#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 13 _journal_issue 4 _journal_year 2022 _journal_page_first 387 _journal_page_last 392 #============================================================================= data_ss-401 _audit_creation_date 2016-12-08 _audit_creation_method ; Olex2 1.2-alpha (compiled 2016.01.25 svn.r3250 for OlexSys, GUI svn.r5148) ; _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C17 H13 N4 O8 V2, C3 H12 Li N O4, H7 Li O4, C3 H7 N O' _chemical_formula_sum 'C23 H39 Li2 N6 O17 V2' _chemical_formula_weight 787.36 _chemical_melting_point ? _chemical_oxdiff_formula C23H25O8N6V2 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' 'Li' 'Li' -0.0003 0.0001 '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' 'V' 'V' 0.3005 0.5294 '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 10.8273(5) _cell_length_b 11.4677(6) _cell_length_c 15.0366(8) _cell_angle_alpha 81.591(4) _cell_angle_beta 83.018(4) _cell_angle_gamma 76.326(4) _cell_volume 1787.23(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4082 _cell_measurement_temperature 292.5(2) _cell_measurement_theta_max 28.3420 _cell_measurement_theta_min 3.2650 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'metallic light brown' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 814 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_unetI/netI 0.0506 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.837 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 11730 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.837 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.031 _diffrn_reflns_theta_min 3.118 _diffrn_ambient_environment air _diffrn_ambient_temperature 292.5(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0640 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.837 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -51.00 44.00 1.00 3.30 -- 19.77 -37.00 -60.00 95 2 \w -17.00 22.00 1.00 3.30 -- -17.51 -99.00 90.00 39 3 \w -6.00 86.00 1.00 3.30 -- 19.77 37.00 120.00 92 4 \w -88.00 13.00 1.00 3.30 -- -17.51 -77.00-150.00 101 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0524928000 _diffrn_orient_matrix_UB_12 -0.0167353000 _diffrn_orient_matrix_UB_13 0.0276087000 _diffrn_orient_matrix_UB_21 0.0065915000 _diffrn_orient_matrix_UB_22 0.0372026000 _diffrn_orient_matrix_UB_23 0.0321019000 _diffrn_orient_matrix_UB_31 -0.0422401000 _diffrn_orient_matrix_UB_32 0.0494879000 _diffrn_orient_matrix_UB_33 -0.0223556000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6252 _reflns_number_total 7981 _reflns_odcompleteness_completeness 99.15 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _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 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.630 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.061 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 481 _refine_ls_number_reflns 7981 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0496 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.7851P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1151 _refine_ls_wR_factor_ref 0.1255 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2.a Free rotating group: O11(H11A), O16(H16A,H16B), O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O12(H12) 2.b Secondary CH2 refined with riding coordinates: C9(H9A,H9B) 2.c Aromatic/amide H refined with riding coordinates: N3(H3), C11(H11), C7(H7), C14(H14), C5(H5), C17(H17), C4(H4), C2(H2), C15(H15), C16(H16), C20(H20), C3(H3A), C23(H23) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C19(H19A,H19B, H19C) ; _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 V1 V 0.26660(4) 0.80845(4) 0.54811(3) 0.02512(11) Uani 1 1 d . . . . . V2 V 0.27461(4) 0.71956(4) 0.13965(3) 0.02886(12) Uani 1 1 d . . . . . O1 O 0.29610(17) 0.94815(15) 0.58908(13) 0.0344(4) Uani 1 1 d . . . . . O2 O 0.30895(17) 0.69065(16) 0.45933(12) 0.0346(4) Uani 1 1 d . . . . . O11 O 0.77580(18) 0.48613(17) 0.24237(13) 0.0374(4) Uani 1 1 d . . . . . H11A H 0.7787 0.4143 0.2673 0.056 Uiso 1 1 d G . . . . O6 O 0.29116(17) 0.68889(17) 0.01643(12) 0.0352(4) Uani 1 1 d . . . . . O5 O 0.31368(17) 0.64982(18) 0.26392(12) 0.0394(5) Uani 1 1 d . . . . . O3 O 0.13237(18) 0.87626(17) 0.50620(13) 0.0397(5) Uani 1 1 d . . . . . N4 N 0.47128(19) 0.63000(18) 0.13195(13) 0.0265(4) Uani 1 1 d . . . . . O4 O 0.2381(2) 0.72353(17) 0.64006(12) 0.0420(5) Uani 1 1 d . . . . . O16 O 0.1074(2) 1.14928(17) 0.53639(17) 0.0495(5) Uani 1 1 d . . . . . H16A H 0.0393 1.1301 0.5272 0.074 Uiso 1 1 d G . . . . H16B H 0.1609 1.0861 0.5554 0.074 Uiso 1 1 d G . . . . N2 N 0.5216(2) 0.68320(18) 0.45991(13) 0.0286(4) Uani 1 1 d . . . . . N3 N 0.5213(2) 0.58590(19) 0.21466(13) 0.0297(5) Uani 1 1 d . . . . . H3 H 0.6004 0.5547 0.2219 0.036 Uiso 1 1 calc R . . . . N1 N 0.47038(19) 0.77350(17) 0.51620(13) 0.0255(4) Uani 1 1 d . . . . . O13 O 0.0529(2) 0.4965(2) 0.15485(15) 0.0520(6) Uani 1 1 d . . . . . H13A H 0.0789 0.5543 0.1705 0.078 Uiso 1 1 d G . . . . H13B H 0.0772 0.4326 0.1905 0.078 Uiso 1 1 d G . . . . O14 O 0.1264(2) 0.5584(2) -0.03061(15) 0.0563(6) Uani 1 1 d . . . . . H14A H 0.1757 0.5993 -0.0168 0.084 Uiso 1 1 d G . . . . H14B H 0.0662 0.6055 -0.0581 0.084 Uiso 1 1 d G . . . . O7 O 0.2758(2) 0.85940(18) 0.13550(14) 0.0510(6) Uani 1 1 d . . . . . O8 O 0.12790(19) 0.7014(2) 0.16497(14) 0.0486(5) Uani 1 1 d . . . . . O17 O 0.0915(2) 0.6463(2) 0.38529(16) 0.0538(6) Uani 1 1 d . . . . . H17A H 0.0995 0.6698 0.3291 