#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 12 _journal_issue 4 _journal_year 2021 _journal_page_first 382 _journal_page_last 388 #============================================================================== data_bb_s3_1_lt_mo _audit_creation_date 2021-09-26 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '4(C26 H12 Cl N O6), 2(C2 H6 O S), 2(H2 O)' _chemical_formula_sum 'C108 H64 Cl4 N4 O29 S2' _chemical_formula_weight 2087.55 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8182(6) _cell_length_b 12.7608(11) _cell_length_c 17.1455(11) _cell_angle_alpha 77.158(6) _cell_angle_beta 73.729(5) _cell_angle_gamma 66.373(7) _cell_volume 2256.2(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description ? _exptl_crystal_F_000 1072 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 11884 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 1.756 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6738 _reflns_number_total 7896 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 1.689 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef 0.0040(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 721 _refine_ls_number_reflns 7896 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0799 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 3.787 _refine_ls_shift/su_mean 0.010 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+10.1105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1899 _refine_ls_wR_factor_ref 0.1962 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances S1-C92 = S1-C93 = S1'-C92' = S1'-C93' 1.8 with sigma of 0.02 S1-O91 = S1'-O91' 1.52 with sigma of 0.02 O93-H93G = O93-H93H = O92-H92H = O92-H92G 0.9 with sigma of 0.02 H93H-H93G = H92G-H92H 1.47 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints O93 \\sim H93H \\sim H93G: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A O92 \\sim H92G \\sim H92H: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A 4. Others Fixed Sof: C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C93(0.5) H93A(0.5) H93B(0.5) H93C(0.5) O91(0.5) O93(0.5) S1(0.5) C92'(0.5) H92D(0.5) H92E(0.5) H92F(0.5) C93'(0.5) H93D(0.5) H93E(0.5) H93F(0.5) O91'(0.5) O92(0.5) S1'(0.5) H92H(0.5) H93G(0.5) H93H(0.5) 5.a Aromatic/amide H refined with riding coordinates: C10(H10), C11(H11), C12(H12), C13(H13), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C28(H28), N23(H23), C44(H44), C45(H45), C46(H46), C47(H47), C53(H53), C54(H54), C55(H55), C56(H56), C60(H60), C62(H62), C63(H63), N57(H57) 5.b Idealised Me refined as rotating group: C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C92'(H92D,H92E,H92F), C93'(H93D, H93E,H93F) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3395(4) 0.4065(4) 0.5759(3) 0.0223(10) Uani 1 1 d . . . . . C3 C 0.3181(4) 0.5850(4) 0.4860(3) 0.0235(10) Uani 1 1 d . . . . . C4 C 0.2451(4) 0.5578(4) 0.4437(3) 0.0201(9) Uani 1 1 d . . . . . C5 C 0.1974(4) 0.6428(4) 0.3715(3) 0.0206(9) Uani 1 1 d . . . . . C6 C 0.1155(4) 0.6001(4) 0.3431(3) 0.0194(9) Uani 1 1 d . . . . . C7 C 0.0548(4) 0.6706(4) 0.2759(3) 0.0238(10) Uani 1 1 d . . . . . C9 C -0.0350(4) 0.5285(4) 0.2822(3) 0.0235(10) Uani 1 1 d . . . . . C10 C -0.1107(5) 0.4965(4) 0.2509(3) 0.0288(11) Uani 1 1 d . . . . . H10 H -0.1458 0.5420 0.2069 0.035 Uiso 1 1 calc R U . . . C11 C -0.1336(5) 0.3969(5) 0.2854(3) 0.0315(12) Uani 1 1 d . . . . . H11 H -0.1860 0.3761 0.2653 0.038 Uiso 1 1 calc R U . . . C12 C -0.0795(5) 0.3270(4) 0.3498(3) 0.0293(11) Uani 1 1 d . . . . . H12 H -0.0943 0.2590 0.3719 0.035 Uiso 1 1 calc R U . . . C13 C -0.0038(4) 0.3585(4) 0.3813(3) 0.0258(10) Uani 1 1 d . . . . . H13 H 0.0325 0.3121 0.4245 0.031 Uiso 1 1 calc R U . . . C14 C 0.0178(4) 0.4615(4) 0.3472(3) 0.0212(10) Uani 1 1 d . . . . . C15 C 0.0952(4) 0.5015(4) 0.3762(3) 0.0215(10) Uani 1 1 d . . . . . C17 C 0.2186(4) 0.4613(4) 0.4720(3) 0.0210(10) Uani 1 1 d . . . . . C18 C 0.2628(4) 0.3813(4) 0.5399(3) 0.0216(10) Uani 1 1 d . . . . . C19 C 0.2316(4) 0.2827(4) 0.5723(3) 0.0251(10) Uani 1 1 d . . . . . H19 H 0.1807 0.2645 0.5488 0.030 Uiso 1 1 calc R U . . . C20 C 0.2771(5) 0.2128(4) 0.6393(3) 0.0293(11) Uani 1 1 d . . . . . H20 H 0.2554 0.1483 0.6620 0.035 Uiso 1 1 calc R U . . . C21 C 0.3558(5) 0.2391(4) 0.6731(3) 0.0304(11) Uani 1 1 d . . . . . H21 H 0.3869 0.1910 0.7177 0.037 Uiso 1 1 calc R U . . . C22 C 0.3885(4) 0.3349(4) 0.6415(3) 0.0272(11) Uani 1 1 d . . . . . H22 H 0.4421 0.3510 0.6638 0.033 Uiso 1 1 calc R U . . . C24 C 0.2869(4) 0.7803(4) 0.2936(3) 0.0212(10) Uani 1 1 d . . . . . C25 C 0.3673(4) 0.8253(4) 0.2332(3) 0.0248(10) Uani 1 1 d . . . . . H25 H 0.3570 0.9026 0.2277 0.030 Uiso 1 1 calc R U . . . C26 C 0.4636(4) 0.7509(4) 0.1814(3) 0.0251(10) Uani 1 1 d . . . . . H26 H 0.5187 0.7783 0.1398 0.030 Uiso 1 1 calc R U . . . C27 C 0.4778(4) 0.6353(4) 0.1916(3) 0.0244(10) Uani 1 1 d . . . . . C28 C 0.3983(4) 0.5902(4) 0.2525(3) 0.0212(10) Uani 1 1 d . . . . . H28 H 0.4094 0.5126 0.2588 0.025 Uiso 1 1 calc R U . . . C29 C 0.3026(4) 0.6642(4) 0.3032(3) 0.0191(9) Uani 1 1 d . . . . . C30 C 0.1207(4) 0.7666(4) 0.3967(3) 0.0231(10) Uani 1 1 d . . . . . N23 N 0.1812(4) 0.8373(3) 0.3503(2) 0.0235(9) Uani 1 1 d . . . . . H23 H 0.1571 0.9091 0.3553 0.028 Uiso 1 1 calc R U . . . O2 O 0.3680(3) 0.5047(3) 0.54803(19) 0.0253(7) Uani 1 1 d . . . . . O8 O -0.0146(3) 0.6294(3) 0.2465(2) 0.0265(7) Uani 1 1 d . . . . . O16 O 0.1453(3) 0.4292(3) 0.43967(19) 0.0241(7) Uani 1 1 d . . . . . O31 O 0.0238(3) 0.7929(3) 0.4490(2) 0.0299(8) Uani 1 1 d . . . . . O33 O 0.0616(3) 0.7630(3) 0.2435(2) 0.0342(9) Uani 1 1 d . . . . . O34 O 0.3394(3) 0.6736(3) 0.4718(2) 0.0315(8) Uani 1 1 d . . . . . Cl32 Cl 0.59884(13) 0.54537(12) 0.12435(9) 0.0431(4) Uani 1 1 d . . . . . C35 C 0.0431(4) 0.7018(4) 0.9469(3) 0.0224(10) Uani 1 1 d . . . . . C37 C 0.2168(4) 0.7459(4) 0.8519(3) 0.0242(10) Uani 1 1 d . . . . . C38 C 0.2203(4) 0.8088(4) 0.9116(3) 0.0188(9) Uani 1 1 d . . . . . C39 C 0.3199(4) 0.8636(4) 0.8879(3) 0.0185(9) Uani 1 1 d . . . . . C40 C 0.2981(4) 0.9344(4) 0.9548(3) 0.0186(9) Uani 1 1 d . . . . . C41 C 0.3739(4) 1.0051(4) 0.9414(3) 0.0200(9) Uani 1 1 d . . . . . C43 C 0.2676(4) 1.0653(4) 1.0746(3) 0.0204(9) Uani 1 1 d . . . . . C44 C 0.2576(4) 1.1321(4) 1.1316(3) 0.0243(10) Uani 1 1 d . . . . . H44 H 0.3127 1.1711 1.1228 0.029 Uiso 1 1 calc R U . . . C45 C 0.1630(5) 1.1392(4) 1.2021(3) 0.0269(11) Uani 1 1 d . . . . . H45 H 0.1546 1.1838 1.2410 0.032 Uiso 1 1 calc R U . . . C46 C 0.0807(4) 1.0811(4) 1.2157(3) 0.0246(10) Uani 1 1 d . . . . . H46 H 0.0171 1.0879 1.2628 0.029 Uiso 1 1 calc R U . . . C47 C 0.0934(4) 1.0133(4) 1.1592(3) 0.0224(10) Uani 1 1 d . . . . . H47 H 0.0399 0.9725 1.1689 0.027 Uiso 1 1 calc R U . . . C48 C 0.1870(4) 1.0057(4) 1.0874(3) 0.0186(9) Uani 1 1 d . . . . . C49 C 0.2084(4) 0.9381(4) 1.0239(3) 0.0191(9) Uani 1 1 d . . . . . C51 C 0.1335(4) 0.8195(4) 0.9824(3) 0.0193(9) Uani 1 1 d . . . . . C52 C 0.0390(4) 0.7683(4) 1.0026(3) 0.0202(9) Uani 1 1 d . . . . . C53 C -0.0575(4) 0.7826(4) 1.0737(3) 0.0236(10) Uani 1 1 d . . . . . H53 H -0.0619 0.8260 1.1122 0.028 Uiso 1 1 calc R U . . . C54 C -0.1461(4) 0.7318(4) 1.0862(3) 0.0284(11) Uani 1 1 d . . . . . H54 H -0.2112 0.7427 1.1326 0.034 Uiso 1 1 calc R U . . . C55 C -0.1380(5) 0.6645(4) 1.0297(3) 0.0295(11) Uani 1 1 d . . . . . H55 H -0.1971 0.6297 1.0391 0.035 Uiso 1 1 calc R U . . . C56 C -0.0435(4) 0.6488(4) 0.9599(3) 0.0274(11) Uani 1 1 d . . . . . H56 H -0.0381 0.6036 0.9223 0.033 Uiso 1 1 calc R U . . . C58 C 0.3082(5) 0.9431(4) 0.8039(3) 0.0245(10) Uani 1 1 d . . . . . C59 C 0.4549(4) 0.7760(4) 0.8665(3) 0.0194(9) Uani 1 1 d . . . . . C60 C 0.5198(4) 0.6796(4) 0.9124(3) 0.0239(10) Uani 1 1 d . . . . . H60 H 0.4843 0.6596 0.9665 0.029 Uiso 1 1 calc R U . . . C61 C 0.6410(5) 0.6125(4) 0.8752(3) 0.0304(11) Uani 1 1 d . . . . . C62 C 0.6948(5) 0.6426(5) 0.7953(3) 0.0340(12) Uani 1 1 d . . . . . H62 H 0.7770 0.5976 0.7726 0.041 Uiso 1 1 calc R U . . . C63 C 0.6281(5) 0.7390(5) 0.7485(3) 0.0318(12) Uani 1 1 d . . . . . H63 H 0.6634 0.7586 0.6942 0.038 Uiso 1 1 calc R U . . . C64 C 0.5071(4) 0.8051(4) 0.7852(3) 0.0246(10) Uani 1 1 d . . . . . N57 N 0.4211(4) 0.9029(3) 0.7503(2) 0.0255(9) Uani 1 1 d . . . . . H57 H 0.4374 0.9344 0.7007 0.031 Uiso 1 1 calc R U . . . O36 O 0.1328(3) 0.6883(3) 0.8751(2) 0.0265(7) Uani 1 1 d . . . . . O42 O 0.3589(3) 1.0643(3) 1.00371(19) 0.0228(7) Uani 1 1 d . . . . . O50 O 0.1256(3) 0.8810(3) 1.04044(19) 0.0225(7) Uani 1 1 d . . . . . O65 O 0.2135(3) 1.0223(3) 0.7908(2) 0.0334(8) Uani 1 1 d . . . . . O67 O 0.4480(3) 1.0170(3) 0.8788(2) 0.0274(8) Uani 1 1 d . . . . . O68 O 0.2824(3) 0.7380(3) 0.7843(2) 0.0309(8) Uani 1 1 d . . . . . Cl66 Cl 0.72882(14) 0.48550(13) 0.92831(10) 0.0512(4) Uani 1 1 d . . . . . C92 C -0.2226(13) 1.0130(11) 0.4566(7) 0.054(3) Uani 0.5 1 d D . P A 1 H92A H -0.2209 1.0883 0.4539 0.080 Uiso 0.5 1 calc R U P A 1 H92B H -0.2991 1.0201 0.4431 0.080 Uiso 0.5 1 calc R U P A 1 H92C H -0.1511 0.9701 0.4183 0.080 Uiso 0.5 1 calc R U P A 1 C93 C -0.3628(9) 1.0362(10) 0.6087(8) 0.046(3) Uani 0.5 1 d D . P A 1 H93A H -0.3719 1.0154 0.6669 0.069 Uiso 0.5 1 calc R U P A 1 H93B H -0.4316 1.0316 0.5921 0.069 Uiso 0.5 1 calc R U P A 1 H93C H -0.3635 1.1136 0.5945 0.069 Uiso 0.5 1 calc R U P A 1 O91 O -0.1135(8) 0.9550(7) 0.5851(5) 0.0334(18) Uani 0.5 1 d D . P A 1 O93 O -0.5332(10) 1.1055(9) 0.4243(5) 0.050(2) Uani 0.5 1 d D U P B 1 S1 S -0.2163(3) 0.9394(2) 0.55776(17) 0.0345(6) Uani 0.5 1 d D . P A 1 C92' C -0.2374(12) 1.0943(14) 0.4128(12) 0.085(6) Uani 0.5 1 d D . P C 2 H92D H -0.1957 1.0132 0.4276 0.128 Uiso 0.5 1 calc R U P C 2 H92E H -0.2032 1.1368 0.4333 0.128 