# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- 1.cif' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_email rosa.pedrido@usc.es _publ_contact_author_name 'Rosa Pedrido' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2012-07-12 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? loop_ _publ_author_name Martinez-Calvo 'Maria J. Romero' 'Rosa Pedrido' 'Ana M. Gonzalez-Noya' ; G.Zaragoza ; 'Manuel R. Bermejo' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_6CoLMe _database_code_depnum_ccdc_archive 'CCDC 893868' #TrackingRef '- 1.cif' _audit_creation_date 2012-07-12T10:10:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H36 Co2 N12 S4' _chemical_formula_sum 'C28 H36 Co2 N12 S4' _chemical_formula_weight 786.83 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.4792(13) _cell_length_b 15.5345(14) _cell_length_c 15.9289(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3582.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1381 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 21.73 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.785543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_unetI/netI 0.0775 _diffrn_reflns_number 19797 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 3573 _reflns_number_gt 2206 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Saint' _computing_structure_solution 'SIR97 (Altomare et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+6.9100P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3573 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1979 _refine_ls_wR_factor_gt 0.176 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.001 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.10214(6) 0.34799(6) 0.63395(5) 0.0317(3) Uani 1 1 d . . . C1 C 0.1733(5) 0.6890(5) 0.6268(5) 0.052(2) Uani 1 1 d . . . H1A H 0.1374 0.6958 0.5751 0.078 Uiso 1 1 calc R . . H1B H 0.2225 0.7324 0.6284 0.078 Uiso 1 1 calc R . . H1C H 0.1327 0.6966 0.6754 0.078 Uiso 1 1 calc R . . C2 C 0.1659(4) 0.5299(5) 0.6281(4) 0.0414(18) Uani 1 1 d . . . C3 C -0.1127(5) 0.3817(4) 0.6063(5) 0.0420(17) Uani 1 1 d . . . H3A H -0.0683 0.3364 0.5921 0.063 Uiso 1 1 calc R . . H3B H -0.1616 0.3833 0.5638 0.063 Uiso 1 1 calc R . . H3C H -0.1398 0.3697 0.6614 0.063 Uiso 1 1 calc R . . C4 C -0.0641(4) 0.4673(4) 0.6087(4) 0.0330(15) Uani 1 1 d . . . C5 C -0.1221(4) 0.5455(4) 0.6051(4) 0.0292(14) Uani 1 1 d . . . C6 C -0.2073(5) 0.5441(5) 0.6460(4) 0.0476(19) Uani 1 1 d . . . H6 H -0.2265 0.4933 0.6742 0.057 Uiso 1 1 calc R . . C7 C -0.2634(6) 0.6142(5) 0.6459(4) 0.054(2) Uani 1 1 d . . . H7 H -0.3211 0.6123 0.6743 0.064 Uiso 1 1 calc R . . C8 C -0.2359(6) 0.6904(5) 0.6035(4) 0.0489(19) Uani 1 1 d . . . H8 H -0.2735 0.7406 0.605 0.059 Uiso 1 1 calc R . . C9 C -0.1536(5) 0.6900(4) 0.5602(3) 0.0319(15) Uani 1 1 d . . . C10 C -0.0959(4) 0.6197(4) 0.5620(3) 0.0281(14) Uani 1 1 d . . . H10 H -0.0381 0.6217 0.5339 0.034 Uiso 1 1 calc R . . C11 C 0.1292(6) 0.1454(4) 0.4427(4) 0.047(2) Uani 1 1 d . . . H11A H 0.0669 0.1207 0.4408 0.07 Uiso 1 1 calc R . . H11B H 0.1702 0.1067 0.4737 0.07 Uiso 1 1 calc R . . H11C H 0.1524 0.1528 0.3853 0.07 Uiso 1 1 calc R . . C12 C 0.1259(5) 0.2312(4) 0.4858(4) 0.0361(16) Uani 1 1 d . . . C13 C 0.0424(4) 0.1716(4) 0.6789(4) 0.0335(15) Uani 1 1 d . . . C14 C 0.0019(5) 0.0185(4) 0.6750(4) 0.0468(18) Uani 1 1 d . . . H14A H 0.0641 -0.0052 0.6674 0.07 Uiso 1 1 calc R . . H14B H -0.0276 0.026 0.6201 0.07 Uiso 1 1 calc R . . H14C H -0.035 -0.0211 0.7092 0.07 Uiso 1 1 calc R . . N1 N 0.2141(5) 0.6031(4) 0.6291(4) 0.0446(15) Uani 1 1 d . . . H1N H 0.280(5) 0.606(5) 0.637(4) 0.054 Uiso 1 1 d . . . N2 N 0.0742(4) 0.5387(3) 0.6180(3) 0.0383(14) Uani 1 1 d . . . N3 N 0.0288(4) 0.4614(4) 0.6150(3) 0.0419(15) Uani 1 1 d . . . N4 N 0.0967(4) 0.2398(3) 0.5624(3) 0.0328(12) Uani 1 1 d . . . N5 N 0.0667(4) 0.1637(3) 0.6000(3) 0.0396(14) Uani 1 1 d . . . N6 N 0.0081(4) 0.1009(3) 0.7168(3) 0.0337(13) Uani 1 1 d . . . H6N H -0.004(4) 0.103(4) 0.778(4) 0.04 Uiso 1 1 d . . . S1 S 0.22936(13) 0.43344(13) 0.63898(12) 0.0499(5) Uani 1 1 d . . . S2 S 0.04988(14) 0.26424(11) 0.74063(9) 0.0430(5) 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 Co1 0.0369(5) 0.0288(5) 0.0295(4) -0.0122(3) 0.0009(4) -0.0008(4) C1 0.054(5) 0.042(5) 0.061(5) -0.007(4) 0.001(4) -0.022(4) C2 0.025(3) 0.075(6) 0.024(3) -0.013(3) -0.009(3) 0.009(4) C3 0.040(4) 0.025(4) 0.062(4) 0.008(3) -0.003(3) -0.002(3) C4 0.033(3) 0.040(4) 0.026(3) 0.001(3) -0.002(3) -0.014(3) C5 0.043(4) 0.018(4) 0.027(3) -0.008(2) 0.004(3) -0.010(3) C6 0.060(5) 0.027(4) 0.055(4) -0.002(3) 0.027(4) 0.002(4) C7 0.061(5) 0.047(5) 0.052(4) -0.006(4) 0.031(4) -0.003(4) C8 0.072(5) 0.028(4) 0.047(4) -0.004(3) 0.022(4) 0.009(4) C9 0.045(4) 0.021(4) 0.030(3) -0.004(2) 0.006(3) -0.008(3) C10 0.039(4) 0.022(4) 0.024(3) -0.008(2) 0.005(2) -0.008(3) C11 0.085(6) 0.018(4) 0.038(4) -0.004(3) 0.016(4) 0.002(4) C12 0.057(4) 0.025(4) 0.026(3) -0.009(2) 0.004(3) -0.003(3) C13 0.039(4) 0.030(4) 0.032(3) -0.002(3) 0.001(3) 0.011(3) C14 0.063(5) 0.031(4) 0.047(4) 0.001(3) 0.011(4) -0.004(4) N1 0.051(4) 0.033(4) 0.049(3) -0.012(3) -0.001(3) 0.007(3) N2 0.055(4) 0.028(3) 0.032(3) -0.003(2) 0.002(2) -0.003(3) N3 0.063(4) 0.038(4) 0.025(3) -0.004(2) 0.018(2) -0.020(3) N4 0.046(3) 0.023(3) 0.029(3) -0.003(2) 0.004(2) -0.002(3) N5 0.065(4) 0.025(3) 0.029(3) -0.004(2) 0.012(3) 0.002(3) N6 0.047(3) 0.030(3) 0.024(2) 0.002(2) 0.003(2) 0.003(3) S1 0.0402(10) 0.0451(12) 0.0644(12) -0.0261(9) -0.0048(9) -0.0061(9) S2 0.0703(13) 0.0354(11) 0.0232(7) -0.0058(7) 0.0030(7) 0.0065(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Co1 N4 2.033(5) . ? Co1 N3 2.078(6) . ? Co1 S2 2.2700(19) . ? Co1 S1 2.272(2) . ? C1 N1 1.461(10) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 N1 1.333(9) . ? C2 N2 1.344(8) . ? C2 S1 1.766(8) . ? C3 C4 1.504(9) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 N3 1.352(8) . ? C4 C5 1.478(9) . ? C5 C10 1.393(8) . ? C5 C6 1.396(9) . ? C6 C7 1.359(10) . ? C6 H6 0.95 . ? C7 C8 1.420(10) . ? C7 H7 0.95 . ? C8 C9 1.377(9) . ? C8 H8 0.95 . ? C9 C10 1.376(9) . ? C9 C12 1.481(8) 5_566 ? C10 H10 0.95 . ? C11 C12 1.500(8) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 N4 1.299(7) . ? C12 C9 1.481(8) 5_566 ? C13 N5 1.310(8) . ? C13 N6 1.348(8) . ? C13 S2 1.747(6) . ? C14 N6 1.445(8) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? N1 H1N 0.96(7) . ? N2 N3 1.370(7) . ? N4 N5 1.394(7) . ? N6 H6N 0.99(6) . ? 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 N4 Co1 N3 126.9(2) . . ? N4 Co1 S2 86.13(14) . . ? N3 Co1 S2 115.09(15) . . ? N4 Co1 S1 122.32(16) . . ? N3 Co1 S1 85.65(17) . . ? S2 Co1 S1 125.36(8) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 115.6(7) . . ? N1 C2 S1 116.7(5) . . ? N2 C2 S1 127.7(6) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 128.6(6) . . ? N3 C4 C3 114.0(6) . . ? C5 C4 C3 117.4(6) . . ? C10 C5 C6 118.9(6) . . ? C10 C5 C4 123.0(6) . . ? C6 C5 C4 118.1(6) . . ? C7 C6 C5 121.0(7) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.1(7) . . ? C6 C7 H7 120 . . ? C8 C7 H7 120 . . ? C9 C8 C7 118.5(7) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C10 C9 C8 121.2(6) . . ? C10 C9 C12 120.2(6) . 5_566 ? C8 C9 C12 118.6(6) . 5_566 ? C9 C10 C5 120.2(6) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C9 117.9(5) . 5_566 ? N4 C12 C11 122.1(6) . . ? C9 C12 C11 119.9(5) 5_566 . ? N5 C13 N6 116.9(6) . . ? N5 C13 S2 126.9(5) . . ? N6 C13 S2 116.2(4) . . ? N6 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 N1 C1 124.6(6) . . ? C2 N1 H1N 124(5) . . ? C1 N1 H1N 111(5) . . ? C2 N2 N3 112.9(6) . . ? C4 N3 N2 114.8(6) . . ? C4 N3 Co1 125.2(4) . . ? N2 N3 Co1 119.5(5) . . ? C12 N4 N5 114.7(5) . . ? C12 N4 Co1 126.8(4) . . ? N5 N4 Co1 118.2(3) . . ? C13 N5 N4 114.6(5) . . ? C13 N6 C14 122.5(5) . . ? C13 N6 H6N 119(4) . . ? C14 N6 H6N 118(4) . . ? C2 S1 Co1 94.0(2) . . ? C13 S2 Co1 94.1(2) . . ? 