#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 1 _journal_year 2020 _journal_page_first 68 _journal_page_last 79 #=============================================================================== data_1942-15386-8-ed _audit_creation_date 2020-02-14 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133) ; _shelxl_version_number 2013-4 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C24 H20 N6 O2), C3 H6 O' _chemical_formula_sum 'C51 H46 N12 O5' _chemical_formula_weight 907.00 _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' _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 9.9554(3) _cell_length_b 14.0875(4) _cell_length_c 17.4572(4) _cell_angle_alpha 79.676(2) _cell_angle_beta 85.283(2) _cell_angle_gamma 72.647(2) _cell_volume 2297.97(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5429 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 23.63 _cell_measurement_theta_min 2.98 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description cube _exptl_crystal_F_000 952 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_Laue_measured_fraction_full 0.944 _diffrn_reflns_Laue_measured_fraction_max 0.914 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 29732 _diffrn_reflns_point_group_measured_fraction_full 0.944 _diffrn_reflns_point_group_measured_fraction_max 0.914 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.534 _diffrn_reflns_theta_min 2.087 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.944 _diffrn_measured_fraction_theta_max 0.914 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'graphite' _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 6124 _reflns_number_total 10681 _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 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.469 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.044 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 627 _refine_ls_number_reflns 10681 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0566 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0276P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1436 _refine_ls_wR_factor_ref 0.1667 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3A), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46) 2.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C48(H48A,H48B,H48C), C49(H49A,H49B, H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C) ; _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 O1 O 0.60102(13) 0.38318(11) 0.11168(7) 0.0568(4) Uani 1 1 d . . . . . O2 O 0.10895(13) 0.53215(11) 0.14925(8) 0.0632(4) Uani 1 1 d . . . . . N1 N 0.28660(15) 0.38029(12) -0.05213(9) 0.0481(4) Uani 1 1 d . . . . . N2 N 0.63398(15) 0.36224(12) -0.13126(9) 0.0481(4) Uani 1 1 d . . . . . N3 N 0.37301(17) 0.38482(13) 0.10171(9) 0.0473(4) Uani 1 1 d . . . . . H3 H 0.311(2) 0.3875(17) 0.0701(12) 0.069(7) Uiso 1 1 d . . . . . N8 N 0.49565(15) 0.36488(11) -0.13413(8) 0.0440(4) Uani 1 1 d . . . . . N9 N 0.18866(17) 0.46491(13) 0.27432(9) 0.0564(4) Uani 1 1 d . . . . . N10 N 0.29613(16) 0.38044(13) 0.30865(9) 0.0536(4) Uani 1 1 d . . . . . C1 C 0.5065(2) 0.35260(15) -0.27458(11) 0.0509(5) Uani 1 1 d . . . . . C2 C 0.4354(2) 0.40479(18) -0.34201(12) 0.0641(6) Uani 1 1 d . . . . . H2 H 0.3439 0.4467 -0.3382 0.077 Uiso 1 1 calc R . . . . C3 C 0.4997(3) 0.3947(2) -0.41449(13) 0.0757(7) Uani 1 1 d . . . . . H3A H 0.4504 0.4284 -0.4591 0.091 Uiso 1 1 calc R . . . . C4 C 0.6358(3) 0.3355(2) -0.42101(13) 0.0814(8) Uani 1 1 d . . . . . H4 H 0.6796 0.3298 -0.4698 0.098 Uiso 1 1 calc R . . . . C5 C 0.7070(3) 0.2846(2) -0.35498(14) 0.0787(7) Uani 1 1 d . . . . . H5 H 0.7992 0.2441 -0.3594 0.094 Uiso 1 1 calc R . . . . C6 C 0.6439(2) 0.29248(18) -0.28177(13) 0.0656(6) Uani 1 1 d . . . . . H6 H 0.6935 0.2575 -0.2375 0.079 Uiso 1 1 calc R . . . . C7 C 0.42886(19) 0.36182(14) -0.19908(10) 0.0464(4) Uani 1 1 d . . . . . C8 C 0.2891(2) 0.36805(15) -0.18768(11) 0.0533(5) Uani 1 1 d . . . . . H8 H 0.2377 0.3660 -0.2292 0.064 Uiso 1 1 calc R . . . . C9 C 0.2221(2) 0.37745(15) -0.11443(11) 0.0536(5) Uani 1 1 d . . . . . H9 H 0.1268 0.3819 -0.1094 0.064 Uiso 1 1 calc R . . . . C10 C 0.42519(18) 0.37333(13) -0.06238(10) 0.0416(4) Uani 1 1 d . . . . . C11 C 0.52478(18) 0.37436(13) -0.01121(10) 0.0418(4) Uani 1 1 d . . . . . C12 C 0.64766(19) 0.36803(14) -0.05730(10) 0.0466(4) Uani 1 1 d . . . . . H12 H 0.7320 0.3679 -0.0379 0.056 Uiso 1 1 calc R . . . . C13 C 0.50525(18) 0.38163(13) 0.07200(10) 0.0433(4) Uani 1 1 d . . . . . C14 C 0.32699(19) 0.39827(15) 0.17851(10) 0.0465(4) Uani 1 1 d . . . . . C15 C 0.0752(2) 0.51516(17) 0.32062(11) 0.0534(5) Uani 1 1 d . . . . . C16 