Uiso 0.5 1 calc R U P C 2 H92F H -0.2243 1.1112 0.3543 0.128 Uiso 0.5 1 calc R U P C 2 C93' C -0.4511(6) 1.2840(6) 0.3967(4) 0.0039(14) Uani 0.5 1 d D . P C 2 H93D H -0.3987 1.2816 0.3425 0.006 Uiso 0.5 1 calc R U P C 2 H93E H -0.4406 1.3365 0.4241 0.006 Uiso 0.5 1 calc R U P C 2 H93F H -0.5380 1.3097 0.3932 0.006 Uiso 0.5 1 calc R U P C 2 O91' O -0.4452(10) 1.0559(9) 0.4261(5) 0.045(2) Uani 0.5 1 d D . P C 2 O92 O -0.0545(10) 0.9718(8) 0.5553(6) 0.049(2) Uani 0.5 1 d D U P D 2 S1' S -0.4036(4) 1.1346(3) 0.45642(18) 0.0570(10) Uani 0.5 1 d D . P C 2 H92G H 0.0000 1.0000 0.5000 0.054(10) Uiso 1 2 d DS U P E 2 H92H H -0.062(10) 0.916(7) 0.535(3) 0.047(10) Uiso 0.5 1 d D U P F 2 H93G H -0.455(6) 1.072(10) 0.394(6) 0.054(11) Uiso 0.5 1 d D U P G 1 H93H H -0.543(10) 1.060(8) 0.472(4) 0.054(11) Uiso 0.5 1 d D U P H 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(2) 0.023(2) 0.022(2) 0.0001(19) -0.0021(18) -0.0068(19) C3 0.023(2) 0.024(2) 0.020(2) 0.0041(19) -0.0052(19) -0.008(2) C4 0.017(2) 0.024(2) 0.019(2) 0.0009(18) -0.0032(17) -0.0086(18) C5 0.019(2) 0.022(2) 0.021(2) -0.0016(18) -0.0036(18) -0.0092(19) C6 0.019(2) 0.021(2) 0.017(2) -0.0009(18) -0.0033(17) -0.0066(18) C7 0.025(2) 0.021(2) 0.024(2) 0.0039(19) -0.0079(19) -0.009(2) C9 0.023(2) 0.023(2) 0.023(2) -0.0017(19) -0.0026(19) -0.0079(19) C10 0.030(3) 0.037(3) 0.023(2) -0.004(2) -0.009(2) -0.013(2) C11 0.037(3) 0.041(3) 0.026(3) -0.010(2) -0.002(2) -0.023(2) C12 0.036(3) 0.030(3) 0.026(3) -0.006(2) -0.001(2) -0.018(2) C13 0.025(2) 0.027(3) 0.025(2) -0.002(2) -0.002(2) -0.012(2) C14 0.018(2) 0.025(2) 0.017(2) -0.0045(18) 0.0015(18) -0.0073(19) C15 0.020(2) 0.023(2) 0.018(2) 0.0007(18) -0.0040(18) -0.0059(19) C17 0.024(2) 0.023(2) 0.018(2) -0.0005(18) -0.0048(18) -0.0110(19) C18 0.020(2) 0.021(2) 0.022(2) 0.0003(18) -0.0051(18) -0.0059(19) C19 0.024(2) 0.026(2) 0.023(2) 0.0022(19) -0.0050(19) -0.010(2) C20 0.032(3) 0.022(2) 0.029(3) 0.007(2) -0.009(2) -0.008(2) C21 0.031(3) 0.028(3) 0.026(3) 0.007(2) -0.012(2) -0.006(2) C22 0.022(2) 0.032(3) 0.025(3) 0.005(2) -0.009(2) -0.008(2) C24 0.024(2) 0.019(2) 0.022(2) 0.0002(18) -0.0077(19) -0.0089(19) C25 0.028(3) 0.023(2) 0.025(2) 0.0022(19) -0.009(2) -0.012(2) C26 0.023(2) 0.028(3) 0.024(2) 0.005(2) -0.0066(19) -0.012(2) C27 0.024(2) 0.024(2) 0.023(2) 0.0003(19) -0.0046(19) -0.008(2) C28 0.024(2) 0.018(2) 0.023(2) 0.0006(18) -0.0078(19) -0.0085(19) C29 0.025(2) 0.021(2) 0.017(2) 0.0041(17) -0.0086(18) -0.0142(19) C30 0.025(2) 0.026(2) 0.019(2) 0.0001(19) -0.007(2) -0.011(2) N23 0.029(2) 0.0188(19) 0.022(2) -0.0017(16) -0.0040(17) -0.0095(17) O2 0.0261(17) 0.0280(18) 0.0242(17) 0.0068(14) -0.0102(14) -0.0142(14) O8 0.0283(18) 0.0301(18) 0.0255(18) 0.0045(14) -0.0117(14) -0.0151(15) O16 0.0303(18) 0.0239(17) 0.0227(17) 0.0062(13) -0.0134(14) -0.0143(14) O31 0.0293(19) 0.0282(18) 0.0269(18) -0.0010(15) -0.0028(15) -0.0086(15) O33 0.039(2) 0.031(2) 0.038(2) 0.0127(16) -0.0218(17) -0.0179(17) O34 0.038(2) 0.0311(19) 0.032(2) 0.0059(15) -0.0157(16) -0.0194(16) Cl32 0.0364(7) 0.0330(7) 0.0467(8) -0.0107(6) 0.0164(6) -0.0130(6) C35 0.018(2) 0.021(2) 0.026(2) 0.0014(19) -0.0077(19) -0.0057(19) C37 0.019(2) 0.022(2) 0.032(3) -0.001(2) -0.008(2) -0.0076(19) C38 0.017(2) 0.016(2) 0.024(2) 0.0019(17) -0.0088(18) -0.0050(18) C39 0.018(2) 0.020(2) 0.017(2) -0.0005(17) -0.0047(17) -0.0066(18) C40 0.018(2) 0.015(2) 0.022(2) 0.0028(17) -0.0093(18) -0.0048(17) C41 0.015(2) 0.017(2) 0.025(2) -0.0031(18) -0.0056(19) -0.0016(18) C43 0.017(2) 0.018(2) 0.022(2) -0.0007(18) -0.0063(18) -0.0015(18) C44 0.024(2) 0.024(2) 0.027(3) -0.004(2) -0.008(2) -0.009(2) C45 0.028(3) 0.025(2) 0.025(3) -0.005(2) -0.008(2) -0.004(2) C46 0.022(2) 0.023(2) 0.020(2) -0.0030(19) -0.0025(19) -0.0003(19) C47 0.021(2) 0.020(2) 0.024(2) 0.0002(19) -0.0064(19) -0.0061(19) C48 0.019(2) 0.015(2) 0.019(2) 0.0009(17) -0.0080(18) -0.0016(17) C49 0.019(2) 0.017(2) 0.022(2) 0.0017(17) -0.0091(18) -0.0055(18) C51 0.020(2) 0.014(2) 0.022(2) 0.0022(17) -0.0093(18) -0.0035(18) C52 0.019(2) 0.015(2) 0.024(2) 0.0046(18) -0.0094(18) -0.0037(18) C53 0.024(2) 0.025(2) 0.020(2) 0.0049(19) -0.0071(19) -0.010(2) C54 0.020(2) 0.031(3) 0.030(3) 0.005(2) -0.007(2) -0.009(2) C55 0.027(3) 0.029(3) 0.036(3) 0.010(2) -0.014(2) -0.016(2) C56 0.027(3) 0.020(2) 0.038(3) -0.001(2) -0.010(2) -0.010(2) C58 0.033(3) 0.021(2) 0.024(2) 0.0010(19) -0.010(2) -0.013(2) C59 0.021(2) 0.022(2) 0.020(2) -0.0047(18) -0.0054(18) -0.0100(19) C60 0.022(2) 0.027(3) 0.024(2) -0.006(2) -0.0052(19) -0.009(2) C61 0.025(3) 0.031(3) 0.036(3) -0.013(2) -0.009(2) -0.003(2) C62 0.021(3) 0.043(3) 0.038(3) -0.022(3) 0.003(2) -0.009(2) C63 0.028(3) 0.045(3) 0.026(3) -0.015(2) 0.007(2) -0.019(2) C64 0.024(2) 0.028(3) 0.027(3) -0.006(2) -0.003(2) -0.015(2) N57 0.035(2) 0.031(2) 0.0128(19) 0.0027(16) -0.0019(16) -0.0195(19) O36 0.0224(17) 0.0283(18) 0.0306(18) -0.0068(14) -0.0021(14) -0.0119(14) O42 0.0229(16) 0.0217(16) 0.0254(17) -0.0037(13) -0.0042(13) -0.0097(13) O50 0.0221(17) 0.0269(17) 0.0227(17) -0.0019(13) -0.0039(13) -0.0143(14) O65 0.039(2) 0.0249(19) 0.031(2) 0.0053(15) -0.0163(16) -0.0052(17) O67 0.0255(18) 0.0304(18) 0.0269(18) -0.0040(14) 0.0011(15) -0.0150(15) O68 0.0336(19) 0.036(2) 0.0267(19) -0.0076(15) -0.0027(16) -0.0171(16) Cl66 0.0414(8) 0.0426(8) 0.0477(9) -0.0144(7) -0.0161(7) 0.0161(7) C92 0.051(8) 0.048(8) 0.050(8) -0.001(6) -0.022(6) -0.001(6) C93 0.031(6) 0.057(8) 0.062(8) -0.035(6) 0.005(5) -0.024(6) O91 0.044(5) 0.025(4) 0.032(5) -0.012(4) -0.012(4) -0.006(4) O93 0.062(6) 0.062(6) 0.028(4) 0.000(4) -0.011(4) -0.027(5) S1 0.0397(15) 0.0259(13) 0.0395(15) -0.0076(11) -0.0095(12) -0.0110(11) C92' 0.069(11) 0.063(10) 0.142(17) 0.033(11) -0.064(12) -0.038(9) C93' 0.002(3) 0.013(4) 0.000(3) -0.004(3) 0.002(3) -0.006(3) O91' 0.074(7) 0.065(6) 0.018(4) -0.001(4) -0.006(4) -0.052(6) O92 0.058(6) 0.040(5) 0.042(5) -0.014(4) 0.007(4) -0.018(5) S1' 0.099(3) 0.076(2) 0.0277(15) 0.0042(15) -0.0185(16) -0.065(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C18 1.394(6) . ? C1 C22 1.385(6) . ? C1 O2 1.376(5) . ? C3 C4 1.447(6) . ? C3 O2 1.383(5) . ? C3 O34 1.214(6) . ? C4 C5 1.525(6) . ? C4 C17 1.345(6) . ? C5 C6 1.509(6) . ? C5 C29 1.518(6) . ? C5 C30 1.562(6) . ? C6 C7 1.462(6) . ? C6 C15 1.345(6) . ? C7 O8 1.379(6) . ? C7 O33 1.211(6) . ? C9 C10 1.383(7) . ? C9 C14 1.379(6) . ? C9 O8 1.380(6) . ? C10 H10 0.9300 . ? C10 C11 1.375(7) . ? C11 H11 0.9300 . ? C11 C12 1.388(7) . ? C12 H12 0.9300 . ? C12 C13 1.381(7) . ? C13 H13 0.9300 . ? C13 C14 1.406(6) . ? C14 C15 1.444(6) . ? C15 O16 1.366(5) . ? C17 C18 1.433(6) . ? C17 O16 1.371(5) . ? C18 C19 1.406(6) . ? C19 H19 0.9300 . ? C19 C20 1.383(7) . ? C20 H20 0.9300 . ? C20 C21 1.396(7) . ? C21 H21 0.9300 . ? C21 C22 1.380(7) . ? C22 H22 0.9300 . ? C24 C25 1.388(6) . ? C24 C29 1.394(6) . ? C24 N23 1.393(6) . ? C25 H25 0.9300 . ? C25 C26 1.389(7) . ? C26 H26 0.9300 . ? C26 C27 1.392(7) . ? C27 C28 1.386(6) . ? C27 Cl32 1.744(5) . ? C28 H28 0.9300 . ? C28 C29 1.373(6) . ? C30 N23 1.356(6) . ? C30 O31 1.216(6) . ? N23 H23 0.8600 . ? C35 C52 1.391(7) . ? C35 C56 1.384(6) . ? C35 O36 1.373(6) . ? C37 C38 1.452(6) . ? C37 O36 1.384(5) . ? C37 O68 1.201(6) . ? C38 C39 1.518(6) . ? C38 C51 1.345(6) . ? C39 C40 1.519(6) . ? C39 C58 1.572(6) . ? C39 C59 1.534(6) . ? C40 C41 1.453(6) . ? C40 C49 1.346(6) . ? C41 O42 1.374(5) . ? C41 O67 1.204(5) . ? C43 C44 1.385(6) . ? C43 C48 1.387(6) . ? C43 O42 1.379(5) . ? C44 H44 0.9300 . ? C44 C45 1.390(7) . ? C45 H45 0.9300 . ? C45 C46 1.387(7) . ? C46 H46 0.9300 . ? C46 C47 1.376(7) . ? C47 H47 0.9300 . ? C47 C48 1.398(6) . ? C48 C49 1.443(6) . ? C49 O50 1.375(5) . ? C51 C52 1.435(6) . ? C51 O50 1.361(5) . ? C52 C53 1.405(6) . ? C53 H53 0.9300 . ? C53 C54 1.385(7) . ? C54 H54 0.9300 . ? C54 C55 1.393(7) . ? C55 H55 0.9300 . ? C55 C56 1.377(7) . ? C56 H56 0.9300 . ? C58 N57 1.364(6) . ? C58 O65 1.207(6) . ? C59 C60 1.368(6) . ? C59 C64 1.391(6) . ? C60 H60 0.9300 . ? C60 C61 1.393(7) . ? C61 C62 1.378(7) . ? C61 Cl66 1.749(5) . ? C62 H62 0.9300 . ? C62 C63 1.385(8) . ? C63 H63 0.9300 . ? C63 C64 1.385(7) . ? C64 N57 1.393(6) . ? N57 H57 0.8600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C92 S1 1.786(11) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C93 S1 1.790(10) . ? O91 S1 1.512(8) . ? O93 H93G 0.90(2) . ? O93 H93H 0.90(2) . ? C92' H92D 0.9600 . ? C92' H92E 0.9600 . ? C92' H92F 0.9600 . ? C92' S1' 1.795(13) . ? C93' H93D 0.9600 . ? C93' H93E 0.9600 . ? C93' H93F 0.9600 . ? C93' S1' 1.896(7) . ? O91' S1' 1.513(8) . ? O92 H92G 1.066(9) . ? O92 H92H 0.91(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 C1 C18 121.5(4) . . ? O2 C1 C18 120.9(4) . . ? O2 C1 C22 117.6(4) . . ? O2 C3 C4 118.3(4) . . ? O34 C3 C4 125.3(4) . . ? O34 C3 O2 116.4(4) . . ? C3 C4 C5 118.3(4) . . ? C17 C4 C3 118.2(4) . . ? C17 C4 C5 123.4(4) . . ? C4 C5 C30 111.0(4) . . ? C6 C5 C4 107.8(4) . . ? C6 C5 C29 113.2(4) . . ? C6 C5 C30 110.5(4) . . ? C29 C5 C4 113.4(4) . . ? C29 C5 C30 100.9(3) . . ? C7 C6 C5 117.7(4) . . ? C15 C6 C5 123.8(4) . . ? C15 C6 C7 118.5(4) . . ? O8 C7 C6 118.2(4) . . ? O33 C7 C6 124.7(4) . . ? O33 C7 O8 117.1(4) . . ? C14 C9 C10 120.7(4) . . ? C14 C9 O8 121.3(4) . . ? O8 C9 C10 117.9(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 C9 119.4(5) . . ? C11 C10 H10 120.3 . . ? C10 C11 H11 119.6 . . ? C10 C11 C12 120.8(5) . . ? C12 C11 H11 119.6 . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(5) . . ? C13 C12 H12 120.0 . . ? C12 C13 H13 120.3 . . ? C12 C13 C14 119.4(5) . . ? C14 C13 H13 120.3 . . ? C9 C14 C13 119.7(4) . . ? C9 C14 C15 117.1(4) . . ? C13 C14 C15 123.2(4) . . ? C6 C15 C14 122.8(4) . . ? C6 C15 O16 123.9(4) . . ? O16 C15 C14 113.3(4) . . ? C4 C17 C18 123.7(4) . . ? C4 C17 O16 123.7(4) . . ? O16 C17 C18 112.6(4) . . ? C1 C18 C17 116.5(4) . . ? C1 C18 C19 119.2(4) . . ? C19 C18 C17 124.3(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 C18 119.5(5) . . ? C20 C19 H19 120.3 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 119.9(5) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 119.3 . . ? C22 C21 C20 121.4(4) . . ? C22 C21 H21 119.3 . . ? C1 C22 H22 120.8 . . ? C21 C22 C1 118.4(5) . . ? C21 C22 H22 120.8 . . ? C25 C24 C29 121.6(4) . . ? C25 C24 N23 128.7(4) . . ? N23 C24 C29 109.7(4) . . ? C24 C25 H25 121.2 . . ? C26 C25 C24 117.7(4) . . ? C26 C25 H25 121.2 . . ? C25 C26 H26 120.0 . . ? C25 C26 C27 120.0(4) . . ? C27 C26 H26 120.0 . . ? C26 C27 Cl32 118.4(4) . . ? C28 C27 C26 122.3(4) . . ? C28 C27 Cl32 119.3(4) . . ? C27 C28 H28 121.2 . . ? C29 C28 C27 117.5(4) . . ? C29 C28 H28 121.2 . . ? C24 C29 C5 109.2(4) . . ? C28 C29 C5 129.9(4) . . ? C28 C29 C24 120.9(4) . . ? N23 C30 C5 108.0(4) . . ? O31 C30 C5 125.0(4) . . ? O31 C30 N23 127.0(4) . . ? C24 N23 H23 123.9 . . ? C30 N23 C24 112.2(4) . . ? C30 N23 H23 123.9 . . ? C1 O2 C3 122.1(4) . . ? C9 O8 C7 121.9(4) . . ? C15 O16 C17 117.3(3) . . ? C56 C35 C52 122.2(4) . . ? O36 C35 C52 120.8(4) . . ? O36 C35 C56 117.0(4) . . ? O36 C37 C38 117.6(4) . . ? O68 C37 C38 125.4(4) . . ? O68 C37 O36 117.0(4) . . ? C37 C38 C39 117.1(4) . . ? C51 C38 C37 119.1(4) . . ? C51 C38 C39 123.8(4) . . ? C38 C39 C40 108.2(4) . . ? C38 C39 C58 109.5(3) . . ? C38 C39 C59 112.9(4) . . ? C40 C39 C58 110.2(4) . . ? C40 C39 C59 114.6(4) . . ? C59 C39 C58 101.3(3) . . ? C41 C40 C39 118.1(4) . . ? C49 C40 C39 122.9(4) . . ? C49 C40 C41 118.9(4) . . ? O42 C41 C40 118.1(4) . . ? O67 C41 C40 124.6(4) . . ? O67 C41 O42 117.4(4) . . ? C44 C43 C48 121.5(4) . . ? O42 C43 C44 116.5(4) . . ? O42 C43 C48 121.9(4) . . ? C43 C44 H44 121.0 . . ? C43 C44 C45 118.1(4) . . ? C45 C44 H44 121.0 . . ? C44 C45 H45 119.3 . . ? C46 C45 C44 121.3(4) . . ? C46 C45 H45 119.3 . . ? C45 C46 H46 120.1 . . ? C47 C46 C45 119.9(4) . . ? C47 C46 H46 120.1 . . ? C46 C47 H47 120.0 . . ? C46 C47 C48 119.9(4) . . ? C48 C47 H47 120.0 . . ? C43 C48 C47 119.3(4) . . ? C43 C48 C49 116.0(4) . . ? C47 C48 C49 124.7(4) . . ? C40 C49 C48 123.0(4) . . ? C40 C49 O50 123.9(4) . . ? O50 C49 C48 113.1(4) . . ? C38 C51 C52 122.6(4) . . ? C38 C51 O50 123.4(4) . . ? O50 C51 C52 114.0(4) . . ? C35 C52 C51 117.2(4) . . ? C35 C52 C53 118.4(4) . . ? C53 C52 C51 124.4(4) . . ? C52 C53 H53 120.1 . . ? C54 C53 C52 119.7(5) . . ? C54 C53 H53 120.1 . . ? C53 C54 H54 119.9 . . ? C53 C54 C55 120.3(5) . . ? C55 C54 H54 119.9 . . ? C54 C55 H55 119.6 . . ? C56 C55 C54 120.8(5) . . ? C56 C55 H55 119.6 . . ? C35 C56 H56 120.7 . . ? C55 C56 C35 118.5(5) . . ? C55 C56 H56 120.7 . . ? N57 C58 C39 107.5(4) . . ? O65 C58 C39 124.6(4) . . ? O65 C58 N57 127.9(4) . . ? C60 C59 C39 130.4(4) . . ? C60 C59 C64 121.2(4) . . ? C64 C59 C39 108.3(4) . . ? C59 C60 H60 121.2 . . ? C59 C60 C61 117.7(4) . . ? C61 C60 H60 121.2 . . ? C60 C61 Cl66 120.7(4) . . ? C62 C61 C60 121.4(5) . . ? C62 C61 Cl66 117.9(4) . . ? C61 C62 H62 119.6 . . ? C61 C62 C63 120.9(5) . . ? C63 C62 H62 119.6 . . ? C62 C63 H63 121.1 . . ? C64 C63 C62 117.7(5) . . ? C64 C63 H63 121.1 . . ? C59 C64 N57 110.7(4) . . ? C63 C64 C59 121.1(5) . . ? C63 C64 N57 128.2(4) . . ? C58 N57 C64 112.2(4) . . ? C58 N57 H57 123.9 . . ? C64 N57 H57 123.9 . . ? C35 O36 C37 122.2(4) . . ? C41 O42 C43 121.7(3) . . ? C51 O50 C49 117.7(3) . . ? H92A C92 H92B 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? S1 C92 H92A 109.5 . . ? S1 C92 H92B 109.5 . . ? S1 C92 H92C 109.5 . . ? H93A C93 H93B 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? S1 C93 H93A 109.5 . . ? S1 C93 H93B 109.5 . . ? S1 C93 H93C 109.5 . . ? H93G O93 H93H 109(3) . . ? C92 S1 C93 96.9(6) . . ? O91 S1 C92 108.2(6) . . ? O91 S1 C93 106.0(5) . . ? H92D C92' H92E 109.5 . . ? H92D C92' H92F 109.5 . . ? H92E C92' H92F 109.5 . . ? S1' C92' H92D 109.5 . . ? S1' C92' H92E 109.5 . . ? S1' C92' H92F 109.5 . . ? H93D C93' H93E 109.5 . . ? H93D C93' H93F 109.5 . . ? H93E C93' H93F 109.5 . . ? S1' C93' H93D 109.5 . . ? S1' C93' H93E 109.5 . . ? S1' C93' H93F 109.5 . . ? H92G O92 H92H 96(2) . . ? C92' S1' C93' 95.9(6) . . ? O91' S1' C92' 105.0(7) . . ? O91' S1' C93' 110.9(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N23 H23 O91 0.86 2.02 2.829(8) 155.4 2_576 N23 H23 O92 0.86 2.16 2.875(10) 140.9 2_576 N57 H57 O93 0.86 2.19 2.923(10) 142.7 2_576 N57 H57 O91' 0.86 2.13 2.905(9) 150.0 2_576 C92 H92B O93 0.96 2.62 3.542(17) 160.9 . C92 H92C O31 0.96 2.45 3.127(13) 127.5 . C93 H93B O93 0.96 2.04 2.780(15) 132.0 2_476 C93' H93D O68 0.96 2.23 3.186(7) 174.4 2_576 C93' H93E O34 0.96 2.37 3.146(7) 137.9 2_576 O92 H92G O92 1.066(9) 1.066(9) 2.131(18) 180.0(10) 2_576 O92 H92H O31 0.91(2) 2.14(5) 2.933(10) 146(6) . O93 H93G N57 0.90(2) 2.36(11) 2.923(10) 120(10) 2_576 O93 H93H O93 0.90(2) 2.48(6) 3.307(19) 153(9) 2_476 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C18 C19 C20 0.2(7) . . . . ? C3 C4 C5 C6 -175.2(4) . . . . ? C3 C4 C5 C29 58.7(5) . . . . ? C3 C4 C5 C30 -54.1(5) . . . . ? C3 C4 C17 C18 -2.6(7) . . . . ? C3 C4 C17 O16 176.8(4) . . . . ? C4 C3 O2 C1 -6.9(6) . . . . ? C4 C5 C6 C7 177.7(4) . . . . ? C4 C5 C6 C15 -2.2(6) . . . . ? C4 C5 C29 C24 -118.0(4) . . . . ? C4 C5 C29 C28 65.2(6) . . . . ? C4 C5 C30 N23 118.5(4) . . . . ? C4 C5 C30 O31 -61.6(6) . . . . ? C4 C17 C18 C1 -1.4(7) . . . . ? C4 C17 C18 C19 177.2(5) . . . . ? C4 C17 O16 C15 -1.3(6) . . . . ? C5 C4 C17 C18 -179.9(4) . . . . ? C5 C4 C17 O16 -0.5(7) . . . . ? C5 C6 C7 O8 176.5(4) . . . . ? C5 C6 C7 O33 -2.9(7) . . . . ? C5 C6 C15 C14 -179.0(4) . . . . ? C5 C6 C15 O16 0.7(7) . . . . ? C5 C30 N23 C24 2.6(5) . . . . ? C6 C5 C29 C24 118.8(4) . . . . ? C6 C5 C29 C28 -58.0(6) . . . . ? C6 C5 C30 N23 -122.0(4) . . . . ? C6 C5 C30 O31 57.9(6) . . . . ? C6 C7 O8 C9 4.5(6) . . . . ? C6 C15 O16 C17 1.3(6) . . . . ? C7 C6 C15 C14 1.1(7) . . . . ? C7 C6 C15 O16 -179.2(4) . . . . ? C9 C10 C11 C12 -1.4(8) . . . . ? C9 C14 C15 C6 0.8(7) . . . . ? C9 C14 C15 O16 -179.0(4) . . . . ? C10 C9 C14 C13 1.0(7) . . . . ? C10 C9 C14 C15 -179.8(4) . . . . ? C10 C9 O8 C7 177.0(4) . . . . ? C10 C11 C12 C13 1.4(8) . . . . ? C11 C12 C13 C14 -0.2(7) . . . . ? C12 C13 C14 C9 -1.0(7) . . . . ? C12 C13 C14 C15 179.8(4) . . . . ? C13 C14 C15 C6 179.9(4) . . . . ? C13 C14 C15 O16 0.2(6) . . . . ? C14 C9 C10 C11 0.2(7) . . . . ? C14 C9 O8 C7 -2.7(6) . . . . ? C14 C15 O16 C17 -179.0(4) . . . . ? C15 C6 C7 O8 -3.7(6) . . . . ? C15 C6 C7 O33 177.0(5) . . . . ? C17 C4 C5 C6 2.1(6) . . . . ? C17 C4 C5 C29 -124.0(5) . . . . ? C17 C4 C5 C30 123.2(5) . . . . ? C17 C18 C19 C20 -178.4(4) . . . . ? C18 C1 C22 C21 -2.4(7) . . . . ? C18 C1 O2 C3 3.0(6) . . . . ? C18 C17 O16 C15 178.1(4) . . . . ? C18 C19 C20 C21 -1.5(7) . . . . ? C19 C20 C21 C22 0.8(8) . . . . ? C20 C21 C22 C1 1.1(7) . . . . ? C22 C1 C18 C17 -179.5(4) . . . . ? C22 C1 C18 C19 1.8(7) . . . . ? C22 C1 O2 C3 -176.3(4) . . . . ? C24 C25 C26 C27 -0.7(7) . . . . ? C25 C24 C29 C5 -177.6(4) . . . . ? C25 C24 C29 C28 -0.4(7) . . . . ? C25 C24 N23 C30 176.0(5) . . . . ? C25 C26 C27 C28 0.0(7) . . . . ? C25 C26 C27 Cl32 179.2(4) . . . . ? C26 C27 C28 C29 0.5(7) . . . . ? C27 C28 C29 C5 176.3(4) . . . . ? C27 C28 C29 C24 -0.3(7) . . . . ? C29 C5 C6 C7 -56.1(5) . . . . ? C29 C5 C6 C15 124.0(5) . . . . ? C29 C5 C30 N23 -2.0(5) . . . . ? C29 C5 C30 O31 177.9(4) . . . . ? C29 C24 C25 C26 0.9(7) . . . . ? C29 C24 N23 C30 -2.1(5) . . . . ? C30 C5 C6 C7 56.3(5) . . . . ? C30 C5 C6 C15 -123.6(5) . . . . ? C30 C5 C29 C24 0.8(5) . . . . ? C30 C5 C29 C28 -176.1(4) . . . . ? N23 C24 C25 C26 -177.0(4) . . . . ? N23 C24 C29 C5 0.7(5) . . . . ? N23 C24 C29 C28 177.9(4) . . . . ? O2 C1 C18 C17 1.3(6) . . . . ? O2 C1 C18 C19 -177.4(4) . . . . ? O2 C1 C22 C21 176.8(4) . . . . ? O2 C3 C4 C5 -176.0(4) . . . . ? O2 C3 C4 C17 6.6(6) . . . . ? O8 C9 C10 C11 -179.6(4) . . . . ? O8 C9 C14 C13 -179.2(4) . . . . ? O8 C9 C14 C15 0.0(6) . . . . ? O16 C17 C18 C1 179.2(4) . . . . ? O16 C17 C18 C19 -2.2(6) . . . . ? O31 C30 N23 C24 -177.3(5) . . . . ? O33 C7 O8 C9 -176.0(4) . . . . ? O34 C3 C4 C5 4.3(7) . . . . ? O34 C3 C4 C17 -173.1(5) . . . . ? O34 C3 O2 C1 172.9(4) . . . . ? Cl32 C27 C28 C29 -178.7(3) . . . . ? C35 C52 C53 C54 -0.6(6) . . . . ? C37 C38 C39 C40 174.3(4) . . . . ? C37 C38 C39 C58 54.2(5) . . . . ? C37 C38 C39 C59 -57.8(5) . . . . ? C37 C38 C51 C52 1.8(6) . . . . ? C37 C38 C51 O50 -177.1(4) . . . . ? C38 C37 O36 C35 9.0(6) . . . . ? C38 C39 C40 C41 -173.5(4) . . . . ? C38 C39 C40 C49 3.6(6) . . . . ? C38 C39 C58 N57 -121.0(4) . . . . ? C38 C39 C58 O65 56.9(6) . . . . ? C38 C39 C59 C60 -58.7(6) . . . . ? C38 C39 C59 C64 117.8(4) . . . . ? C38 C51 C52 C35 2.5(6) . . . . ? C38 C51 C52 C53 -176.3(4) . . . . ? C38 C51 O50 C49 2.4(6) . . . . ? C39 C38 C51 C52 179.0(4) . . . . ? C39 C38 C51 O50 0.1(7) . . . . ? C39 C40 C41 O42 -176.6(4) . . . . ? C39 C40 C41 O67 4.6(6) . . . . ? C39 C40 C49 C48 -179.7(4) . . . . ? C39 C40 C49 O50 -1.6(7) . . . . ? C39 C58 N57 C64 1.7(5) . . . . ? C39 C59 C60 C61 177.1(4) . . . . ? C39 C59 C64 C63 -178.6(4) . . . . ? C39 C59 C64 N57 0.1(5) . . . . ? C40 C39 C58 N57 120.1(4) . . . . ? C40 C39 C58 O65 -62.0(6) . . . . ? C40 C39 C59 C60 65.8(6) . . . . ? C40 C39 C59 C64 -117.7(4) . . . . ? C40 C41 O42 C43 -5.4(6) . . . . ? C40 C49 O50 C51 -1.7(6) . . . . ? C41 C40 C49 C48 -2.7(6) . . . . ? C41 C40 C49 O50 175.5(4) . . . . ? C43 C44 C45 C46 0.1(7) . . . . ? C43 C48 C49 C40 -1.9(6) . . . . ? C43 C48 C49 O50 179.8(4) . . . . ? C44 