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 N3 C4 C5 C10 37.9(9) . . . . ? C3 C4 C5 C10 -143.0(6) . . . . ? N3 C4 C5 C6 -142.9(7) . . . . ? C3 C4 C5 C6 36.1(8) . . . . ? C10 C5 C6 C7 -1.7(10) . . . . ? C4 C5 C6 C7 179.2(6) . . . . ? C5 C6 C7 C8 0.4(11) . . . . ? C6 C7 C8 C9 2.5(11) . . . . ? C7 C8 C9 C10 -4.1(10) . . . . ? C7 C8 C9 C12 178.5(6) . . . 5_566 ? C8 C9 C10 C5 2.9(9) . . . . ? C12 C9 C10 C5 -179.8(5) 5_566 . . . ? C6 C5 C10 C9 0.1(9) . . . . ? C4 C5 C10 C9 179.2(5) . . . . ? N2 C2 N1 C1 5.1(9) . . . . ? S1 C2 N1 C1 -175.5(5) . . . . ? N1 C2 N2 N3 178.2(5) . . . . ? S1 C2 N2 N3 -1.1(7) . . . . ? C5 C4 N3 N2 -0.4(8) . . . . ? C3 C4 N3 N2 -179.5(5) . . . . ? C5 C4 N3 Co1 172.2(4) . . . . ? C3 C4 N3 Co1 -6.8(7) . . . . ? C2 N2 N3 C4 177.2(5) . . . . ? C2 N2 N3 Co1 4.1(6) . . . . ? N4 Co1 N3 C4 55.5(5) . . . . ? S2 Co1 N3 C4 -49.5(5) . . . . ? S1 Co1 N3 C4 -176.7(5) . . . . ? N4 Co1 N3 N2 -132.2(4) . . . . ? S2 Co1 N3 N2 122.9(4) . . . . ? S1 Co1 N3 N2 -4.4(4) . . . . ? C9 C12 N4 N5 176.4(6) 5_566 . . . ? C11 C12 N4 N5 -1.5(9) . . . . ? C9 C12 N4 Co1 -9.9(9) 5_566 . . . ? C11 C12 N4 Co1 172.2(5) . . . . ? N3 Co1 N4 C12 67.8(6) . . . . ? S2 Co1 N4 C12 -173.5(6) . . . . ? S1 Co1 N4 C12 -43.4(6) . . . . ? N3 Co1 N4 N5 -118.7(5) . . . . ? S2 Co1 N4 N5 0.0(4) . . . . ? S1 Co1 N4 N5 130.1(4) . . . . ? N6 C13 N5 N4 176.4(5) . . . . ? S2 C13 N5 N4 -3.7(9) . . . . ? C12 N4 N5 C13 176.2(6) . . . . ? Co1 N4 N5 C13 1.9(7) . . . . ? N5 C13 N6 C14 2.9(9) . . . . ? S2 C13 N6 C14 -176.9(5) . . . . ? N1 C2 S1 Co1 178.8(5) . . . . ? N2 C2 S1 Co1 -1.9(5) . . . . ? N4 Co1 S1 C2 134.3(3) . . . . ? N3 Co1 S1 C2 2.7(2) . . . . ? S2 Co1 S1 C2 -115.1(2) . . . . ? N5 C13 S2 Co1 3.3(6) . . . . ? N6 C13 S2 Co1 -176.9(5) . . . . ? N4 Co1 S2 C13 -1.3(3) . . . . ? N3 Co1 S2 C13 127.9(3) . . . . ? S1 Co1 S2 C13 -128.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6N N2 0.99(6) 2.19(6) 3.046(7) 145(5) 4_546 N1 H1N N5 0.96(7) 2.47(8) 3.342(9) 151(6) 7_665 # END of CIF # Attachment '- 2.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-07-11 at 10:17:26 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : 2 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_9ZnLEt _database_code_depnum_ccdc_archive 'CCDC 893869' #TrackingRef '- 2.cif' _audit_creation_date 2012-07-11T10:17:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H44 N12 S4 Zn2' _chemical_formula_sum 'C32 H44 N12 S4 Zn2' _chemical_formula_weight 855.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6969(4) _cell_length_b 14.6726(5) _cell_length_c 11.8716(4) _cell_angle_alpha 90 _cell_angle_beta 90.6800(10) _cell_angle_gamma 90 _cell_volume 1863.13(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.55 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 0.93 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_unetI/netI 0.0441 _diffrn_reflns_number 31071 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.3 _diffrn_reflns_theta_full 28.3 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 4617 _reflns_number_gt 3558 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.4421P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4617 _refine_ls_number_parameters 255 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.608 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.52693(4) 0.37707(3) -0.25263(5) 0.01288(10) Uani 0.910(2) 1 d P . 1 C1 C 0.9634(2) 0.38851(15) -0.56972(19) 0.0210(5) Uani 1 1 d . . . H1A H 0.9614 0.3371 -0.6197 0.032 Uiso 1 1 calc R . . H1B H 1.0337 0.4264 -0.5873 0.032 Uiso 1 1 calc R . . H1C H 0.8877 0.423 -0.5786 0.032 Uiso 1 1 calc R . . C2 C 0.97536(19) 0.35530(14) -0.44852(18) 0.0162(4) Uani 1 1 d . . . H2A H 1.0502 0.3183 -0.4413 0.019 Uiso 1 1 calc R . . H2B H 0.9856 0.4077 -0.3994 0.019 Uiso 1 1 calc R . . N1 N 0.86873(17) 0.30219(12) -0.41064(16) 0.0166(4) Uani 1 1 d . . . C3 C 0.76158(19) 0.33997(14) -0.37535(17) 0.0147(4) Uani 1 1 d . . . S1 S 0.64430(5) 0.26277(4) -0.33337(5) 0.01834(13) Uani 1 1 d . . . N2 N 0.75516(16) 0.42980(12) -0.37624(15) 0.0142(4) Uani 1 1 d . . . N3 N 0.64627(16) 0.46519(12) -0.33092(15) 0.0142(4) Uani 1 1 d . . . C4 C 0.6951(2) 0.60619(15) -0.4345(2) 0.0237(5) Uani 1 1 d . . . H4A H 0.7565 0.6406 -0.3929 0.035 Uiso 1 1 calc R . . H4B H 0.6402 0.6472 -0.4742 0.035 Uiso 1 1 calc R . . H4C H 0.7362 0.5673 -0.4874 0.035 Uiso 1 1 calc R . . C5 C 0.62087(19) 0.54942(14) -0.35494(18) 0.0152(4) Uani 1 1 d . . . C6 C 0.51480(19) 0.59185(13) -0.29540(19) 0.0148(4) Uani 1 1 d . . . C7 C 0.4210(2) 0.63778(14) -0.35556(19) 0.0176(5) Uani 1 1 d . . . H7 H 0.4259 0.644 -0.4333 0.021 Uiso 1 1 calc R . . C8 C 0.32080(19) 0.67374(14) -0.29810(19) 0.0175(5) Uani 1 1 d . . . H8 H 0.257 0.7031 -0.3377 0.021 Uiso 1 1 calc R . . C9 C 0.3145(2) 0.66637(14) -0.18184(19) 0.0164(4) Uani 1 1 d . . . H10 H 0.2454 0.6897 -0.1448 0.02 Uiso 1 1 calc R . . C10 C 0.40994(19) 0.62461(14) -0.11934(18) 0.0147(4) Uani 1 1 d . . . C11 C 0.50999(19) 0.58686(13) -0.17879(18) 0.0142(4) Uani 1 1 d . . . H11 H 0.5743 0.558 -0.1393 0.017 Uiso 1 1 calc R . . C12 C 0.2697(2) 0.61729(16) 0.05321(19) 0.0211(5) Uani 1 1 d . . . H12A H 0.2743 0.5994 0.1309 0.032 Uiso 1 1 calc R . . H12B H 0.2202 0.5739 0.0117 0.032 Uiso 1 1 calc R . . H12C H 0.2319 0.6765 0.0473 0.032 Uiso 1 1 calc R . . C13 C 0.3993(2) 0.62059(14) 0.00560(19) 0.0174(4) Uani 1 1 d . . . S2 S 0.68410(6) 0.60380(4) 0.26223(8) 0.01485(17) Uani 0.910(2) 1 d P . 1 C14 C 0.6999(2) 0.61441(15) 0.1171(2) 0.0128(5) Uani 0.910(2) 1 d P . 1 N6 N 0.8165(2) 0.6155(2) 0.07463(18) 0.0166(5) Uani 0.910(2) 1 d PD . 1 C15 C 0.9322(2) 0.61067(15) 0.13912(19) 0.0200(5) Uani 1 1 d D . . H15A H 0.9218 0.6432 0.2095 0.024 Uiso 1 1 calc R . 1 H15B H 0.9977 0.641 0.0974 0.024 Uiso 1 1 calc R . 1 C16 C 0.9728(2) 0.51370(16) 0.16461(19) 0.0223(5) Uani 1 1 d . . . H16A H 0.9103 0.4841 0.2089 0.033 Uiso 1 1 calc R . . H16B H 1.0507 0.5146 0.2057 0.033 Uiso 1 1 calc R . . H16C H 0.9833 0.481 0.0953 0.033 Uiso 1 1 calc R . . N4 N 0.48933(17) 0.61926(12) 0.07941(17) 0.0129(4) Uani 0.910(2) 1 d P . 1 N5 N 0.61068(19) 0.62286(13) 0.03919(17) 0.0139(4) Uani 0.910(2) 1 d P . 1 Zn1C Zn 0.5154(5) 0.3694(3) -0.2884(5) 0.01288(10) Uani 0.090(2) 1 d P . 2 S2B S 0.7048(7) 0.6080(5) 0.3120(8) 0.01485(17) Uani 0.090(2) 1 d P . 2 C14B C 0.688(2) 0.6129(17) 0.171(2) 0.0128(5) Uani 0.090(2) 1 d PD . 2 N4B N 0.548(2) 0.6236(14) 0.0262(19) 0.0129(4) Uani 0.090(2) 1 d P . 2 N5B N 0.5624(18) 0.6248(13) 0.1349(17) 0.0139(4) Uani 0.090(2) 1 d P . 2 N6B N 0.7865(16) 0.614(3) 0.102(2) 0.0166(5) Uani 0.090(2) 1 d PD . 2 H66N H 0.7704 0.616 0.0306 0.02 Uiso 0.090(2) 1 calc PR . 2 H1N H 0.873(2) 0.2454(17) -0.419(2) 0.02 Uiso 1 1 d . . . H6N H 0.823(2) 0.6313(17) 0.0081(15) 0.02 Uiso 0.910(2) 1 d PD . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01317(14) 0.01296(14) 0.0126(2) -0.00077(16) 0.00323(15) -0.00114(11) C1 0.0167(11) 0.0251(12) 0.0214(12) 0.0012(9) 0.0027(9) -0.0003(9) C2 0.0136(10) 0.0145(10) 0.0206(12) 0.0008(8) 0.0026(9) 0.0023(8) N1 0.0170(9) 0.0104(9) 0.0224(10) 0.0003(8) 0.0048(8) 0.0014(7) C3 0.0168(10) 0.0154(10) 0.0119(10) 0.0014(8) 0.0019(9) 0.0008(8) S1 0.0204(3) 0.0120(3) 0.0228(3) -0.0006(2) 0.0078(2) -0.0015(2) N2 0.0135(8) 0.0129(9) 0.0163(9) 0.0011(7) 0.0024(7) 0.0009(7) N3 0.0123(8) 0.0159(9) 0.0143(9) -0.0013(7) 0.0022(7) -0.0011(7) C4 0.0199(11) 0.0178(12) 0.0334(14) 0.0082(10) 0.0080(10) 0.0022(9) C5 0.0135(10) 0.0144(10) 0.0178(11) 0.0004(8) -0.0019(9) -0.0009(8) C6 0.0136(10) 0.0083(9) 0.0226(12) -0.0008(8) -0.0011(9) -0.0016(8) C7 0.0208(11) 0.0121(10) 0.0199(12) 0.0019(8) -0.0008(9) -0.0001(8) C8 0.0138(10) 0.0135(10) 0.0250(13) 0.0013(9) -0.0041(9) 0.0027(8) C9 0.0133(10) 0.0130(10) 0.0227(12) -0.0044(9) -0.0008(9) 0.0005(8) C10 0.0137(9) 0.0099(9) 0.0206(11) -0.0024(9) -0.0023(8) -0.0016(8) C11 0.0135(10) 0.0088(9) 0.0202(12) -0.0007(8) -0.0030(9) -0.0008(8) C12 0.0223(11) 0.0238(12) 0.0171(11) -0.0024(9) 0.0007(9) 0.0033(9) C13 0.0206(11) 0.0102(10) 