C 0.0288(2) 0.61864(18) 0.30638(13) 0.0633(6) Uani 1 1 d . . . . . H16 H 0.0688 0.6548 0.2659 0.076 Uiso 1 1 calc R . . . . C17 C -0.0789(3) 0.6683(2) 0.35334(14) 0.0738(7) Uani 1 1 d . . . . . H17 H -0.1105 0.7383 0.3440 0.089 Uiso 1 1 calc R . . . . C18 C -0.1388(2) 0.6172(2) 0.41239(14) 0.0745(7) Uani 1 1 d . . . . . H18 H -0.2097 0.6519 0.4438 0.089 Uiso 1 1 calc R . . . . C19 C -0.0942(2) 0.5138(2) 0.42576(13) 0.0716(7) Uani 1 1 d . . . . . H19 H -0.1359 0.4784 0.4661 0.086 Uiso 1 1 calc R . . . . C20 C 0.0125(2) 0.46145(19) 0.37949(12) 0.0637(6) Uani 1 1 d . . . . . H20 H 0.0415 0.3914 0.3880 0.076 Uiso 1 1 calc R . . . . C21 C 0.5116(2) 0.25873(17) 0.26204(12) 0.0664(6) Uani 1 1 d . . . . . H21A H 0.5375 0.2262 0.2169 0.100 Uiso 1 1 calc GR . . . . H21B H 0.4936 0.2114 0.3056 0.100 Uiso 1 1 calc GR . . . . H21C H 0.5869 0.2828 0.2737 0.100 Uiso 1 1 calc GR . . . . C22 C 0.3623(2) 0.4006(2) 0.37340(12) 0.0776(7) Uani 1 1 d . . . . . H22A H 0.4289 0.3396 0.3966 0.116 Uiso 1 1 calc GR . . . . H22B H 0.2914 0.4248 0.4117 0.116 Uiso 1 1 calc GR . . . . H22C H 0.4099 0.4506 0.3544 0.116 Uiso 1 1 calc GR . . . . C23 C 0.38239(19) 0.34508(15) 0.24637(11) 0.0487(5) Uani 1 1 d . . . . . C24 C 0.1979(2) 0.47429(16) 0.19407(11) 0.0501(5) Uani 1 1 d . . . . . O3 O 0.17367(14) 0.14697(12) 0.01513(8) 0.0646(4) Uani 1 1 d . . . . . O4 O 0.28296(15) 0.12307(12) 0.28194(8) 0.0701(4) Uani 1 1 d . . . . . N4 N 0.28526(18) 0.18043(13) 0.11139(10) 0.0504(4) Uani 1 1 d . . . . . H4A H 0.367(2) 0.1770(15) 0.1263(11) 0.052(6) Uiso 1 1 d . . . . . N5 N 0.59887(17) 0.13173(12) 0.08850(9) 0.0518(4) Uani 1 1 d . . . . . N6 N 0.56670(16) 0.10766(12) -0.10861(9) 0.0509(4) Uani 1 1 d . . . . . N7 N 0.63898(15) 0.11045(11) -0.04572(8) 0.0439(4) Uani 1 1 d . . . . . N12 N 0.05196(16) 0.22638(13) 0.27677(9) 0.0542(4) Uani 1 1 d . . . . . N13 N -0.04422(15) 0.27389(12) 0.21653(9) 0.0507(4) Uani 1 1 d . . . . . C25 C 0.8520(2) 0.03862(16) -0.17295(12) 0.0603(5) Uani 1 1 d . . . . . H25 H 0.7797 0.0083 -0.1668 0.072 Uiso 1 1 calc R . . . . C26 C 0.9428(2) 0.02886(18) -0.23710(14) 0.0718(6) Uani 1 1 d . . . . . H26 H 0.9306 -0.0079 -0.2739 0.086 Uiso 1 1 calc R . . . . C27 C 1.0505(3) 0.0723(2) -0.24765(14) 0.0741(7) Uani 1 1 d . . . . . H27 H 1.1119 0.0641 -0.2907 0.089 Uiso 1 1 calc R . . . . C28 C 1.0667(2) 0.1285(2) -0.19342(14) 0.0746(7) Uani 1 1 d . . . . . H28 H 1.1383 0.1595 -0.2006 0.089 Uiso 1 1 calc R . . . . C29 C 0.9770(2) 0.13874(17) -0.12869(12) 0.0605(5) Uani 1 1 d . . . . . H29 H 0.9895 0.1760 -0.0923 0.073 Uiso 1 1 calc R . . . . C30 C 0.86848(19) 0.09394(14) -0.11729(11) 0.0488(5) Uani 1 1 d . . . . . C31 C 0.77908(18) 0.10484(14) -0.04588(11) 0.0449(4) Uani 1 1 d . . . . . C32 C 0.8260(2) 0.11183(15) 0.02437(11) 0.0534(5) Uani 1 1 d . . . . . H32 H 0.9201 0.1076 0.0289 0.064 Uiso 1 1 calc R . . . . C33 C 0.7340(2) 0.12514(15) 0.08850(12) 0.0548(5) Uani 1 1 d . . . . . H33 H 0.7702 0.1297 0.1347 0.066 Uiso 1 1 calc R . . . . C34 C 0.55103(19) 0.12495(13) 0.02003(10) 0.0439(4) Uani 1 1 d . . . . . C35 C 0.41679(19) 0.13039(13) -0.00230(10) 0.0447(4) Uani 1 1 d . . . . . C36 C 0.4362(2) 0.11898(14) -0.08012(11) 0.0503(5) Uani 1 1 d . . . . . H36 H 0.3630 0.1192 -0.1101 0.060 Uiso 1 1 calc R . . . . C37 C 0.2813(2) 0.15166(14) 0.04137(11) 0.0476(4) Uani 1 1 d . . . . . C38 C 0.16936(19) 0.21162(15) 0.16213(11) 0.0465(4) Uani 1 1 d . . . . . C39 C 0.1825(2) 0.18031(15) 0.24446(11) 0.0506(5) Uani 1 1 d . . . . . C41 C 0.0000(2) 0.19151(16) 0.35175(11) 0.0554(5) Uani 1 1 d . . . . . C42 C 0.0789(3) 0.18123(18) 0.41567(13) 0.0708(6) Uani 1 1 d . . . . . H42 H 0.1633 0.1979 0.4097 0.085 Uiso 1 1 calc R . . . . C43 C 0.0312(4) 0.1458(2) 0.48902(14) 0.0899(8) Uani 1 1 d . . . . . H43 H 0.0843 0.1376 0.5324 0.108 Uiso 1 1 calc R . . . . C44 C -0.0946(4) 0.1227(2) 0.49761(16) 0.0963(9) Uani 1 1 d . . . . . H44 H -0.1267 0.1001 0.5470 0.116 Uiso 1 1 calc R . . . . C45 C -0.1734(3) 0.1327(2) 0.43390(16) 0.0898(8) Uani 1 1 d . . . . . H45 H -0.2583 0.1168 0.4401 0.108 Uiso 1 1 calc R . . . . C46 C -0.1252(2) 0.16669(18) 0.36026(13) 0.0689(6) Uani 1 1 d . . . . . H46 H -0.1770 0.1727 0.3168 0.083 Uiso 1 1 calc R . . . . C47 C 0.03641(19) 0.27092(15) 0.14722(11) 0.0488(5) Uani 1 1 d . . . . . C48 C -0.0270(2) 0.33230(18) 0.07359(12) 0.0651(6) Uani 1 1 d . . . . . H48A H -0.0238 0.4003 0.0706 0.098 Uiso 1 1 calc GR . . . . H48B H -0.1230 0.3318 0.0726 0.098 Uiso 1 1 calc GR . . . . H48C H 0.0250 0.3044 0.0300 0.098 Uiso 1 1 calc GR . . . . C49 C -0.1419(2) 0.37185(16) 0.23038(12) 0.0612(6) Uani 1 1 d . . . . . H49A H -0.0904 0.4202 0.2274 0.092 Uiso 1 1 calc