C43 C48 C47 0.1(6) . . . . ? C44 C43 C48 C49 -179.2(4) . . . . ? C44 C43 O42 C41 -177.2(4) . . . . ? C44 C45 C46 C47 1.1(7) . . . . ? C45 C46 C47 C48 -1.8(7) . . . . ? C46 C47 C48 C43 1.2(6) . . . . ? C46 C47 C48 C49 -179.6(4) . . . . ? C47 C48 C49 C40 178.9(4) . . . . ? C47 C48 C49 O50 0.5(6) . . . . ? C48 C43 C44 C45 -0.7(7) . . . . ? C48 C43 O42 C41 0.7(6) . . . . ? C48 C49 O50 C51 176.6(4) . . . . ? C49 C40 C41 O42 6.2(6) . . . . ? C49 C40 C41 O67 -172.6(4) . . . . ? C51 C38 C39 C40 -2.9(6) . . . . ? C51 C38 C39 C58 -123.0(4) . . . . ? C51 C38 C39 C59 125.0(4) . . . . ? C51 C52 C53 C54 178.2(4) . . . . ? C52 C35 C56 C55 1.2(7) . . . . ? C52 C35 O36 C37 -4.8(6) . . . . ? C52 C51 O50 C49 -176.6(4) . . . . ? C52 C53 C54 C55 1.5(7) . . . . ? C53 C54 C55 C56 -1.1(7) . . . . ? C54 C55 C56 C35 -0.3(7) . . . . ? C56 C35 C52 C51 -179.7(4) . . . . ? C56 C35 C52 C53 -0.7(7) . . . . ? C56 C35 O36 C37 173.8(4) . . . . ? C58 C39 C40 C41 -53.8(5) . . . . ? C58 C39 C40 C49 123.3(4) . . . . ? C58 C39 C59 C60 -175.7(5) . . . . ? C58 C39 C59 C64 0.9(5) . . . . ? C59 C39 C40 C41 59.6(5) . . . . ? C59 C39 C40 C49 -123.4(4) . . . . ? C59 C39 C58 N57 -1.5(4) . . . . ? C59 C39 C58 O65 176.3(4) . . . . ? C59 C60 C61 C62 0.9(7) . . . . ? C59 C60 C61 Cl66 -178.0(4) . . . . ? C59 C64 N57 C58 -1.2(5) . . . . ? C60 C59 C64 C63 -1.7(7) . . . . ? C60 C59 C64 N57 177.0(4) . . . . ? C60 C61 C62 C63 -2.2(8) . . . . ? C61 C62 C63 C64 1.4(7) . . . . ? C62 C63 C64 C59 0.4(7) . . . . ? C62 C63 C64 N57 -178.0(5) . . . . ? C63 C64 N57 C58 177.3(5) . . . . ? C64 C59 C60 C61 1.0(7) . . . . ? O36 C35 C52 C51 -1.2(6) . . . . ? O36 C35 C52 C53 177.7(4) . . . . ? O36 C35 C56 C55 -177.4(4) . . . . ? O36 C37 C38 C39 175.2(4) . . . . ? O36 C37 C38 C51 -7.4(6) . . . . ? O42 C43 C44 C45 177.2(4) . . . . ? O42 C43 C48 C47 -177.8(4) . . . . ? O42 C43 C48 C49 2.9(6) . . . . ? O50 C51 C52 C35 -178.5(4) . . . . ? O50 C51 C52 C53 2.7(6) . . . . ? O65 C58 N57 C64 -176.0(5) . . . . ? O67 C41 O42 C43 173.6(4) . . . . ? O68 C37 C38 C39 -3.5(7) . . . . ? O68 C37 C38 C51 173.9(4) . . . . ? O68 C37 O36 C35 -172.2(4) . . . . ? Cl66 C61 C62 C63 176.8(4) . . . . ? _shelx_res_file ; bb_s3_1_lt_mo.res created by SHELXL-2014/7 TITL bb_s3_1_lt_mo_a.res in P-1 CELL 0.71073 11.8182 12.7608 17.1455 77.158 73.729 66.373 ZERR 1 0.0006 0.0011 0.0011 0.006 0.005 0.007 LATT 1 SFAC C H N O Cl S UNIT 108 64 4 29 4 2 EQIV $1 -X,2-Y,1-Z EQIV $2 -1-X,2-Y,1-Z DFIX 1.8 S1 C92 S1 C93 S1' C92' S1' C93' DFIX 1.52 S1 O91 S1' O91' DFIX 0.9 O93 H93g O93 H93h O92 H92h O92 H92g DFIX 1.47 H93h H93g H92g H92h SIMU 0.02 0.04 2 O93 H93h H93g SIMU 0.02 0.04 2 O92 H92g H92h L.S. 11 PLAN 2 HTAB N23 O91_$1 HTAB N23 O92_$1 HTAB N57 O93_$1 HTAB N57 O91'_$1 HTAB C92 O93 HTAB C92 O31 HTAB C93 O93_$2 HTAB C93' O68_$1 HTAB C93' O34_$1 HTAB O92 O92_$1 HTAB O92 O31 HTAB O93 N57_$1 HTAB O93 O93_$2 CONF BOND $H fmap 2 acta MORE -1 MERG 2 OMIT -3 50 REM REM REM WGHT 0.042700 10.110500 EXTI 0.003993 FVAR 0.44226 C1 1 0.339517 0.406497 0.575947 11.00000 0.01789 0.02304 = 0.02248 0.00010 -0.00209 -0.00684 C3 1 0.318087 0.584986 0.485994 11.00000 0.02260 0.02386 = 0.02032 0.00409 -0.00523 -0.00783 C4 1 0.245070 0.557845 0.443652 11.00000 0.01691 0.02357 = 0.01873 0.00094 -0.00324 -0.00856 C5 1 0.197449 0.642764 0.371506 11.00000 0.01949 0.02219 = 0.02058 -0.00158 -0.00357 -0.00916 C6 1 0.115464 0.600076 0.343136 11.00000 0.01894 0.02056 = 0.01704 -0.00091 -0.00328 -0.00657 C7 1 0.054756 0.670625 0.275947 11.00000 0.02503 0.02115 = 0.02369 0.00395 -0.00791 -0.00854 C9 1 -0.034980 0.528483 0.282170 11.00000 0.02273 0.02263 = 0.02265 -0.00170 -0.00255 -0.00792 C10 1 -0.110680 0.496485 0.250905 11.00000 0.03017 0.03664 = 0.02253 -0.00385 -0.00940 -0.01262 AFIX 43 H10 2 -0.145770 0.541955 0.206933 11.00000 -1.20000 AFIX 0 C11 1 -0.133612 0.396893 0.285380 11.00000 0.03714 0.04076 = 0.02565 -0.01031 -0.00194 -0.02331 AFIX 43 H11 2 -0.186007 0.376104 0.265259 11.00000 -1.20000 AFIX 0 C12 1 -0.079525 0.327000 0.349844 11.00000 0.03586 0.02953 = 0.02559 -0.00551 -0.00083 -0.01781 AFIX 43 H12 2 -0.094252 0.258978 0.371869 11.00000 -1.20000 AFIX 0 C13 1 -0.003814 0.358530 0.381266 11.00000 0.02529 0.02690 = 0.02488 -0.00245 -0.00201 -0.01183 AFIX 43 H13 2 0.032498 0.312120 0.424545 11.00000 -1.20000 AFIX 0 C14 1 0.017826 0.461497 0.347176 11.00000 0.01840 0.02516 = 0.01712 -0.00450 0.00147 -0.00734 C15 1 0.095178 0.501479 0.376160 11.00000 0.01978 0.02333 = 0.01789 0.00070 -0.00396 -0.00594 C17 1 0.218578 0.461315 0.472002 11.00000 0.02445 0.02272 = 0.01756 -0.00053 -0.00483 -0.01096 C18 1 0.262836 0.381349 0.539868 11.00000 0.02004 0.02062 = 0.02157 0.00027 -0.00511 -0.00592 C19 1 0.231582 0.282662 0.572280 11.00000 0.02394 0.02631 = 0.02306 0.00216 -0.00500 -0.00985 AFIX 43 H19 2 0.180713 0.264544 0.548821 11.00000 -1.20000 AFIX 0 C20 1 0.277130 0.212766 0.639344 11.00000 0.03209 0.02186 = 0.02900 0.00678 -0.00941 -0.00804 AFIX 43 H20 2 0.255365 0.148312 0.661953 11.00000 -1.20000 AFIX 0 C21 1 0.355829 0.239090 0.673061 11.00000 0.03124 0.02805 = 0.02590 0.00733 -0.01197 -0.00614 AFIX 43 H21 2 0.386870 0.191038 0.717706 11.00000 -1.20000 AFIX 0 C22 1 0.388491 0.334888 0.641526 11.00000 0.02227 0.03172 = 0.02474 0.00453 -0.00902 -0.00827 AFIX 43 H22 2 0.442139 0.351007 0.663782 11.00000 -1.20000 AFIX 0 C24 1 0.286945 0.780263 0.293609 11.00000 0.02411 0.01891 = 0.02203 0.00024 -0.00766 -0.00886 C25 1 0.367318 0.825275 0.233217 11.00000 0.02836 0.02304 = 0.02531 0.00220 -0.00860 -0.01232 AFIX 43 H25 2 0.357033 0.902552 0.227653 11.00000 -1.20000 AFIX 0 C26 1 0.463647 0.750881 0.181382 11.00000 0.02251 0.02818 = 0.02405 0.00550 -0.00658 -0.01196 AFIX 43 H26 2 0.518710 0.778266 0.139834 11.00000 -1.20000 AFIX 0 C27 1 0.477750 0.635285 0.191644 11.00000 0.02406 0.02357 = 0.02315 0.00030 -0.00463 -0.00803 C28 1 0.398306 0.590166 0.252540 11.00000 0.02408 0.01755 = 0.02315 0.00064 -0.00779 -0.00852 AFIX 43 H28 2 0.409408 0.512601 0.258841 11.00000 -1.20000 AFIX 0 C29 1 0.302569 0.664213 0.303247 11.00000 0.02468 0.02142 = 0.01657 0.00409 -0.00860 -0.01422 C30 1 0.120745 0.766560 0.396744 11.00000 0.02504 0.02582 = 0.01941 0.00013 -0.00661 -0.01057 N23 3 0.181230 0.837318 0.350298 11.00000 0.02932 0.01876 = 0.02194 -0.00174 -0.00397 -0.00950 AFIX 43 H23 2 0.157112 0.909112 0.355266 11.00000 -1.20000 AFIX 0 O2 4 0.368029 0.504667 0.548026 11.00000 0.02615 0.02801 = 0.02417 0.00681 -0.01022 -0.01422 O8 4 -0.014639 0.629378 0.246469 11.00000 0.02833 0.03010 = 0.02554 0.00445 -0.01171 -0.01513 O16 4 0.145341 0.429208 0.439672 11.00000 0.03034 0.02393 = 0.02272 0.00617 -0.01337 -0.01432 O31 4 0.023789 0.792916 0.449006 11.00000 0.02929 0.02818 = 0.02692 -0.00096 -0.00277 -0.00859 O33 4 0.061645 0.762986 0.243462 11.00000 0.03905 0.03081 = 0.03817 0.01265 -0.02185 -0.01793 O34 4 0.339380 0.673601 0.471837 11.00000 0.03809 0.03107 = 0.03229 0.00592 -0.01570 -0.01937 CL32 5 0.598838 0.545374 0.124349 11.00000 0.03640 0.03299 = 0.04672 -0.01067 0.01645 -0.01298 C35 1 0.043117 0.701819 0.946948 11.00000 0.01782 0.02150 = 0.02622 0.00143 -0.00770 -0.00565 C37 1 0.216778 0.745900 0.851922 11.00000 0.01904 0.02238 = 0.03167 -0.00128 -0.00763 -0.00756 C38 1 0.220280 0.808832 0.911563 11.00000 0.01707 0.01559 = 0.02363 0.00188 -0.00881 -0.00501 C39 1 0.319908 0.863581 0.887906 11.00000 0.01771 0.01993 = 0.01748 -0.00052 -0.00475 -0.00665 C40 1 0.298081 0.934403 0.954781 11.00000 0.01839 0.01538 = 0.02154 0.00279 -0.00935 -0.00482 C41 1 0.373883 1.005114 0.941381 11.00000 0.01483 0.01719 = 0.02505 -0.00312 -0.00559 -0.00157 C43 1 0.267615 1.065304 1.074618 11.00000 0.01706 0.01809 = 0.02162 -0.00068 -0.00631 -0.00147 C44 1 0.257629 1.132134 1.131551 11.00000 0.02356 0.02445 = 0.02699 -0.00386 -0.00810 -0.00856 AFIX 43 H44 2 0.312659 1.171138 1.122820 11.00000 -1.20000 AFIX 0 C45 1 0.162975 1.139212 1.202113 11.00000 0.02808 0.02517 = 0.02525 -0.00547 -0.00826 -0.00439 AFIX 43 H45 2 0.154639 1.183802 1.240999 11.00000 -1.20000 AFIX 0 C46 1 0.080713 1.081089 1.215671 11.00000 0.02157 0.02296 = 0.02037 -0.00305 -0.00250 -0.00033 AFIX 43 H46 2 0.017059 1.087942 1.262816 11.00000 -1.20000 AFIX 0 C47 1 0.093444 1.013267 1.159247 11.00000 0.02148 0.01978 = 0.02402 0.00017 -0.00641 -0.00606 AFIX 43 H47 2 0.039892 0.972528 1.168920 11.00000 -1.20000 AFIX 0 C48 1 0.187008 1.005697 1.087355 11.00000 0.01880 0.01496 = 0.01878 0.00092 -0.00804 -0.00165 C49 1 0.208351 0.938111 1.023880 11.00000 0.01866 0.01710 = 0.02150 0.00174 -0.00910 -0.00547 C51 1 0.133484 0.819526 0.982362 11.00000 0.02024 0.01412 = 0.02183 0.00220 -0.00929 -0.00354 C52 1 0.039047 0.768301 1.002627 11.00000 0.01880 0.01460 = 0.02429 0.00458 -0.00944 -0.00367 C53 1 -0.057490 0.782600 1.073703 11.00000 0.02421 0.02453 = 0.02047 0.00487 -0.00714 -0.00951 AFIX 43 H53 2 -0.061912 0.825995 1.112196 11.00000 -1.20000 AFIX 0 C54 1 -0.146052 0.731811 1.086218 11.00000 0.02039 0.03136 = 0.02989 0.00524 -0.00734 -0.00921 AFIX 43 H54 2 -0.211220 0.742693 1.132595 11.00000 -1.20000 AFIX 0 C55 1 -0.137957 0.664502 1.029652 11.00000 0.02657 0.02941 = 0.03631 0.01006 -0.01419 -0.01631 AFIX 43 H55 2 -0.197096 0.629718 1.039123 11.00000 -1.20000 AFIX 0 C56 1 -0.043519 0.648806 0.959897 11.00000 0.02687 0.01960 = 0.03806 -0.00052 -0.01024 -0.01030 AFIX 43 H56 2 -0.038050 0.603580 0.922301 11.00000 -1.20000 AFIX 0 C58 1 0.308231 0.943114 0.803923 11.00000 0.03252 0.02137 = 0.02365 0.00104 -0.01017 -0.01310 C59 1 0.454879 0.775954 0.866540 11.00000 0.02060 0.02162 = 0.02005 -0.00471 -0.00543 -0.00998 C60 1 0.519849 0.679611 0.912374 11.00000 0.02188 0.02737 = 0.02425 -0.00646 -0.00519 -0.00899 AFIX 