0.081 Uiso 1 1 d G . . . . H17B H 0.1524 0.6595 0.4102 0.081 Uiso 1 1 d G . . . . O15 O 0.7897(2) 0.6458(3) 0.3747(2) 0.0599(7) Uani 1 1 d . . . . . O10 O 0.8061(3) 0.6932(2) 0.09302(19) 0.0677(7) Uani 1 1 d . . . . . C10 C 0.4303(2) 0.5994(2) 0.27835(16) 0.0270(5) Uani 1 1 d . . . . . O9 O 0.0947(3) 0.3032(2) 0.28451(16) 0.0649(7) Uani 1 1 d . . . . . C8 C 0.4280(2) 0.6469(2) 0.43519(15) 0.0261(5) Uani 1 1 d . . . . . C12 C 0.5158(3) 0.6538(2) -0.02920(17) 0.0319(6) Uani 1 1 d . . . . . C6 C 0.5204(2) 0.9137(2) 0.60230(16) 0.0297(5) Uani 1 1 d . . . . . O12 O 0.1130(3) 0.3944(2) 0.44049(17) 0.0789(9) Uani 1 1 d . . . . . H12 H 0.1065 0.3809 0.3874 0.118 Uiso 1 1 d G . . . . C11 C 0.5511(2) 0.6180(2) 0.06160(17) 0.0310(6) Uani 1 1 d . . . . . H11 H 0.6365 0.5844 0.0698 0.037 Uiso 1 1 calc R . . . . N5 N 0.0619(3) 0.1304(2) 0.24594(18) 0.0508(7) Uani 1 1 d . . . . . C13 C 0.3875(3) 0.6871(2) -0.04832(17) 0.0307(5) Uani 1 1 d . . . . . N6 N 0.7774(3) 0.8951(2) 0.07230(19) 0.0564(7) Uani 1 1 d . . . . . C7 C 0.5533(2) 0.8197(2) 0.54561(16) 0.0292(5) Uani 1 1 d . . . . . H7 H 0.6392 0.7899 0.5288 0.035 Uiso 1 1 calc R . . . . C1 C 0.3928(3) 0.9736(2) 0.62324(16) 0.0303(5) Uani 1 1 d . . . . . C9 C 0.4589(3) 0.5499(2) 0.37349(16) 0.0311(6) Uani 1 1 d . . . . . H9A H 0.5487 0.5107 0.3740 0.037 Uiso 1 1 calc R . . . . H9B H 0.4098 0.4894 0.3959 0.037 Uiso 1 1 calc R . . . . C14 C 0.3610(3) 0.7123(2) -0.13861(18) 0.0395(7) Uani 1 1 d . . . . . H14 H 0.2767 0.7323 -0.1527 0.047 Uiso 1 1 calc R . . . . C5 C 0.6188(3) 0.9503(3) 0.6362(2) 0.0427(7) Uani 1 1 d . . . . . H5 H 0.7033 0.9122 0.6218 0.051 Uiso 1 1 calc R . . . . C17 C 0.6125(3) 0.6492(3) -0.10026(19) 0.0457(7) Uani 1 1 d . . . . . H17 H 0.6974 0.6265 -0.0875 0.055 Uiso 1 1 calc R . . . . C4 C 0.5923(3) 1.0409(3) 0.6901(2) 0.0515(8) Uani 1 1 d . . . . . H4 H 0.6582 1.0639 0.7124 0.062 Uiso 1 1 calc R . . . . C2 C 0.3680(3) 1.0653(3) 0.67881(19) 0.0410(7) Uani 1 1 d . . . . . H2 H 0.2842 1.1046 0.6941 0.049 Uiso 1 1 calc R . . . . C15 C 0.4577(3) 0.7078(3) -0.20664(19) 0.0469(8) Uani 1 1 d . . . . . H15 H 0.4377 0.7255 -0.2663 0.056 Uiso 1 1 calc R . . . . C16 C 0.5843(3) 0.6777(3) -0.1887(2) 0.0509(8) Uani 1 1 d . . . . . H16 H 0.6491 0.6768 -0.2354 0.061 Uiso 1 1 calc R . . . . C20 C 0.0623(3) 0.2055(3) 0.3029(2) 0.0510(8) Uani 1 1 d . . . . . H20 H 0.0358 0.1837 0.3629 0.061 Uiso 1 1 calc R . . . . C3 C 0.4674(4) 1.0979(3) 0.7112(2) 0.0505(8) Uani 1 1 d . . . . . H3A H 0.4497 1.1594 0.7480 0.061 Uiso 1 1 calc R . . . . C23 C 0.8420(3) 0.7848(3) 0.0957(2) 0.0550(9) Uani 1 1 d . . . . . H23 H 0.9218 0.7763 0.1159 0.066 Uiso 1 1 calc R . . . . C18 C 0.0244(5) 0.0167(4) 0.2763(3) 0.0802(13) Uani 1 1 d . . . . . H18A H 0.0284 -0.0018 0.3404 0.120 Uiso 1 1 calc GR . . . . H18B H 0.0813 -0.0465 0.2466 0.120 Uiso 1 1 calc GR . . . . H18C H -0.0612 0.0233 0.2620 0.120 Uiso 1 1 calc GR . . . . C21 C 0.6513(4) 0.9188(4) 0.0429(3) 0.0805(13) Uani 1 1 d . . . . . H21A H 0.6219 0.8450 0.0509 0.121 Uiso 1 1 calc GR . . . . H21B H 0.6535 0.9511 -0.0198 0.121 Uiso 1 1 calc GR . . . . H21C H 0.5943 0.9763 0.0779 0.121 Uiso 1 1 calc GR . . . . C22 C 0.8281(6) 0.9975(4) 0.0799(4) 0.111(2) Uani 1 1 d . . . . . H22A H 0.7765 1.0429 0.1252 0.167 Uiso 1 1 calc GR . . . . H22B H 0.8278 1.0479 0.0230 0.167 Uiso 1 1 calc GR . . . . H22C H 0.9140 0.9703 0.0965 0.167 Uiso 1 1 calc GR . . . . C19 C 0.0980(6) 0.1588(4) 0.1508(3) 0.105(2) Uani 1 1 d . . . . . H19A H 0.0241 0.2024 0.1212 0.158 Uiso 1 1 calc GR . . . . H19B H 0.1337 0.0852 0.1246 0.158 Uiso 1 1 calc GR . . . . H19C H 0.1603 0.2076 0.1434 0.158 Uiso 1 1 calc GR . . . . H15A H 0.775(6) 0.607(5) 0.432(5) 0.15(3) Uiso 1 1 d . . . . . H15B H 0.794(5) 0.593(5) 0.342(4) 0.12(2) Uiso 1 1 d . . . . . Li1 Li 0.8770(5) 0.5260(4) 0.1324(3) 0.0411(11) Uani 1 1 d . . . . . Li2 Li 0.0862(5) 0.3134(4) 0.5606(4) 0.0453(12) Uani 1 1 d . . . . . 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 V1 0.0216(2) 0.0279(2) 0.0256(2) -0.00285(17) -0.00259(16) -0.00490(16) V2 0.0264(2) 0.0334(2) 0.0267(2) -0.00574(18) -0.00535(17) -0.00367(17) O1 0.0258(9) 0.0328(9) 0.0466(11) -0.0134(8) -0.0041(8) -0.0051(7) O2 0.0248(9) 0.0430(10) 0.0392(10) -0.0176(8) -0.0024(8) -0.0065(8) O11 0.0356(11) 0.0384(10) 0.0360(11) 0.0014(9) -0.0026(8) -0.0077(8) O6 0.0307(10) 0.0491(11) 0.0290(9) -0.0093(8) -0.0077(8) -0.0096(8) O5 0.0296(10) 0.0587(12) 0.0242(9) -0.0018(9) -0.0014(7) -0.0009(9) O3 0.0294(10) 0.0419(11) 0.0472(12) -0.0091(9) -0.0111(8) -0.0007(8) N4 0.0285(11) 0.0306(11) 0.0225(10) -0.0034(8) -0.0071(8) -0.0077(8) O4 0.0505(13) 0.0409(11) 0.0333(10) 0.0011(9) 0.0014(9) -0.0142(9) O16 0.0420(12) 0.0315(10) 0.0772(16) -0.0069(11) -0.0186(11) -0.0058(9) N2 0.0277(11) 0.0304(11) 0.0265(11) -0.0049(9) -0.0013(8) -0.0040(9) N3 0.0256(11) 0.0374(11) 0.0243(10) -0.0027(9) -0.0071(8) -0.0018(9) N1 0.0253(10) 0.0278(10) 0.0231(10) -0.0027(8) -0.0021(8) -0.0058(8) O13 0.0446(13) 0.0656(14) 0.0502(13) -0.0019(11) -0.0098(10) -0.0213(12) O14 0.0544(15) 0.0825(17) 0.0439(13) -0.0192(12) -0.0013(10) -0.0332(13) O7 0.0695(16) 0.0360(11) 0.0477(13) -0.0072(9) -0.0107(11) -0.0081(10) O8 0.0279(11) 0.0749(15) 0.0446(12) -0.0098(11) -0.0049(9) -0.0124(10) O17 0.0423(13) 0.0622(14) 0.0626(14) -0.0224(12) 0.0117(11) -0.0223(11) O15 0.0432(14) 0.0737(17) 0.0722(19) -0.0362(16) -0.0037(12) -0.0158(12) O10 0.0675(17) 0.0432(13) 0.094(2) 0.0090(13) -0.0256(15) -0.0166(12) C10 0.0304(13) 0.0250(12) 0.0262(12) -0.0051(10) -0.0043(10) -0.0056(10) O9 