GR . . . . H49B H -0.1863 0.3639 0.2811 0.092 Uiso 1 1 calc GR . . . . H49C H -0.2125 0.3950 0.1916 0.092 Uiso 1 1 calc GR . . . . O5 O 0.6737(3) 0.9195(4) 0.38998(18) 0.251(3) Uani 1 1 d . . . . . C50 C 0.5664(4) 0.9225(3) 0.3656(2) 0.1095(11) Uani 1 1 d . . . . . C51 C 0.4453(5) 0.9246(4) 0.4178(2) 0.1738(19) Uani 1 1 d . . . . . H51A H 0.4747 0.8809 0.4661 0.261 Uiso 1 1 calc GR . . . . H51B H 0.3787 0.9022 0.3945 0.261 Uiso 1 1 calc GR . . . . H51C H 0.4022 0.9922 0.4276 0.261 Uiso 1 1 calc GR . . . . C52 C 0.5497(4) 0.9210(3) 0.2854(2) 0.1356(14) Uani 1 1 d . . . . . H52A H 0.5815 0.9737 0.2537 0.203 Uiso 1 1 calc GR . . . . H52B H 0.4522 0.9314 0.2763 0.203 Uiso 1 1 calc GR . . . . H52C H 0.6043 0.8570 0.2723 0.203 Uiso 1 1 calc GR . . . . 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 O1 0.0453(8) 0.0767(10) 0.0549(8) -0.0142(7) -0.0080(6) -0.0239(7) O2 0.0434(8) 0.0816(11) 0.0574(8) -0.0065(7) -0.0083(7) -0.0081(7) N1 0.0376(9) 0.0521(10) 0.0542(9) -0.0065(7) -0.0076(7) -0.0121(7) N2 0.0402(9) 0.0561(11) 0.0511(9) -0.0100(7) -0.0019(7) -0.0177(7) N3 0.0393(9) 0.0607(11) 0.0458(9) -0.0141(7) -0.0031(8) -0.0165(7) N8 0.0405(8) 0.0455(9) 0.0470(9) -0.0059(6) -0.0060(7) -0.0137(7) N9 0.0489(10) 0.0675(12) 0.0479(9) -0.0127(8) -0.0002(8) -0.0081(8) N10 0.0486(10) 0.0656(12) 0.0476(9) -0.0122(7) -0.0052(8) -0.0151(8) C1 0.0581(12) 0.0509(12) 0.0492(11) -0.0102(8) -0.0084(9) -0.0210(10) C2 0.0662(14) 0.0753(16) 0.0547(13) -0.0084(10) -0.0101(11) -0.0254(12) C3 0.0889(19) 0.095(2) 0.0504(13) -0.0048(12) -0.0109(13) -0.0386(16) C4 0.095(2) 0.111(2) 0.0534(14) -0.0270(13) 0.0093(14) -0.0468(17) C5 0.0726(16) 0.099(2) 0.0675(16) -0.0332(13) 0.0020(13) -0.0183(14) C6 0.0648(15) 0.0717(16) 0.0593(13) -0.0187(10) -0.0060(11) -0.0127(12) C7 0.0484(11) 0.0441(11) 0.0473(10) -0.0052(8) -0.0117(9) -0.0128(8) C8 0.0510(12) 0.0570(13) 0.0542(12) -0.0059(9) -0.0159(9) -0.0173(9) C9 0.0415(11) 0.0558(13) 0.0634(13) -0.0049(9) -0.0097(10) -0.0146(9) C10 0.0388(10) 0.0369(10) 0.0475(10) -0.0050(7) -0.0040(8) -0.0093(7) C11 0.0410(10) 0.0396(11) 0.0464(10) -0.0071(7) -0.0039(8) -0.0132(8) C12 0.0417(10) 0.0512(12) 0.0494(11) -0.0092(8) -0.0067(9) -0.0153(8) C13 0.0400(10) 0.0421(11) 0.0487(10) -0.0068(7) -0.0050(8) -0.0128(8) C14 0.0380(10) 0.0583(13) 0.0469(10) -0.0124(8) -0.0021(8) -0.0172(9) C15 0.0451(11) 0.0697(15) 0.0508(11) -0.0190(9) 0.0007(9) -0.0200(10) C16 0.0598(14) 0.0692(17) 0.0648(13) -0.0176(11) 0.0019(11) -0.0218(11) C17 0.0720(16) 0.0727(17) 0.0770(16) -0.0263(12) -0.0013(13) -0.0135(13) C18 0.0599(15) 0.098(2) 0.0666(15) -0.0320(13) 0.0038(12) -0.0154(14) C19 0.0559(14) 0.107(2) 0.0565(13) -0.0165(13) 0.0072(11) -0.0311(14) C20 0.0626(14) 0.0754(16) 0.0595(13) -0.0172(11) 0.0013(11) -0.0269(12) C21 0.0562(13) 0.0732(16) 0.0636(13) -0.0086(11) -0.0063(11) -0.0099(11) C22 0.0728(16) 0.105(2) 0.0586(13) -0.0234(12) -0.0139(12) -0.0213(14) C23 0.0419(10) 0.0571(13) 0.0501(11) -0.0090(9) -0.0040(9) -0.0177(9) C24 0.0423(11) 0.0616(13) 0.0510(11) -0.0123(9) -0.0036(9) -0.0197(9) O3 0.0462(8) 0.0789(11) 0.0790(10) -0.0277(8) -0.0014(7) -0.0254(7) O4 0.0496(9) 0.0793(11) 0.0706(9) -0.0056(8) -0.0100(7) -0.0042(7) N4 0.0375(9) 0.0583(11) 0.0584(10) -0.0136(8) 0.0019(8) -0.0166(8) N5 0.0503(10) 0.0533(10) 0.0508(9) -0.0092(7) -0.0035(8) -0.0128(8) N6 0.0481(10) 0.0547(11) 0.0523(9) -0.0119(7) -0.0024(8) -0.0163(8) N7 0.0419(9) 0.0408(9) 0.0483(9) -0.0074(6) -0.0016(7) -0.0106(7) N12 0.0412(9) 0.0652(12) 0.0520(9) -0.0083(8) -0.0023(8) -0.0094(8) N13 0.0413(9) 0.0557(11) 0.0522(9) -0.0105(7) -0.0033(7) -0.0084(7) C25 0.0563(13) 0.0550(14) 0.0707(14) -0.0147(10) 0.0146(11) -0.0198(10) C26 0.0759(16) 0.0686(16) 0.0729(15) -0.0236(11) 0.0228(12) -0.0233(13) C27 0.0671(15) 0.0808(18) 0.0710(15) -0.0120(12) 0.0235(12) -0.0230(13) C28 0.0547(14) 0.094(2) 0.0784(16) -0.0052(14) 0.0095(12) -0.0347(13) C29 0.0486(12) 0.0715(15) 0.0635(13) -0.0082(10) -0.0017(10) -0.0223(10) C30 0.0410(11) 0.0440(12) 0.0556(11) -0.0041(8) 0.0017(9) -0.0067(8) C31 0.0377(10) 0.0381(11) 0.0556(11) -0.0052(8) -0.0010(8) -0.0073(8) C32 0.0396(11) 0.0560(13) 0.0608(12) -0.0074(9) -0.0059(9) -0.0084(9) C33 0.0495(12) 0.0580(13) 0.0556(12) -0.0095(9) -0.0108(10) -0.0112(9) C34 0.0450(11) 0.0377(11) 0.0466(10) -0.0055(7) 0.0024(8) -0.0102(8) C35 0.0432(11) 0.0382(11) 0.0531(11) -0.0076(8) -0.0004(8) -0.0128(8) C36 0.0484(12) 0.0469(12) 0.0582(12) -0.0096(8) -0.0049(9) -0.0162(9) C37 0.0445(11) 0.0420(11) 0.0581(12) -0.0095(8) -0.0008(9) -0.0145(8) C38 0.0391(10) 0.0475(12) 0.0561(11) -0.0110(8) 0.0010(9) -0.0164(8) C39 0.0390(11) 0.0543(13) 0.0598(12) -0.0110(9) -0.0043(9) -0.0137(9) C41 