43 H60 2 0.484326 0.659617 0.966502 11.00000 -1.20000 AFIX 0 C61 1 0.641042 0.612492 0.875179 11.00000 0.02472 0.03050 = 0.03555 -0.01339 -0.00902 -0.00288 C62 1 0.694814 0.642613 0.795337 11.00000 0.02117 0.04325 = 0.03796 -0.02205 0.00298 -0.00943 AFIX 43 H62 2 0.776980 0.597612 0.772623 11.00000 -1.20000 AFIX 0 C63 1 0.628119 0.738976 0.748508 11.00000 0.02758 0.04525 = 0.02595 -0.01545 0.00728 -0.01947 AFIX 43 H63 2 0.663375 0.758645 0.694248 11.00000 -1.20000 AFIX 0 C64 1 0.507117 0.805064 0.785235 11.00000 0.02423 0.02795 = 0.02665 -0.00619 -0.00269 -0.01504 N57 3 0.421133 0.902934 0.750336 11.00000 0.03484 0.03143 = 0.01284 0.00269 -0.00186 -0.01954 AFIX 43 H57 2 0.437361 0.934385 0.700738 11.00000 -1.20000 AFIX 0 O36 4 0.132850 0.688302 0.875139 11.00000 0.02243 0.02827 = 0.03065 -0.00675 -0.00206 -0.01192 O42 4 0.358852 1.064305 1.003708 11.00000 0.02286 0.02165 = 0.02541 -0.00375 -0.00417 -0.00974 O50 4 0.125638 0.881009 1.040445 11.00000 0.02207 0.02691 = 0.02268 -0.00190 -0.00391 -0.01435 O65 4 0.213544 1.022331 0.790830 11.00000 0.03893 0.02490 = 0.03131 0.00533 -0.01630 -0.00518 O67 4 0.448044 1.017038 0.878834 11.00000 0.02554 0.03036 = 0.02687 -0.00403 0.00105 -0.01503 O68 4 0.282357 0.737972 0.784269 11.00000 0.03360 0.03630 = 0.02674 -0.00761 -0.00266 -0.01713 CL66 5 0.728818 0.485500 0.928314 11.00000 0.04138 0.04258 = 0.04771 -0.01439 -0.01613 0.01605 PART 1 C92 1 -0.222583 1.012982 0.456560 10.50000 0.05124 0.04757 = 0.04991 -0.00136 -0.02240 -0.00051 AFIX 137 H92A 2 -0.220936 1.088326 0.453860 10.50000 -1.50000 H92B 2 -0.299109 1.020102 0.443076 10.50000 -1.50000 H92C 2 -0.151071 0.970072 0.418347 10.50000 -1.50000 AFIX 0 C93 1 -0.362818 1.036213 0.608714 10.50000 0.03103 0.05652 = 0.06216 -0.03452 0.00520 -0.02395 AFIX 137 H93A 2 -0.371922 1.015432 0.666878 10.50000 -1.50000 H93B 2 -0.431586 1.031556 0.592075 10.50000 -1.50000 H93C 2 -0.363507 1.113569 0.594512 10.50000 -1.50000 AFIX 0 O91 4 -0.113546 0.954959 0.585063 10.50000 0.04431 0.02501 = 0.03206 -0.01244 -0.01203 -0.00641 O93 4 -0.533209 1.105485 0.424350 10.50000 0.06216 0.06178 = 0.02811 -0.00026 -0.01082 -0.02711 S1 6 -0.216318 0.939397 0.557760 10.50000 0.03970 0.02591 = 0.03950 -0.00762 -0.00950 -0.01101 PART 2 C92' 1 -0.237379 1.094256 0.412818 10.50000 0.06892 0.06254 = 0.14173 0.03251 -0.06394 -0.03812 AFIX 137 H92D 2 -0.195707 1.013199 0.427575 10.50000 -1.50000 H92E 2 -0.203163 1.136805 0.433283 10.50000 -1.50000 H92F 2 -0.224343 1.111161 0.354272 10.50000 -1.50000 AFIX 0 C93' 1 -0.451074 1.284033 0.396688 10.50000 0.00195 0.01312 = 0.00001 -0.00364 0.00194 -0.00609 AFIX 137 H93D 2 -0.398680 1.281620 0.342539 10.50000 -1.50000 H93E 2 -0.440598 1.336457 0.424060 10.50000 -1.50000 H93F 2 -0.537976 1.309666 0.393220 10.50000 -1.50000 AFIX 0 O91' 4 -0.445179 1.055926 0.426121 10.50000 0.07419 0.06549 = 0.01837 -0.00130 -0.00554 -0.05232 O92 4 -0.054548 0.971827 0.555289 10.50000 0.05808 0.04019 = 0.04236 -0.01378 0.00687 -0.01807 S1' 6 -0.403614 1.134642 0.456422 10.50000 0.09866 0.07551 = 0.02774 0.00417 -0.01847 -0.06501 H92G 2 0.000000 1.000000 0.500000 10.50000 0.05421 H92H 2 -0.062379 0.915702 0.535067 10.50000 0.04679 PART 1 H93G 2 -0.455268 1.072371 0.394061 10.50000 0.05373 H93H 2 -0.543456 1.060184 0.472214 10.50000 0.05368 HKLF 4 REM bb_s3_1_lt_mo_a.res in P-1 REM R1 = 0.0799 for 6738 Fo > 4sig(Fo) and 0.0906 for all 7896 data REM 721 parameters refined using 38 restraints END WGHT 0.0463 9.7324 REM Highest difference peak 1.689, deepest hole -0.386, 1-sigma level 0.085 Q1 1 0.7538 0.5561 0.9576 11.00000 0.05 0.35 Q2 1 -0.3766 1.0982 0.5352 11.00000 0.05 0.31 ; _shelx_res_checksum 91629 _shelx_hkl_file ; 0 0 2 590.10 7.78 0 0 2 608.29 8.60 0 0 -2 601.95 7.84 0 0 -3 220.64 4.40 0 0 3 219.17 5.05 0 0 3 206.83 4.29 0 0 4 42.20 2.55 0 0 -4 44.91 2.12 0 0 4 42.52 2.09 0 0 5 112.32 4.42 0 0 5 111.55 3.72 0 0 -5 110.79 3.70 0 0 6 1897.19 26.65 0 0 6 1935.51 24.72 0 0 -6 1889.88 24.60 0 0 -7 12.03 1.64 0 0 7 11.22 2.00 0 0 7 14.90 1.75 0 0 8 6.89 1.65 0 0 -8 4.19 1.16 0 0 9 1056.04 20.38 0 0 -9 1062.74 18.07 0 0 10 478.39 13.47 0 0 -10 487.42 11.56 0 0 -11 102.65 5.30 0 0 11 107.01 6.36 0 0 12 299.39 11.41 0 0 -12 281.03 9.28 0 0 13 -2.24 1.51 0 0 -13 2.01 1.23 0 0 14 69.72 5.83 0 0 -14 67.07 4.92 0 0 -15 59.93 4.85 0 0 15 55.93 5.57 0 0 16 81.79 6.93 0 0 -16 79.12 5.90 0 0 17 5.30 2.25 0 0 18 24.42 4.24 0 0 19 72.52 7.35 0 0 20 16.93 4.22 0 0 21 20.74 4.42 0 -1 21 4.89 2.45 0 -1 20 45.78 6.07 0 -1 19 32.63 5.09 0 -1 18 0.67 1.87 0 -1 17 49.65 5.60 0 1 -17 52.96 4.98 0 -1 16 6.51 2.18 0 1 -16 7.58 2.17 0 1 -15 8.80 2.14 0 -1 15 8.03 2.34 0 1 -14 4.10 1.44 0 -1 14 4.58 1.88 0 1 -13 47.28 3.86 0 -1 13 42.66 4.39 0 -1 12 7.47 2.25 0 1 -12 6.98 1.72 0 -1 11 11.69 2.40 0 -1 11 11.05 2.01 0 1 -11 10.20 1.70 0 1 -10 553.25 12.37 0 -1 10 554.99 13.01 0 -1 10 551.45 14.56 0 -1 9 31.97 3.23 0 -1 9 30.20 2.66 0 1 -9 32.68 2.68 0 1 -8 84.62 3.99 0 -1 8 85.96 5.07 0 -1 8 86.95 4.25 0 -1 7 103.34 5.16 0 1 -7 104.63 4.12 0 -1 7 106.45 4.50 0 -1 6 24.02 2.49 0 -1 6 27.09 2.13 0 1 -6 26.58 1.92 0 -1 5 943.95 15.66 0 -1 5 887.16 13.94 0 1 -5 890.27 13.21 0 -1 4 95.03 3.41 0 -1 4 95.34 3.94 0 1 -4 99.48 3.13 0 -1 3 80.75 2.86 0 -1 3 81.46 3.34 0 1 -3 77.47 2.42 0 1 -2 3153.95 33.63 0 -1 2 3208.23 34.86 0 -1 1 1160.39 13.84 0 1 0 175.04 3.29 0 -1 0 168.63 3.13 0 -1 -1 1503.73 16.75 0 1 1 1524.62 17.51 0 1 2 1092.06 14.18 0 -1 -2 1101.86 13.31 0 1 3 342.95 6.62 0 -1 -3 341.88 5.85 0 1 4 616.80 11.00 0 -1 -4 646.63 9.05 0 -1 -4 601.24 9.88 0 1 5 1693.40 23.30 0 -1 -5 1621.87 19.95 0 -1 -5 1660.16 21.49 0 1 6 1.10 0.81 0 -1 -6 1.40 0.82 0 1 7 365.17 9.96 0 -1 -7 380.31 8.69 0 1 8 179.23 7.18 0 -1 -8 190.38 6.30 0 1 9 241.02 8.81 0 -1 -9 238.20 7.45 0 -1 -10 8.22 1.63 0 1 10 8.77 1.92 0 1 11 212.14 9.10 0 -1 -11 226.37 7.99 0 -1 -12 48.03 3.87 0 1 12 45.70 4.36 0 -1 -13 84.79 5.46 0 1 13 81.17 6.15 0 -1 -14 21.10 3.02 0 1 14 22.08 3.47 0 -1 -15 23.90 3.29 0 1 15 24.09 3.79 0 1 16 148.31 9.34 0 1 17 3.92 2.06 0 1 18 45.02 5.68 0 1 19 18.41 4.00 0 1 20 2.41 2.03 0 1 21 7.42 3.04 0 -2 21 3.53 2.44 0 -2 20 14.28 3.74 0 -2 19 2.01 1.95 0 -2 18 8.73 2.83 0 -2 17 42.06 5.48 0 2 -16 94.42 6.25 0 -2 16 79.62 7.15 0 2 -15 3.05 1.31 0 -2 15 1.89 1.46 0 2 -14 7.14 1.91 0 -2 14 7.72 2.23 0 -2 14 8.56 2.08 0 2 -13 1.83 1.22 0 -2 13 1.38 1.30 0 -2 13 1.61 1.36 0 2 -12 1.92 1.14 0 -2 12 3.11 1.36 0 -2 12 3.38 1.80 0 -2 11 23.12 3.12 0 -2 11 21.80 2.70 0 2 -11 20.26 2.42 0 2 -10 52.97 3.47 0 -2 10 49.91 4.33 0 -2 10 54.24 3.96 0 -2 9 12.07 2.26 0 2 -9 15.36 1.83 0 -2 9 12.44 2.03 0 -2 8 392.55 11.46 0 2 -8 424.20 9.46 0 -2 8 421.09 10.57 0 -2 7 66.61 4.36 0 2 -7 69.78 3.35 0 -2 7 71.91 3.98 0 2 -6 1040.28 15.50 0 -2 6 1056.18 19.04 0 -2 6 1047.00 17.27 0 2 -5 234.86 5.49 0 -2 5 228.34 6.53 0 -2 5 228.68 7.28 0 2 -4 664.96 10.03 0 -2 4 667.25 11.88 0 -2 3 301.10 6.85 0 2 -3 297.06 5.43 0 -2 2 1121.60 15.36 0 2 -2 1088.93 13.32 0 -2 1 947.36 13.20 0 -2 0 126.41 3.48 0 2 0 129.18 3.70 0 -2 -1 1143.44 14.65 0 2 1 1151.67 15.48 0 -2 -2 977.92 13.00 0 2 2 963.21 14.19 0 -2 -3 532.51 8.58 0 2 3 518.80 9.81 0 -2 -3 533.61 7.84 0 -2 -4 899.65 11.67 0 -2 -4 860.87 13.20 0 2 4 867.96 14.60 0 -2 -5 991.82 15.24 0 2 5 1028.75 16.99 0 -2 -5 1001.83 13.75 0 -2 -6 62.25 3.26 0 -2 -6 64.59 2.67 0 2 6 63.50 3.83 0 2 7 44.76 3.44 0 -2 -7 37.32 2.42 0 -2 -7 53.52 3.17 0 2 8 26.06 2.92 0 -2 -8 25.22 2.33 0 2 9 10.00 2.00 0 -2 -9 7.66 1.57 0 -2 -10 62.03 4.09 0 2 10 64.90 4.88 0 2 11 68.93 5.24 0 -2 -11 57.91 4.17 0 -2 -12 59.11 4.44 0 2 12 49.25 4.70 0 -2 -13 53.57 4.43 0 2 13 51.65 4.95 0 2 14 21.33 3.43 0 2 15 25.81 3.97 0 2 16 19.35 3.67 0 2 17 73.18 7.04 0 2 18 17.64 3.72 0 2 19 4.20 2.34 0 2 20 38.98 5.72 0 2 21 1.82 1.78 0 -3 20 0.59 1.85 0 -3 19 32.06 4.79 0 -3 18 12.15 3.32 0 -3 17 7.55 2.59 0 -3 16 8.71 2.68 0 -3 15 30.01 4.13 0 -3 15 35.92 4.21 0 -3 14 39.94 4.22 0 -3 14 32.74 4.45 0 3 -13 51.39 3.87 0 -3 13 59.71 5.00 0 -3 13 45.02 4.80 0 3 -12 25.40 2.74 0 -3 12 23.88 3.38 0 -3 12 28.57 3.41 0 3 -11 132.39 5.72 0 -3 11 121.03 7.38 0 -3 11 116.97 6.42 0 -3 10 31.76 3.65 0 -3 10 33.91 3.38 0 3 -10 31.09 2.75 0 -3 9 609.70 16.16 0 3 -9 650.28 12.76 0 -3 9 641.24 14.96 0 3 -8 85.47 3.94 0 -3 8 78.09 5.42 0 -3 8 91.64 5.03 0 -3 7 66.80 4.08 0 -3 7 67.17 4.63 0 3 -7 67.71 3.28 0 3 -6 70.70 3.20 0 -3 6 77.14 4.43 0 3 -5 985.13 14.13 0 -3 5 960.24 16.91 0 -3 4 256.01 7.31 0 3 -4 261.39 5.55 0 -3 3 207.35 6.25 0 3 -3 203.73 4.55 0 -3 2 563.51 10.67 0 -3 1 155.25 4.90 0 3 0 276.97 6.86 0 -3 0 287.65 6.59 0 -3 -1 134.29 4.32 0 3 1 136.39 4.72 0 3 2 634.53 11.79 0 -3 -2 645.34 10.73 0 -3 -3 103.43 3.74 0 3 3 103.87 4.55 0 -3 -4 124.96 3.74 0 3 4 125.64 5.15 0 -3 -4 121.64 4.14 0 -3 -5 14.16 1.27 0 3 5 13.49 1.89 0 -3 -5 12.42 1.39 0 -3 -6 262.40 5.82 0 3 6 240.24 8.12 0 3 7 100.68 5.43 0 -3 -7 100.13 3.72 0 3 8 -0.46 0.96 0 -3 -8 0.56 0.52 0 -3 -9 41.70 2.70 0 3 9 55.54 4.49 0 3 10 231.38 9.59 0 3 11 14.30 2.71 0 3 12 78.38 6.04 0 3 13 20.75 3.49 0 3 14 96.82 7.24 0 3 15 10.11 2.90 0 3 16 9.56 2.87 0 3 17 6.92 2.75 0 3 18 10.05 2.96 0 3 19 38.93 5.95 0 3 20 6.32 3.31 0 3 21 4.56 2.52 0 -4 18 62.01 6.91 0 -4 17 7.76 2.80 0 -4 16 1.44 1.70 0 -4 15 11.41 3.22 0 -4 15 16.60 3.24 0 -4 14 15.93 2.96 0 -4 14 7.26 2.37 0 -4 13 50.67 4.77 0 -4 13 46.93 5.14 0 -4 12 23.39 3.24 0 -4 12 13.23 2.78 0 -4 11 154.53 7.75 0 -4 11 150.14 8.75 0 4 -11 153.49 6.16 0 -4 10 36.39 3.73 0 -4 10 40.94 4.30 0 4 -10 37.06 2.83 0 -4 9 47.32 4.16 0 -4 9 42.22 4.29 0 4 -9 45.33 3.05 0 4 -8 100.28 4.26 0 -4 8 109.43 5.95 0 -4 8 104.73 6.52 0 4 -7 145.87 4.88 0 -4 7 142.21 6.57 0 -4 6 140.31 6.23 0 