0.0851(19) 0.0598(15) 0.0525(14) -0.0074(12) -0.0072(13) -0.0208(14) C8 0.0292(13) 0.0287(12) 0.0190(11) 0.0011(10) -0.0031(9) -0.0058(10) C12 0.0369(15) 0.0380(14) 0.0231(12) -0.0028(11) -0.0037(10) -0.0130(11) C6 0.0344(14) 0.0320(13) 0.0244(12) 0.0012(10) -0.0077(10) -0.0111(11) O12 0.143(3) 0.0526(15) 0.0478(15) -0.0058(12) -0.0082(17) -0.0353(16) C11 0.0247(13) 0.0415(14) 0.0279(13) -0.0051(11) -0.0035(10) -0.0085(11) N5 0.0550(17) 0.0558(16) 0.0404(14) -0.0082(13) 0.0061(12) -0.0139(13) C13 0.0382(15) 0.0310(13) 0.0263(13) -0.0046(10) -0.0053(11) -0.0128(11) N6 0.070(2) 0.0407(15) 0.0553(17) 0.0031(13) -0.0203(15) -0.0040(13) C7 0.0231(12) 0.0354(13) 0.0288(13) -0.0001(11) -0.0039(10) -0.0070(10) C1 0.0372(14) 0.0309(13) 0.0248(12) 0.0001(10) -0.0052(10) -0.0126(11) C9 0.0352(14) 0.0310(13) 0.0240(12) -0.0013(10) -0.0033(10) -0.0023(11) C14 0.0475(17) 0.0410(15) 0.0323(15) 0.0001(12) -0.0140(13) -0.0115(13) C5 0.0402(16) 0.0502(17) 0.0427(16) -0.0035(14) -0.0152(13) -0.0151(13) C17 0.0392(17) 0.066(2) 0.0331(15) -0.0044(14) 0.0022(12) -0.0186(15) C4 0.061(2) 0.057(2) 0.0480(18) -0.0095(16) -0.0196(16) -0.0268(17) C2 0.0520(18) 0.0364(15) 0.0364(15) -0.0080(12) -0.0017(13) -0.0124(13) C15 0.067(2) 0.0537(18) 0.0236(14) 0.0024(13) -0.0101(14) -0.0224(16) C16 0.058(2) 0.070(2) 0.0274(15) -0.0002(14) 0.0039(13) -0.0276(17) C20 0.0450(19) 0.067(2) 0.0358(17) -0.0006(16) -0.0013(13) -0.0070(16) C3 0.077(2) 0.0467(18) 0.0372(16) -0.0120(14) -0.0091(16) -0.0254(17) C23 0.055(2) 0.0466(19) 0.065(2) 0.0018(16) -0.0248(17) -0.0080(15) C18 0.094(3) 0.075(3) 0.077(3) -0.013(2) 0.017(2) -0.039(2) C21 0.059(3) 0.084(3) 0.081(3) 0.018(2) -0.016(2) 0.005(2) C22 0.158(6) 0.053(2) 0.138(5) -0.004(3) -0.066(4) -0.030(3) C19 0.195(6) 0.081(3) 0.043(2) -0.012(2) 0.024(3) -0.054(3) Li1 0.041(3) 0.048(3) 0.034(2) -0.002(2) -0.005(2) -0.011(2) Li2 0.042(3) 0.042(3) 0.052(3) -0.008(2) -0.002(2) -0.010(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 V1 O1 1.9042(18) . ? V1 O2 1.9757(18) . ? V1 O3 1.6306(18) . ? V1 O4 1.6125(18) . ? V1 N1 2.154(2) . ? V2 O6 1.9154(18) . ? V2 O5 1.9761(18) . ? V2 N4 2.132(2) . ? V2 O7 1.599(2) . ? V2 O8 1.642(2) . ? O1 C1 1.328(3) . ? O2 C8 1.295(3) . ? O11 H11A 0.8488 . ? O11 Li1 1.929(5) . ? O6 C13 1.336(3) . ? O5 C10 1.289(3) . ? N4 N3 1.395(3) . ? N4 C11 1.284(3) . ? O16 H16A 0.8499 . ? O16 H16B 0.8501 . ? O16 Li2 1.925(5) 1_565 ? N2 N1 1.402(3) . ? N2 C8 1.294(3) . ? N3 H3 0.8600 . ? N3 C10 1.286(3) . ? N1 C7 1.293(3) . ? O13 H13A 0.8510 . ? O13 H13B 0.8496 . ? O13 Li1 1.917(5) 1_455 ? O14 H14A 0.8498 . ? O14 H14B 0.8497 . ? O14 Li1 1.934(5) 2_665 ? O17 H17A 0.8492 . ? O17 H17B 0.8497 . ? O17 Li2 1.971(6) 2_566 ? O15 H15A 0.93(7) . ? O15 H15B 0.83(6) . ? O15 Li2 1.929(6) 2_666 ? O10 C23 1.210(4) . ? O10 Li1 1.923(5) . ? C10 C9 1.501(3) . ? O9 C20 1.234(4) . ? C8 C9 1.503(3) . ? C12 C11 1.438(3) . ? C12 C13 1.404(4) . ? C12 C17 1.400(4) . ? C6 C7 1.424(4) . ? C6 C1 1.410(4) . ? C6 C5 1.406(4) . ? O12 H12 0.8495 . ? O12 Li2 1.928(6) . ? C11 H11 0.9300 . ? N5 C20 1.301(4) . ? N5 C18 1.451(4) . ? N5 C19 1.447(4) . ? C13 C14 1.396(4) . ? N6 C23 1.313(4) . ? N6 C21 1.439(5) . ? N6 C22 1.432(5) . ? C7 H7 0.9300 . ? C1 C2 1.394(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C14 H14 0.9300 . ? C14 C15 1.369(4) . ? C5 H5 0.9300 . ? C5 C4 1.366(4) . ? C17 H17 0.9300 . ? C17 C16 1.376(4) . ? C4 H4 0.9300 . ? C4 C3 1.376(5) . ? C2 H2 0.9300 . ? C2 C3 1.381(4) . ? C15 H15 0.9300 . ? C15 C16 1.382(5) . ? C16 H16 0.9300 . ? C20 H20 0.9300 . ? C3 H3A 0.9300 . ? C23 H23 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Li1 O13 1.917(5) 1_655 ? Li1 O14 1.934(5) 2_665 ? Li2 O16 1.925(5) 1_545 ? Li2 O17 1.971(6) 2_566 ? Li2 O15 1.929(6) 2_666 ? 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 O1 V1 O2 148.87(8) . . ? O1 V1 N1 82.01(8) . . ? O2 V1 N1 73.14(7) . . ? O3 V1 O1 95.72(9) . . ? O3 V1 O2 92.74(9) . . ? O3 V1 N1 142.18(9) . . ? O4 V1 O1 103.77(9) . . ? O4 V1 O2 101.49(9) . . ? O4 V1 O3 109.44(11) . . ? O4 V1 N1 107.73(9) . . ? O6 V2 O5 145.19(8) . . ? O6 V2 N4 82.41(8) . . ? O5 V2 N4 73.29(8) . . ? O7 V2 O6 105.43(10) . . ? O7 V2 O5 104.49(10) . . ? O7 V2 N4 104.31(10) . . ? O7 V2 O8 109.50(12) . . ? O8 V2 O6 97.14(9) . . ? O8 V2 O5 89.25(9) . . ? O8 V2 N4 144.92(10) . . ? C1 O1 V1 134.79(16) . . ? C8 O2 V1 118.68(16) . . ? Li1 O11 H11A 123.5 . . ? C13 O6 V2 131.93(16) . . ? C10 O5 V2 118.64(16) . . ? N3 N4 V2 115.46(15) . . ? C11 N4 V2 128.39(17) . . ? C11 N4 N3 116.0(2) . . ? H16A O16 H16B 109.5 . . ? Li2 O16 H16A 114.9 1_565 . ? Li2 O16 H16B 129.4 1_565 . ? C8 N2 N1 108.1(2) . . ? N4 N3 H3 125.4 . . ? C10 N3 N4 109.2(2) . . ? C10 N3 H3 125.4 . . ? N2 N1 V1 115.79(15) . . ? C7 N1 V1 128.93(17) . . ? C7 N1 N2 115.2(2) . . ? H13A O13 H13B 109.4 . . ? Li1 O13 H13A 117.5 1_455 . ? Li1 O13 H13B 113.6 1_455 . ? H14A O14 H14B 109.4 . . ? Li1 O14 H14A 134.5 2_665 . ? Li1 O14 H14B 78.1 2_665 . ? H17A O17 H17B 109.5 . . ? Li2 O17 H17A 113.3 2_566 . ? Li2 O17 H17B 121.3 2_566 . ? H15A O15 H15B 103(5) . . ? Li2 O15 H15A 78(4) 2_666 . ? Li2 O15 H15B 133(4) 2_666 . ? C23 O10 Li1 132.3(3) . . ? O5 C10 C9 118.0(2) . . ? N3 C10 O5 122.9(2) . . ? N3 C10 C9 119.1(2) . . ? O2 C8 C9 118.1(2) . . ? N2 C8 O2 123.8(2) . . ? N2 C8 C9 118.2(2) . . ? C13 C12 C11 121.7(2) . . ? C17 C12 C11 118.7(2) . . ? C17 C12 C13 119.5(2) . . ? C1 C6 C7 122.1(2) . . ? C5 C6 C7 118.8(3) . . ? C5 C6 C1 119.0(2) . . ? Li2 O12 H12 135.7 . . ? N4 C11 C12 123.7(2) . . ? N4 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C20 N5 C18 120.8(3) . . ? C20 N5 C19 120.8(3) . . ? C19 N5 C18 118.5(3) . . ? O6 C13 C12 122.3(2) . . ? O6 C13 C14 119.3(2) . . ? C14 C13 C12 118.3(2) . . ? C23 N6 C21 122.0(3) . . ? C23 N6 C22 120.7(3) . . ? C22 N6 C21 117.3(3) . . ? N1 C7 C6 123.7(2) . . ? N1 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? O1 C1 C6 121.9(2) . . ? O1 C1 C2 119.1(2) . . ? C2 C1 C6 118.9(2) . . ? C10 C9 C8 112.2(2) . . ? C10 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C13 C14 H14 119.6 . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C6 C5 H5 119.5 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.5 . . ? C12 C17 H17 119.4 . . ? C16 C17 C12 121.2(3) . . ? C16 C17 H17 119.4 . . ? C5 C4 H4 120.2 . . ? C5 C4 C3 119.6(3) . . ? C3 C4 H4 120.2 . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C14 C15 H15 119.3 . . ? C14 C15 C16 121.5(3) . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 118.6(3) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? O9 C20 N5 126.0(3) . . ? O9 C20 H20 117.0 . . ? N5 C20 H20 117.0 . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? O10 C23 N6 125.4(3) . . ? O10 C23 H23 117.3 . . ? N6 C23 H23 117.3 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 H22A 109.5 . . ? N6 C22 H22B 109.5 . . ? N6 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O11 Li1 O14 117.6(3) . 2_665 ? O13 Li1 O11 109.9(2) 1_655 . ? O13 Li1 O14 106.0(3) 1_655 2_665 ? O13 Li1 O10 112.9(3) 1_655 . ? O10 Li1 O11 105.6(3) . . ? O10 Li1 O14 105.0(2) . 2_665 ? O16 Li2 O17 103.2(3) 1_545 2_566 ? O16 Li2 O15 119.4(3) 1_545 2_666 ? O16 Li2 O12 101.2(3) 1_545 . ? O15 Li2 O17 115.1(3) 2_666 2_566 ? O12 Li2 O17 114.1(3) . 2_566 ? O12 Li2 O15 103.3(3) . 2_666 ? 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 V1 O1 C1 C6 28.1(4) . . . . ? V1 O1 C1 C2 -154.3(2) . . . . ? V1 O2 C8 N2 -6.1(3) . . . . ? V1 O2 C8 C9 175.10(15) . . . . ? V1 N1 C7 C6 -5.1(3) . . . . ? V2 O6 C13 C12 30.5(4) . . . . ? V2 O6 C13 C14 -153.3(2) . . . . ? V2 O5 C10 N3 -4.3(3) . . . . ? V2 O5 C10 C9 178.32(16) . . . . ? V2 N4 N3 C10 6.7(2) . . . . ? V2 N4 C11 C12 -7.3(4) . . . . ? O1 C1 C2 C3 -176.5(2) . . . . ? O2 C8 C9 C10 74.0(3) . . . . ? O6 C13 C14 C15 -178.1(3) . . . . ? O5 C10 C9 C8 -62.1(3) . . . . ? N4 N3 C10 O5 -2.0(3) . . . . ? N4 N3 C10 C9 175.4(2) . . . . ? N2 N1 C7 C6 178.9(2) . . . . ? N2 C8 C9 C10 -104.8(3) . . . . ? N3 N4 C11 C12 177.5(2) . . . . ? N3 C10 C9 C8 120.4(3) . . . . ? N1 N2 C8 O2 0.8(3) . . . . ? N1 N2 C8 C9 179.61(19) . . . . ? C8 N2 N1 V1 4.2(2) . . . . ? C8 N2 N1 C7 -179.3(2) . . . . ? C12 C13 C14 C15 -1.8(4) . . . . ? C12 C17 C16 C15 -1.9(5) . . . . ? C6 C1 C2 C3 1.2(4) . . . . ? C6 C5 C4 C3 -0.3(5) . . . . ? C11 N4 N3 C10 -177.4(2) . . . . ? C11 C12 C13 O6 0.8(4) . . . . ? C11 C12 C13 C14 -175.4(2) . . . . ? C11 C12 C17 C16 177.4(3) . . . . ? C13 C12 C11 N4 -10.3(4) . . . . ? C13 C12 C17 C16 0.6(5) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C7 C6 C1 O1 -2.0(4) . . . . ? C7 C6 C1 C2 -179.6(2) . . . . ? C7 C6 C5 C4 179.3(3) . . . . ? C1 C6 C7 N1 -7.1(4) . . . . ? C1 C6 C5 C4 1.2(4) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? C14 C15 C16 C17 1.4(5) . . . . ? C5 C6 C7 N1 174.9(2) . . . . ? C5 C6 C1 O1 176.0(2) . . . . ? C5 C6 C1 C2 -1.6(4) . . . . ? C5 C4 C3 C2 -0.1(5) . . . . ? C17 C12 C11 N4 172.9(3) . . . . ? C17 C12 C13 O6 177.5(2) . . . . ? C17 C12 C13 C14 1.3(4) . . . . ? C18 N5 C20 O9 178.6(4) . . . . ? C21 N6 C23 O10 2.1(6) . . . . ? C22 N6 C23 O10 178.7(4) . . . . ? C19 N5 C20 O9 -1.9(6) . . . . ? Li1 O10 C23 N6 -174.2(3) . . . . ? _shelx_res_file ; ss-401.res created by SHELXL-2014/7 TITL ss-401_a.res in P-1 REM Old TITL SS-401 in P-1 REM SHELXT solution in P-1 REM R1 0.151, Rweak 0.017, Alpha 0.085, Orientation as input REM Formula found by SHELXT: C26 N12 O10 V2 CELL 0.71073 10.827284 11.46769 15.036639 81.5915 83.0179 76.3263 ZERR 2 0.000534 0.000585 0.000795 0.0043 0.0042 0.0043 LATT 1 SFAC C H Li N O V UNIT 46 78 4 12 34 4 L.S. 6 PLAN 20 TEMP 17.49 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 OMIT -1 3 0 OMIT -2 -2 3 OMIT 3 1 1 REM REM REM WGHT 0.054700 0.785100 FVAR 0.49787 V1 6 0.266598 0.808454 0.548109 11.00000 0.02157 0.02791 = 0.02558 -0.00285 -0.00259 -0.00490 V2 6 0.274609 0.719562 0.139652 11.00000 0.02638 0.03337 = 0.02672 -0.00574 -0.00535 -0.00367 O1 5 0.296098 0.948147 0.589076 11.00000 0.02582 0.03275 = 0.04661 -0.01340 -0.00409 -0.00507 O2 5 0.308950 0.690647 0.459328 11.00000 0.02481 0.04296 = 0.03924 -0.01763 -0.00242 -0.00651 AFIX 6 O11 5 0.775801 0.486135 0.242366 11.00000 0.03555 0.03837 = 0.03597 0.00144 -0.00263 -0.00766 H11A 2 0.778719 0.414284 0.267265 11.00000 -1.50000 AFIX 0 O6 5 0.291163 0.688891 0.016432 11.00000 0.03069 0.04906 = 0.02897 -0.00926 -0.00769 -0.00964 O5 5 0.313676 0.649817 0.263915 11.00000 0.02960 0.05872 = 0.02421 -0.00183 -0.00141 -0.00086 O3 5 0.132375 0.876260 0.506198 11.00000 0.02940 0.04186 = 0.04722 -0.00909 -0.01111 -0.00065 N4 4 0.471279 0.629999 0.131947 11.00000 0.02846 0.03056 = 0.02246 -0.00341 -0.00708 -0.00769 O4 5 0.238050 0.723535 0.640059 11.00000 0.05052 0.04095 = 0.03334 0.00112 0.00144 -0.01418 AFIX 6 O16 5 0.107432 1.149281 0.536392 11.00000 0.04198 0.03148 = 0.07723 -0.00685 -0.01859 -0.00580 H16A 2 0.039275 1.130118 0.527190 11.00000 -1.50000 H16B 2 0.160924 1.086133 0.555363 11.00000 -1.50000 AFIX 0 N2 4 0.521553 0.683200 0.459907 11.00000 0.02769 0.03040 = 0.02649 -0.00490 -0.00129 -0.00404 N3 4 