0.0560(13) 0.0523(13) 0.0548(12) -0.0144(9) 0.0023(10) -0.0090(9) C42 0.0829(16) 0.0700(16) 0.0623(14) -0.0121(11) -0.0124(12) -0.0229(12) C43 0.123(2) 0.084(2) 0.0581(16) -0.0097(12) -0.0126(15) -0.0199(17) C44 0.116(3) 0.091(2) 0.0667(18) -0.0094(14) 0.0257(18) -0.0165(18) C45 0.0813(19) 0.102(2) 0.0806(19) -0.0130(15) 0.0266(16) -0.0271(15) C46 0.0584(14) 0.0809(17) 0.0641(14) -0.0146(11) 0.0091(11) -0.0162(12) C47 0.0437(11) 0.0517(12) 0.0545(11) -0.0121(8) -0.0009(9) -0.0168(9) C48 0.0588(13) 0.0702(16) 0.0594(13) -0.0064(10) -0.0054(10) -0.0096(11) C49 0.0486(12) 0.0614(14) 0.0705(13) -0.0199(10) -0.0035(10) -0.0057(10) O5 0.135(3) 0.514(8) 0.157(3) -0.123(4) 0.004(2) -0.137(4) C50 0.078(2) 0.160(3) 0.107(2) -0.049(2) 0.0021(19) -0.045(2) C51 0.153(4) 0.234(6) 0.140(3) -0.011(3) 0.046(3) -0.089(4) C52 0.104(3) 0.168(4) 0.126(3) -0.066(3) -0.008(2) -0.001(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 O1 C13 1.231(2) . ? O2 C24 1.231(2) . ? N1 C9 1.320(2) . ? N1 C10 1.353(2) . ? N2 N8 1.3713(19) . ? N2 C12 1.329(2) . ? N3 H3 0.85(2) . ? N3 C13 1.366(2) . ? N3 C14 1.408(2) . ? N8 C7 1.374(2) . ? N8 C10 1.391(2) . ? N9 N10 1.418(2) . ? N9 C15 1.417(2) . ? N9 C24 1.381(2) . ? N10 C22 1.463(3) . ? N10 C23 1.397(2) . ? C1 C2 1.394(3) . ? C1 C6 1.387(3) . ? C1 C7 1.478(3) . ? C2 H2 0.9300 . ? C2 C3 1.381(3) . ? C3 H3A 0.9300 . ? C3 C4 1.371(3) . ? C4 H4 0.9300 . ? C4 C5 1.371(3) . ? C5 H5 0.9300 . ? C5 C6 1.385(3) . ? C6 H6 0.9300 . ? C7 C8 1.368(3) . ? C8 H8 0.9300 . ? C8 C9 1.402(3) . ? C9 H9 0.9300 . ? C10 C11 1.393(2) . ? C11 C12 1.397(2) . ? C11 C13 1.467(2) . ? C12 H12 0.9300 . ? C14 C23 1.346(3) . ? C14 C24 1.448(3) . ? C15 C16 1.374(3) . ? C15 C20 1.384(3) . ? C16 H16 0.9300 . ? C16 C17 1.387(3) . ? C17 H17 0.9300 . ? C17 C18 1.351(3) . ? C18 H18 0.9300 . ? C18 C19 1.372(4) . ? C19 H19 0.9300 . ? C19 C20 1.390(3) . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21 C23 1.488(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O3 C37 1.223(2) . ? O4 C39 1.232(2) . ? N4 H4A 0.86(2) . ? N4 C37 1.362(2) . ? N4 C38 1.406(2) . ? N5 C33 1.321(2) . ? N5 C34 1.351(2) . ? N6 N7 1.374(2) . ? N6 C36 1.327(2) . ? N7 C31 1.373(2) . ? N7 C34 1.392(2) . ? N12 N13 1.415(2) . ? N12 C39 1.391(2) . ? N12 C41 1.426(2) . ? N13 C47 1.396(2) . ? N13 C49 1.480(2) . ? C25 H25 0.9300 . ? C25 C26 1.380(3) . ? C25 C30 1.397(3) . ? C26 H26 0.9300 . ? C26 C27 1.370(3) . ? C27 H27 0.9300 . ? C27 C28 1.386(4) . ? C28 H28 0.9300 . ? C28 C29 1.382(3) . ? C29 H29 0.9300 . ? C29 C30 1.390(3) . ? C30 C31 1.475(2) . ? C31 C32 1.377(3) . ? C32 H32 0.9300 . ? C32 C33 1.390(3) . ? C33 H33 0.9300 . ? C34 C35 1.399(3) . ? C35 C36 1.388(3) . ? C35 C37 1.470(2) . ? C36 H36 0.9300 . ? C38 C39 1.431(3) . ? C38 C47 1.355(2) . ? C41 C42 1.379(3) . ? C41 C46 1.381(3) . ? C42 H42 0.9300 . ? C42 C43 1.388(3) . ? C43 H43 0.9300 . ? C43 C44 1.375(4) . ? C44 H44 0.9300 . ? C44 C45 1.376(4) . ? C45 H45 0.9300 . ? C45 C46 1.388(3) . ? C46 H46 0.9300 . ? C47 C48 1.486(3) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? O5 C50 1.168(3) . ? C50 C51 1.447(4) . ? C50 C52 1.428(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? 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 C9 N1 C10 115.84(16) . . ? C12 N2 N8 103.34(14) . . ? C13 N3 H3 117.6(14) . . ? C13 N3 C14 124.55(16) . . ? C14 N3 H3 117.2(14) . . ? N2 N8 C7 125.92(15) . . ? N2 N8 C10 112.15(14) . . ? C7 N8 C10 121.92(15) . . ? C15 N9 N10 120.53(15) . . ? C24 N9 N10 110.77(15) . . ? C24 N9 C15 127.45(16) . . ? N9 N10 C22 113.35(17) . . ? C23 N10 N9 105.25(14) . . ? C23 N10 C22 118.16(16) . . ? C2 C1 C7 117.81(18) . . ? C6 C1 C2 118.67(19) . . ? C6 C1 C7 123.48(17) . . ? C1 C2 H2 119.8 . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2 119.8 . . ? C2 C3 H3A 119.8 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3A 119.8 . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 119.5 . . ? C4 C5 C6 121.1(2) . . ? C6 C5 H5 119.5 . . ? C1 C6 H6 120.1 . . ? C5 C6 C1 119.9(2) . . ? C5 C6 H6 120.1 . . ? N8 C7 C1 120.75(16) . . ? C8 C7 N8 115.04(16) . . ? C8 C7 C1 124.21(17) . . ? C7 C8 H8 119.5 . . ? C7 C8 C9 121.05(17) . . ? C9 C8 H8 119.5 . . ? N1 C9 C8 123.77(18) . . ? N1 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? N1 C10 N8 122.37(15) . . ? N1 C10 C11 131.74(16) . . ? N8 C10 C11 105.88(15) . . ? C10 C11 C12 104.28(15) . . ? C10 C11 C13 128.06(16) . . ? C12 C11 C13 127.66(16) . . ? N2 C12 C11 114.34(16) . . ? N2 C12 H12 122.8 . . ? C11 C12 H12 122.8 . . ? O1 C13 N3 123.06(17) . . ? O1 C13 C11 122.55(16) . . ? N3 C13 C11 114.37(16) . . ? N3 C14 C24 121.04(16) . . ? C23 C14 N3 129.44(18) . . ? C23 C14 C24 109.41(16) . . ? C16 C15 N9 118.75(18) . . ? C16 C15 C20 120.4(2) . . ? C20 C15 N9 120.9(2) . . ? C15 C16 H16 120.5 . . ? C15 C16 C17 118.9(2) . . ? C17 C16 H16 120.5 . . ? C16 C17 H17 119.3 . . ? C18 C17 C16 121.5(3) . . ? C18 C17 H17 119.3 . . ? C17 C18 H18 120.2 . . ? C17 C18 C19 119.6(2) . . ? C19 C18 H18 120.2 . . ? C18 C19 H19 119.7 . . ? C18 C19 C20 120.5(2) . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 119.0(2) . . ? C15 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C21 H21A 109.5 . . ? C23 C21 H21B 109.5 . . ? C23 C21 H21C 109.5 . . ? N10 C22 H22A 109.5 . . ? N10 C22 H22B 109.5 . . ? N10 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N10 C23 C21 119.60(16) . . ? C14 C23 N10 109.90(17) . . ? C14 C23 C21 130.48(18) . . ? O2 C24 N9 125.29(18) . . ? O2 C24 C14 130.40(18) . . ? N9 C24 C14 104.21(16) . . ? C37 N4 H4A 116.4(13) . . ? C37 N4 C38 126.10(17) . . ? C38 N4 H4A 117.4(13) . . ? C33 N5 C34 115.53(16) . . ? C36 N6 N7 103.22(15) . . ? N6 N7 C34 111.76(14) . . ? C31 N7 N6 125.94(15) . . ? C31 N7 C34 122.24(15) . . ? N13 N12 C41 119.13(15) . . ? C39 N12 N13 109.40(14) . . ? C39 N12 C41 124.40(16) . . ? N12 N13 C49 113.85(15) . . ? C47 N13 N12 105.77(14) . . ? C47 N13 C49 118.22(16) . . ? C26 C25 H25 119.9 . . ? C26 C25 C30 120.1(2) . . ? C30 C25 H25 119.9 . . ? C25 C26 H26 119.4 . . ? C27 C26 C25 121.3(2) . . ? C27 C26 H26 119.4 . . ? C26 C27 H27 120.4 . . ? C26 C27 C28 119.2(2) . . ? C28 C27 H27 120.4 . . ? C27 C28 H28 119.9 . . ? C29 C28 C27 120.3(2) . . ? C29 C28 H28 119.9 . . ? C28 C29 H29 119.6 . . ? C28 C29 C30 120.8(2) . . ? C30 C29 H29 119.6 . . ? C25 C30 C31 123.33(17) . . ? C29 C30 C25 118.40(18) . . ? C29 C30 C31 118.24(19) . . ? N7 C31 C30 121.13(16) . . ? N7 C31 C32 114.81(16) . . ? C32 C31 C30 124.05(17) . . ? C31 C32 H32 119.7 . . ? C31 C32 C33 120.61(18) . . ? C33 C32 H32 119.7 . . ? N5 C33 C32 124.65(18) . . ? N5 C33 H33 117.7 . . ? C32 C33 H33 117.7 . . ? N5 C34 N7 122.14(16) . . ? N5 C34 C35 131.75(17) . . ? N7 C34 C35 106.11(15) . . ? C34 C35 C37 130.17(17) . . ? C36 C35 C34 103.82(16) . . ? C36 C35 C37 125.82(17) . . ? N6 C36 C35 115.08(18) . . ? N6 C36 H36 122.5 . . ? C35 C36 H36 122.5 . . ? O3 C37 N4 123.36(18) . . ? O3 C37 C35 122.16(18) . . ? N4 C37 C35 114.44(17) . . ? N4 C38 C39 120.26(17) . . ? C47 C38 N4 130.71(18) . . ? C47 C38 C39 109.03(16) . . ? O4 C39 N12 124.77(18) . . ? O4 C39 C38 129.87(18) . . ? N12 C39 C38 105.33(16) . . ? C42 C41 N12 118.5(2) . . ? C42 C41 C46 120.6(2) . . ? C46 C41 N12 120.91(19) . . ? C41 C42 H42 120.3 . . ? C41 C42 C43 119.3(2) . . ? C43 C42 H42 120.3 . . ? C42 C43 H43 120.0 . . ? C44 C43 C42 120.1(3) . . ? C44 C43 H43 120.0 . . ? C43 C44 H44 119.6 . . ? C43 C44 C45 120.7(3) . . ? C45 C44 H44 119.6 . . ? C44 C45 H45 120.3 . . ? C44 C45 C46 119.5(3) . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 119.8(2) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? N13 C47 C48 119.71(16) . . ? C38 C47 N13 109.46(16) . . ? C38 C47 C48 130.74(18) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N13 C49 H49A 109.5 . . ? N13 C49 H49B 109.5 . . ? N13 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O5 C50 C51 119.9(4) . . ? O5 C50 C52 122.5(3) . . ? C52 C50 C51 117.6(3) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? 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 N1 C10 C11 C12 -177.95(18) . . . . ? N1 C10 C11 C13 1.4(3) . . . . ? N2 N8 C7 C1 1.5(3) . . . . ? N2 N8 C7 C8 -178.41(16) . . . . ? N2 N8 C10 N1 177.99(16) . . . . ? N2 N8 C10 C11 -1.03(19) . . . . ? N3 C14 C23 N10 -175.60(18) . . . . ? N3 C14 C23 C21 2.8(4) . . . . ? N3 C14 C24 O2 3.9(3) . . . . ? N3 C14 C24 N9 -179.84(16) . . . . ? N8 N2 C12 C11 0.0(2) . . . . ? N8 C7 C8 C9 0.4(3) . . . . ? N8 C10 C11 C12 0.94(18) . . . . ? N8 C10 C11 C13 -179.70(16) . . . . ? N9 N10 C23 C14 -4.5(2) . . . . ? N9 N10 C23 C21 176.95(18) . . . . ? N9 C15 C16 C17 -177.70(18) . . . . ? N9 C15 C20 C19 177.18(18) . . . . ? N10 N9 C15 C16 138.88(19) . . . . ? N10 N9 C15 C20 -40.7(3) . . . . ? N10 N9 C24 O2 170.12(18) . . . . ? N10 N9 C24 C14 -6.4(2) . . . . ? C1 C2 C3 C4 -1.8(4) . . . . ? C1 C7 C8 C9 -179.51(18) . . . . ? C2 C1 C6 C5 -0.6(3) . . . . ? C2 C1 C7 N8 -143.47(19) . . . . ? C2 C1 C7 C8 36.4(3) . . . . ? C2 C3 C4 C5 1.2(4) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C4 C5 C6 C1 0.0(4) . . . . ? C6 C1 C2 C3 1.5(3) . . . . ? C6 C1 C7 N8 38.7(3) . . . . ? C6 C1 C7 C8 -141.4(2) . . . . ? C7 N8 C10 N1 -0.8(3) . . . . ? C7 N8 C10 C11 -179.84(16) . . . . ? C7 C1 C2 C3 -176.42(19) . . . . ? C7 C1 C6 C5 177.2(2) . . . . ? C7 C8 C9 N1 -0.5(3) . . . . ? C9 