4 -6 142.43 4.53 0 4 -5 25.71 1.78 0 -4 5 29.35 2.90 0 -4 4 256.99 7.97 0 4 -4 257.93 5.74 0 -4 3 81.70 4.22 0 -4 2 10.17 1.57 0 -4 1 2090.58 28.11 0 -4 0 592.07 11.52 0 -4 -1 277.61 7.26 0 4 1 284.23 7.91 0 -4 -2 14.70 1.71 0 4 2 14.81 1.91 0 4 3 1138.06 19.31 0 -4 -3 1179.57 17.64 0 4 4 162.00 6.46 0 -4 -4 174.48 5.51 0 -4 -5 299.84 6.95 0 4 5 302.24 9.22 0 -4 -5 315.17 7.66 0 -4 -6 213.00 5.74 0 -4 -6 217.75 6.38 0 4 6 224.18 8.16 0 -4 -7 120.90 4.84 0 4 7 110.87 5.96 0 -4 -7 131.78 4.31 0 4 8 29.28 3.33 0 -4 -8 28.64 2.09 0 -4 -9 2.59 0.72 0 4 9 2.85 1.55 0 4 10 10.57 2.40 0 4 11 228.74 10.34 0 4 12 121.34 7.78 0 4 13 512.08 16.94 0 4 14 158.83 9.58 0 4 15 164.50 10.06 0 4 16 18.03 3.76 0 4 17 8.60 2.98 0 4 18 6.23 2.84 0 4 19 14.49 3.98 0 4 20 0.18 1.76 0 -5 17 -0.15 1.60 0 -5 16 30.45 4.71 0 -5 15 4.52 1.93 0 -5 15 5.59 1.94 0 -5 14 33.26 4.27 0 -5 14 39.90 5.05 0 -5 13 4.83 1.94 0 -5 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12 11.79 3.39 1 -9 13 6.14 2.61 1 -9 13 3.51 2.49 1 -9 14 71.48 8.14 1 -9 14 75.50 7.56 1 -9 15 15.42 3.92 -1 8 17 9.82 3.28 -1 8 16 -0.25 2.16 -1 8 15 14.40 3.98 -1 8 14 62.98 7.16 -1 8 13 99.32 8.52 -1 8 12 38.66 5.36 -1 8 11 23.36 4.03 -1 8 10 20.36 3.73 1 -8 -9 45.32 4.19 -1 8 9 50.34 5.57 1 -8 -8 6.73 1.80 -1 8 8 6.79 2.26 1 -8 -7 23.53 3.06 -1 8 7 25.06 3.77 1 -8 -6 10.55 2.15 -1 8 6 12.50 2.58 -1 8 5 609.90 18.12 1 -8 -5 590.47 15.89 -1 8 4 376.79 13.86 1 -8 -4 374.83 12.32 1 -8 -3 52.33 4.63 -1 8 3 54.08 5.12 -1 8 2 113.41 7.27 1 -8 -2 101.74 6.41 1 -8 -1 15.36 2.74 1 -8 0 65.83 5.20 1 -8 1 31.53 3.81 1 -8 2 164.00 8.39 1 -8 3 5.55 1.92 1 -8 4 168.57 8.77 1 -8 5 967.18 22.82 1 -8 6 854.74 21.61 1 -8 7 50.61 5.18 1 -8 8 19.21 3.41 1 -8 9 16.64 3.33 1 -8 10 46.96 5.30 1 -8 11 85.96 7.21 1 -8 12 16.10 3.71 1 -8 12 10.87 3.13 1 -8 13 71.05 7.08 1 -8 13 66.54 7.50 1 -8 14 97.78 9.10 1 -8 14 102.99 8.58 1 -8 15 51.09 6.19 1 -8 15 33.47 5.66 1 -8 16 61.74 7.36 1 -8 16 72.74 7.48 -1 7 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6 16 24.96 4.63 -1 6 15 34.32 5.28 -1 6 14 44.83 5.56 -1 6 13 106.71 8.23 -1 6 12 47.22 5.34 -1 6 11 13.27 3.16 -1 6 10 77.51 6.46 1 -6 -10 72.62 4.76 -1 6 9 20.52 3.38 1 -6 -9 20.44 2.56 1 -6 -8 102.25 5.56 -1 6 8 97.99 6.77 1 -6 -7 8.76 1.76 -1 6 7 11.39 2.52 -1 6 6 8.13 2.10 1 -6 -6 8.69 1.83 1 -6 -5 47.42 3.73 -1 6 5 35.24 3.78 -1 6 4 28.28 3.33 1 -6 -4 33.27 3.17 -1 6 3 19.15 2.89 1 -6 -3 15.26 2.26 1 -6 -2 273.61 9.19 -1 6 2 272.27 10.04 1 -6 -1 194.68 7.79 -1 6 1 194.29 8.30 1 -6 0 183.29 7.58 1 -6 1 43.88 3.74 1 -6 2 196.80 7.98 1 -6 3 18.70 2.61 1 -6 4 16.72 2.72 1 -6 5 283.97 10.34 1 -6 6 13.45 2.41 1 -6 7 11.39 2.31 1 -6 8 87.61 6.00 1 -6 9 2.31 1.20 1 -6 10 59.62 5.26 1 -6 11 45.00 4.88 1 -6 11 38.51 5.25 1 -6 12 165.09 10.49 1 -6 12 184.22 9.77 1 -6 13 3.06 1.89 1 -6 13 5.16 2.08 1 -6 14 15.72 3.66 1 -6 14 10.31 2.79 1 -6 15 13.66 3.08 1 -6 15 11.02 3.28 1 -6 16 14.02 3.44 1 -6 17 43.50 6.11 1 -6 18 5.99 2.66 -1 5 20 16.90 4.36 -1 5 19 26.47 5.06 -1 5 18 -0.12 1.75 -1 5 17 5.62 2.58 -1 5 16 -0.38 2.17 -1 5 15 24.91 4.24 -1 5 14 0.21 1.85 -1 5 13 218.79 11.35 -1 5 12 196.40 10.48 1 -5 -11 325.27 10.26 -1 5 11 334.21 13.26 1 -5 -10 5.78 1.48 -1 5 10 6.03 2.16 -1 5 9 324.99 12.26 1 -5 -9 323.63 9.97 1 -5 -8 13.90 2.09 -1 5 8 12.72 2.44 -1 5 7 34.69 3.84 1 -5 -7 38.73 3.20 1 -5 -7 35.61 2.23 -1 5 6 1.31 1.14 1 -5 -6 0.73 0.44 1 -5 -6 2.87 1.22 1 -5 -5 148.30 6.20 -1 5 5 151.83 7.22 1 -5 -4 191.91 7.02 -1 5 4 172.39 7.53 1 -5 -3 132.35 5.82 -1 5 3 132.41 6.49 1 -5 -2 28.84 2.78 -1 5 2 29.70 3.10 -1 5 1 507.35 12.91 1 -5 -1 508.02 12.16 1 -5 0 338.01 9.67 1 -5 1 673.46 14.57 1 -5 2 1108.30 20.03 1 -5 3 351.19 10.27 -1 5 -4 55.65 1.93 1 -5 4 51.81 3.87 -1 5 -5 64.55 2.18 1 -5 5 65.38 4.52 1 -5 6 116.76 6.20 1 -5 7 239.02 9.25 1 -5 8 44.68 4.07 1 -5 9 183.88 8.50 1 -5 10 26.36 3.91 1 -5 10 30.00 3.52 1 -5 11 292.50 13.17 1 -5 11 320.23 11.94 1 -5 12 121.57 7.54 1 -5 12 117.05 8.44 1 -5 13 47.07 4.94 1 -5 13 41.65 5.35 1 -5 14 9.02 2.96 1 -5 14 13.01 2.92 1 -5 15 3.64 1.95 1 -5 15 8.40 2.97 1 -5 16 7.89 3.01 1 -5 17 7.34 2.63 1 -5 18 4.37 2.49 1 -5 19 9.04 2.99 -1 4 20 12.52 3.73 -1 4 19 -1.85 2.36 -1 4 18 33.34 5.26 -1 4 17 1.18 1.70 -1 4 16 3.15 1.97 -1 4 15 13.49 3.22 -1 4 14 276.05 12.87 -1 4 13 946.47 24.24 -1 4 12 554.19 17.32 -1 4 11 105.40 7.10 -1 4 10 90.45 6.37 1 -4 -10 96.91 5.54 -1 4 9 4.66 1.59 1 -4 -9 4.58 1.53 -1 4 8 31.51 3.51 1 -4 -8 31.36 2.98 -1 4 7 223.00 8.96 1 -4 -7 247.51 5.13 1 -4 -7 233.78 7.71 -1 4 6 504.43 13.07 1 -4 -6 484.25 11.01 1 -4 -5 590.99 9.85 -1 4 5 576.06 14.02 1 -4 -5 573.59 12.35 1 -4 -4 1191.05 19.49 -1 4 4 1205.21 21.32 -1 4 3 9.87 1.80 1 -4 -3 14.16 1.83 1 -4 -2 34.60 2.79 -1 4 2 36.61 3.12 1 -4 -1 482.95 10.89 -1 4 1 479.05 11.55 1 -4 0 40.34 2.98 1 -4 1 124.55 5.22 1 -4 2 182.77 6.54 -1 4 -3 4.00 0.54 1 -4 3 2.18 0.95 1 -4 4 9.13 1.72 -1 4 -4 8.71 0.71 -1 4 -5 123.07 3.06 1 -4 5 118.41 5.55 -1 4 -6 62.00 2.34 1 -4 6 60.13 4.13 -1 4 -7 132.09 3.87 1 -4 7 133.41 6.30 1 -4 8 359.50 11.00 -1 4 -8 358.81 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376.31 7.75 -1 1 3 1207.08 17.12 1 -1 -3 1231.21 16.33 1 -1 -2 335.89 6.14 -1 1 2 347.91 6.88 1 -1 -1 252.48 4.51 -1 1 1 252.61 5.30 -1 1 0 1565.49 19.04 1 -1 0 1535.99 16.84 1 -1 0 1583.68 19.08 1 -1 1 37.77 1.83 1 -1 2 457.89 7.64 1 -1 3 1531.44 19.02 -1 1 -3 1506.05 16.52 1 -1 4 113.16 3.64 -1 1 -4 107.17 2.67 1 -1 5 129.94 5.44 -1 1 -5 132.39 3.47 1 -1 5 139.33 4.36 1 -1 6 233.20 6.15 1 -1 6 225.85 7.77 -1 1 -6 228.94 5.27 1 -1 7 604.27 13.92 1 -1 7 602.20 11.36 -1 1 -7 588.31 10.31 1 -1 8 993.82 19.67 -1 1 -8 976.68 15.30 1 -1 8 994.26 16.49 -1 1 -9 10.09 1.46 1 -1 9 7.91 1.74 1 -1 9 7.14 1.33 1 -1 10 124.44 5.48 -1 1 -10 126.93 5.14 1 -1 10 126.06 6.95 1 -1 11 46.15 3.44 1 -1 11 44.14 4.32 -1 1 -11 47.13 3.35 -1 1 -12 12.56 1.98 1 -1 12 14.10 2.88 1 -1 12 12.90 2.04 1 -1 13 54.85 4.15 -1 1 -13 61.85 4.26 1 -1 13 55.81 5.34 1 -1 14 28.36 4.00 1 -1 15 11.09 2.76 1 -1 16 15.24 3.31 1 -1 17 15.24 3.60 1 -1 18 62.49 6.70 1 -1 19 53.49 6.58 1 -1 20 6.50 2.81 1 -1 21 2.59 2.18 -1 0 20 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-1 6 30.14 2.56 -1 -1 6 32.55 2.62 1 1 -6 34.69 2.48 1 1 -5 1587.16 21.73 -1 -1 5 1597.30 22.32 -1 -1 5 1630.38 22.55 1 1 -4 1.89 0.72 -1 -1 4 1.29 0.76 -1 -1 4 2.34 0.75 -1 -1 3 908.13 13.55 -1 -1 3 900.17 12.78 1 1 -3 911.85 13.15 1 1 -2 5.48 0.84 -1 -1 2 4.17 0.78 -1 -1 2 3.91 0.60 -1 -1 1 22.10 1.34 1 1 -1 22.44 1.32 -1 -1 0 170.72 3.36 -1 -1 -1 587.33 8.34 -1 -1 -2 32.00 1.57 1 1 2 31.44 1.52 1 1 3 385.66 7.30 -1 -1 -3 407.50 7.23 1 1 4 3.90 1.00 -1 -1 -4 4.06 0.82 1 1 5 1071.53 15.69 -1 -1 -5 758.85 12.94 -1 -1 -6 290.06 7.30 1 1 6 293.03 8.12 -1 -1 -7 196.11 5.97 1 1 7 186.48 6.85 1 1 8 351.04 10.19 1 1 9 68.31 4.62 1 1 10 14.63 2.40 1 1 11 99.53 6.23 1 1 12 227.37 10.02 1 1 13 74.27 5.91 1 1 14 8.13 2.29 1 1 15 21.97 3.60 1 1 16 10.35 2.79 1 1 17 3.85 2.36 1 1 18 3.67 1.90 1 1 19 19.19 3.91 1 1 20 30.86 5.15 1 1 21 -1.82 2.39 -1 -2 18 55.78 6.22 -1 -2 17 2.00 1.85 1 2 -17 4.96 2.01 -1 -2 16 23.17 3.85 1 2 -16 17.08 2.75 -1 -2 15 39.62 4.76 1 2 -15 43.97 4.27 1 2 -14 23.67 3.11 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22.71 3.19 10 1 8 221.51 9.87 -10 -1 -8 234.78 11.50 10 1 9 78.09 6.80 -10 -1 -9 85.63 7.01 -10 -1 -10 16.10 3.55 10 1 10 15.13 3.17 10 1 11 105.75 8.46 -10 -1 -11 114.72 8.49 10 1 12 10.10 2.87 10 1 13 1.46 1.75 10 1 14 1.27 1.62 10 1 15 22.22 4.54 10 1 16 104.05 9.45 10 1 17 43.05 6.43 10 1 18 38.58 6.57 10 2 -11 15.14 3.70 10 2 -10 22.34 4.32 10 2 -9 37.36 5.02 10 2 -8 7.86 2.81 10 2 -7 5.52 2.24 10 2 -6 39.16 4.88 10 2 -5 22.71 3.73 10 2 -4 22.03 3.57 10 2 -3 9.46 2.48 10 2 -2 29.89 4.16 10 2 -1 366.08 13.54 -10 -2 0 358.64 13.31 10 2 0 409.65 14.05 -10 -2 -1 100.40 7.09 10 2 1 127.03 7.52 10 2 2 7.92 1.95 -10 -2 -2 7.63 2.08 10 2 3 4.65 1.79 -10 -2 -3 6.02 2.07 10 2 4 18.92 2.98 -10 -2 -4 17.19 3.33 -10 -2 -5 48.69 5.19 -10 -2 -6 7.84 2.38 10 2 6 5.24 1.30 -10 -2 -7 24.40 4.07 10 2 7 26.57 3.54 10 2 7 31.10 3.60 -10 -2 -8 11.79 3.02 10 2 8 10.58 2.55 10 2 8 10.81 2.23 10 2 9 116.54 7.91 -10 -2 -9 116.10 8.37 10 2 10 62.91 6.04 -10 -2 -10 64.35 6.23 -10 -2 -11 6.53 2.37 10 2 11 1.65 1.29 -10 -2 -12 3.74 2.07 10 2 12 5.25 2.15 -10 -2 -13 29.39 4.53 10 2 13 22.25 4.17 -10 -2 -14 61.78 6.66 10 2 14 61.63 6.79 10 2 15 173.83 11.64 10 2 16 126.30 10.14 10 2 17 12.10 3.65 10 2 18 42.63 6.49 10 3 -11 3.88 2.14 10 3 -10 4.98 2.44 10 3 -9 13.69 3.32 10 3 -8 21.61 3.76 10 3 -7 8.57 2.65 10 3 -6 52.93 5.71 10 3 -5 47.31 5.25 10 3 -4 60.47 5.86 10 3 -3 3.64 1.92 10 3 -2 184.90 9.75 10 3 -1 8.47 2.71 -10 -3 1 3.61 1.47 10 3 0 3.30 1.86 -10 -3 0 1.95 1.62 -10 -3 -1 59.59 5.47 10 3 1 54.82 5.02 10 3 2 11.17 2.28 -10 -3 -2 7.28 2.40 10 3 3 3.81 1.29 -10 -3 -3 10.07 2.89 -10 -3 -4 15.66 3.40 -10 -3 -5 22.23 3.64 -10 -3 -6 -1.23 1.34 10 3 7 75.87 5.61 10 3 7 66.65 5.09 -10 -3 -7 85.47 7.11 10 3 8 36.69 4.07 10 3 8 32.64 3.49 -10 -3 -8 36.51 4.82 10 3 9 5.01 1.50 -10 -3 -9 2.61 1.91 -10 -3 -10 107.23 8.46 10 3 10 93.54 6.86 10 3 11 18.25 3.40 -10 -3 -11 22.00 4.10 -10 -3 -12 41.60 5.73 10 3 12 46.67 5.32 -10 -3 -13 39.58 5.53 10 3 13 46.13 5.45 -10 -3 -14 79.12 7.51 10 3 14 75.72 7.18 10 3 15 34.72 5.18 -10 -3 -15 29.58 5.00 10 3 16 23.97 4.47 -10 -3 -16 16.22 3.84 10 3 17 2.51 2.10 10 3 18 31.91 5.47 10 3 19 2.84 2.59 10 4 -11 1.91 1.93 10 4 -10 26.06 4.60 10 4 -9 7.61 2.82 10 4 -8 3.85 2.34 10 4 -7 5.03 2.13 10 4 -6 26.04 4.02 10 4 -5 52.65 5.62 10 4 -4 36.55 4.69 10 4 -3 8.38 2.57 10 4 -2 5.14 1.87 -10 -4 1 128.52 7.75 10 4 -1 133.17 8.29 -10 -4 0 0.35 1.24 10 4 0 1.99 1.75 -10 -4 -1 3.04 1.72 10 4 1 5.13 1.53 10 4 2 4.08 1.36 -10 -4 -2 4.57 2.17 -10 -4 -3 39.14 4.73 -10 -4 -4 72.71 6.44 -10 -4 -5 -0.78 1.45 -10 -4 -6 65.59 6.53 -10 -4 -7 25.75 4.26 -10 -4 -8 15.75 3.53 -10 -4 -9 56.53 6.12 10 4 9 59.05 5.13 -10 -4 -10 47.13 5.53 10 4 10 41.92 4.42 -10 -4 -11 151.80 10.00 10 4 11 140.26 8.47 -10 -4 -12 58.53 6.15 10 4 12 64.30 5.87 10 4 13 4.84 1.83 -10 -4 -13 5.50 2.57 -10 -4 -14 91.60 8.29 10 4 14 95.46 7.73 10 4 15 37.57 5.18 -10 -4 -15 41.30 5.45 -10 -4 -16 41.17 5.96 10 4 16 46.55 5.89 10 4 17 28.82 4.77 -10 -4 -17 20.28 4.15 10 4 18 25.37 4.65 -10 -4 -18 26.95 4.66 10 4 19 2.21 2.17 10 5 -10 25.24 4.40 10 5 -9 70.21 6.96 10 5 -8 3.59 1.84 10 5 -7 16.16 3.42 10 5 -6 41.86 5.13 10 5 -5 27.02 4.12 10 5 -4 72.78 6.48 10 5 -3 53.06 5.51 10 5 -2 12.70 2.91 -10 -5 2 21.50 3.49 -10 -5 1 63.79 5.87 10 5 -1 69.32 6.12 10 5 0 6.34 2.23 -10 -5 0 6.67 2.07 10 5 1 5.70 1.85 -10 -5 -1 5.89 1.98 -10 -5 -2 39.19 4.49 -10 -5 -3 2.53 1.67 -10 -5 -4 3.67 1.89 -10 -5 -5 62.79 6.19 -10 -5 -6 6.34 2.53 -10 -5 -7 11.68 3.08 -10 -5 -8 4.43 2.39 -10 -5 -9 16.68 3.57 10 5 10 20.14 2.80 -10 -5 -10 22.86 4.26 -10 -5 -11 109.94 8.55 10 5 11 111.15 7.13 -10 -5 -12 202.53 11.79 10 5 12 186.76 9.72 10 5 13 24.86 3.71 -10 -5 -13 31.87 5.03 -10 -5 -14 49.86 6.01 10 5 14 43.01 5.01 10 5 15 30.90 4.47 -10 -5 -15 36.44 5.23 10 5 16 4.91 2.36 -10 -5 -16 2.95 2.29 -10 -5 -17 87.98 8.41 10 5 17 93.84 8.31 10 5 18 0.85 1.84 -10 -5 -18 -0.42 1.76 10 5 19 4.40 2.44 -10 -5 -19 0.38 1.84 10 5 20 26.22 5.25 10 6 -10 22.32 4.09 10 6 -9 7.09 2.54 10 6 -8 0.06 1.81 10 6 -7 30.12 4.48 10 6 -6 -0.92 1.47 10 6 -5 4.15 2.01 10 6 -4 133.49 9.03 -10 -6 3 40.17 4.73 10 6 -3 49.85 5.44 -10 -6 2 60.29 5.83 10 6 -2 71.08 6.47 -10 -6 1 63.06 5.86 10 6 -1 60.11 5.92 -10 -6 0 63.38 5.91 10 6 0 61.90 5.89 -10 -6 -1 87.18 6.85 -10 -6 -2 -1.96 1.68 -10 -6 -3 68.35 6.15 -10 -6 -4 1.81 2.05 -10 -6 -5 43.47 4.90 -10 -6 -6 10.54 2.80 -10 -6 -7 0.28 1.59 -10 -6 -8 81.52 7.32 -10 -6 -9 38.96 5.23 -10 -6 -10 11.71 3.22 -10 -6 -11 303.17 14.79 10 6 11 296.58 11.57 -10 -6 -12 242.23 13.34 10 6 12 245.19 10.93 -10 -6 -13 223.99 12.86 10 6 13 239.91 11.31 -10 -6 -14 363.56 16.46 10 6 14 362.28 14.66 -10 -6 -15 47.29 6.26 10 6 15 50.47 5.61 10 6 16 14.00 3.53 -10 -6 -16 10.98 3.40 10 6 17 1.50 1.69 -10 -6 -17 2.68 2.22 10 6 18 6.18 2.78 -10 -6 -18 3.43 1.68 10 6 19 1.69 2.17 -10 -6 -19 3.77 2.32 10 6 20 22.45 4.68 -10 -6 -20 21.44 4.47 10 7 -10 15.47 3.40 10 7 -9 -2.16 2.06 10 7 -8 -2.43 2.14 10 7 -7 3.68 2.15 10 7 -6 73.05 6.89 10 7 -5 -0.78 1.89 10 7 -4 46.02 5.45 -10 -7 4 44.34 5.29 10 7 -3 311.81 14.00 -10 -7 3 338.38 14.37 10 7 -2 34.16 4.68 -10 -7 2 37.73 4.77 -10 -7 1 124.36 8.54 10 7 -1 127.31 8.66 -10 -7 0 146.62 9.25 -10 -7 -1 109.46 8.02 -10 -7 -2 4.78 2.22 -10 -7 -3 19.11 3.88 -10 -7 -4 6.81 2.24 -10 -7 -5 161.41 9.85 -10 -7 -6 10.22 3.10 -10 -7 -7 40.96 5.04 -10 -7 -8 4.12 2.40 -10 -7 -9 43.84 5.47 -10 -7 -10 171.82 10.89 -10 -7 -11 36.19 5.14 -10 -7 -12 266.02 14.22 10 7 13 14.92 3.13 -10 -7 -13 14.65 3.67 10 7 14 22.28 3.67 -10 -7 -14 24.66 4.50 10 7 15 0.25 1.59 -10 -7 -15 -0.96 1.66 -10 -7 -16 1.08 2.35 10 7 16 0.90 1.68 -10 -7 -17 -2.27 2.22 10 7 17 0.76 1.91 -10 -7 -18 5.46 2.96 10 7 18 2.88 1.92 -10 -7 -19 1.69 2.18 10 7 19 0.79 1.72 -10 -7 -20 2.07 2.14 10 7 20 5.20 2.05 10 8 -9 63.90 6.92 10 8 -8 8.89 2.86 10 8 -7 0.37 1.49 10 8 -6 4.71 1.87 10 8 -5 31.85 4.55 -10 -8 4 52.47 6.14 10 8 -4 68.78 6.69 10 8 -3 93.87 7.79 -10 -8 3 114.61 8.59 10 8 -2 66.76 6.49 -10 -8 2 58.63 6.34 10 8 -1 45.79 5.32 -10 -8 1 54.97 5.88 -10 -8 0 4.84 2.96 -10 -8 -1 5.53 2.45 -10 -8 -2 28.47 4.42 -10 -8 -3 44.20 5.38 -10 -8 -4 1.20 1.84 -10 -8 -5 7.49 2.71 -10 -8 -6 8.06 2.68 -10 -8 -7 12.34 3.00 -10 -8 -8 4.44 1.66 -10 -8 -9 13.42 3.40 -10 -8 -10 122.27 9.45 -10 -8 -11 0.20 1.75 -10 -8 -12 9.77 3.14 -10 -8 -13 53.14 6.67 -10 -8 -14 8.35 2.81 10 8 14 13.02 2.86 -10 -8 -15 0.29 1.78 10 8 15 -1.56 1.59 -10 -8 -16 7.43 2.92 10 8 16 10.40 2.76 -10 -8 -17 8.09 3.39 10 8 17 12.23 3.08 -10 -8 -18 3.60 2.89 10 8 18 10.51 3.34 -10 -8 -19 0.76 2.09 10 8 19 -0.67 1.71 -10 -8 -20 7.96 3.07 10 8 20 7.99 3.09 10 9 -9 6.00 2.57 10 9 -8 -1.56 2.24 10 9 -7 103.31 8.57 10 9 -6 7.45 2.46 10 9 -5 6.12 2.37 -10 -9 5 7.71 2.78 10 9 -4 28.17 4.55 -10 -9 4 25.33 4.47 10 9 -3 20.05 3.74 -10 -9 3 20.26 4.26 10 9 -2 5.52 2.01 -10 -9 2 5.63 2.92 -10 -9 1 31.72 5.07 -10 -9 0 135.69 9.76 -10 -9 -1 73.07 7.07 -10 -9 -2 43.02 5.52 -10 -9 -3 20.09 3.94 -10 -9 -4 203.08 11.72 -10 -9 -5 20.95 4.08 -10 -9 -6 4.04 2.16 -10 -9 -7 32.16 4.87 -10 -9 -8 -0.57 1.65 -10 -9 -9 28.69 4.94 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-0.09 1.79 11 -3 -1 -0.30 1.64 11 -3 0 2.71 1.84 11 -3 1 4.45 2.76 11 -3 2 0.93 1.85 11 -3 3 40.39 5.45 11 -3 4 0.82 1.92 11 -3 5 29.54 4.68 11 -3 6 12.77 3.50 11 -3 7 76.87 7.29 11 -3 8 18.86 3.74 11 -3 9 40.33 5.31 11 -2 -8 25.70 4.25 11 -2 -7 19.77 3.75 11 -2 -6 39.38 4.85 11 -2 -4 20.75 4.33 11 -2 -3 9.31 3.12 11 -2 -2 3.00 2.65 11 -2 -1 27.46 4.72 11 -2 0 9.90 3.16 11 -2 1 22.18 4.17 11 -2 2 151.39 10.11 11 -2 3 24.67 4.07 11 -2 4 10.02 2.75 11 -2 5 35.25 4.67 11 -2 6 19.92 3.92 11 -2 7 18.74 3.41 11 -2 8 9.33 3.00 11 -2 9 111.71 8.35 11 -2 12 1.36 1.88 11 -2 13 -0.94 2.42 11 -2 14 20.31 4.90 11 -1 -9 18.54 3.77 11 -1 -8 51.97 5.96 11 -1 -7 1.27 1.23 11 -1 -6 33.64 4.56 11 -1 -5 17.94 3.45 11 -1 -4 1.55 1.43 11 -1 -3 0.73 1.80 11 -1 0 7.30 2.54 11 -1 1 1.23 1.76 11 -1 2 25.22 4.44 11 -1 3 14.13 3.19 11 -1 4 8.66 2.94 11 -1 5 71.32 6.52 11 -1 6 58.91 6.02 11 -1 7 9.22 2.95 11 -1 8 51.61 5.53 11 -1 9 14.95 2.98 11 -1 11 3.57 2.32 11 -1 12 -0.09 1.98 11 -1 13 30.59 5.40 11 -1 14 12.10 3.52 11 -1 15 7.79 3.48 11 0 -9 34.95 5.03 11 0 -8 -0.67 1.86 11 0 -7 31.03 4.50 11 0 -6 12.06 2.97 11 0 -5 8.56 2.24 11 0 -4 30.66 4.08 11 0 -3 50.36 5.15 11 0 -2 151.00 8.70 11 0 -1 22.51 3.54 11 0 0 6.59 2.13 11 0 2 7.45 2.70 -11 0 -3 5.83 1.83 11 0 3 2.32 1.84 11 0 4 102.24 7.64 -11 0 -4 95.00 7.32 -11 0 -5 15.81 2.86 11 0 5 18.11 3.20 -11 0 -6 -0.38 1.51 11 0 6 2.45 2.04 11 0 7 163.25 9.38 11 0 8 2.57 1.67 11 0 10 10.22 2.83 11 0 11 17.27 3.99 11 0 12 -1.93 2.45 11 0 13 11.32 3.52 11 0 14 0.54 2.03 11 0 15 0.60 2.39 11 0 16 21.31 4.71 11 1 -9 9.68 2.64 11 1 -8 31.48 4.82 11 1 -7 3.16 1.89 11 1 -6 19.45 3.75 11 1 -5 -1.04 1.65 11 1 -4 8.56 2.41 11 1 -3 -0.28 1.63 11 1 -2 0.68 1.43 11 1 -1 32.17 4.14 11 1 0 141.68 8.34 11 1 1 81.74 6.16 11 1 2 13.18 2.64 11 1 3 9.28 2.22 -11 -1 -3 10.61 2.49 -11 -1 -4 7.98 2.56 11 1 4 -3.05 2.26 11 1 5 47.65 5.09 -11 -1 -5 51.37 5.49 11 1 6 175.38 9.62 -11 -1 -6 192.10 10.51 11 1 7 258.09 11.64 -11 -1 -7 271.82 12.67 11 1 8 101.31 7.06 -11 -1 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2.33 11 2 17 2.73 2.68 11 2 18 3.47 2.33 11 3 -9 3.13 2.60 11 3 -8 38.31 5.35 11 3 -7 -3.77 2.45 11 3 -6 5.72 2.51 11 3 -5 43.97 5.33 11 3 -4 7.75 2.28 11 3 -3 13.03 3.09 11 3 -2 109.49 7.85 11 3 -1 88.82 7.01 11 3 0 3.14 1.87 11 3 1 6.25 2.11 -11 -3 -1 6.35 1.98 11 3 2 35.37 4.24 -11 -3 -2 28.10 4.37 11 3 3 -0.33 1.51 -11 -3 -3 2.55 2.31 11 3 4 11.78 2.50 -11 -3 -4 13.91 3.31 -11 -3 -5 126.60 8.96 -11 -3 -6 12.11 3.20 -11 -3 -7 -2.47 2.27 11 3 7 1.56 1.17 -11 -3 -8 49.92 5.82 -11 -3 -9 11.30 3.21 11 3 10 1.27 1.40 -11 -3 -10 1.08 2.07 11 3 11 4.98 2.15 -11 -3 -11 6.25 2.45 11 3 12 4.79 2.06 -11 -3 -12 8.75 2.81 11 3 13 8.98 2.74 -11 -3 -13 4.66 2.45 -11 -3 -14 55.19 6.39 11 3 14 60.62 6.68 -11 -3 -15 12.70 3.44 11 3 15 19.63 4.29 -11 -3 -16 0.53 1.62 11 3 16 7.83 3.13 11 3 17 7.60 3.26 11 3 18 2.37 2.18 11 4 -9 54.44 6.29 11 4 -8 10.15 2.74 11 4 -7 2.21 1.89 11 4 -6 49.00 5.77 11 4 -5 -0.19 1.86 11 4 -4 10.62 2.96 11 4 -3 1.67 1.75 11 4 -2 44.78 5.14 11 4 -1 85.04 6.90 11 4 0 41.49 4.88 -11 -4 0 35.05 4.35 -11 -4 -1 123.30 8.45 11 4 1 137.90 8.61 -11 -4 -2 48.34 5.32 11 4 2 55.10 5.43 11 4 3 4.28 1.70 -11 -4 -3 6.92 2.74 -11 -4 -4 2.99 1.85 -11 -4 -5 10.73 3.23 -11 -4 -6 0.68 1.64 -11 -4 -7 21.62 4.06 -11 -4 -8 -1.14 1.61 -11 -4 -9 3.89 2.55 -11 -4 -10 19.62 3.94 -11 -4 -11 39.48 5.58 -11 -4 -12 64.67 6.95 11 4 12 72.49 6.39 -11 -4 -13 37.84 5.34 11 4 13 44.01 5.27 -11 -4 -14 168.16 11.25 11 4 14 158.92 10.15 -11 -4 -15 160.18 11.12 11 4 15 177.87 11.16 11 4 16 3.04 2.17 -11 -4 -16 5.21 3.01 11 4 17 3.03 2.32 -11 -4 -17 0.37 2.09 11 4 18 0.75 1.73 -11 -4 -18 1.99 2.37 11 4 19 9.78 3.45 11 5 -9 3.11 1.92 11 5 -8 20.96 4.18 11 5 -7 20.98 4.08 11 5 -6 3.29 1.62 11 5 -5 2.37 2.14 11 5 -4 33.88 4.89 11 5 -3 4.23 2.47 11 5 -2 28.41 4.25 -11 -5 1 269.33 12.15 11 5 -1 273.36 12.74 -11 -5 0 10.27 2.41 11 5 0 13.17 3.17 -11 -5 -1 1.26 1.36 11 5 1 -1.55 1.99 -11 -5 -2 18.76 3.54 11 5 2 24.10 3.77 -11 -5 -3 -0.75 1.91 -11 -5 -4 -2.35 1.99 -11 -5 -5 40.27 5.30 -11 -5 -6 28.79 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-10 -7 25.56 4.95 -12 -10 -8 6.25 2.70 -12 -10 -9 7.64 2.99 -12 -10 -10 19.55 4.49 -12 -10 -11 1.18 2.00 -12 -10 -12 9.05 3.53 -12 -10 -13 13.84 5.29 -12 -10 -14 -0.77 2.42 -12 -10 -15 -1.12 2.19 -12 -10 -16 6.45 3.73 12 11 -3 17.46 4.13 -12 -11 3 15.21 4.18 -12 -11 2 0.70 1.95 12 11 -2 2.68 2.33 -12 -11 1 23.98 5.08 12 11 -1 15.72 3.76 12 11 0 4.57 2.38 -12 -11 0 3.06 2.14 -12 -11 -1 2.72 3.31 -12 -11 -2 19.80 4.37 -12 -11 -3 2.12 2.10 -12 -11 -4 5.74 3.00 -12 -11 -5 0.35 2.26 -12 -11 -6 8.01 3.19 -12 -11 -7 61.84 7.42 -12 -11 -8 7.19 2.82 -12 -11 -9 13.19 3.70 -12 -11 -10 5.75 3.17 -12 -11 -11 42.92 7.12 -12 -11 -12 2.32 2.62 -12 -11 -13 12.02 4.04 -12 -11 -14 1.07 2.12 -12 -11 -15 7.54 3.22 -12 -12 3 6.87 3.29 -12 -12 2 -1.97 2.45 12 12 -1 27.03 4.79 -12 -12 1 25.88 5.33 -12 -12 0 23.88 5.02 -12 -12 -1 4.46 2.79 -12 -12 -2 1.44 