0.0213(11) -0.0025(9) -0.0058(9) 0.0017(8) S2 0.0136(3) 0.0188(3) 0.0122(4) 0.0009(3) 0.0006(3) -0.0025(2) C14 0.0156(11) 0.0084(10) 0.0143(13) 0.0000(10) 0.0007(11) -0.0022(8) N6 0.0150(11) 0.0241(11) 0.0107(12) 0.0012(11) 0.0034(8) 0.0018(11) C15 0.0147(10) 0.0272(12) 0.0181(11) 0.0009(9) 0.0014(9) 0.0001(9) C16 0.0214(12) 0.0280(13) 0.0176(12) 0.0009(10) -0.0005(10) 0.0046(10) N4 0.0110(9) 0.0122(9) 0.0157(10) -0.0005(8) 0.0036(8) -0.0007(8) N5 0.0100(10) 0.0163(10) 0.0155(10) -0.0005(8) 0.0040(8) -0.0005(8) Zn1C 0.01317(14) 0.01296(14) 0.0126(2) -0.00077(16) 0.00323(15) -0.00114(11) S2B 0.0136(3) 0.0188(3) 0.0122(4) 0.0009(3) 0.0006(3) -0.0025(2) C14B 0.0156(11) 0.0084(10) 0.0143(13) 0.0000(10) 0.0007(11) -0.0022(8) N4B 0.0110(9) 0.0122(9) 0.0157(10) -0.0005(8) 0.0036(8) -0.0007(8) N5B 0.0100(10) 0.0163(10) 0.0155(10) -0.0005(8) 0.0040(8) -0.0005(8) N6B 0.0150(11) 0.0241(11) 0.0107(12) 0.0012(11) 0.0034(8) 0.0018(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 N3 2.0477(17) . ? Zn1 N4 2.067(2) 3_665 ? Zn1 S2 2.2763(7) 3_665 ? Zn1 S1 2.3100(7) . ? C1 C2 1.523(3) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 N1 1.457(3) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? N1 C3 1.345(3) . ? N1 H1N 0.84(2) . ? C3 N2 1.320(3) . ? C3 S1 1.766(2) . ? S1 Zn1C 2.157(5) . ? N2 N3 1.390(2) . ? N3 C5 1.296(3) . ? N3 Zn1C 2.051(5) . ? C4 C5 1.494(3) . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 C6 1.481(3) . ? C6 C11 1.388(3) . ? C6 C7 1.398(3) . ? C7 C8 1.382(3) . ? C7 H7 0.93 . ? C8 C9 1.387(3) . ? C8 H8 0.93 . ? C9 C10 1.396(3) . ? C9 H10 0.93 . ? C10 C11 1.403(3) . ? C10 C13 1.490(3) . ? C11 H11 0.93 . ? C12 C13 1.504(3) . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 N4 1.295(3) . ? C13 N4B 1.60(2) . ? S2 C14 1.741(3) . ? S2 Zn1 2.2763(7) 3_665 ? C14 N5 1.326(3) . ? C14 N6 1.351(3) . ? N6 C15 1.449(3) . ? N6 H6N 0.826(17) . ? C15 C16 1.517(3) . ? C15 N6B 1.616(18) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? N4 N5 1.389(3) . ? N4 Zn1 2.067(2) 3_665 ? Zn1C N5B 2.01(2) 3_665 ? Zn1C S2B 2.392(8) 3_665 ? S2B C14B 1.69(3) . ? S2B Zn1C 2.392(8) 3_665 ? C14B N6B 1.340(18) . ? C14B N5B 1.42(3) . ? N4B N5B 1.30(3) . ? N5B Zn1C 2.01(2) 3_665 ? N6B H66N 0.86 . ? N6B H6N 1.21(3) . ? 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 N3 Zn1 N4 119.71(7) . 3_665 ? N3 Zn1 S2 121.51(5) . 3_665 ? N4 Zn1 S2 87.22(6) 3_665 3_665 ? N3 Zn1 S1 85.72(5) . . ? N4 Zn1 S1 118.97(6) 3_665 . ? S2 Zn1 S1 127.75(3) 3_665 . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 113.93(18) . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C3 N1 C2 123.30(18) . . ? C3 N1 H1N 119.8(16) . . ? C2 N1 H1N 116.5(16) . . ? N2 C3 N1 116.97(19) . . ? N2 C3 S1 127.27(16) . . ? N1 C3 S1 115.75(16) . . ? C3 S1 Zn1C 93.62(14) . . ? C3 S1 Zn1 92.45(7) . . ? C3 N2 N3 114.45(17) . . ? C5 N3 N2 116.46(17) . . ? C5 N3 Zn1 124.86(14) . . ? N2 N3 Zn1 118.02(12) . . ? C5 N3 Zn1C 124.4(2) . . ? N2 N3 Zn1C 114.65(18) . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 117.10(19) . . ? N3 C5 C4 123.98(19) . . ? C6 C5 C4 118.87(18) . . ? C11 C6 C7 120.0(2) . . ? C11 C6 C5 119.44(18) . . ? C7 C6 C5 120.5(2) . . ? C8 C7 C6 119.2(2) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 120.56(19) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 121.3(2) . . ? C8 C9 H10 119.4 . . ? C10 C9 H10 119.4 . . ? C9 C10 C11 117.6(2) . . ? C9 C10 C13 118.83(19) . . ? C11 C10 C13 123.57(19) . . ? C6 C11 C10 121.23(19) . . ? C6 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C10 127.5(2) . . ? N4 C13 C12 115.3(2) . . ? C10 C13 C12 117.21(18) . . ? C10 C13 N4B 93.7(8) . . ? C12 C13 N4B 149.1(8) . . ? C14 S2 Zn1 92.70(8) . 3_665 ? N5 C14 N6 113.5(2) . . ? N5 C14 S2 128.40(19) . . ? N6 C14 S2 118.10(18) . . ? C14 N6 C15 126.1(2) . . ? C14 N6 H6N 116.3(19) . . ? C15 N6 H6N 116.3(19) . . ? N6 C15 C16 113.1(2) . . ? C16 C15 N6B 110.7(13) . . ? N6 C15 H15A 109 . . ? C16 C15 H15A 109 . . ? N6B C15 H15A 95.9 . . ? N6 C15 H15B 109 . . ? C16 C15 H15B 109 . . ? N6B C15 H15B 123.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 N4 N5 117.2(2) . . ? C13 N4 Zn1 127.04(16) . 3_665 ? N5 N4 Zn1 115.53(14) . 3_665 ? C14 N5 N4 115.10(19) . . ? N5B Zn1C N3 118.9(6) 3_665 . ? N5B Zn1C S1 121.8(6) 3_665 . ? N3 Zn1C S1 89.76(19) . . ? N5B Zn1C S2B 71.6(6) 3_665 3_665 ? N3 Zn1C S2B 123.4(3) . 3_665 ? S1 Zn1C S2B 134.7(3) . 3_665 ? C14B S2B Zn1C 77.7(9) . 3_665 ? N6B C14B N5B 124(2) . . ? N6B C14B S2B 122(2) . . ? N5B C14B S2B 113.1(16) . . ? N5B N4B C13 105.1(18) . . ? N4B N5B C14B 114(2) . . ? N4B N5B Zn1C 148.5(18) . 3_665 ? C14B N5B Zn1C 97.7(15) . 3_665 ? C14B N6B C15 126(2) . . ? C14B N6B H66N 116.9 . . ? C15 N6B H66N 116.9 . . ? C14B N6B H6N 146(3) . . ? C15 N6B H6N 86.6(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 N1 C3 -80.8(3) . . . . ? C2 N1 C3 N2 0.2(3) . . . . ? C2 N1 C3 S1 179.90(16) . . . . ? N2 C3 S1 Zn1C -1.6(3) . . . . ? N1 C3 S1 Zn1C 178.8(2) . . . . ? N2 C3 S1 Zn1 -12.5(2) . . . . ? N1 C3 S1 Zn1 167.78(16) . . . . ? N3 Zn1 S1 C3 10.87(9) . . . . ? N4 Zn1 S1 C3 -110.90(9) 3_665 . . . ? S2 Zn1 S1 C3 138.09(7) 3_665 . . . ? N3 Zn1 S1 Zn1C -85.5(7) . . . . ? N4 Zn1 S1 Zn1C 152.8(7) 3_665 . . . ? S2 Zn1 S1 Zn1C 41.8(7) 3_665 . . . ? N1 C3 N2 N3 -175.31(17) . . . . ? S1 C3 N2 N3 5.0(3) . . . . ? C3 N2 N3 C5 -163.17(19) . . . . ? C3 N2 N3 Zn1 8.0(2) . . . . ? C3 N2 N3 Zn1C -5.8(3) . . . . ? N4 Zn1 N3 C5 -81.20(19) 3_665 . . . ? S2 Zn1 N3 C5 25.3(2) 3_665 . . . ? S1 Zn1 N3 C5 157.71(18) . . . . ? N4 Zn1 N3 N2 108.48(14) 3_665 . . . ? S2 Zn1 N3 N2 -145.01(12) 3_665 . . . ? S1 Zn1 N3 N2 -12.61(13) . . . . ? N4 Zn1 N3 Zn1C -173.7(7) 3_665 . . . ? S2 Zn1 N3 Zn1C -67.2(6) 3_665 . . . ? S1 Zn1 N3 Zn1C 65.2(6) . . . . ? N2 N3 C5 C6 -172.07(17) . . . . ? Zn1 N3 C5 C6 17.5(3) . . . . ? Zn1C N3 C5 C6 33.0(3) . . . . ? N2 N3 C5 C4 5.2(3) . . . . ? Zn1 N3 C5 C4 -165.23(16) . . . . ? Zn1C N3 C5 C4 -149.7(3) . . . . ? N3 C5 C6 C11 51.4(3) . . . . ? C4 C5 C6 C11 -126.0(2) . . . . ? N3 C5 C6 C7 -129.5(2) . . . . ? C4 C5 C6 C7 53.1(3) . . . . ? C11 C6 C7 C8 -3.3(3) . . . . ? C5 C6 C7 C8 177.61(19) . . . . ? C6 C7 C8 C9 1.5(3) . . . . ? C7 C8 C9 C10 1.5(3) . . . . ? C8 C9 C10 C11 -2.7(3) . . . . ? C8 C9 C10 C13 178.64(19) . . . . ? C7 C6 C11 C10 2.2(3) . . . . ? C5 C6 C11 C10 -178.75(18) . . . . ? C9 C10 C11 C6 0.8(3) . . . . ? C13 C10 C11 C6 179.44(19) . . . . ? C9 C10 C13 N4 -150.7(2) . . . . ? C11 C10 C13 N4 30.7(3) . . . . ? C9 C10 C13 C12 29.6(3) . . . . ? C11 C10 C13 C12 -149.1(2) . . . . ? C9 C10 C13 N4B -149.6(8) . . . . ? C11 C10 C13 N4B 31.8(8) . . . . ? Zn1 S2 C14 N5 -4.6(2) 3_665 . . . ? Zn1 S2 C14 N6 174.6(2) 3_665 . . . ? N5 C14 N6 C15 177.9(2) . . . . ? S2 C14 N6 C15 -1.4(4) . . . . ? C14 N6 C15 C16 85.9(3) . . . . ? C14 N6 C15 N6B 1(5) . . . . ? C10 C13 N4 N5 0.7(3) . . . . ? C12 C13 N4 N5 -179.56(18) . . . . ? N4B C13 N4 N5 -1.3(14) . . . . ? C10 C13 N4 Zn1 175.28(15) . . . 3_665 ? C12 C13 N4 Zn1 -5.0(3) . . . 3_665 ? N4B C13 N4 Zn1 173.3(14) . . . 3_665 ? N6 C14 N5 N4 178.2(2) . . . . ? S2 C14 N5 N4 -2.6(3) . . . . ? C13 N4 N5 C14 -175.1(2) . . . . ? Zn1 N4 N5 C14 9.6(2) 3_665 . . . ? C5 N3 Zn1C N5B -73.7(7) . . . 3_665 ? N2 N3 Zn1C N5B 131.0(7) . . . 3_665 ? Zn1 N3 Zn1C N5B 22.7(8) . . . 3_665 ? C5 N3 Zn1C S1 159.47(18) . . . . ? N2 N3 Zn1C S1 4.1(3) . . . . ? Zn1 N3 Zn1C S1 -104.2(7) . . . . ? C5 N3 Zn1C S2B 12.4(4) . . . 3_665 ? N2 N3 Zn1C S2B -143.0(3) . . . 3_665 ? Zn1 N3 Zn1C S2B 108.7(8) . . . 3_665 ? C3 S1 Zn1C N5B -125.9(7) . . . 3_665 ? Zn1 S1 Zn1C N5B -41.6(8) . . . 3_665 ? C3 S1 Zn1C N3 -1.36(19) . . . . ? Zn1 S1 Zn1C N3 82.9(7) . . . . ? C3 S1 Zn1C S2B 139.0(4) . . . 3_665 ? Zn1 S1 Zn1C S2B -136.8(9) . . . 3_665 ? Zn1C S2B C14B N6B 173(3) 3_665 . . . ? Zn1C S2B C14B N5B -1.0(16) 3_665 . . . ? N4 C13 N4B N5B -4.2(9) . . . . ? C10 C13 N4B N5B 177.3(14) . . . . ? C12 C13 N4B N5B -1(3) . . . . ? C13 N4B N5B C14B 170.5(16) . . . . ? C13 N4B N5B Zn1C -5(4) . . . 