N1 C10 N8 0.7(2) . . . . ? C9 N1 C10 C11 179.46(19) . . . . ? C10 N1 C9 C8 -0.1(3) . . . . ? C10 N8 C7 C1 -179.88(16) . . . . ? C10 N8 C7 C8 0.2(2) . . . . ? C10 C11 C12 N2 -0.6(2) . . . . ? C10 C11 C13 O1 -179.04(19) . . . . ? C10 C11 C13 N3 2.0(3) . . . . ? C12 N2 N8 C7 179.40(17) . . . . ? C12 N2 N8 C10 0.64(18) . . . . ? C12 C11 C13 O1 0.2(3) . . . . ? C12 C11 C13 N3 -178.79(17) . . . . ? C13 N3 C14 C23 -55.0(3) . . . . ? C13 N3 C14 C24 129.2(2) . . . . ? C13 C11 C12 N2 -179.98(17) . . . . ? C14 N3 C13 O1 5.3(3) . . . . ? C14 N3 C13 C11 -175.71(16) . . . . ? C15 N9 N10 C22 -54.4(2) . . . . ? C15 N9 N10 C23 175.03(17) . . . . ? C15 N9 C24 O2 3.0(3) . . . . ? C15 N9 C24 C14 -173.54(19) . . . . ? C15 C16 C17 C18 -0.1(3) . . . . ? C16 C15 C20 C19 -2.4(3) . . . . ? C16 C17 C18 C19 -1.1(4) . . . . ? C17 C18 C19 C20 0.5(3) . . . . ? C18 C19 C20 C15 1.2(3) . . . . ? C20 C15 C16 C17 1.9(3) . . . . ? C22 N10 C23 C14 -132.2(2) . . . . ? C22 N10 C23 C21 49.2(3) . . . . ? C23 C14 C24 O2 -172.7(2) . . . . ? C23 C14 C24 N9 3.6(2) . . . . ? C24 N9 N10 C22 137.48(18) . . . . ? C24 N9 N10 C23 6.9(2) . . . . ? C24 N9 C15 C16 -55.1(3) . . . . ? C24 N9 C15 C20 125.3(2) . . . . ? C24 C14 C23 N10 0.6(2) . . . . ? C24 C14 C23 C21 179.0(2) . . . . ? N4 C38 C39 O4 -3.7(3) . . . . ? N4 C38 C39 N12 178.20(16) . . . . ? N4 C38 C47 N13 175.42(18) . . . . ? N4 C38 C47 C48 -8.1(4) . . . . ? N5 C34 C35 C36 179.4(2) . . . . ? N5 C34 C35 C37 4.2(3) . . . . ? N6 N7 C31 C30 -0.5(3) . . . . ? N6 N7 C31 C32 178.47(17) . . . . ? N6 N7 C34 N5 -178.97(16) . . . . ? N6 N7 C34 C35 0.71(19) . . . . ? N7 N6 C36 C35 0.8(2) . . . . ? N7 C31 C32 C33 -1.0(3) . . . . ? N7 C34 C35 C36 -0.22(19) . . . . ? N7 C34 C35 C37 -175.42(18) . . . . ? N12 N13 C47 C38 9.2(2) . . . . ? N12 N13 C47 C48 -167.76(17) . . . . ? N12 C41 C42 C43 -178.9(2) . . . . ? N12 C41 C46 C45 179.9(2) . . . . ? N13 N12 C39 O4 -170.97(18) . . . . ? N13 N12 C39 C38 7.3(2) . . . . ? N13 N12 C41 C42 -155.78(18) . . . . ? N13 N12 C41 C46 25.4(3) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C25 C30 C31 N7 -34.8(3) . . . . ? C25 C30 C31 C32 146.3(2) . . . . ? C26 C25 C30 C29 0.4(3) . . . . ? C26 C25 C30 C31 -177.78(18) . . . . ? C26 C27 C28 C29 1.4(4) . . . . ? C27 C28 C29 C30 -0.7(3) . . . . ? C28 C29 C30 C25 -0.2(3) . . . . ? C28 C29 C30 C31 178.10(19) . . . . ? C29 C30 C31 N7 147.03(18) . . . . ? C29 C30 C31 C32 -31.9(3) . . . . ? C30 C25 C26 C27 0.3(3) . . . . ? C30 C31 C32 C33 177.99(17) . . . . ? C31 N7 C34 N5 -1.8(3) . . . . ? C31 N7 C34 C35 177.87(16) . . . . ? C31 C32 C33 N5 0.2(3) . . . . ? C33 N5 C34 N7 0.9(3) . . . . ? C33 N5 C34 C35 -178.65(19) . . . . ? C34 N5 C33 C32 -0.2(3) . . . . ? C34 N7 C31 C30 -177.27(16) . . . . ? C34 N7 C31 C32 1.7(2) . . . . ? C34 C35 C36 N6 -0.4(2) . . . . ? C34 C35 C37 O3 -174.91(19) . . . . ? C34 C35 C37 N4 7.5(3) . . . . ? C36 N6 N7 C31 -177.92(17) . . . . ? C36 N6 N7 C34 -0.89(19) . . . . ? C36 C35 C37 O3 10.8(3) . . . . ? C36 C35 C37 N4 -166.78(18) . . . . ? C37 N4 C38 C39 139.9(2) . . . . ? C37 N4 C38 C47 -40.4(3) . . . . ? C37 C35 C36 N6 175.13(17) . . . . ? C38 N4 C37 O3 -2.2(3) . . . . ? C38 N4 C37 C35 175.40(16) . . . . ? C39 N12 N13 C47 -10.2(2) . . . . ? C39 N12 N13 C49 -141.68(17) . . . . ? C39 N12 C41 C42 56.8(3) . . . . ? C39 N12 C41 C46 -122.0(2) . . . . ? C39 C38 C47 N13 -4.9(2) . . . . ? C39 C38 C47 C48 171.6(2) . . . . ? C41 N12 N13 C47 -162.11(17) . . . . ? C41 N12 N13 C49 66.4(2) . . . . ? C41 N12 C39 O4 -20.9(3) . . . . ? C41 N12 C39 C38 157.38(18) . . . . ? C41 C42 C43 C44 -1.0(4) . . . . ? C42 C41 C46 C45 1.1(3) . . . . ? C42 C43 C44 C45 1.1(4) . . . . ? C43 C44 C45 C46 -0.1(4) . . . . ? C44 C45 C46 C41 -1.0(4) . . . . ? C46 C41 C42 C43 -0.1(3) . . . . ? C47 C38 C39 O4 176.6(2) . . . . ? C47 C38 C39 N12 -1.5(2) . . . . ? C49 N13 C47 C38 138.13(18) . . . . ? C49 N13 C47 C48 -38.8(3) . . . . ? _shelx_res_file ; TITL SKF-01_0m in P-1 CELL 0.71073 9.9554 14.0875 17.4572 79.676 85.283 72.647 ZERR 2 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 102 92 24 10 L.S. 20 PLAN 1 TEMP 23 BOND MORE -1 BOND $H CONF fmap 2 acta OMIT 0 0 1 OMIT 2 10 3 OMIT 3 10 4 REM REM REM WGHT 0.080700 0.027600 FVAR 0.40646 O1 4 0.601018 0.383176 0.111682 11.00000 0.04532 0.07672 = 0.05494 -0.01421 -0.00800 -0.02388 O2 4 0.108950 0.532155 0.149248 11.00000 0.04341 0.08155 = 0.05738 -0.00649 -0.00832 -0.00812 N1 3 0.286596 0.380286 -0.052133 11.00000 0.03758 0.05206 = 0.05425 -0.00648 -0.00764 -0.01211 N2 3 0.633978 0.362242 -0.131258 11.00000 0.04020 0.05614 = 0.05111 -0.01002 -0.00193 -0.01773 N3 3 0.373005 0.384818 0.101714 11.00000 0.03926 0.06066 = 0.04580 -0.01412 -0.00306 -0.01654 H3 2 0.310995 0.387499 0.070080 11.00000 0.06919 N8 3 0.495650 0.364878 -0.134135 11.00000 0.04051 0.04549 = 0.04700 -0.00595 -0.00602 -0.01369 N9 3 0.188665 0.464907 0.274320 11.00000 0.04893 0.06750 = 0.04794 -0.01267 -0.00015 -0.00806 N10 3 0.296131 0.380441 0.308650 11.00000 0.04858 0.06557 = 0.04763 -0.01224 -0.00517 -0.01505 C1 1 0.506473 0.352601 -0.274582 11.00000 0.05809 0.05090 = 0.04920 -0.01021 -0.00842 -0.02105 C2 1 0.435361 0.404788 -0.342013 11.00000 0.06619 0.07528 = 0.05472 -0.00838 -0.01013 -0.02542 AFIX 43 H2 2 0.343932 0.446671 -0.338171 11.00000 -1.20000 AFIX 0 C3 1 0.499728 0.394734 -0.414492 11.00000 0.08891 0.09476 = 0.05035 -0.00483 -0.01093 -0.03857 AFIX 43 H3A 2 0.450429 0.428373 -0.459146 11.00000 -1.20000 AFIX 0 C4 1 0.635844 0.335469 -0.421008 11.00000 0.09477 0.11075 = 0.05344 -0.02702 0.00926 -0.04681 AFIX 43 H4 2 0.679555 0.329830 -0.469836 11.00000 -1.20000 AFIX 0 C5 1 0.706993 0.284594 -0.354981 11.00000 0.07259 0.09859 = 0.06753 -0.03322 0.00203 -0.01832 AFIX 43 H5 2 0.799153 0.244130 -0.359423 11.00000 -1.20000 AFIX 0 C6 1 0.643851 0.292478 -0.281766 11.00000 0.06479 0.07173 = 0.05935 -0.01873 -0.00596 -0.01274 AFIX 43 H6 2 0.693495 0.257516 -0.237511 11.00000 -1.20000 AFIX 0 C7 1 0.428856 0.361819 -0.199079 11.00000 0.04844 0.04406 = 0.04731 -0.00521 -0.01173 -0.01282 C8 1 0.289107 0.368053 -0.187675 11.00000 0.05103 0.05703 = 0.05423 -0.00586 -0.01595 -0.01727 AFIX 43 H8 2 0.237694 0.366026 -0.229180 11.00000 -1.20000 AFIX 0 C9 1 0.222145 0.377451 -0.114427 11.00000 0.04152 0.05576 = 0.06343 -0.00492 -0.00967 -0.01460 AFIX 43 H9 2 0.126810 0.381946 -0.109442 11.00000 -1.20000 AFIX 0 C10 1 0.425189 0.373327 -0.062377 11.00000 0.03885 0.03690 = 0.04754 -0.00497 -0.00397 -0.00925 C11 1 0.524778 0.374362 -0.011214 11.00000 0.04096 0.03957 = 0.04637 -0.00711 -0.00391 -0.01319 C12 1 0.647663 0.368033 -0.057303 11.00000 0.04172 0.05120 = 0.04941 -0.00920 -0.00669 -0.01529 AFIX 43 H12 2 0.731958 0.367883 -0.037866 11.00000 -1.20000 AFIX 0 C13 1 0.505245 0.381631 0.071998 11.00000 0.04004 0.04214 = 0.04871 -0.00679 -0.00502 -0.01284 C14 1 0.326993 0.398270 0.178515 11.00000 0.03801 0.05833 = 0.04687 -0.01241 -0.00212 -0.01723 C15 1 0.075200 0.515159 0.320624 11.00000 0.04507 0.06966 = 0.05082 -0.01897 0.00071 -0.02004 C16 1 0.028751 0.618645 0.306379 11.00000 0.05985 0.06924 = 0.06481 -0.01760 0.00191 -0.02181 AFIX 43 H16 2 0.068845 0.654836 0.265880 11.00000 -1.20000 AFIX 0 C17 1 -0.078852 0.668265 0.353344 11.00000 0.07203 0.07267 = 0.07698 -0.02634 -0.00131 -0.01348 AFIX 43 H17 2 -0.110505 0.738311 0.343990 11.00000 -1.20000 AFIX 0 C18 1 -0.138760 0.617155 0.412393 11.00000 0.05985 0.09831 = 0.06664 -0.03199 0.00378 -0.01542 AFIX 43 H18 2 -0.209744 0.651852 0.443785 11.00000 -1.20000 AFIX 0 C19 1 -0.094246 0.513764 0.425765 11.00000 0.05593 0.10703 = 0.05648 -0.01647 0.00719 -0.03110 AFIX 43 H19 2 -0.135869 0.478426 0.466106 11.00000 -1.20000 AFIX 0 C20 1 0.012549 0.461449 0.379491 11.00000 0.06263 0.07536 = 0.05946 -0.01720 0.00127 -0.02690 AFIX 43 H20 2 0.041503 0.391354 0.387960 11.00000 -1.20000 AFIX 0 C21 1 0.511560 0.258732 0.262045 11.00000 0.05617 0.07322 = 0.06362 -0.00860 -0.00627 -0.00990 AFIX 137 H21A 2 0.537503 0.226231 0.216939 11.00000 -1.50000 H21B 2 0.493595 0.211411 0.305600 11.00000 -1.50000 H21C 2 0.586924 0.282840 0.273707 11.00000 -1.50000 AFIX 0 C22 1 0.362294 0.400608 0.373403 11.00000 0.07279 0.10471 = 0.05859 -0.02343 -0.01394 -0.02134 AFIX 137 H22A 2 0.428943 0.339631 0.396594 11.00000 -1.50000 H22B 2 0.291402 0.424783 0.411697 11.00000 -1.50000 H22C 2 0.409941 0.450641 0.354397 11.00000 -1.50000 AFIX 0 C23 1 0.382388 0.345083 0.246373 11.00000 0.04185 0.05706 = 0.05006 -0.00904 -0.00405 -0.01775 C24 1 0.197945 0.474291 0.194072 11.00000 0.04234 0.06162 = 0.05099 -0.01233 -0.00358 -0.01968 O3 4 0.173672 0.146968 0.015128 11.00000 0.04620 0.07894 = 0.07904 -0.02769 -0.00143 -0.02540 O4 4 0.282958 0.123074 0.281945 11.00000 0.04958 0.07932 = 0.07058 -0.00561 -0.01001 -0.00422 N4 3 0.285262 0.180431 0.111391 11.00000 0.03745 0.05829 = 0.05839 -0.01356 0.00188 -0.01659 H4A 2 0.366597 0.176960 0.126325 11.00000 0.05244 N5 3 0.598866 0.131729 0.088503 11.00000 0.05032 0.05333 = 0.05078 -0.00923 -0.00345 -0.01277 N6 3 0.566701 0.107657 -0.108611 11.00000 0.04809 0.05474 = 0.05228 -0.01189 -0.00244 -0.01635 N7 3 0.638984 0.110450 -0.045716 11.00000 0.04192 0.04084 = 0.04828 -0.00740 -0.00164 -0.01065 N12 3 0.051962 0.226385 0.276769 11.00000 0.04125 0.06519 = 0.05201 -0.00833 -0.00228 -0.00941 N13 3 -0.044215 0.273885 0.216534 11.00000 0.04135 0.05573 = 0.05220 -0.01050 -0.00334 -0.00844 C25 1 0.851998 0.038621 -0.172948 11.00000 0.05631 0.05505 = 0.07073 -0.01475 0.01456 -0.01982 AFIX 43 H25 2 0.779746 0.008332 -0.166750 11.00000 -1.20000 AFIX 0 C26 1 0.942763 0.028861 -0.237102 11.00000 0.07591 0.06857 = 0.07290 -0.02357 0.02280 -0.02325 AFIX 43 H26 2 0.930571 -0.007912 -0.273882 11.00000 -1.20000 AFIX 0 C27 1 1.050450 0.072281 -0.247655 11.00000 0.06709 0.08075 = 0.07102 -0.01200 0.02349 -0.02300 AFIX 43 H27 2 1.111898 0.064129 -0.290675 11.00000 -1.20000 AFIX 0 C28 1 1.066705 0.128519 -0.193420 11.00000 0.05473 0.09391 = 0.07838 -0.00519 0.00946 -0.03472 AFIX 43 H28 2 1.138255 0.159510 -0.200612 11.00000 -1.20000 AFIX 0 C29 1 0.977032 0.138741 -0.128691 11.00000 0.04864 0.07149 = 0.06349 -0.00822 -0.00170 -0.02227 AFIX 43 H29 2 0.989459 0.176025 -0.092345 11.00000 -1.20000 AFIX 0 C30 1 0.868480 0.093935 -0.117292 11.00000 0.04104 0.04405 = 0.05563 -0.00412 0.00171 -0.00670 C31 1 0.779077 0.104842 -0.045881 11.00000 0.03772 0.03810 = 0.05556 -0.00521 -0.00095 -0.00732 C32 1 0.826011 0.111828 0.024365 11.00000 0.03961 0.05602 = 0.06082 -0.00736 -0.00594 -0.00844 AFIX 43 H32 2 0.920119 0.107602 0.028922 11.00000 -1.20000 AFIX 0 C33 1 0.734040 0.125135 0.088503 11.00000 0.04950 0.05799 = 0.05561 -0.00946 -0.01076 -0.01123 AFIX 43 H33 2 0.770230 0.129724 0.134705 11.00000 -1.20000 AFIX 0 C34 1 0.551034 0.124952 0.020029 11.00000 0.04498 0.03774 = 0.04662 -0.00546 0.00242 -0.01016 C35 1 0.416795 0.130392 -0.002301 11.00000 0.04324 0.03817 = 0.05314 -0.00760 -0.00039 -0.01280 C36 1 0.436160 0.118978 -0.080124 11.00000 0.04843 0.04690 = 0.05817 -0.00961 -0.00491 -0.01625 AFIX 43 H36 2 0.363002 0.119244 -0.110113 11.00000 -1.20000 AFIX 0 C37 1 0.281307 0.151658 0.041366 11.00000 0.04449 0.04200 = 0.05806 -0.00953 -0.00085 -0.01451 C38 1 0.169355 0.211623 0.162133 11.00000 0.03907 0.04751 = 0.05614 -0.01100 0.00105 -0.01644 C39 1 0.182454 0.180306 0.244462 11.00000 0.03898 0.05428 = 0.05978 -0.01100 -0.00426 -0.01375 C41 1 0.000017 0.191508 0.351754 11.00000 0.05602 0.05226 = 0.05485 -0.01436 0.00232 -0.00898 C42 1 0.078940 0.181234 0.415666 11.00000 0.08293 0.07004 = 0.06226 -0.01206 -0.01243 -0.02288 AFIX 43 H42 2 0.163267 0.197878 0.409695 11.00000 -1.20000 AFIX 0 C43 1 0.031192 0.145782 0.489018 11.00000 0.12256 0.08351 = 0.05814 -0.00974 -0.01256 -0.01995 AFIX 43 H43 2 0.084339 0.137633 0.532390 11.00000 -1.20000 AFIX 0 C44 1 -0.094578 0.122709 0.497612 11.00000 0.11640 0.09060 = 0.06668 -0.00936 0.02574 -0.01647 AFIX 43 H44 2 -0.126737 0.100091 0.547020 11.00000 -1.20000 AFIX 0 C45 1 -0.173408 0.132716 0.433902 11.00000 0.08132 0.10204 = 0.08063 -0.01304 0.02662 -0.02707 AFIX 43 H45 2 -0.258299 0.116848 0.440129 11.00000 -1.20000 AFIX 0 C46 1 -0.125161 0.166694 0.360257 11.00000 0.05839 0.08085 = 0.06406 -0.01465 0.00911 -0.01623 AFIX 43 H46 2 -0.176984 0.172731 0.316768 11.00000 -1.20000 AFIX 0 C47 1 0.036408 0.270924 0.147217 11.00000 0.04367 0.05165 = 0.05445 -0.01208 -0.00094 -0.01680 C48 1 -0.026959 0.332302 0.073592 11.00000 0.05882 0.07015 = 0.05944 -0.00640 -0.00539 -0.00959 AFIX 137 H48A 2 -0.023837 0.400334 0.070554 11.00000 -1.50000 H48B 2 -0.123035 0.331847 0.072601 11.00000 -1.50000 H48C 2 0.025049 0.304384 0.030045 11.00000 -1.50000 AFIX 0 C49 1 -0.141921 0.371849 0.230380 11.00000 0.04858 0.06145 = 0.07048 -0.01987 -0.00347 -0.00570 AFIX 137 H49A 2 -0.090393 0.420214 0.227435 11.00000 -1.50000 H49B 2 -0.186252 0.363851 0.281118 11.00000 -1.50000 H49C 2 -0.212510 0.395043 0.191571 11.00000 -1.50000 AFIX 0 O5 4 0.673684 0.919486 0.389975 11.00000 0.13531 0.51433 = 0.15681 -0.12316 0.00437 -0.13665 C50 1 0.566447 0.922452 0.365600 11.00000 0.07760 0.16049 = 0.10722 -0.04883 0.00210 -0.04506 C51 1 0.445315 0.924615 0.417844 11.00000 0.15271 0.23425 = 0.14001 -0.01118 0.04616 -0.08905 AFIX 137 H51A 2 0.474719 0.880917 0.466104 11.00000 -1.50000 H51B 2 0.378687 0.902177 0.394504 11.00000 -1.50000 H51C 2 0.402181 0.992186 0.427583 11.00000 -1.50000 AFIX 0 C52 1 0.549750 0.921024 0.285404 11.00000 0.10448 0.16795 = 0.12625 -0.06609 -0.00806 -0.00138 AFIX 137 H52A 2 0.581487 0.973710 0.253652 11.00000 -1.50000 H52B 2 0.452223 0.931383 0.276324 11.00000 -1.50000 H52C 2 0.604312 0.857017 0.272314 11.00000 -1.50000 AFIX 0 HKLF 4 REM SKF-01_0m in P-1 REM R1 = 0.0566 for 6124 Fo > 4sig(Fo) and 0.1032 for all 10681 data REM 627 parameters refined using 0 restraints END WGHT 0.0807 0.0276 REM Highest difference peak 0.469, deepest hole -0.297, 1-sigma level 0.044 Q1 1 0.5861 0.8500 0.5704 11.00000 0.05 0.47 ; _shelx_res_checksum 66601 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