2.11 -12 -12 -3 -0.93 2.20 -12 -12 -4 12.07 3.54 -12 -12 -5 16.16 4.33 -12 -12 -6 51.07 7.05 -12 -12 -7 10.52 3.96 -12 -12 -8 5.80 3.15 -12 -12 -9 32.54 5.75 -12 -12 -10 36.13 6.36 -12 -12 -11 -0.84 1.88 -12 -12 -12 4.02 3.09 -12 -12 -13 -0.35 2.64 -12 -13 1 52.90 7.60 -12 -13 0 0.13 2.60 -12 -13 -1 16.85 4.71 -12 -13 -2 8.59 3.60 -12 -13 -3 1.96 1.93 -12 -13 -4 8.32 3.22 -12 -13 -5 14.68 4.01 -12 -13 -6 3.25 2.15 -12 -13 -7 95.90 9.82 -12 -13 -8 5.85 3.26 -12 -13 -9 31.33 5.86 -12 -13 -10 57.08 7.92 -12 -13 -11 69.49 8.68 13 -2 3 13.12 3.88 13 -2 4 83.37 8.15 13 -2 5 61.91 7.14 13 -2 6 30.67 5.01 13 -2 7 9.78 3.34 13 -2 8 1.24 2.53 13 -1 0 23.23 4.61 13 -1 1 22.52 4.60 13 -1 2 148.40 10.92 13 -1 3 4.46 2.61 13 -1 4 15.40 4.04 13 -1 5 5.73 2.55 13 -1 6 10.67 2.94 13 -1 7 6.29 2.90 13 0 0 2.44 2.10 13 0 1 24.17 4.48 13 0 2 74.52 7.70 13 0 3 137.54 10.20 13 0 4 9.07 2.96 13 0 5 24.35 4.44 13 0 6 6.98 2.47 13 0 7 9.16 3.03 13 1 -5 30.16 4.69 13 1 -4 -1.71 1.78 13 1 -3 6.67 2.47 13 1 2 0.01 2.48 13 1 3 22.54 4.18 13 1 4 -2.32 2.36 13 1 5 15.59 3.62 -13 -1 -6 3.24 2.18 13 1 6 2.33 1.94 -13 -1 -7 5.74 2.53 13 1 7 2.52 1.56 -13 -1 -8 19.71 4.31 13 2 -5 -2.99 2.09 13 2 -4 4.94 2.64 13 2 -3 24.95 4.27 13 2 -2 -3.71 2.14 13 2 -1 17.66 3.42 13 2 0 2.51 1.63 13 2 4 13.62 3.18 -13 -2 -5 2.38 1.77 13 2 5 2.83 1.81 -13 -2 -6 -1.47 1.56 13 2 6 1.24 1.71 -13 -2 -7 3.34 2.14 -13 -2 -8 5.80 2.55 -13 -2 -9 17.96 3.83 -13 -2 -10 3.57 2.25 -13 -2 -11 4.61 2.41 -13 -2 -12 35.93 5.67 13 3 -5 35.12 4.99 13 3 -4 4.57 2.46 13 3 -3 -2.94 2.38 13 3 -2 13.91 3.29 13 3 -1 0.69 1.91 13 3 0 21.46 3.64 13 3 1 20.01 3.71 13 3 2 143.98 9.21 13 3 3 10.02 2.99 -13 -3 -4 24.19 4.33 -13 -3 -5 4.55 2.46 -13 -3 -6 4.74 2.55 13 3 6 5.17 1.88 -13 -3 -7 15.69 3.86 -13 -3 -8 8.00 3.09 -13 -3 -9 66.46 7.12 -13 -3 -10 5.47 2.95 -13 -3 -11 7.87 2.76 -13 -3 -12 3.87 2.42 -13 -3 -13 15.98 3.91 -13 -3 -14 71.76 7.91 13 4 -5 1.04 1.63 13 4 -4 51.24 6.19 13 4 -3 3.01 2.13 13 4 -2 7.22 2.63 13 4 -1 41.38 5.36 13 4 0 3.17 2.09 13 4 1 3.91 2.02 13 4 2 0.27 1.60 13 4 3 23.42 3.92 13 4 4 22.40 3.75 -13 -4 -4 19.46 3.86 13 4 5 1.12 1.80 -13 -4 -5 1.87 2.54 13 4 6 3.99 1.60 -13 -4 -6 9.62 3.17 -13 -4 -7 10.56 3.12 -13 -4 -8 40.96 5.72 -13 -4 -9 3.62 2.05 -13 -4 -10 26.59 4.92 -13 -4 -11 29.55 5.21 -13 -4 -12 2.22 2.05 -13 -4 -13 2.79 2.14 -13 -4 -14 19.75 4.23 13 5 -5 9.57 3.29 13 5 -4 182.52 11.72 13 5 -3 12.71 3.40 13 5 -2 9.48 2.89 13 5 -1 17.57 3.74 13 5 0 3.65 2.21 13 5 1 4.95 2.42 13 5 2 4.74 2.10 13 5 3 -2.17 1.89 -13 -5 -3 -1.74 2.23 13 5 4 27.14 4.16 -13 -5 -4 31.35 5.41 -13 -5 -5 58.28 7.30 13 5 5 67.11 6.42 -13 -5 -6 29.07 5.17 -13 -5 -7 25.10 4.93 -13 -5 -8 35.19 5.36 -13 -5 -9 25.09 4.74 -13 -5 -10 21.44 4.87 -13 -5 -11 5.36 2.66 -13 -5 -12 8.77 3.55 -13 -5 -13 31.35 5.57 -13 -5 -14 0.43 2.03 13 6 -4 113.02 9.34 13 6 -3 147.25 10.61 13 6 -2 5.23 2.64 13 6 -1 51.78 6.23 13 6 0 12.52 3.32 13 6 1 2.52 1.76 13 6 2 0.82 1.72 -13 -6 -2 -3.80 2.76 13 6 3 38.65 5.20 -13 -6 -3 24.36 4.71 13 6 4 19.10 3.95 -13 -6 -4 15.82 3.86 -13 -6 -5 6.32 2.83 -13 -6 -6 26.62 4.90 -13 -6 -7 0.58 2.17 -13 -6 -8 8.52 3.05 -13 -6 -9 5.64 2.80 -13 -6 -10 -1.55 2.47 -13 -6 -11 12.05 3.70 -13 -6 -12 67.91 8.31 -13 -6 -13 5.24 3.38 -13 -6 -14 1.96 2.50 -13 -6 -15 94.50 9.48 13 7 -4 41.95 5.73 13 7 -3 36.97 5.56 13 7 -2 57.26 6.71 13 7 -1 8.54 2.89 13 7 0 -0.40 1.89 -13 -7 -1 68.91 7.24 13 7 1 72.36 7.30 -13 -7 -2 15.96 3.71 13 7 2 14.09 3.32 -13 -7 -3 61.99 6.86 13 7 3 61.06 6.53 -13 -7 -4 34.64 5.59 -13 -7 -5 10.46 3.45 -13 -7 -6 3.52 2.24 -13 -7 -7 21.97 4.32 -13 -7 -8 -0.95 1.85 -13 -7 -9 4.24 2.22 -13 -7 -10 7.96 3.30 -13 -7 -11 5.51 3.04 -13 -7 -12 -2.82 2.51 -13 -7 -13 -0.56 2.22 -13 -7 -14 1.48 2.32 -13 -7 -15 7.92 3.91 13 8 -3 29.25 4.93 13 8 -2 21.58 4.19 13 8 -1 9.38 3.43 13 8 0 0.02 1.93 13 8 1 9.65 3.07 -13 -8 -1 4.86 2.28 13 8 2 32.22 5.05 -13 -8 -2 25.67 4.68 -13 -8 -3 6.28 2.81 -13 -8 -4 5.64 2.61 -13 -8 -5 6.07 2.83 -13 -8 -6 -2.58 2.32 -13 -8 -7 11.63 3.71 -13 -8 -8 11.89 3.71 -13 -8 -9 8.40 3.27 -13 -8 -10 -3.34 2.71 -13 -8 -11 3.35 2.45 -13 -8 -12 5.37 3.72 -13 -8 -13 0.69 2.01 -13 -8 -14 1.13 2.29 13 9 -2 5.62 2.96 13 9 -1 8.72 3.18 13 9 0 1.26 1.94 -13 -9 0 10.91 3.37 13 9 1 15.56 4.04 -13 -9 -1 5.41 2.64 -13 -9 -2 2.22 1.95 -13 -9 -3 0.36 1.75 -13 -9 -4 6.25 2.84 -13 -9 -5 30.65 4.90 -13 -9 -6 2.03 1.82 -13 -9 -7 2.06 1.81 -13 -9 -8 -2.73 2.36 -13 -9 -9 5.28 2.99 -13 -9 -10 12.27 3.62 -13 -9 -11 -0.83 1.98 -13 -9 -12 1.19 2.61 -13 -9 -13 7.20 4.07 -13 -9 -14 -0.76 2.74 13 10 -1 15.34 3.89 -13 -10 1 4.36 2.80 13 10 0 2.96 2.39 -13 -10 0 0.99 1.99 13 10 1 32.80 5.31 -13 -10 -1 40.48 6.01 -13 -10 -2 26.40 5.20 -13 -10 -3 20.52 4.71 -13 -10 -4 17.88 4.27 -13 -10 -5 11.88 3.82 -13 -10 -6 18.44 4.22 -13 -10 -7 11.16 3.62 -13 -10 -8 3.55 2.06 -13 -10 -9 4.48 2.62 -13 -10 -10 -0.59 1.94 -13 -10 -11 15.41 4.49 -13 -10 -12 -1.49 2.38 -13 -10 -13 0.70 2.06 -13 -11 1 -0.62 2.07 13 11 0 -0.12 2.00 -13 -11 0 -0.80 2.21 13 11 1 6.13 2.83 -13 -11 -1 7.17 3.17 -13 -11 -2 4.22 2.46 -13 -11 -3 -0.53 2.25 -13 -11 -4 41.86 6.31 -13 -11 -5 3.96 2.50 -13 -11 -6 22.33 4.87 -13 -11 -7 55.10 7.17 -13 -11 -8 2.53 2.51 -13 -11 -9 28.51 5.55 -13 -11 -10 27.50 5.75 -13 -11 -11 15.98 4.56 -13 -11 -12 6.65 3.54 -13 -12 2 3.49 2.49 -13 -12 1 -1.99 2.65 -13 -12 0 12.55 4.25 -13 -12 -1 -1.29 2.26 -13 -12 -2 23.81 5.22 -13 -12 -3 8.22 3.38 -13 -12 -4 1.10 2.92 -13 -12 -5 -2.32 2.83 -13 -12 -6 6.90 2.83 -13 -12 -7 14.11 4.02 -13 -12 -8 23.35 5.28 -13 -12 -9 111.94 10.64 -13 -12 -10 2.05 2.35 14 0 3 40.27 5.84 14 0 4 65.87 7.33 14 0 5 19.64 4.41 14 0 6 0.35 1.89 14 1 1 -1.72 2.90 14 1 2 19.94 4.24 14 1 3 29.27 5.07 14 1 4 44.64 6.07 14 1 5 -1.18 1.79 14 1 6 2.46 1.99 14 2 -3 5.67 2.32 14 2 3 4.67 1.90 14 2 4 7.90 2.55 14 2 5 35.29 5.19 14 2 6 4.47 1.91 -14 -2 -7 3.67 2.36 -14 -2 -8 17.94 4.25 -14 -2 -9 2.62 2.10 -14 -2 -10 3.99 2.79 14 3 -3 4.12 2.22 14 3 -2 4.11 2.28 14 3 -1 1.19 1.99 14 3 0 10.13 3.03 14 3 1 -0.73 1.60 14 3 5 1.43 1.76 -14 -3 -6 19.65 4.34 -14 -3 -7 17.55 4.44 -14 -3 -8 11.23 3.50 -14 -3 -9 3.77 2.88 -14 -3 -10 -1.31 1.95 -14 -3 -11 6.02 2.90 14 4 -2 1.87 1.75 14 4 -1 12.72 3.46 14 4 0 1.17 1.47 14 4 1 -0.45 1.80 14 4 2 8.42 2.75 14 4 3 86.01 7.45 -14 -4 -5 54.85 6.58 -14 -4 -6 1.06 1.79 -14 -4 -7 7.74 3.25 -14 -4 -8 51.12 6.83 -14 -4 -9 42.53 6.27 -14 -4 -10 -1.13 2.27 -14 -4 -11 13.59 3.73 -14 -4 -12 4.17 2.44 14 5 -2 4.89 2.30 14 5 -1 5.42 2.77 14 5 0 8.97 2.86 14 5 1 -3.06 2.35 14 5 2 19.03 4.05 14 5 3 58.80 6.50 14 5 4 19.34 3.86 -14 -5 -5 67.49 7.49 14 5 5 60.33 6.62 14 5 6 20.91 4.05 -14 -5 -6 25.84 4.84 -14 -5 -7 79.88 8.25 -14 -5 -8 32.03 5.20 -14 -5 -9 12.38 4.03 -14 -5 -10 12.25 3.86 -14 -5 -11 5.06 2.75 -14 -5 -12 86.70 9.06 14 6 -2 46.99 6.24 14 6 -1 21.87 4.16 14 6 0 2.78 2.39 14 6 1 -3.56 2.44 14 6 2 35.22 5.14 14 6 3 4.92 2.29 14 6 4 11.32 3.40 -14 -6 -4 6.42 2.98 14 6 5 9.34 2.64 -14 -6 -5 15.87 4.06 -14 -6 -6 28.10 5.07 -14 -6 -7 19.77 4.36 -14 -6 -8 94.07 9.22 -14 -6 -9 -2.06 2.38 -14 -6 -10 29.66 5.58 -14 -6 -11 7.47 3.75 -14 -6 -12 4.32 2.79 14 7 -1 10.56 3.24 14 7 0 11.73 3.33 14 7 1 3.48 2.17 14 7 2 44.63 5.99 14 7 3 18.56 3.95 -14 -7 -3 17.85 3.96 14 7 4 4.52 2.18 -14 -7 -4 13.41 3.89 -14 -7 -5 11.95 3.64 -14 -7 -6 4.62 2.54 -14 -7 -7 10.36 3.66 -14 -7 -8 3.52 2.70 -14 -7 -9 1.55 2.29 -14 -7 -10 3.48 2.86 -14 -7 -11 -0.11 2.44 -14 -7 -12 2.95 2.53 14 8 0 63.84 7.23 14 8 1 20.69 4.29 -14 -8 -2 4.40 2.60 14 8 2 0.47 1.83 -14 -8 -3 20.18 4.29 14 8 3 2.30 1.94 -14 -8 -4 6.37 3.11 -14 -8 -5 4.82 2.63 -14 -8 -6 8.72 3.29 -14 -8 -7 69.15 8.17 -14 -8 -8 -1.39 2.25 -14 -8 -9 12.63 4.36 -14 -8 -10 4.44 3.28 -14 -8 -11 6.39 3.27 -14 -8 -12 0.00 2.13 14 9 1 6.46 2.35 14 9 2 7.62 3.06 -14 -9 -2 4.35 2.51 -14 -9 -3 10.28 3.36 14 9 3 7.16 2.55 -14 -9 -4 8.67 3.28 -14 -9 -5 1.12 2.03 -14 -9 -6 19.63 4.62 -14 -9 -7 16.38 4.33 -14 -9 -8 4.12 2.91 -14 -9 -9 9.24 3.64 -14 -9 -10 1.57 2.89 -14 -9 -11 -1.86 2.46 -14 -10 -1 28.36 5.59 -14 -10 -2 -0.61 2.58 -14 -10 -3 -1.01 2.20 -14 -10 -4 2.27 2.11 -14 -10 -5 -1.36 2.19 -14 -10 -6 9.96 3.20 -14 -10 -7 7.54 3.75 -14 -10 -8 32.24 5.85 -14 -10 -9 7.09 3.29 -14 -10 -10 46.77 7.43 -14 -11 0 1.52 2.61 -14 -11 -1 10.48 3.81 -14 -11 -2 9.78 3.99 -14 -11 -3 -0.96 2.15 -14 -11 -4 -1.76 2.26 -14 -11 -5 11.81 3.75 -14 -11 -6 -3.12 2.86 -14 -11 -7 17.50 4.29 -14 -11 -8 80.19 9.14 15 2 5 26.55 4.78 15 3 4 5.00 2.70 -15 -3 -8 28.52 5.29 -15 -3 -9 7.83 3.27 -15 -4 -7 2.77 1.97 -15 -4 -8 6.24 3.35 -15 -4 -9 4.15 2.75 15 5 1 3.52 2.46 15 5 2 13.39 3.44 15 5 3 29.54 4.83 -15 -5 -6 4.47 2.53 -15 -5 -7 -0.70 1.77 -15 -5 -8 6.91 3.67 -15 -5 -9 11.31 3.72 15 6 2 43.61 6.09 15 6 3 11.31 3.31 15 6 4 18.37 4.12 15 6 5 6.55 2.91 15 6 6 0.88 1.79 -15 -6 -6 0.83 2.68 -15 -6 -7 6.08 3.23 -15 -6 -8 2.22 2.29 -15 -6 -9 8.95 3.42 15 7 3 4.76 2.78 15 7 4 11.66 3.17 15 7 5 4.52 2.64 -15 -7 -5 3.96 2.23 15 7 6 3.81 2.21 -15 -7 -6 7.37 2.95 -15 -7 -7 67.43 8.27 -15 -7 -8 2.83 2.29 -15 -7 -9 3.75 2.88 15 8 4 1.85 2.12 -15 -8 -4 4.89 3.09 15 8 5 33.79 5.57 -15 -8 -5 30.72 5.67 -15 -8 -6 3.68 2.35 -15 -8 -7 4.87 2.44 -15 -8 -8 -3.55 2.65 -15 -9 -3 25.14 5.17 -15 -9 -4 36.03 6.28 -15 -9 -5 29.87 5.47 -15 -9 -6 7.46 3.16 -15 -9 -7 1.97 2.84 -15 -10 -3 5.65 3.06 -15 -10 -4 11.24 3.64 0 0 0 0.00 0.00 TITL BB_S3_1_Lt_Mo in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 11.818237 12.760805 17.145483 77.1582 73.7295 66.3731 ZERR 1.00 0.000579 0.001079 0.001060 0.0062 0.0051 0.0065 LATT 1 SFAC C H N O UNIT 42.00 42.00 42.00 42.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65348 _olex2_submission_special_instructions 'No special instructions were received'