3_665 ? N6B C14B N5B N4B 9(4) . . . . ? S2B C14B N5B N4B -176.4(17) . . . . ? N6B C14B N5B Zn1C -173(3) . . . 3_665 ? S2B C14B N5B Zn1C 1.2(18) . . . 3_665 ? N5B C14B N6B C15 173(2) . . . . ? S2B C14B N6B C15 0(5) . . . . ? N6 C15 N6B C14B -177(8) . . . . ? C16 C15 N6B C14B 81(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N5 0.84(2) 2.30(2) 3.051(3) 149(2) 2_644 # END of CIF # Attachment '- 3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-07-11 at 11:09:45 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : 3 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_11ZnLPh _database_code_depnum_ccdc_archive 'CCDC 893870' #TrackingRef '- 3.cif' _audit_creation_date 2012-07-11T11:09:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H44 N12 S4 Zn2, 2(C H Cl3)' _chemical_formula_sum 'C50 H46 Cl6 N12 S4 Zn2' _chemical_formula_weight 1286.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9266(2) _cell_length_b 12.5924(3) _cell_length_c 13.3789(3) _cell_angle_alpha 107.0830(10) _cell_angle_beta 104.0560(10) _cell_angle_gamma 99.2360(10) _cell_volume 1350.20(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4948 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 24.91 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.389 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.960 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_unetI/netI 0.0820 _diffrn_reflns_number 28152 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 6659 _reflns_number_gt 4280 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR2004 (Giacovazzo et all, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6659 _refine_ls_number_parameters 342 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.572 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3402(4) 0.7626(3) 0.3445(3) 0.0204(8) Uani 1 1 d . . . C2 C 0.2795(4) 0.7702(3) 0.4325(3) 0.0241(8) Uani 1 1 d . . . H2 H 0.2629 0.7082 0.4562 0.029 Uiso 1 1 calc R . . C3 C 0.2442(5) 0.8721(3) 0.4843(3) 0.0301(9) Uani 1 1 d . . . H3 H 0.2016 0.8767 0.5418 0.036 Uiso 1 1 calc R . . C4 C 0.2703(6) 0.9652(4) 0.4529(3) 0.0383(11) Uani 1 1 d . . . H4 H 0.2468 1.0325 0.4893 0.046 Uiso 1 1 calc R . . C5 C 0.3323(5) 0.9589(3) 0.3661(3) 0.0299(10) Uani 1 1 d . . . H5 H 0.35 1.0222 0.3443 0.036 Uiso 1 1 calc R . . C6 C 0.3675(5) 0.8596(3) 0.3125(3) 0.0253(9) Uani 1 1 d . . . H6 H 0.4096 0.8562 0.2548 0.03 Uiso 1 1 calc R . . C7 C 0.3653(4) 0.5575(3) 0.2872(3) 0.0186(8) Uani 1 1 d . . . C8 C 0.2813(4) 0.2730(3) 0.4397(3) 0.0213(8) Uani 1 1 d . . . H8A H 0.3356 0.2399 0.3894 0.032 Uiso 1 1 calc R . . H8B H 0.1736 0.2276 0.4162 0.032 Uiso 1 1 calc R . . H8C H 0.3354 0.2749 0.5119 0.032 Uiso 1 1 calc R . . C9 C 0.2802(4) 0.3932(3) 0.4426(3) 0.0166(7) Uani 1 1 d . . . C10 C 0.2332(4) 0.4654(3) 0.5328(3) 0.0169(7) Uani 1 1 d . . . C11 C 0.1114(4) 0.4139(3) 0.5664(3) 0.0213(8) Uani 1 1 d . . . H11 H 0.0637 0.3358 0.532 0.026 Uiso 1 1 calc R . . C12 C 0.0618(4) 0.4773(3) 0.6495(3) 0.0232(8) Uani 1 1 d . . . H12 H -0.0199 0.4419 0.6697 0.028 Uiso 1 1 calc R . . C13 C 0.1327(4) 0.5932(3) 0.7031(3) 0.0202(8) Uani 1 1 d . . . H13 H 0.0964 0.6361 0.7574 0.024 Uiso 1 1 calc R . . C14 C 0.2590(4) 0.6457(3) 0.6756(3) 0.0186(8) Uani 1 1 d . . . C15 C 0.3057(4) 0.5817(3) 0.5893(3) 0.0159(7) Uani 1 1 d . . . H15 H 0.3871 0.6174 0.5692 0.019 Uiso 1 1 calc R . . C16 C 0.2443(4) 0.8534(3) 0.7648(3) 0.0234(8) Uani 1 1 d . . . H16A H 0.2531 0.8756 0.8415 0.035 Uiso 1 1 calc R . . H16B H 0.1346 0.8195 0.7217 0.035 Uiso 1 1 calc R . . H16C H 0.2836 0.9199 0.7484 0.035 Uiso 1 1 calc R . . C17 C 0.3407(4) 0.7681(3) 0.7380(3) 0.0182(8) Uani 1 1 d . . . C18 C 0.7166(4) 0.9396(3) 0.8760(3) 0.0190(8) Uani 1 1 d . . . C19 C 0.7274(4) 1.1487(3) 0.9565(3) 0.0206(8) Uani 1 1 d . . . C20 C 0.5700(5) 1.1460(3) 0.9553(3) 0.0238(8) Uani 1 1 d . . . H20 H 0.4982 1.0769 0.9403 0.029 Uiso 1 1 calc R . . C21 C 0.5220(5) 1.2473(3) 0.9767(3) 0.0262(9) Uani 1 1 d . . . H21 H 0.4168 1.2454 0.9751 0.031 Uiso 1 1 calc R . . C22 C 0.6254(5) 1.3501(3) 0.9999(3) 0.0287(9) Uani 1 1 d . . . H22 H 0.5911 1.4174 1.0147 0.034 Uiso 1 1 calc R . . C23 C 0.7818(5) 1.3534(3) 1.0014(3) 0.0295(9) Uani 1 1 d . . . H23 H 0.8525 1.423 1.0162 0.035 Uiso 1 1 calc R . . C24 C 0.8327(5) 1.2537(3) 0.9809(3) 0.0276(9) Uani 1 1 d . . . H24 H 0.9383 1.2566 0.9834 0.033 Uiso 1 1 calc R . . C25 C 0.0911(5) 0.2036(4) 0.7596(3) 0.0378(11) Uani 1 1 d . . . H25 H -0.0134 0.1978 0.7105 0.045 Uiso 1 1 calc R . . N1 N 0.3743(4) 0.6644(3) 0.2814(2) 0.0226(7) Uani 1 1 d D . . H1N H 0.413(4) 0.672(3) 0.232(2) 0.027 Uiso 1 1 d D . . N2 N 0.3271(3) 0.5358(2) 0.3691(2) 0.0167(6) Uani 1 1 d . . . N3 N 0.3225(3) 0.4230(2) 0.3664(2) 0.0162(6) Uani 1 1 d . . . N4 N 0.4952(3) 0.7956(2) 0.7705(2) 0.0158(6) Uani 1 1 d . . . N5 N 0.5629(3) 0.9116(2) 0.8300(2) 0.0175(6) Uani 1 1 d . . . N6 N 0.7898(4) 1.0512(3) 0.9381(2) 0.0215(7) Uani 1 1 d . . . H6N H 0.886(5) 1.066(3) 0.956(3) 0.026 Uiso 1 1 d . . . S1 S 0.40936(14) 0.46583(9) 0.17717(8) 0.0302(3) Uani 1 1 d . . . S2 S 0.84715(11) 0.84911(8) 0.86934(8) 0.0254(2) Uani 1 1 d . . . Zn1 Zn 0.35587(5) 0.31271(3) 0.22879(3) 0.01748(13) Uani 1 1 d . . . Cl1 Cl 0.15326(15) 0.33670(10) 0.86802(10) 0.0467(3) Uani 1 1 d . . . Cl2 Cl 0.07559(14) 0.08982(10) 0.81081(9) 0.0418(3) Uani 1 1 d . . . Cl3 Cl 0.22864(17) 0.19416(12) 0.68532(10) 0.0558(4) 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 C1 0.025(2) 0.017(2) 0.0164(16) 0.0055(14) 0.0029(14) 0.0029(16) C2 0.028(2) 0.018(2) 0.0269(18) 0.0081(16) 0.0100(16) 0.0041(17) C3 0.043(3) 0.028(2) 0.0206(18) 0.0070(17) 0.0122(17) 0.012(2) C4 0.059(3) 0.022(2) 0.029(2) 0.0026(18) 0.011(2) 0.014(2) C5 0.048(3) 0.015(2) 0.0246(18) 0.0106(16) 0.0051(18) 0.0048(19) C6 0.030(2) 0.023(2) 0.0221(17) 0.0085(16) 0.0084(16) 0.0037(18) C7 0.0203(19) 0.0142(19) 0.0233(17) 0.0073(15) 0.0077(15) 0.0070(16) C8 0.026(2) 0.021(2) 0.0197(16) 0.0106(15) 0.0059(15) 0.0072(17) C9 0.0111(17) 0.0144(18) 0.0203(16) 0.0039(14) 0.0028(13) -0.0002(14) C10 0.0130(18) 0.0187(19) 0.0175(15) 0.0072(14) 0.0010(13) 0.0038(15) C11 0.023(2) 0.016(2) 0.0239(17) 0.0081(15) 0.0056(15) 0.0033(16) C12 0.018(2) 0.030(2) 0.0250(17) 0.0129(16) 0.0095(15) 0.0042(17) C13 0.0157(19) 0.029(2) 0.0189(16) 0.0091(15) 0.0058(14) 0.0092(16) C14 0.0158(19) 0.022(2) 0.0162(15) 0.0067(14) 0.0007(14) 0.0056(16) C15 0.0101(17) 0.021(2) 0.0154(15) 0.0064(14) 0.0030(13) 0.0027(15) C16 0.0191(19) 0.025(2) 0.0243(17) 0.0041(16) 0.0067(15) 0.0097(17) C17 0.022(2) 0.019(2) 0.0151(15) 0.0059(14) 0.0068(14) 0.0066(16) C18 0.019(2) 0.018(2) 0.0179(16) 0.0050(14) 0.0014(14) 0.0060(16) C19 0.028(2) 0.015(2) 0.0167(16) 0.0026(14) 0.0066(15) 0.0064(17) C20 0.026(2) 0.020(2) 0.0204(17) 0.0020(15) 0.0054(15) 0.0056(17) C21 0.032(2) 0.032(2) 0.0185(17) 0.0083(16) 0.0092(16) 0.0163(19) C22 0.045(3) 0.024(2) 0.0273(19) 0.0117(17) 0.0179(18) 0.021(2) C23 0.046(3) 0.019(2) 0.0280(19) 0.0104(16) 0.0150(18) 0.0113(19) C24 0.028(2) 0.025(2) 0.0271(19) 0.0024(16) 0.0116(17) 0.0065(18) C25 0.042(3) 0.037(3) 0.038(2) 0.008(2) 0.020(2) 0.017(2) N1 0.036(2) 0.0194(17) 0.0214(15) 0.0122(13) 0.0165(14) 0.0102(15) N2 0.0164(15) 0.0144(16) 0.0199(14) 0.0052(12) 0.0069(12) 0.0047(13) N3 0.0149(15) 0.0129(16) 0.0176(13) 0.0032(12) 0.0021(11) 0.0030(12) N4 0.0181(16) 0.0161(16) 0.0134(12) 0.0057(11) 0.0045(11) 0.0046(13) N5 0.0208(16) 0.0128(16) 0.0169(13) 0.0029(12) 0.0041(12) 0.0054(13) N6 0.0170(16) 0.0185(17) 0.0249(15) 0.0034(13) 0.0037(13) 0.0053(14) S1 0.0533(7) 0.0246(6) 0.0257(5) 0.0125(4) 0.0243(5) 0.0188(5) S2 0.0186(5) 0.0181(5) 0.0290(5) -0.0020(4) -0.0001(4) 0.0067(4) Zn1 0.0190(2) 0.0147(2) 0.01660(19) 0.00287(16) 0.00396(16) 0.00579(17) Cl1 0.0538(8) 0.0312(7) 0.0522(7) 0.0066(5) 0.0208(6) 0.0107(6) Cl2 0.0499(7) 0.0360(7) 0.0526(6) 0.0214(5) 0.0257(6) 0.0195(6) Cl3 0.0694(9) 0.0703(9) 0.0483(7) 0.0273(6) 0.0395(7) 0.0276(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.397(5) . ? C1 N1 1.402(5) . ? C1 C6 1.413(5) . ? C2 C3 1.392(5) . ? C2 H2 0.93 . ? C3 C4 1.361(6) . ? C3 H3 0.93 . ? C4 C5 1.391(6) . ? C4 H4 0.93 . ? C5 C6 1.373(5) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 N2 1.310(4) . ? C7 N1 1.362(5) . ? C7 S1 1.756(4) . ? C8 C9 1.504(5) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 N3 1.300(4) . ? C9 C10 1.478(5) . ? C10 C15 1.393(5) . ? C10 C11 1.410(5) . ? C11 C12 1.378(5) . ? C11 H11 0.93 . ? C12 C13 1.383(5) . ? C12 H12 0.93 . ? C13 C14 1.396(5) . ? C13 H13 0.93 . ? C14 C15 1.397(5) . ? C14 C17 1.480(5) . ? C15 H15 0.93 . ? C16 C17 1.497(5) . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C17 N4 1.296(4) . ? C18 N5 1.301(4) . ? C18 N6 1.360(5) . ? C18 S2 1.756(4) . ? C19 C24 1.392(5) . ? C19 C20 1.396(5) . ? C19 N6 1.408(5) . ? C20 C21 1.383(5) . ? C20 H20 0.93 . ? C21 C22 1.366(6) . ? C21 H21 0.93 . ? C22 C23 1.385(6) . ? C22 H22 0.93 . ? C23 C24 1.378(5) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 Cl3 1.755(4) . ? C25 Cl2 1.760(5) . ? C25 Cl1 1.762(4) . ? C25 H25 0.98 . ? N1 H1N 0.840(18) . ? N2 N3 1.404(4) . ? N3 Zn1 2.074(3) . ? N4 N5 1.391(4) . ? N4 Zn1 2.052(3) 2_666 ? N6 H6N 0.81(4) . ? S1 Zn1 2.2516(11) . ? S2 Zn1 2.2907(10) 2_666 ? Zn1 N4 2.052(3) 2_666 ? Zn1 S2 2.2907(10) 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 C2 C1 N1 125.5(3) . . ? C2 C1 C6 118.9(3) . . ? N1 C1 C6 115.7(3) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 121.8(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.4(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? N2 C7 N1 119.2(3) . . ? N2 C7 S1 129.1(3) . . ? N1 C7 S1 111.8(2) . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 126.9(3) . . ? N3 C9 C8 116.7(3) . . ? C10 C9 C8 116.5(3) . . ? C15 C10 C11 117.6(3) . . ? C15 C10 C9 123.7(3) . . ? C11 C10 C9 118.6(3) . . ? C12 C11 C10 121.1(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 119.3(3) . . ? C13 C14 C17 119.5(3) . . ? C15 C14 C17 121.2(3) . . ? C10 C15 C14 121.5(3) . . ? C10 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C14 117.4(3) . . ? N4 C17 C16 122.8(3) . . ? C14 C17 C16 119.8(3) . . ? N5 C18 N6 118.4(3) . . ? N5 C18 S2 127.8(3) . . ? N6 C18 S2 113.8(3) . . ? C24 C19 C20 119.0(3) . . ? C24 C19 N6 117.0(3) . . ? C20 C19 N6 124.0(3) . . ? C21 C20 C19 119.3(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 121.5(4) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 119.5(4) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C23 C24 C19 120.6(4) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? Cl3 C25 Cl2 109.6(2) . . ? Cl3 C25 Cl1 109.6(2) . . ? Cl2 C25 Cl1 110.6(2) . . ? Cl3 C25 H25 109 . . ? Cl2 C25 H25 109 . . ? Cl1 C25 H25 109 . . ? C7 N1 C1 132.8(3) . . ? C7 N1 H1N 112(3) . . ? C1 N1 H1N 116(3) . . ? C7 N2 N3 113.9(3) . . ? C9 N3 N2 117.8(3) . . ? C9 N3 Zn1 125.4(2) . . ? N2 N3 Zn1 116.2(2) . . ? C17 N4 N5 113.9(3) . . ? C17 N4 Zn1 127.7(2) . 2_666 ? N5 N4 Zn1 117.2(2) . 2_666 ? C18 N5 N4 115.4(3) . . ? C18 N6 C19 130.1(3) . . ? C18 N6 H6N 115(3) . . ? C19 N6 H6N 114(3) . . ? C7 S1 Zn1 93.16(12) . . ? C18 S2 Zn1 93.07(12) . 2_666 ? N4 Zn1 N3 125.87(11) 2_666 . ? N4 Zn1 S1 120.84(8) 2_666 . ? N3 Zn1 S1 87.23(8) . . ? N4 Zn1 S2 86.31(8) 2_666 2_666 ? N3 Zn1 S2 115.53(8) . 2_666 ? S1 Zn1 S2 125.46(4) . 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 N1 C1 C2 C3 -176.9(3) . . . . ? C6 C1 C2 C3 1.6(5) . . . . ? C1 C2 C3 C4 -1.4(6) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C3 C4 C5 C6 -0.2(6) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C2 C1 C6 C5 -1.1(5) . . . . ? N1 C1 C6 C5 177.5(3) . . . . ? N3 C9 C10 C15 -38.4(5) . . . . ? C8 C9 C10 C15 140.7(3) . . . . ? N3 C9 C10 C11 143.6(4) . . . . ? C8 C9 C10 C11 -37.3(4) . . . . ? C15 C10 C11 C12 2.4(5) . . . . ? C9 C10 C11 C12 -179.5(3) . . . . ? C10 C11 C12 C13 -1.0(5) . . . . ? C11 C12 C13 C14 -2.2(5) . . . . ? C12 C13 C14 C15 3.8(5) . . . . ? C12 C13 C14 C17 -176.2(3) . . . . ? C11 C10 C15 C14 -0.6(5) . . . . ? C9 C10 C15 C14 -178.7(3) . . . . ? C13 C14 C15 C10 -2.5(5) . . . . ? C17 C14 C15 C10 177.6(3) . . . . ? C13 C14 C17 N4 133.5(3) . . . . ? C15 C14 C17 N4 -46.6(5) . . . . ? C13 C14 C17 C16 -44.2(5) . . . . ? C15 C14 C17 C16 135.7(3) . . . . ? C24 C19 C20 C21 1.0(5) . . . . ? N6 C19 C20 C21 178.7(3) . . . . ? C19 C20 C21 C22 -0.7(5) . . . . ? C20 C21 C22 C23 0.6(5) . . . . ? C21 C22 C23 C24 -0.8(5) . . . . ? C22 C23 C24 C19 1.3(6) . . . . ? C20 C19 C24 C23 -1.3(5) . . . . ? N6 C19 C24 C23 -179.1(3) . . . . ? N2 C7 N1 C1 -4.9(6) . . . . ? S1 C7 N1 C1 175.2(3) . . . . ? C2 C1 N1 C7 -2.3(7) . . . . ? C6 C1 N1 C7 179.2(4) . . . . ? N1 C7 N2 N3 -179.7(3) . . . . ? S1 C7 N2 N3 0.3(5) . . . . ? C10 C9 N3 N2 1.0(5) . . . . ? C8 C9 N3 N2 -178.1(3) . . . . ? C10 C9 N3 Zn1 -170.6(2) . . . . ? C8 C9 N3 Zn1 10.3(4) . . . . ? C7 N2 N3 C9 -177.7(3) . . . . ? C7 N2 N3 Zn1 -5.4(4) . . . . ? C14 C17 N4 N5 -179.1(3) . . . . ? C16 C17 N4 N5 -1.4(4) . . . . ? C14 C17 N4 Zn1 -12.2(4) . . . 2_666 ? C16 C17 N4 Zn1 165.4(2) . . . 2_666 ? N6 C18 N5 N4 -178.1(3) . . . . ? S2 C18 N5 N4 1.4(4) . . . . ? C17 N4 N5 C18 171.3(3) . . . . ? Zn1 N4 N5 C18 3.1(4) 2_666 . . . ? N5 C18 N6 C19 -5.2(6) . . . . ? S2 C18 N6 C19 175.2(3) . . . . ? C24 C19 N6 C18 -152.3(4) . . . . ? C20 C19 N6 C18 30.0(6) . . . . ? N2 C7 S1 Zn1 4.0(3) . . . . ? N1 C7 S1 Zn1 -176.0(3) . . . . ? N5 C18 S2 Zn1 -4.2(3) . . . 2_666 ? N6 C18 S2 Zn1 175.3(2) . . . 2_666 ? C9 N3 Zn1 N4 -55.2(3) . . . 2_666 ? N2 N3 Zn1 N4 133.1(2) . . . 2_666 ? C9 N3 Zn1 S1 178.0(3) . . . . ? N2 N3 Zn1 S1 6.4(2) . . . . ? C9 N3 Zn1 S2 49.7(3) . . . 2_666 ? N2 N3 Zn1 S2 -122.0(2) . . . 2_666 ? C7 S1 Zn1 N4 -135.46(15) . . . 2_666 ? C7 S1 Zn1 N3 -4.60(14) . . . . ? C7 S1 Zn1 S2 115.09(12) . . . 2_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6N S2 0.81(4) 2.70(4) 3.384(3) 144(4) 2_777 # END of CIF # Attachment '- 4.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-07-11 at 11:35:13 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : 4 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_13ZnLPhNO2 _database_code_depnum_ccdc_archive 'CCDC 893871' #TrackingRef '- 4.cif' _audit_creation_date 2012-07-11T11:35:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C48 H40 N16 O8 S4 Zn2), 5(C3 H6 O)' _chemical_formula_sum 'C111 H110 N32 O21 S8 Zn4' _chemical_formula_weight 2746.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1425(7) _cell_length_b 15.4703(10) _cell_length_c 18.6236(11) _cell_angle_alpha 97.906(3) _cell_angle_beta 91.450(2) _cell_angle_gamma 107.563(2) _cell_volume 3024.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1371 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 17.88 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.1378 _diffrn_reflns_av_unetI/netI 0.1538 _diffrn_reflns_number 38469 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 8384 _reflns_number_gt 4701 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+11.6395P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8384 _refine_ls_number_parameters 796 _refine_ls_number_restraints 483 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.895 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1526(6) 0.3723(5) 0.2105(4) 0.0139(17) Uani 1 1 d U . . C2 C 0.1433(7) 0.2849(5) 0.2227(4) 0.0213(19) Uani 1 1 d U . . H2 H 0.1293 0.2361 0.1833 0.026 Uiso 1 1 calc R . . C3 C 0.1546(7) 0.2698(5) 0.2933(4) 0.0214(19) Uani 1 1 d U . . H3 H 0.1482 0.2097 0.3024 0.026 Uiso 1 1 calc R . . C4 C 0.1750(7) 0.3396(5) 0.3511(4) 0.0159(18) Uani 1 1 d U . . C5 C 0.1824(6) 0.4282(5) 0.3384(4) 0.0157(18) Uani 1 1 d U . . H5 H 0.1962 0.4768 0.3778 0.019 Uiso 1 1 calc R . . C6 C 0.1695(6) 0.4440(5) 0.2672(4) 0.0148(18) Uani 1 1 d U . . H6 H 0.1722 0.5033 0.2576 0.018 Uiso 1 1 calc R . . C7 C 0.2344(6) 0.3680(5) 0.4862(4) 0.0108(17) Uani 1 1 d U . . C8 C 0.4761(7) 0.6361(5) 0.6324(4) 0.0211(19) Uani 1 1 d U . . H8A H 0.422 0.6689 0.6566 0.032 Uiso 1 1 calc R . . H8B H 0.5578 0.68 0.6259 0.032 Uiso 1 1 calc R . . H8C H 0.4889 0.5917 0.6621 0.032 Uiso 1 1 calc R . . C9 C 0.4135(6) 0.5861(5) 0.5587(4) 0.0109(17) Uani 1 1 d U . . C10 C 0.4264(6) 0.6427(4) 0.4983(4) 0.0102(16) Uani 1 1 d U . . C11 C 0.4250(6) 0.7327(5) 0.5148(4) 0.0170(18) Uani 1 1 d U . . H11 H 0.4192 0.7574 0.5637 0.02 Uiso 1 1 calc R . . C12 C 0.4320(7) 0.7872(5) 0.4601(4) 0.0195(19) Uani 1 1 d U . . H12 H 0.4292 0.8483 0.4714 0.023 Uiso 1 1 calc R . . C13 C 0.4432(6) 0.7507(5) 0.3889(4) 0.0137(17) Uani 1 1 d U . . H13 H 0.4462 0.787 0.3514 0.016 Uiso 1 1 calc R . . C14 C 0.4500(6) 0.6628(5) 0.3718(4) 0.0111(17) Uani 1 1 d U . . C15 C 0.4399(6) 0.6084(5) 0.4276(3) 0.0102(16) Uani 1 1 d U . . H15 H 0.4425 0.5473 0.4163 0.012 Uiso 1 1 calc R . . C16 C 0.4001(7) 0.6487(5) 0.2342(4) 0.0209(19) Uani 1 1 d U . . H16A H 0.4617 0.6905 0.2082 0.031 Uiso 1 1 calc R . . H16B H 0.3383 0.6782 0.2527 0.031 Uiso 1 1 calc R . . H16C H 0.3567 0.5922 0.201 0.031 Uiso 1 1 calc R . . C17 C 0.4670(6) 0.6260(4) 0.2968(4) 0.0110(17) Uani 1 1 d U . . C18 C 0.6393(7) 0.5048(5) 0.2043(4) 0.0145(18) Uani 1 1 d U . . C19 C 0.5561(7) 0.4202(5) 0.0782(4) 0.0151(18) Uani 1 1 d U . . C20 C 0.4422(7) 0.4384(5) 0.0713(4) 0.0185(18) Uani 1 1 d U . . H20 H 0.4205 0.4788 0.1082 0.022 Uiso 1 1 calc R . . C21 C 0.3600(7) 0.3975(5) 0.0105(4) 0.0197(19) Uani 1 1 d U . . H21 H 0.2816 0.4093 0.0056 0.024 Uiso 1 1 calc R . . C22 C 0.3935(6) 0.3395(5) -0.0429(4) 0.0140(17) Uani 1 1 d U . . C23 C 0.5081(6) 0.3224(5) -0.0378(4) 0.0167(18) Uani 1 1 d U . . H23 H 0.5306 0.2834 -0.0754 0.02 Uiso 1 1 calc R . . C24 C 0.5879(7) 0.3627(5) 0.0221(4) 0.0142(18) Uani 1 1 d U . . H24 H 0.667 0.3516 0.026 0.017 Uiso 1 1 calc R . . C25 C 0.8814(7) 0.3071(5) 0.5056(4) 0.0160(18) Uani 1 1 d U . . C26 C 0.8889(6) 0.3896(5) 0.4821(4) 0.0162(18) Uani 1 1 d U . . H26 H 0.902 0.4439 0.5161 0.019 Uiso 1 1 calc R . . C27 C 0.8770(6) 0.3917(5) 0.4084(4) 0.0173(18) Uani 1 1 d U . . H27 H 0.8826 0.4479 0.3915 0.021 Uiso 1 1 calc R . . C28 C 0.8568(6) 0.3117(5) 0.3585(4) 0.0111(17) Uani 1 1 d U . . C29 C 0.8514(7) 0.2295(5) 0.3830(4) 0.0197(19) Uani 1 1 d U . . H29 H 0.839 0.1751 0.3493 0.024 Uiso 1 1 calc R . . C30 C 0.8644(6) 0.2278(5) 0.4576(4) 0.0170(18) Uani 1 1 d U . . H30 H 0.8615 0.1724 0.475 0.02 Uiso 1 1 calc R . . C31 C 0.8281(6) 0.2601(5) 0.2226(4) 0.0110(17) Uani 1 1 d U . . C32 C 0.9184(7) 0.0312(5) 0.2175(4) 0.0209(19) Uani 1 1 d U . . H32A H 1.0061 0.07 0.2178 0.031 Uiso 1 1 calc R . . H32B H 0.9153 -0.0334 0.2111 0.031 Uiso 1 1 calc R . . H32C H 0.884 0.0467 0.2637 0.031 Uiso 1 1 calc R . . C33 C 0.8419(6) 0.0470(5) 0.1565(4) 0.0142(17) Uani 1 1 d U . . C34 C 0.8042(6) -0.0216(5) 0.0899(4) 0.0131(17) Uani 1 1 d U . . C35 C 0.8840(7) -0.0702(5) 0.0627(4) 0.0186(18) Uani 1 1 d U . . H35 H 0.9641 -0.0597 0.0872 0.022 Uiso 1 1 calc R . . C36 C 0.8474(7) -0.1334(5) 0.0003(4) 0.025(2) Uani 1 1 d U . . H36 H 0.9028 -0.1658 -0.0183 0.03 Uiso 1 1 calc R . . C37 C 0.7307(7) -0.1501(5) -0.0353(4) 0.0200(19) Uani 1 1 d U . . H37 H 0.7076 -0.1926 -0.079 0.024 Uiso 1 1 calc R . . C38 C 0.6464(6) -0.1054(5) -0.0079(4) 0.0125(17) Uani 1 1 d U . . C39 C 0.6857(6) -0.0412(4) 0.0550(3) 0.0107(17) Uani 1 1 d U . . H39 H 0.6295 -0.01 0.0746 0.013 Uiso 1 1 calc R . . C40 C 0.5139(7) -0.1475(5) -0.1283(3) 0.0185(18) Uani 1 1 d U . . H40A H 0.437 -0.1387 -0.1484 0.028 Uiso 1 1 calc R . . H40B H 0.5124 -0.2111 -0.1432 0.028 Uiso 1 1 calc R . . H40C H 0.5878 -0.1059 -0.1465 0.028 Uiso 1 1 calc R . . C41 C 0.5209(6) -0.1270(5) -0.0467(4) 0.0130(17) Uani 1 1 d U . . C42 C 0.3118(7) -0.1181(5) 0.0850(4) 0.0159(18) Uani 1 1 d U . . C43 C 0.4042(6) -0.0770(5) 0.2152(4) 0.0140(18) Uani 1 1 d U . . C44 C 0.5186(6) -0.0941(5) 0.2075(4) 0.0167(18) Uani 1 1 d U . . H44 H 0.5375 -0.12 0.1615 0.02 Uiso 1 1 calc R . . C45 C 0.6059(7) -0.0735(5) 0.2669(4) 0.0225(19) Uani 1 1 d U . . H45 H 0.6839 -0.086 0.2621 0.027 Uiso 1 1 calc R . . C46 C 0.5777(7) -0.0345(5) 0.3331(4) 0.0196(19) Uani 1 1 d U . . C47 C 0.4653(7) -0.0181(5) 0.3422(4) 0.027(2) Uani 1 1 d U . . H47 H 0.4473 0.0072 0.3885 0.032 Uiso 1 1 calc R . . C48 C 0.3775(7) -0.0386(5) 0.2837(4) 0.0204(19) Uani 1 1 d U . . H48 H 0.2992 -0.0267 0.2897 0.024 Uiso 1 1 calc R . . N1 N 0.1407(6) 0.3893(4) 0.1357(3) 0.0205(15) Uani 1 1 d U . . N2 N 0.1806(5) 0.3152(4) 0.4207(3) 0.0189(15) Uani 1 1 d U . . H2A H 0.1438 0.2567 0.4229 0.023 Uiso 1 1 calc R . . N3 N 0.2947(5) 0.4541(4) 0.4867(3) 0.0143(14) Uani 1 1 d U . . N4 N 0.3527(5) 0.5004(4) 0.5542(3) 0.0130(14) Uani 1 1 d U . . N5 N 0.5421(5) 0.5763(4) 0.2876(3) 0.0165(15) Uani 1 1 d U . . N6 N 0.5442(5) 0.5356(4) 0.2162(3) 0.0173(15) Uani 1 1 d U . . N7 N 0.6463(5) 0.4572(4) 0.1373(3) 0.0185(15) Uani 1 1 d U . . H7 H 0.7198 0.4484 0.1303 0.022 Uiso 1 1 calc R . . N8 N 0.3055(6) 0.2943(4) -0.1054(3) 0.0234(16) Uani 1 1 d U . . N9 N 0.8880(6) 0.3047(4) 0.5841(3) 0.0241(16) Uani 1 1 d U . . N10 N 0.8429(5) 0.3210(4) 0.2857(3) 0.0144(14) Uani 1 1 d U . . H10 H 0.8437 0.3763 0.2788 0.017 Uiso 1 1 calc R . . N11 N 0.8261(5) 0.1766(4) 0.2257(3) 0.0149(15) Uani 1 1 d U . . N12 N 0.8063(5) 0.1200(4) 0.1586(3) 0.0131(14) Uani 1 1 d U . . N13 N 0.4162(5) -0.1297(4) -0.0169(3) 0.0111(14) Uani 1 1 d U . . N14 N 0.4200(5) -0.1119(4) 0.0588(3) 0.0137(14) Uani 1 1 d U . . N15 N 0.3089(5) -0.0971(4) 0.1596(3) 0.0188(15) Uani 1 1 d U . . H15A H 0.2348 -0.0963 0.1745 0.023 Uiso 1 1 calc R . . N16 N 0.6684(6) -0.0136(4) 0.3964(3) 0.0255(16) Uani 1 1 d U . . O1 O 0.1153(5) 0.3225(4) 0.0864(3) 0.0268(13) Uani 1 1 d U . . O2 O 0.1607(5) 0.4697(3) 0.1251(3) 0.0275(13) Uani 1 1 d U . . O3 O 0.3326(5) 0.2388(4) -0.1505(3) 0.0289(14) Uani 1 1 d U . . O4 O 0.2050(5) 0.3116(4) -0.1106(3) 0.0311(14) Uani 1 1 d U . . O5 O 0.8652(5) 0.2292(3) 0.6042(3) 0.0261(13) Uani 1 1 d U . . O6 O 0.9106(5) 0.3775(4) 0.6253(3) 0.0330(14) Uani 1 1 d U . . O7 O 0.6405(5) 0.0194(4) 0.4552(3) 0.0315(14) Uani 1 1 d U . . O8 O 0.7677(5) -0.0309(4) 0.3874(3) 0.0441(16) Uani 1 1 d U . . S1 S 0.21122(18) 0.30249(13) 0.55700(10) 0.0210(5) Uani 1 1 d . . . S2 S 0.77317(17) 0.52161(13) 0.26339(10) 0.0175(5) Uani 1 1 d . . . S3 S 0.81915(18) 0.31036(13) 0.14444(10) 0.0187(5) Uani 1 1 d . . . S4 S 0.16161(17) -0.14894(14) 0.04048(10) 0.0194(5) Uani 1 1 d . . . Zn1 Zn 0.31755(8) 0.42488(6) 0.63927(4) 0.0153(2) Uani 1 1 d . . . Zn2 Zn 0.76323(8) 0.17329(6) 0.06942(4) 0.0148(2) Uani 1 1 d . . . C49 C 0.9448(7) 0.2797(5) 0.7885(4) 0.025(2) Uani 1 1 d U . . H49A H 0.9131 0.3024 0.7478 0.038 Uiso 1 1 calc R . . H49B H 1.0176 0.3279 0.8142 0.038 Uiso 1 1 calc R . . H49C H 0.8782 0.2625 0.822 0.038 Uiso 1 1 calc R . . O9 O 0.9235(5) 0.1210(3) 0.7706(3) 0.0248(13) Uani 1 1 d DU . . C50 C 0.9840(7) 0.1972(5) 0.7603(4) 0.0169(18) Uani 1 1 d DU . . C51 C 1.0961(7) 0.2123(5) 0.7180(4) 0.025(2) Uani 1 1 d DU . . H51A H 1.1128 0.1539 0.7038 0.038 Uiso 1 1 calc R . . H51B H 1.169 0.2556 0.7476 0.038 Uiso 1 1 calc R . . H51C H 1.0813 0.2375 0.6743 0.038 Uiso 1 1 calc R . . C52 C 0.0781(8) -0.0309(5) 0.4252(4) 0.038(2) Uani 1 1 d U . . H52A H -0.0143 -0.0505 0.42 0.057 Uiso 1 1 calc R . . H52B H 0.1059 -0.0413 0.4727 0.057 Uiso 1 1 calc R . . H52C H 0.1098 -0.0662 0.3867 0.057 Uiso 1 1 calc R . . O10 O 0.0646(5) 0.1163(4) 0.4077(3) 0.0375(15) Uani 1 1 d U . . C53 C 0.1276(8) 0.0677(6) 0.4197(4) 0.033(2) Uani 1 1 d U . . C54 C 0.2693(8) 0.1129(6) 0.4310(5) 0.056(3) Uani 1 1 d U . . H54A H 0.3045 0.1219 0.3839 0.085 Uiso 1 1 calc R . . H54B H 0.3076 0.0736 0.4543 0.085 Uiso 1 1 calc R . . H54C H 0.2874 0.1725 0.4621 0.085 Uiso 1 1 calc R . . O11 O 0.8753(11) 0.4758(8) 0.0532(7) 0.054(4) Uiso 0.5 1 d PD A -1 C55 C 0.9623(14) 0.4973(10) 0.0182(8) 0.032(5) Uiso 0.5 1 d PD A -1 C56 C 1.0323(10) 0.5869(7) 0.0304(6) 0.083(4) Uiso 1 1 d D A -1 H56A H 0.977 0.6249 0.0412 0.124 Uiso 1 1 calc R A -1 H56B H 1.077 0.6031 -0.0128 0.124 Uiso 1 1 calc R A -1 H56C H 1.0938 0.5975 0.0719 0.124 Uiso 1 1 calc R A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.013(2) 0.016(2) 