0.521278 0.585900 0.214662 11.00000 0.02560 0.03742 = 0.02433 -0.00275 -0.00714 -0.00182 AFIX 43 H3 2 0.600364 0.554683 0.221907 11.00000 -1.20000 AFIX 0 N1 4 0.470375 0.773500 0.516197 11.00000 0.02533 0.02782 = 0.02312 -0.00269 -0.00213 -0.00581 AFIX 6 O13 5 0.052914 0.496452 0.154849 11.00000 0.04459 0.06563 = 0.05017 -0.00192 -0.00977 -0.02127 H13A 2 0.078930 0.554262 0.170493 11.00000 -1.50000 H13B 2 0.077170 0.432572 0.190530 11.00000 -1.50000 AFIX 6 O14 5 0.126365 0.558377 -0.030615 11.00000 0.05438 0.08246 = 0.04390 -0.01918 -0.00134 -0.03320 H14A 2 0.175679 0.599272 -0.016784 11.00000 -1.50000 H14B 2 0.066152 0.605494 -0.058137 11.00000 -1.50000 AFIX 0 O7 5 0.275796 0.859400 0.135502 11.00000 0.06948 0.03600 = 0.04771 -0.00717 -0.01074 -0.00811 O8 5 0.127904 0.701440 0.164965 11.00000 0.02787 0.07493 = 0.04458 -0.00984 -0.00491 -0.01237 AFIX 6 O17 5 0.091499 0.646252 0.385287 11.00000 0.04229 0.06222 = 0.06258 -0.02239 0.01166 -0.02229 H17A 2 0.099485 0.669831 0.329087 11.00000 -1.50000 H17B 2 0.152397 0.659548 0.410151 11.00000 -1.50000 AFIX 0 O15 5 0.789750 0.645771 0.374671 11.00000 0.04325 0.07371 = 0.07218 -0.03624 -0.00367 -0.01579 O10 5 0.806115 0.693234 0.093021 11.00000 0.06754 0.04323 = 0.09379 0.00904 -0.02559 -0.01660 C10 1 0.430275 0.599362 0.278355 11.00000 0.03045 0.02504 = 0.02623 -0.00510 -0.00433 -0.00564 O9 5 0.094697 0.303157 0.284512 11.00000 0.08507 0.05978 = 0.05252 -0.00736 -0.00722 -0.02077 C8 1 0.427972 0.646854 0.435186 11.00000 0.02924 0.02869 = 0.01901 0.00112 -0.00313 -0.00576 C12 1 0.515791 0.653806 -0.029196 11.00000 0.03690 0.03795 = 0.02306 -0.00276 -0.00368 -0.01297 C6 1 0.520437 0.913716 0.602300 11.00000 0.03445 0.03199 = 0.02443 0.00122 -0.00765 -0.01107 AFIX 6 O12 5 0.112992 0.394411 0.440486 11.00000 0.14280 0.05261 = 0.04783 -0.00581 -0.00821 -0.03529 H12 2 0.106518 0.380930 0.387367 11.00000 -1.50000 AFIX 0 C11 1 0.551084 0.618045 0.061600 11.00000 0.02470 0.04147 = 0.02789 -0.00513 -0.00349 -0.00849 AFIX 43 H11 2 0.636506 0.584369 0.069838 11.00000 -1.20000 AFIX 0 N5 4 0.061935 0.130440 0.245937 11.00000 0.05496 0.05584 = 0.04037 -0.00817 0.00612 -0.01388 C13 1 0.387500 0.687110 -0.048319 11.00000 0.03823 0.03098 = 0.02630 -0.00461 -0.00530 -0.01283 N6 4 0.777418 0.895122 0.072298 11.00000 0.06987 0.04070 = 0.05529 0.00306 -0.02026 -0.00399 C7 1 0.553276 0.819710 0.545612 11.00000 0.02306 0.03537 = 0.02875 -0.00015 -0.00395 -0.00705 AFIX 43 H7 2 0.639243 0.789867 0.528798 11.00000 -1.20000 AFIX 0 C1 1 0.392811 0.973615 0.623236 11.00000 0.03723 0.03094 = 0.02482 0.00013 -0.00522 -0.01259 C9 1 0.458946 0.549916 0.373487 11.00000 0.03524 0.03097 = 0.02396 -0.00132 -0.00330 -0.00232 AFIX 23 H9A 2 0.548710 0.510716 0.373950 11.00000 -1.20000 H9B 2 0.409830 0.489375 0.395894 11.00000 -1.20000 AFIX 0 C14 1 0.361031 0.712264 -0.138612 11.00000 0.04746 0.04097 = 0.03226 0.00011 -0.01400 -0.01146 AFIX 43 H14 2 0.276705 0.732266 -0.152702 11.00000 -1.20000 AFIX 0 C5 1 0.618794 0.950311 0.636249 11.00000 0.04023 0.05016 = 0.04266 -0.00348 -0.01516 -0.01514 AFIX 43 H5 2 0.703263 0.912239 0.621804 11.00000 -1.20000 AFIX 0 C17 1 0.612463 0.649212 -0.100260 11.00000 0.03922 0.06625 = 0.03314 -0.00436 0.00218 -0.01864 AFIX 43 H17 2 0.697357 0.626455 -0.087463 11.00000 -1.20000 AFIX 0 C4 1 0.592257 1.040892 0.690108 11.00000 0.06128 0.05689 = 0.04798 -0.00947 -0.01963 -0.02683 AFIX 43 H4 2 0.658201 1.063928 0.712379 11.00000 -1.20000 AFIX 0 C2 1 0.367974 1.065271 0.678806 11.00000 0.05200 0.03637 = 0.03644 -0.00804 -0.00171 -0.01236 AFIX 43 H2 2 0.284205 1.104574 0.694084 11.00000 -1.20000 AFIX 0 C15 1 0.457665 0.707845 -0.206645 11.00000 0.06726 0.05374 = 0.02365 0.00238 -0.01011 -0.02236 AFIX 43 H15 2 0.437683 0.725501 -0.266267 11.00000 -1.20000 AFIX 0 C16 1 0.584264 0.677729 -0.188696 11.00000 0.05780 0.07045 = 0.02744 -0.00024 0.00394 -0.02756 AFIX 43 H16 2 0.649059 0.676759 -0.235433 11.00000 -1.20000 AFIX 0 C20 1 0.062322 0.205540 0.302885 11.00000 0.04496 0.06724 = 0.03580 -0.00057 -0.00130 -0.00702 AFIX 43 H20 2 0.035785 0.183674 0.362910 11.00000 -1.20000 AFIX 0 C3 1 0.467411 1.097878 0.711238 11.00000 0.07670 0.04670 = 0.03717 -0.01197 -0.00905 -0.02541 AFIX 43 H3A 2 0.449676 1.159428 0.748002 11.00000 -1.20000 AFIX 0 C23 1 0.841962 0.784781 0.095680 11.00000 0.05467 0.04659 = 0.06451 0.00182 -0.02480 -0.00802 AFIX 43 H23 2 0.921779 0.776337 0.115945 11.00000 -1.20000 AFIX 0 C18 1 0.024433 0.016741 0.276313 11.00000 0.09434 0.07467 = 0.07659 -0.01272 0.01654 -0.03862 AFIX 137 H18A 2 0.028360 -0.001794 0.340407 11.00000 -1.50000 H18B 2 0.081300 -0.046496 0.246585 11.00000 -1.50000 H18C 2 -0.061176 0.023275 0.262048 11.00000 -1.50000 AFIX 0 C21 1 0.651305 0.918831 0.042886 11.00000 0.05927 0.08443 = 0.08102 0.01838 -0.01634 0.00515 AFIX 137 H21A 2 0.621926 0.844959 0.050898 11.00000 -1.50000 H21B 2 0.653508 0.951102 -0.019760 11.00000 -1.50000 H21C 2 0.594335 0.976253 0.077894 11.00000 -1.50000 AFIX 0 C22 1 0.828124 0.997486 0.079890 11.00000 0.15847 0.05255 = 0.13774 -0.00417 -0.06591 -0.03023 AFIX 137 H22A 2 0.776544 1.042876 0.125239 11.00000 -1.50000 H22B 2 0.827790 1.047885 0.022973 11.00000 -1.50000 H22C 2 0.914022 0.970307 0.096545 11.00000 -1.50000 AFIX 0 C19 1 0.098036 0.158806 0.150808 11.00000 0.19538 0.08112 = 0.04283 -0.01182 0.02402 -0.05371 AFIX 137 H19A 2 0.024070 0.202430 0.121226 11.00000 -1.50000 H19B 2 0.133681 0.085246 0.124641 11.00000 -1.50000 H19C 2 0.160314 0.207567 0.143430 11.00000 -1.50000 AFIX 0 H15A 2 0.774920 0.606785 0.432266 11.00000 0.15307 H15B 2 0.794446 0.592805 0.341891 11.00000 0.11955 LI1 3 0.877007 0.526025 0.132356 11.00000 0.04148 0.04755 = 0.03446 -0.00245 -0.00475 -0.01095 LI2 3 0.086170 0.313433 0.560593 11.00000 0.04182 0.04216 = 0.05233 -0.00843 -0.00168 -0.00991 HKLF 4 REM ss-401_a.res in P-1 REM R1 = 0.0496 for 6252 Fo > 4sig(Fo) and 0.0682 for all 7981 data REM 481 parameters refined using 0 restraints END WGHT 0.0549 0.7416 REM Highest difference peak 0.630, deepest hole -0.513, 1-sigma level 0.061 Q1 1 0.2258 0.6612 0.1397 11.00000 0.05 0.63 Q2 1 0.6944 0.5061 0.2271 11.00000 0.05 0.46 Q3 1 0.6958 0.6528 0.4003 11.00000 0.05 0.40 Q4 1 0.2113 0.8161 0.1548 11.00000 0.05 0.38 Q5 1 0.1011 0.5360 0.0324 11.00000 0.05 0.38 Q6 1 0.1030 0.4812 0.4374 11.00000 0.05 0.33 Q7 1 0.5589 0.9391 0.6119 11.00000 0.05 0.32 Q8 1 0.3187 0.8758 0.5598 11.00000 0.05 0.30 Q9 1 0.2564 0.8936 0.5573 11.00000 0.05 0.30 Q10 1 0.5312 0.6504 0.0149 11.00000 0.05 0.29 Q11 1 0.2844 0.6592 0.1980 11.00000 0.05 0.29 Q12 1 0.2929 0.7226 0.5306 11.00000 0.05 0.29 Q13 1 0.1863 0.7382 0.1731 11.00000 0.05 0.28 Q14 1 0.2753 0.7222 0.5893 11.00000 0.05 0.28 Q15 1 0.4435 0.5947 0.4102 11.00000 0.05 0.27 Q16 1 0.4653 0.6306 0.2557 11.00000 0.05 0.26 Q17 1 0.0228 0.4058 0.4435 11.00000 0.05 0.25 Q18 1 0.2047 0.8735 0.5146 11.00000 0.05 0.25 Q19 1 0.3819 1.0359 0.6286 11.00000 0.05 0.25 Q20 1 0.4533 0.6471 -0.0389 11.00000 0.05 0.25 ; _shelx_res_checksum 4177 _shelx_hkl_file ; 0 0 -3 1156.05 24.06 0 0 -3 1191.64 22.84 0 0 -4 240.87 6.22 0 0 -4 245.16 7.45 0 0 -5 246.44 8.15 0 0 -5 248.89 6.70 0 0 -6 16.74 1.60 0 0 -7 1148.20 24.05 0 0 -7 1114.91 24.31 0 0 -8 153.09 5.95 0 0 -8 151.11 5.71 0 0 -9 3.55 1.08 0 0 -9 3.74 1.11 0 0 -10 827.98 20.05 0 0 10 870.74 24.30 0 0 -11 32.73 2.90 0 0 11 20.48 3.56 0 0 12 571.22 19.94 0 0 -12 549.57 15.48 0 0 -13 182.72 7.87 0 0 13 174.53 10.77 0 0 14 26.97 4.81 0 0 -14 21.62 2.87 0 0 15 21.38 4.43 0 0 16 7.83 3.57 0 0 17 107.44 10.04 0 0 18 14.74 4.90 0 0 19 30.67 6.23 0 -1 18 5.92 4.00 0 -1 17 8.22 3.45 0 -1 16 25.27 5.00 0 -1 15 38.41 5.79 0 -1 14 3.08 2.75 0 -1 13 38.20 5.08 0 1 -13 34.07 2.99 0 1 -12 163.37 6.62 0 -1 12 185.90 10.68 0 1 -11 17.93 2.03 0 -1 11 20.04 3.69 0 1 -10 17.82 1.94 0 -1 10 15.99 3.38 0 1 -10 18.10 2.00 0 1 -9 76.44 3.89 0 1 -9 73.93 3.66 0 1 -8 465.55 11.68 0 1 -8 503.46 12.14 0 1 -7 131.23 4.56 0 1 -7 137.54 4.81 0 1 -6 163.38 4.92 0 1 -6 168.50 5.14 0 1 -5 4.64 0.79 0 1 -5 6.67 1.63 0 1 -5 4.89 0.72 0 1 -4 136.30 5.46 0 1 -4 129.88 3.61 0 1 -3 24.84 2.15 0 -1 -2 2317.16 43.16 0 -1 -3 1028.83 20.78 0 -1 -3 1022.89 20.93 0 1 4 112.54 4.24 0 -1 -4 119.33 4.48 0 -1 -4 124.14 4.32 0 -1 -5 2615.12 51.60 0 1 5 2563.17 50.93 0 -1 -5 2700.54 50.96 0 -1 -6 144.54 5.42 0 -1 -6 140.69 6.01 0 1 6 143.85 5.41 0 -1 -7 474.72 12.48 0 1 7 458.79 13.64 0 -1 -8 20.90 2.30 0 1 8 20.51 2.76 0 1 9 45.68 4.28 0 -1 -9 42.11 3.26 0 -1 -10 168.29 7.15 0 1 10 170.69 8.80 0 -1 -11 19.64 2.59 0 1 11 15.84 2.83 0 1 12 43.02 5.03 0 -1 -12 41.92 3.82 0 1 13 1.70 2.38 0 -1 -13 0.34 1.16 0 1 14 41.01 5.31 0 -1 -14 50.74 4.40 0 1 15 64.77 6.89 0 1 16 50.42 6.41 0 1 17 80.23 8.61 0 1 18 11.18 4.45 0 1 19 8.24 3.57 0 -2 18 27.37 5.99 0 -2 17 6.21 3.12 0 -2 16 87.74 8.88 0 -2 15 76.86 8.03 0 -2 14 3.17 2.41 0 -2 13 93.48 8.03 0 -2 12 70.03 6.66 0 -2 11 121.64 8.36 0 2 -11 118.63 4.69 0 2 -10 55.44 2.91 0 -2 10 65.85 5.78 0 2 -10 60.56 3.22 0 2 -9 12.61 1.41 0 2 -9 14.40 1.43 0 2 -8 1.22 0.60 0 2 -8 0.59 0.59 0 2 -7 875.57 18.14 0 2 -7 902.67 18.23 0 2 -6 875.66 17.47 0 2 -5 463.66 9.49 0 2 -4 1510.26 32.08 0 2 -3 5861.75 109.69 0 2 -2 3817.95 72.03 0 2 -2 4110.96 73.71 0 2 -1 1398.33 26.81 0 -2 1 1348.05 26.60 0 -2 0 2075.46 39.71 0 -2 0 2140.09 38.64 0 2 1 941.86 19.55 0 -2 -1 947.53 19.51 0 -2 -2 15.38 1.47 0 -2 -3 1130.87 23.46 0 2 3 1105.00 21.90 0 -2 -3 1108.81 21.79 0 -2 -4 2277.87 44.01 0 -2 -4 2309.53 45.25 0 2 4 2315.17 44.21 0 2 5 352.73 9.72 0 -2 -5 365.54 10.22 0 2 5 359.26 10.11 0 -2 -5 342.07 9.48 0 2 6 76.26 4.18 0 2 6 84.35 4.37 0 -2 -6 77.63 4.19 0 -2 -6 81.21 4.14 0 -2 -7 67.31 4.03 0 2 7 62.20 4.04 0 -2 -8 7.96 1.74 0 2 8 9.33 2.09 0 2 9 1029.78 26.00 0 -2 -9 1040.77 24.94 0 -2 -10 650.99 17.80 0 2 10 621.18 19.13 0 -2 -11 42.01 3.92 0 2 11 33.97 4.19 0 2 12 285.94 12.79 0 -2 -12 291.25 11.32 0 2 13 1.60 2.23 0 -2 -13 -0.88 1.47 0 -2 -14 69.01 5.65 0 2 14 64.52 6.46 0 -2 -15 15.62 3.16 0 2 15 10.44 3.32 0 2 16 54.50 6.68 0 2 17 19.29 4.54 0 2 18 2.81 2.73 0 2 19 13.70 4.34 0 2 20 62.25 8.20 0 -3 17 7.15 4.33 0 -3 16 8.56 4.01 0 -3 15 32.41 5.71 0 -3 14 44.92 6.17 0 -3 13 2.41 2.50 0 -3 12 6.84 2.60 0 -3 11 24.95 4.51 0 3 -10 252.61 6.54 0 3 -10 250.98 6.64 0 -3 10 266.68 12.40 0 3 -9 7.18 0.88 0 3 -9 7.84 0.85 0 3 -8 236.94 5.62 0 3 -8 239.69 5.98 0 3 -7 75.08 2.73 0 3 -6 5.29 0.75 0 3 -5 3.20 0.63 0 3 -4 1748.17 36.50 0 -3 4 1724.16 36.64 0 3 -4 1714.82 33.09 0 3 -3 2306.14 45.25 0 -3 3 2249.63 45.18 0 3 -3 2220.01 42.81 0 -3 3 2342.30 42.86 0 -3 2 81.45 3.69 0 3 -2 79.27 3.10 0 -3 2 80.29 3.24 0 3 -2 75.29 3.56 0 -3 1 16.69 1.65 0 -3 1 16.62 1.44 0 3 -1 15.17 1.41 0 3 -1 17.45 1.43 0 -3 0 2592.53 50.18 0 3 0 2675.75 48.54 0 -3 0 2601.28 48.52 0 -3 -1 2058.68 40.93 0 3 1 2087.27 41.24 0 3 2 679.02 15.64 0 -3 -2 638.73 15.52 0 -3 -3 236.25 5.42 0 3 3 249.60 5.57 0 -3 -3 242.43 7.83 0 3 3 237.68 7.71 0 3 4 32.38 1.89 0 -3 -4 35.42 1.85 0 -3 -4 32.85 2.70 0 3 5 442.53 10.87 0 -3 -5 434.86 12.36 0 -3 -5 430.09 10.61 0 -3 -6 60.51 3.32 0 3 6 61.33 3.51 0 -3 -6 61.94 4.05 0 -3 -7 339.77 10.16 0 3 7 329.01 10.25 0 -3 -7 333.36 11.02 0 3 8 99.13 5.39 0 -3 -8 102.24 5.72 0 -3 -9 369.73 12.40 0 3 9 350.69 12.12 0 -3 -10 7.77 2.08 0 3 10 12.51 2.63 0 3 11 31.98 3.93 0 -3 -11 33.20 3.79 0 3 12 5.78 2.40 0 -3 -12 4.24 1.80 0 -3 -13 310.37 12.58 0 3 13 279.05 13.13 0 3 14 14.71 3.63 0 -3 -14 22.37 3.43 0 -3 -15 -0.80 1.71 0 3 15 -0.96 2.36 0 -3 -16 6.40 2.65 0 3 16 12.74 4.04 0 3 17 15.71 4.27 0 3 18 13.16 3.76 0 3 19 52.16 7.35 0 3 20 10.39 4.27 0 -4 17 -1.24 2.66 0 -4 16 100.92 10.02 0 -4 15 25.38 5.35 0 -4 14 52.70 6.72 0 -4 13 51.09 6.22 0 -4 12 1.11 2.17 0 -4 11 21.06 3.99 0 -4 10 52.05 5.61 0 4 -9 132.18 3.64 0 4 -9 143.19 3.57 0 -4 8 118.27 7.47 0 4 -8 105.09 3.28 0 -4 7 614.00 18.03 0 4 -7 549.83 11.96 0 4 -6 2594.79 49.47 0 -4 6 2723.00 55.62 0 4 -5 436.22 10.25 0 -4 5 462.38 13.91 0 -4 4 0.55 1.08 0 4 -4 2.48 0.72 0 4 -3 713.31 16.07 0 4 -3 757.24 17.93 0 -4 3 727.53 16.38 0 -4 3 735.48 17.86 0 4 -2 324.14 8.66 0 -4 2 306.37 8.85 0 -4 2 321.62 9.24 0 4 -2 321.80 9.14 0 4 -1 1.60 0.90 0 -4 1 0.45 0.98 0 -4 1 2.26 0.92 0 4 -1 1.27 0.71 0 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203.60 10.50 3 -6 8 125.26 8.39 3 -6 9 4.32 2.19 3 -6 10 24.88 4.50 3 -6 11 143.69 10.29 3 -6 12 3.28 2.59 3 -6 13 -1.02 2.34 3 -6 14 44.12 6.72 3 -6 15 5.11 3.28 3 -5 -18 15.12 4.34 3 -5 -17 5.31 3.26 3 -5 -16 112.59 9.53 3 -5 -15 31.91 5.02 3 -5 -14 32.31 5.19 -3 5 14 25.82 4.34 3 -5 -13 146.22 10.02 -3 5 13 179.40 9.89 3 -5 -12 0.58 1.88 -3 5 12 -2.41 1.85 3 -5 -11 -0.04 2.14 -3 5 11 0.37 1.47 3 -5 -10 177.53 10.16 -3 5 10 189.48 8.81 3 -5 -9 21.83 3.60 -3 5 9 28.85 3.16 -3 5 8 0.37 0.98 3 -5 -8 -0.90 1.55 3 -5 -7 178.70 9.53 3 -5 -6 1105.67 28.92 3 -5 -6 1097.53 25.31 3 -5 -5 88.75 4.59 3 -5 -5 95.61 6.36 3 -5 -4 665.49 19.50 3 -5 -4 670.74 16.45 3 -5 -3 748.00 20.63 3 -5 -3 743.08 17.53 3 -5 -2 102.99 6.01 3 -5 -2 97.68 4.57 3 -5 -1 44.57 3.83 3 -5 0 41.91 3.52 3 -5 1 329.51 10.65 3 -5 2 53.15 3.48 3 -5 2 52.31 4.73 3 -5 2 55.47 3.64 3 -5 3 161.61 6.27 3 -5 3 160.77 6.05 3 -5 3 153.64 8.49 3 -5 3 166.87 7.51 3 -5 4 7.03 1.27 3 -5 4 5.56 1.12 3 -5 4 9.53 2.09 3 -5 5 15.34 1.48 3 -5 5 15.88 1.62 3 -5 5 14.62 2.59 3 -5 6 513.42 11.45 3 -5 6 544.19 12.04 3 -5 7 405.18 15.11 3 -5 8 14.09 3.29 3 -5 9 191.76 10.73 3 -5 10 22.80 4.43 3 -5 11 2.34 2.29 3 -5 12 33.14 5.21 3 -5 13 84.77 8.29 3 -5 14 0.42 2.42 3 -5 15 1.22 3.41 3 -5 16 71.58 8.92 3 -4 -18 17.42 4.52 3 -4 -17 3.62 2.78 3 -4 -16 0.99 2.54 -3 4 16 2.80 2.49 3 -4 -15 8.44 2.99 -3 4 15 5.09 2.21 3 -4 -14 111.38 8.63 -3 4 14 111.04 8.28 3 -4 -13 13.38 3.18 -3 4 13 19.62 3.50 3 -4 -12 2.29 2.19 -3 4 12 5.17 2.28 -3 4 11 83.31 6.17 3 -4 -11 80.96 6.72 3 -4 -10 31.95 4.24 -3 4 10 33.21 3.81 3 -4 -9 128.86 8.17 -3 4 9 134.20 7.20 3 -4 -8 60.49 5.36 -3 4 8 47.41 3.94 3 -4 -7 484.34 16.27 -3 4 7 468.59 13.94 -3 4 6 214.71 8.02 3 -4 -6 216.17 9.79 3 -4 -5 140.06 6.10 3 -4 -5 137.94 7.42 3 -4 -4 55.46 4.48 3 -4 -4 58.26 3.60 3 -4 -3 80.88 5.11 3 -4 -3 70.98 3.86 3 -4 -2 77.45 4.96 3 -4 -2 89.21 4.23 3 -4 -1 71.63 4.48 3 -4 0 101.12 5.14 3 -4 1 46.90 3.32 3 -4 1 46.30 3.17 -3 4 -2 22.58 2.10 3 -4 2 21.28 2.06 3 -4 2 21.54 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56.92 6.62 5 -7 -9 -3.69 2.65 5 -7 -8 6.29 3.23 5 -7 -7 1.67 2.30 5 -7 -6 148.90 9.74 5 -7 -5 0.77 1.94 5 -7 -4 7.59 2.51 5 -7 -3 97.46 7.33 5 -7 -2 17.69 3.37 5 -7 -1 15.95 3.43 5 -7 -1 12.30 2.91 5 -7 0 86.25 6.29 5 -7 0 95.88 7.60 5 -7 1 8.80 2.87 5 -7 1 4.15 1.50 5 -7 2 24.49 4.16 5 -7 2 23.12 3.19 5 -7 3 22.08 3.96 5 -7 3 15.17 2.44 5 -7 3 14.46 2.65 5 -7 4 11.28 2.82 5 -7 4 11.33 2.14 5 -7 4 11.44 2.64 5 -7 5 2.36 2.04 5 -7 5 0.11 0.98 5 -7 5 -0.70 1.43 5 -7 6 98.39 7.48 5 -7 6 95.01 8.24 5 -7 7 6.60 2.56 5 -7 7 2.30 2.05 5 -7 8 2.58 2.45 5 -7 8 3.36 2.37 5 -7 9 112.58 9.09 5 -7 10 -1.68 1.91 5 -7 11 5.74 2.66 5 -7 12 12.93 4.19 5 -7 13 -0.52 2.67 5 -6 -15 12.84 3.64 5 -6 -14 49.53 6.76 5 -6 -13 34.60 5.65 5 -6 -12 2.67 2.46 5 -6 -11 127.20 9.76 5 -6 -10 75.44 7.45 5 -6 -9 17.75 4.04 5 -6 -8 107.63 8.45 5 -6 -7 13.19 3.54 5 -6 -6 22.43 4.08 5 -6 -5 21.86 3.78 5 -6 -4 487.46 17.73 5 -6 -3 176.51 9.59 5 -6 -2 154.27 8.66 5 -6 -1 485.26 16.40 5 -6 -1 463.98 17.24 5 -6 0 61.56 5.16 5 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4.55 -5 5 -3 65.48 4.56 5 -5 3 72.45 6.01 5 -5 4 205.08 8.02 -5 5 -4 201.50 7.98 5 -5 4 194.84 10.53 -5 5 -5 11.59 1.80 5 -5 5 12.56 1.88 5 -5 5 11.40 2.56 5 -5 5 13.10 2.97 -5 5 -6 0.66 0.89 5 -5 6 0.41 0.77 5 -5 6 -0.72 2.13 5 -5 6 0.77 1.55 5 -5 7 334.23 14.25 5 -5 8 18.71 3.57 5 -5 9 119.50 8.74 5 -5 10 78.29 7.34 5 -5 11 35.69 5.64 5 -5 12 29.21 5.18 5 -5 13 72.49 8.16 5 -5 14 32.83 5.74 5 -5 15 4.74 3.62 5 -4 -17 2.29 2.75 5 -4 -16 2.77 2.63 5 -4 -15 12.30 3.80 5 -4 -14 112.50 9.24 -5 4 14 94.36 8.19 5 -4 -13 15.31 3.65 -5 4 13 12.69 3.27 5 -4 -12 73.67 7.24 -5 4 12 71.15 6.48 5 -4 -11 109.98 8.51 -5 4 11 112.91 7.87 5 -4 -10 1.99 1.94 -5 4 10 -0.05 1.48 5 -4 -9 228.54 11.77 -5 4 9 208.14 10.10 5 -4 -8 13.66 3.22 5 -4 -7 153.13 9.08 5 -4 -6 4.21 1.82 5 -4 -5 95.75 6.69 -5 4 4 634.62 19.61 5 -4 -4 624.60 19.38 -5 4 3 90.49 6.23 5 -4 -3 79.77 5.79 -5 4 2 185.54 8.82 5 -4 -2 181.45 8.78 5 -4 -1 588.56 17.52 -5 4 1 607.70 17.71 5 -4 -1 580.82 17.93 5 -4 0 176.50 8.16 -5 4 0 181.52 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64.01 6.76 -12 -1 -8 6.72 2.71 -12 -1 -9 5.29 2.67 -12 -1 -10 24.06 4.20 -12 -2 7 6.97 3.14 -12 -2 6 4.48 2.55 -12 -2 5 62.32 7.30 -12 -2 4 -1.00 2.03 -12 -2 3 16.40 3.99 -12 -2 2 47.37 6.35 -12 -2 1 3.64 2.52 -12 -2 0 3.22 2.66 -12 -2 -1 17.58 3.78 -12 -2 -2 60.47 6.57 -12 -2 -3 2.96 2.13 -12 -2 -4 20.24 3.99 -12 -2 -5 211.94 12.50 -12 -2 -6 3.64 2.79 -12 -2 -7 -0.96 2.28 -12 -2 -8 18.73 3.89 -12 -2 -9 14.66 3.91 -12 -2 -10 5.41 2.82 -12 -2 -11 11.24 3.55 -12 -3 7 9.76 3.57 -12 -3 6 24.13 4.83 -12 -3 5 10.19 3.44 -12 -3 4 3.20 2.70 -12 -3 3 65.89 7.42 -12 -3 2 32.11 5.36 -12 -3 1 10.96 3.83 -12 -3 0 41.40 5.94 -12 -3 -1 28.47 5.01 -12 -3 -2 -2.33 2.48 -12 -3 -3 -1.35 2.01 -12 -3 -4 110.76 9.11 -12 -3 -5 5.30 3.22 -12 -3 -6 5.84 3.07 -12 -3 -7 107.33 8.99 -12 -3 -8 1.20 2.10 -12 -3 -9 25.41 4.68 -12 -3 -10 50.71 6.35 -12 -3 -11 11.42 3.71 -12 -3 -12 29.49 5.03 -12 -4 7 8.64 4.22 -12 -4 6 0.62 2.55 -12 -4 5 18.45 4.28 -12 -4 4 3.35 2.92 -12 -4 3 4.61 2.96 -12 -4 2 51.17 6.64 -12 -4 1 81.68 8.02 -12 -4 0 18.73 4.18 -12 -4 -1 0.98 2.06 -12 -4 -2 51.13 6.23 -12 -4 -3 -1.82 2.19 -12 -4 -4 42.27 5.78 -12 -4 -5 3.30 2.13 -12 -4 -6 18.93 4.09 -12 -4 -7 3.57 2.84 -12 -4 -8 10.36 3.66 -12 -4 -9 108.05 9.17 -12 -4 -10 2.95 2.77 -12 -4 -11 37.71 5.54 -12 -4 -12 19.29 4.61 -12 -4 -13 21.61 4.76 -12 -5 7 0.07 2.07 -12 -5 6 29.08 5.35 -12 -5 5 21.41 4.68 -12 -5 4 -0.39 2.18 -12 -5 3 88.07 8.67 -12 -5 2 10.49 3.56 -12 -5 1 4.73 2.78 -12 -5 0 25.44 4.68 -12 -5 -1 63.03 7.05 -12 -5 -2 4.41 2.71 -12 -5 -3 2.53 2.74 -12 -5 -4 19.03 4.08 -12 -5 -5 4.92 2.69 -12 -5 -6 2.70 2.65 -12 -5 -7 101.33 9.14 -12 -5 -8 18.83 4.32 -12 -5 -9 14.69 3.98 -12 -5 -10 -0.08 2.20 -12 -5 -11 16.14 4.26 -12 -5 -12 3.26 2.35 -12 -5 -13 3.64 2.89 -12 -6 7 6.01 3.46 -12 -6 6 1.27 2.23 -12 -6 5 16.40 4.23 -12 -6 4 47.67 6.50 -12 -6 3 0.68 2.28 -12 -6 2 12.59 3.74 -12 -6 1 216.03 13.56 -12 -6 0 0.45 2.42 -12 -6 -1 2.91 2.91 -12 -6 -2 64.81 7.32 -12 -6 -3 28.86 5.15 -12 -6 -4 8.50 3.12 -12 -6 -5 3.10 3.00 -12 -6 -6 120.30 9.87 -12 -6 -7 5.54 3.58 -12 -6 -8 53.80 6.96 -12 -6 -9 55.08 6.95 -12 -6 -10 -0.93 2.46 -12 -6 -11 73.19 8.15 -12 -6 -12 -13.28 3.97 -12 -7 6 11.96 3.90 -12 -7 5 14.36 3.56 -12 -7 4 0.61 2.28 -12 -7 3 6.71 3.22 -12 -7 2 38.44 5.82 -12 -7 1 5.19 3.70 -12 -7 0 9.63 4.00 -12 -7 -1 91.03 8.83 -12 -7 -2 4.35 3.18 -12 -7 -3 6.35 2.90 -12 -7 -4 6.96 3.26 -12 -7 -5 6.28 3.78 -12 -7 -6 46.15 6.65 -12 -7 -7 33.85 5.83 -12 -7 -8 24.97 5.22 -12 -7 -9 14.34 4.02 -12 -7 -10 17.63 4.70 -12 -8 5 3.24 3.11 -12 -8 4 17.65 4.36 -12 -8 3 1.19 2.59 -12 -8 2 29.36 5.28 -12 -8 1 42.69 6.33 -12 -8 0 4.99 3.00 -12 -8 -1 14.63 4.13 -12 -8 -2 6.17 3.11 -12 -8 -3 29.44 5.38 -12 -8 -4 10.19 3.60 -12 -8 -5 5.63 3.50 -12 -8 -6 73.13 8.37 -12 -8 -7 4.47 3.08 -12 -8 -8 86.81 8.95 -12 -9 4 5.02 2.87 -12 -9 3 7.29 3.42 -12 -9 2 9.67 3.78 -12 -9 1 4.05 2.99 -12 -9 0 11.75 3.76 -12 -9 -1 82.68 8.59 -12 -9 -2 3.53 2.60 -12 -9 -3 1.53 2.80 -12 -9 -4 64.64 7.76 -12 -9 -5 5.34 3.35 -12 -9 -6 9.62 3.67 -13 3 -2 8.43 3.89 -13 3 -3 3.45 2.83 -13 3 -4 10.55 3.63 -13 2 0 15.60 4.47 -13 2 -1 21.46 4.60 -13 2 -2 -0.34 2.33 -13 2 -3 61.77 7.27 -13 2 -4 12.70 4.07 -13 2 -5 9.35 3.39 -13 2 -6 38.30 5.72 -13 1 1 5.90 3.23 -13 1 0 4.83 3.28 -13 1 -1 32.21 5.68 -13 1 -2 24.69 4.94 -13 1 -3 2.95 2.74 -13 1 -4 0.26 2.29 -13 1 -5 24.75 4.68 -13 1 -6 29.23 5.09 -13 1 -7 -0.33 2.28 -13 0 1 0.98 2.78 -13 0 0 9.47 3.55 -13 0 -1 -2.07 2.55 -13 0 -2 7.02 3.57 -13 0 -3 57.17 6.94 -13 0 -4 10.03 3.36 -13 0 -5 2.71 2.69 -13 0 -6 64.59 7.42 -13 0 -7 22.07 4.51 -13 0 -8 2.63 2.87 -13 -1 2 14.80 4.28 -13 -1 1 0.11 2.69 -13 -1 0 15.35 4.11 -13 -1 -1 20.41 4.43 -13 -1 -2 58.99 7.11 -13 -1 -3 28.21 5.24 -13 -1 -4 15.97 4.20 -13 -1 -5 69.94 7.30 -13 -1 -6 5.58 2.88 -13 -1 -7 -4.24 2.67 -13 -1 -8 42.64 5.99 -13 -1 -9 0.43 2.29 -13 -2 2 -4.11 2.54 -13 -2 1 -1.19 2.64 -13 -2 0 63.94 7.57 -13 -2 -1 1.48 2.72 -13 -2 -2 4.80 3.28 -13 -2 -3 35.07 5.58 -13 -2 -4 2.27 2.06 -13 -2 -5 6.88 3.53 -13 -2 -6 -1.39 2.38 -13 -2 -7 35.29 5.45 -13 -2 -8 12.56 4.07 -13 -2 -9 4.40 2.22 -13 -2 -10 59.00 7.11 -13 -3 3 5.42 3.16 -13 -3 2 11.96 3.66 -13 -3 1 10.71 3.86 -13 -3 0 31.33 5.63 -13 -3 -1 4.63 3.23 -13 -3 -2 120.37 10.14 -13 -3 -3 8.18 3.28 -13 -3 -4 -0.81 2.47 -13 -3 -5 47.12 6.32 -13 -3 -6 0.85 3.06 -13 -3 -7 4.78 3.02 -13 -3 -8 2.81 2.49 -13 -3 -9 40.46 5.99 -13 -3 -10 20.58 4.50 -13 -3 -11 14.60 4.18 -13 -4 3 84.50 8.84 -13 -4 2 11.37 3.82 -13 -4 1 7.00 3.52 -13 -4 0 46.42 6.56 -13 -4 -1 35.62 5.64 -13 -4 -2 1.48 2.70 -13 -4 -3 14.34 3.84 -13 -4 -4 58.12 6.98 -13 -4 -5 0.39 2.46 -13 -4 -6 1.83 2.68 -13 -4 -7 139.32 10.93 -13 -4 -8 10.85 3.75 -13 -4 -9 3.50 3.06 -13 -4 -10 5.30 3.23 -13 -4 -11 24.66 4.88 -13 -5 2 5.12 2.91 -13 -5 1 95.04 9.24 -13 -5 0 19.46 4.54 -13 -5 -1 14.94 4.12 -13 -5 -2 31.43 5.65 -13 -5 -3 16.35 4.65 -13 -5 -4 16.05 4.56 -13 -5 -5 3.33 3.22 -13 -5 -6 97.79 9.22 -13 -5 -7 7.27 3.77 -13 -5 -8 -3.04 2.86 -13 -5 -9 82.36 8.70 -13 -6 1 -2.24 2.85 -13 -6 0 51.00 6.94 -13 -6 -1 36.44 5.96 -13 -6 -2 12.21 3.86 -13 -6 -3 26.26 5.46 -13 -6 -4 40.64 6.23 -13 -6 -5 2.69 3.02 -13 -6 -6 10.95 4.00 -13 -6 -7 47.05 6.54 -13 -7 -1 17.08 4.92 -13 -7 -2 1.48 2.97 -13 -7 -3 24.64 5.32 -13 -7 -4 8.24 3.41 0 0 0 0.00 0.00 TITL SS-401 in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 10.827284 11.467690 15.036639 81.5915 83.0179 76.3263 ZERR 3.00 0.000534 0.000585 0.000795 0.0043 0.0042 0.0043 LATT 1 SFAC C H N O V UNIT 69.00 75.00 18.00 24.00 6.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23173 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.144 _oxdiff_exptl_absorpt_empirical_full_min 0.859