0.012(2) 0.0013(18) 0.0001(17) 0.0030(18) C2 0.022(3) 0.023(3) 0.019(3) 0.0021(18) 0.0001(18) 0.0071(18) C3 0.023(3) 0.021(2) 0.019(3) 0.0042(18) 0.0015(18) 0.0052(18) C4 0.015(2) 0.016(2) 0.015(2) 0.0004(18) 0.0006(18) 0.0026(18) C5 0.014(2) 0.017(2) 0.015(2) 0.0015(18) 0.0014(18) 0.0040(18) C6 0.014(2) 0.015(2) 0.014(2) 0.0023(18) 0.0005(17) 0.0033(18) C7 0.010(2) 0.013(2) 0.009(2) 0.0005(18) 0.0000(17) 0.0029(17) C8 0.021(3) 0.021(2) 0.021(3) 0.0028(18) 0.0018(18) 0.0059(18) C9 0.009(2) 0.012(2) 0.011(2) -0.0002(18) 0.0003(17) 0.0042(17) C10 0.008(2) 0.010(2) 0.011(2) 0.0022(18) 0.0013(17) 0.0010(17) C11 0.015(2) 0.019(2) 0.016(2) 0.0017(18) 0.0034(18) 0.0048(18) C12 0.019(2) 0.019(2) 0.020(2) 0.0023(18) 0.0005(18) 0.0058(18) C13 0.015(2) 0.014(2) 0.013(2) 0.0030(18) 0.0011(17) 0.0051(18) C14 0.009(2) 0.011(2) 0.012(2) 0.0014(18) -0.0002(17) 0.0024(17) C15 0.008(2) 0.010(2) 0.012(2) 0.0018(18) 0.0000(17) 0.0021(17) C16 0.021(3) 0.022(2) 0.021(2) 0.0046(18) 0.0006(18) 0.0072(18) C17 0.012(2) 0.010(2) 0.012(2) 0.0038(18) -0.0001(17) 0.0034(18) C18 0.014(2) 0.016(2) 0.013(2) 0.0019(18) 0.0014(18) 0.0044(18) C19 0.016(2) 0.016(2) 0.013(2) 0.0024(18) 0.0015(18) 0.0035(18) C20 0.019(2) 0.019(2) 0.018(2) 0.0007(18) 0.0018(18) 0.0076(18) C21 0.019(2) 0.020(2) 0.020(2) 0.0033(18) 0.0020(18) 0.0067(18) C22 0.015(2) 0.014(2) 0.011(2) 0.0021(18) -0.0006(18) 0.0025(18) C23 0.018(2) 0.016(2) 0.016(2) 0.0021(18) 0.0021(18) 0.0059(18) C24 0.013(2) 0.015(2) 0.015(2) 0.0007(18) 0.0005(18) 0.0070(18) C25 0.015(2) 0.018(2) 0.014(2) 0.0019(18) -0.0001(18) 0.0044(18) C26 0.014(2) 0.017(2) 0.017(2) 0.0000(18) 0.0019(18) 0.0043(18) C27 0.017(2) 0.018(2) 0.017(2) 0.0026(18) 0.0011(18) 0.0049(18) C28 0.010(2) 0.012(2) 0.009(2) 0.0011(18) -0.0007(17) 0.0009(17) C29 0.020(2) 0.019(2) 0.019(2) 0.0017(18) 0.0007(18) 0.0046(18) C30 0.017(2) 0.017(2) 0.017(2) 0.0031(18) 0.0001(18) 0.0055(18) C31 0.010(2) 0.012(2) 0.010(2) -0.0001(18) 0.0008(17) 0.0029(18) C32 0.021(3) 0.020(2) 0.022(3) 0.0030(18) -0.0009(18) 0.0068(18) C33 0.013(2) 0.014(2) 0.015(2) 0.0027(18) 0.0018(17) 0.0025(18) C34 0.012(2) 0.013(2) 0.015(2) 0.0020(18) 0.0012(17) 0.0039(18) C35 0.016(2) 0.019(2) 0.019(2) 0.0012(18) 0.0014(18) 0.0042(18) C36 0.023(3) 0.025(3) 0.027(3) 0.0013(18) 0.0015(18) 0.0099(18) C37 0.019(3) 0.020(2) 0.019(2) 0.0007(18) 0.0007(18) 0.0046(18) C38 0.011(2) 0.013(2) 0.014(2) 0.0028(18) 0.0010(17) 0.0036(18) C39 0.010(2) 0.012(2) 0.011(2) 0.0014(18) 0.0011(17) 0.0040(17) C40 0.018(2) 0.019(2) 0.018(2) 0.0026(18) 0.0026(18) 0.0050(18) C41 0.014(2) 0.013(2) 0.013(2) 0.0028(18) 0.0015(18) 0.0052(18) C42 0.016(2) 0.015(2) 0.016(2) 0.0035(18) 0.0005(18) 0.0039(18) C43 0.013(2) 0.015(2) 0.013(2) 0.0002(18) -0.0004(18) 0.0047(18) C44 0.015(2) 0.018(2) 0.017(2) 0.0016(18) 0.0010(18) 0.0058(18) C45 0.022(3) 0.024(3) 0.022(3) 0.0037(18) 0.0009(18) 0.0083(18) C46 0.019(2) 0.021(2) 0.018(2) 0.0037(18) -0.0017(18) 0.0045(18) C47 0.027(3) 0.028(3) 0.025(3) 0.0011(18) 0.0019(18) 0.0091(19) C48 0.019(3) 0.022(2) 0.020(3) 0.0005(18) 0.0023(18) 0.0074(18) N1 0.020(2) 0.022(2) 0.019(2) 0.0024(17) 0.0018(17) 0.0060(17) N2 0.020(2) 0.018(2) 0.016(2) 0.0037(17) -0.0012(17) 0.0019(17) N3 0.015(2) 0.014(2) 0.014(2) 0.0018(17) 0.0003(16) 0.0034(16) N4 0.012(2) 0.014(2) 0.012(2) 0.0003(17) 0.0014(16) 0.0045(16) N5 0.016(2) 0.018(2) 0.015(2) 0.0031(17) 0.0017(17) 0.0039(17) N6 0.018(2) 0.017(2) 0.016(2) 0.0014(17) 0.0003(17) 0.0054(17) N7 0.016(2) 0.022(2) 0.018(2) -0.0001(17) -0.0002(17) 0.0087(17) N8 0.022(2) 0.025(2) 0.024(2) 0.0030(18) 0.0009(17) 0.0079(17) N9 0.023(2) 0.025(2) 0.023(2) 0.0023(18) 0.0010(17) 0.0061(17) N10 0.016(2) 0.013(2) 0.014(2) 0.0009(17) 0.0002(16) 0.0041(16) N11 0.015(2) 0.015(2) 0.015(2) 0.0011(17) 0.0003(16) 0.0047(17) N12 0.012(2) 0.014(2) 0.013(2) -0.0001(17) 0.0002(16) 0.0035(16) N13 0.011(2) 0.012(2) 0.010(2) 0.0016(16) 0.0003(16) 0.0032(16) N14 0.013(2) 0.016(2) 0.013(2) 0.0006(17) 0.0019(16) 0.0047(16) N15 0.016(2) 0.021(2) 0.017(2) 0.0010(17) 0.0026(17) 0.0048(17) N16 0.025(2) 0.027(2) 0.025(2) 0.0034(18) -0.0001(18) 0.0088(18) O1 0.027(2) 0.028(2) 0.022(2) 0.0006(16) -0.0001(16) 0.0072(16) O2 0.029(2) 0.027(2) 0.027(2) 0.0070(16) 0.0003(16) 0.0072(16) O3 0.027(2) 0.031(2) 0.029(2) 0.0018(17) 0.0001(16) 0.0113(16) O4 0.027(2) 0.037(2) 0.031(2) 0.0008(17) -0.0030(16) 0.0143(17) O5 0.029(2) 0.026(2) 0.025(2) 0.0067(16) -0.0013(16) 0.0084(16) O6 0.038(2) 0.033(2) 0.029(2) 0.0071(17) -0.0009(16) 0.0111(17) O7 0.032(2) 0.032(2) 0.029(2) 0.0028(17) -0.0002(16) 0.0093(16) O8 0.039(2) 0.052(2) 0.041(2) 0.0033(17) -0.0002(17) 0.0169(17) S1 0.0246(12) 0.0198(12) 0.0150(11) 0.0051(9) -0.0009(9) 0.0005(10) S2 0.0145(11) 0.0214(12) 0.0158(11) 0.0019(9) -0.0011(9) 0.0050(9) S3 0.0223(12) 0.0154(11) 0.0168(11) 0.0025(9) -0.0043(9) 0.0041(9) S4 0.0089(11) 0.0309(13) 0.0167(11) 0.0024(10) 0.0001(9) 0.0040(10) Zn1 0.0143(5) 0.0186(5) 0.0118(5) 0.0031(4) -0.0007(4) 0.0030(4) Zn2 0.0115(5) 0.0185(5) 0.0132(5) 0.0012(4) -0.0026(4) 0.0037(4) C49 0.026(3) 0.027(3) 0.023(3) 0.0044(18) 0.0013(18) 0.0074(18) O9 0.023(2) 0.025(2) 0.026(2) 0.0036(16) 0.0037(16) 0.0074(16) C50 0.017(2) 0.018(2) 0.016(2) 0.0057(18) -0.0007(18) 0.0056(18) C51 0.025(3) 0.026(3) 0.024(3) 0.0053(18) 0.0036(18) 0.0069(18) C52 0.039(3) 0.036(3) 0.038(3) 0.0059(19) 0.0011(19) 0.0114(19) O10 0.038(2) 0.036(2) 0.040(2) 0.0068(17) -0.0013(17) 0.0121(17) C53 0.033(3) 0.034(3) 0.033(3) 0.0043(19) 0.0024(19) 0.0111(19) C54 0.055(3) 0.056(3) 0.058(3) 0.007(2) 0.0047(19) 0.017(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.375(9) . ? C1 C6 1.387(9) . ? C1 N1 1.463(8) . ? C2 C3 1.377(9) . ? C2 H2 0.95 . ? C3 C4 1.377(9) . ? C3 H3 0.95 . ? C4 C5 1.401(9) . ? C4 N2 1.403(8) . ? C5 C6 1.393(9) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 N3 1.298(8) . ? C7 N2 1.382(8) . ? C7 S1 1.749(6) . ? C8 C9 1.517(9) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 N4 1.284(8) . ? C9 C10 1.502(8) . ? C10 C15 1.380(9) . ? C10 C11 1.389(9) . ? C11 C12 1.399(9) . ? C11 H11 0.95 . ? C12 C13 1.392(9) . ? C12 H12 0.95 . ? C13 C14 1.379(9) . ? C13 H13 0.95 . ? C14 C15 1.410(8) . ? C14 C17 1.474(9) . ? C15 H15 0.95 . ? C16 C17 1.506(9) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 N5 1.296(8) . ? C18 N6 1.299(8) . ? C18 N7 1.375(8) . ? C18 S2 1.763(7) . ? C19 C20 1.388(9) . ? C19 C24 1.400(9) . ? C19 N7 1.404(8) . ? C20 C21 1.386(9) . ? C20 H20 0.95 . ? C21 C22 1.382(9) . ? C21 H21 0.95 . ? C22 C23 1.384(9) . ? C22 N8 1.453(9) . ? C23 C24 1.359(9) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C30 1.374(9) . ? C25 C26 1.386(9) . ? C25 N9 1.467(9) . ? C26 C27 1.381(9) . ? C26 H26 0.95 . ? C27 C28 1.397(9) . ? C27 H27 0.95 . ? C28 N10 1.393(8) . ? C28 C29 1.394(9) . ? C29 C30 1.398(9) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 N11 1.295(8) . ? C31 N10 1.372(8) . ? C31 S3 1.756(6) . ? C32 C33 1.493(9) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 N12 1.301(8) . ? C33 C34 1.478(9) . ? C34 C39 1.386(9) . ? C34 C35 1.389(9) . ? C35 C36 1.377(10) . ? C35 H35 0.95 . ? C36 C37 1.379(10) . ? C36 H36 0.95 . ? C37 C38 1.393(9) . ? C37 H37 0.95 . ? C38 C39 1.394(9) . ? C38 C41 1.480(9) . ? C39 H39 0.95 . ? C40 C41 1.505(9) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 N13 1.297(8) . ? C42 N14 1.294(8) . ? C42 N15 1.387(8) . ? C42 S4 1.747(7) . ? C43 C44 1.385(9) . ? C43 N15 1.397(8) . ? C43 C48 1.411(9) . ? C44 C45 1.391(9) . ? C44 H44 0.95 . ? C45 C46 1.383(10) . ? C45 H45 0.95 . ? C46 C47 1.360(10) . ? C46 N16 1.467(9) . ? C47 C48 1.381(10) . ? C47 H47 0.95 . ? C48 H48 0.95 . ? N1 O2 1.239(7) . ? N1 O1 1.241(7) . ? N2 H2A 0.88 . ? N3 N4 1.395(7) . ? N4 Zn1 2.072(5) . ? N5 N6 1.394(7) . ? N5 Zn1 2.054(5) 2_666 ? N7 H7 0.88 . ? N8 O3 1.226(7) . ? N8 O4 1.232(7) . ? N9 O6 1.226(7) . ? N9 O5 1.231(7) . ? N10 H10 0.88 . ? N11 N12 1.394(7) . ? N12 Zn2 2.061(5) . ? N13 N14 1.396(7) . ? N13 Zn2 2.076(5) 2_655 ? N15 H15A 0.88 . ? N16 O8 1.224(7) . ? N16 O7 1.232(7) . ? S1 Zn1 2.257(2) . ? S2 Zn1 2.276(2) 2_666 ? S3 Zn2 2.276(2) . ? S4 Zn2 2.258(2) 2_655 ? Zn1 N5 2.054(5) 2_666 ? Zn1 S2 2.276(2) 2_666 ? Zn2 N13 2.076(5) 2_655 ? Zn2 S4 2.258(2) 2_655 ? C49 C50 1.502(10) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? O9 C50 1.213(7) . ? C50 C51 1.470(9) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 C53 1.477(11) . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? O10 C53 1.210(8) . ? C53 C54 1.518(11) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? O11 C55 1.172(13) . ? C55 C56 1.354(15) . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? 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 C2 C1 C6 121.8(6) . . ? C2 C1 N1 119.0(6) . . ? C6 C1 N1 119.2(6) . . ? C1 C2 C3 118.5(7) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C2 C3 C4 121.6(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 N2 116.5(6) . . ? C5 C4 N2 123.8(7) . . ? C6 C5 C4 119.2(7) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C1 C6 C5 119.3(6) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? N3 C7 N2 118.3(6) . . ? N3 C7 S1 130.2(5) . . ? N2 C7 S1 111.5(5) . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 126.3(6) . . ? N4 C9 C8 117.3(6) . . ? C10 C9 C8 116.4(6) . . ? C15 C10 C11 119.3(6) . . ? C15 C10 C9 122.3(6) . . ? C11 C10 C9 118.4(6) . . ? C10 C11 C12 120.6(7) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.2(7) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 121.1(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 118.7(6) . . ? C13 C14 C17 120.8(6) . . ? C15 C14 C17 120.4(6) . . ? C10 C15 C14 121.0(6) . . ? C10 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C14 118.0(6) . . ? N5 C17 C16 122.5(6) . . ? C14 C17 C16 119.5(6) . . ? N6 C18 N7 119.8(6) . . ? N6 C18 S2 127.7(6) . . ? N7 C18 S2 112.3(5) . . ? C20 C19 C24 119.1(7) . . ? C20 C19 N7 124.9(7) . . ? C24 C19 N7 116.0(6) . . ? C21 C20 C19 119.9(7) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 119.3(7) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 121.6(7) . . ? C21 C22 N8 119.2(6) . . ? C23 C22 N8 119.2(6) . . ? C24 C23 C22 118.7(7) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C19 121.4(7) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C30 C25 C26 121.8(6) . . ? C30 C25 N9 119.7(6) . . ? C26 C25 N9 118.5(6) . . ? C27 C26 C25 118.9(7) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 120.4(6) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? N10 C28 C29 124.4(6) . . ? N10 C28 C27 115.8(6) . . ? C29 C28 C27 119.9(6) . . ? C28 C29 C30 119.5(7) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 119.4(6) . . ? C25 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? N11 C31 N10 119.7(6) . . ? N11 C31 S3 127.5(6) . . ? N10 C31 S3 112.8(5) . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N12 C33 C34 117.2(6) . . ? N12 C33 C32 122.8(6) . . ? C34 C33 C32 120.0(6) . . ? C39 C34 C35 118.8(7) . . ? C39 C34 C33 120.0(6) . . ? C35 C34 C33 121.2(6) . . ? C36 C35 C34 120.2(7) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C37 120.4(7) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 120.9(7) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C39 117.8(6) . . ? C37 C38 C41 119.2(6) . . ? C39 C38 C41 123.0(6) . . ? C34 C39 C38 121.9(6) . . ? C34 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N13 C41 C38 126.1(6) . . ? N13 C41 C40 116.8(6) . . ? C38 C41 C40 117.1(6) . . ? N14 C42 N15 118.0(6) . . ? N14 C42 S4 130.0(6) . . ? N15 C42 S4 112.0(5) . . ? C44 C43 N15 124.7(7) . . ? C44 C43 C48 119.4(6) . . ? N15 C43 C48 115.9(6) . . ? C43 C44 C45 120.1(7) . . ? C43 C44 H44 120 . . ? C45 C44 H44 120 . . ? C46 C45 C44 119.2(7) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C47 C46 C45 121.7(7) . . ? C47 C46 N16 118.6(7) . . ? C45 C46 N16 119.6(6) . . ? C46 C47 C48 119.8(8) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C43 119.9(7) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? O2 N1 O1 124.0(6) . . ? O2 N1 C1 118.2(6) . . ? O1 N1 C1 117.8(6) . . ? C7 N2 C4 130.5(6) . . ? C7 N2 H2A 114.8 . . ? C4 N2 H2A 114.8 . . ? C7 N3 N4 114.2(5) . . ? C9 N4 N3 117.5(5) . . ? C9 N4 Zn1 126.7(5) . . ? N3 N4 Zn1 115.6(4) . . ? C17 N5 N6 115.2(5) . . ? C17 N5 Zn1 126.3(5) . 2_666 ? N6 N5 Zn1 117.0(4) . 2_666 ? C18 N6 N5 114.6(6) . . ? C18 N7 C19 131.0(6) . . ? C18 N7 H7 114.5 . . ? C19 N7 H7 114.5 . . ? O3 N8 O4 122.2(6) . . ? O3 N8 C22 118.9(6) . . ? O4 N8 C22 118.9(6) . . ? O6 N9 O5 124.3(6) . . ? O6 N9 C25 118.0(6) . . ? O5 N9 C25 117.7(6) . . ? C31 N10 C28 132.2(6) . . ? C31 N10 H10 113.9 . . ? C28 N10 H10 113.9 . . ? C31 N11 N12 114.8(5) . . ? C33 N12 N11 116.0(5) . . ? C33 N12 Zn2 125.4(5) . . ? N11 N12 Zn2 117.0(4) . . ? C41 N13 N14 117.9(5) . . ? C41 N13 Zn2 126.5(5) . 2_655 ? N14 N13 Zn2 115.2(4) . 2_655 ? C42 N14 N13 114.7(6) . . ? C42 N15 C43 130.7(6) . . ? C42 N15 H15A 114.7 . . ? C43 N15 H15A 114.7 . . ? O8 N16 O7 123.8(6) . . ? O8 N16 C46 117.6(7) . . ? O7 N16 C46 118.6(6) . . ? C7 S1 Zn1 92.1(2) . . ? C18 S2 Zn1 92.6(2) . 2_666 ? C31 S3 Zn2 93.3(2) . . ? C42 S4 Zn2 92.3(3) . 2_655 ? N5 Zn1 N4 122.6(2) 2_666 . ? N5 Zn1 S1 123.62(17) 2_666 . ? N4 Zn1 S1 87.62(17) . . ? N5 Zn1 S2 86.44(17) 2_666 2_666 ? N4 Zn1 S2 117.96(16) . 2_666 ? S1 Zn1 S2 122.61(8) . 2_666 ? N12 Zn2 N13 122.3(2) . 2_655 ? N12 Zn2 S4 123.70(16) . 2_655 ? N13 Zn2 S4 87.55(16) 2_655 2_655 ? N12 Zn2 S3 85.71(17) . . ? N13 Zn2 S3 116.86(16) 2_655 . ? S4 Zn2 S3 124.76(8) 2_655 . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O9 C50 C51 121.4(7) . . ? O9 C50 C49 121.1(7) . . ? C51 C50 C49 117.4(6) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O10 C53 C52 125.5(8) . . ? O10 C53 C54 116.8(8) . . ? C52 C53 C54 117.6(7) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O11 C55 C56 116.4(15) . . ? 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 C6 C1 C2 C3 -1.8(11) . . . . ? N1 C1 C2 C3 180.0(6) . . . . ? C1 C2 C3 C4 -0.1(11) . . . . ? C2 C3 C4 C5 1.0(11) . . . . ? C2 C3 C4 N2 177.9(6) . . . . ? C3 C4 C5 C6 -0.2(10) . . . . ? N2 C4 C5 C6 -176.8(6) . . . . ? C2 C1 C6 C5 2.6(10) . . . . ? N1 C1 C6 C5 -179.2(6) . . . . ? C4 C5 C6 C1 -1.6(10) . . . . ? N4 C9 C10 C15 -37.7(10) . . . . ? C8 C9 C10 C15 143.9(7) . . . . ? N4 C9 C10 C11 142.5(7) . . . . ? C8 C9 C10 C11 -36.0(9) . . . . ? C15 C10 C11 C12 2.5(10) . . . . ? C9 C10 C11 C12 -177.6(6) . . . . ? C10 C11 C12 C13 -1.3(10) . . . . ? C11 C12 C13 C14 -1.3(10) . . . . ? C12 C13 C14 C15 2.7(10) . . . . ? C12 C13 C14 C17 -177.5(6) . . . . ? C11 C10 C15 C14 -1.1(10) . . . . ? C9 C10 C15 C14 179.0(6) . . . . ? C13 C14 C15 C10 -1.5(10) . . . . ? C17 C14 C15 C10 178.7(6) . . . . ? C13 C14 C17 N5 139.9(7) . . . . ? C15 C14 C17 N5 -40.3(9) . . . . ? C13 C14 C17 C16 -38.7(9) . . . . ? C15 C14 C17 C16 141.1(6) . . . . ? C24 C19 C20 C21 2.0(10) . . . . ? N7 C19 C20 C21 -179.7(6) . . . . ? C19 C20 C21 C22 -0.5(10) . . . . ? C20 C21 C22 C23 -1.2(10) . . . . ? C20 C21 C22 N8 178.0(6) . . . . ? C21 C22 C23 C24 1.3(10) . . . . ? N8 C22 C23 C24 -177.9(6) . . . . ? C22 C23 C24 C19 0.2(10) . . . . ? C20 C19 C24 C23 -1.9(10) . . . . ? N7 C19 C24 C23 179.7(6) . . . . ? C30 C25 C26 C27 1.0(11) . . . . ? N9 C25 C26 C27 -177.1(6) . . . . ? C25 C26 C27 C28 0.5(10) . . . . ? C26 C27 C28 N10 178.4(6) . . . . ? C26 C27 C28 C29 -1.4(10) . . . . ? N10 C28 C29 C30 -178.9(6) . . . . ? C27 C28 C29 C30 0.9(10) . . . . ? C26 C25 C30 C29 -1.5(11) . . . . ? N9 C25 C30 C29 176.6(6) . . . . ? C28 C29 C30 C25 0.5(10) . . . . ? N12 C33 C34 C39 -39.0(9) . . . . ? C32 C33 C34 C39 141.5(7) . . . . ? N12 C33 C34 C35 143.7(7) . . . . ? C32 C33 C34 C35 -35.9(9) . . . . ? C39 C34 C35 C36 2.9(10) . . . . ? C33 C34 C35 C36 -179.6(6) . . . . ? C34 C35 C36 C37 -0.8(11) . . . . ? C35 C36 C37 C38 -1.8(11) . . . . ? C36 C37 C38 C39 2.2(10) . . . . ? C36 C37 C38 C41 -178.5(6) . . . . ? C35 C34 C39 C38 -2.5(10) . . . . ? C33 C34 C39 C38 180.0(6) . . . . ? C37 C38 C39 C34 0.0(10) . . . . ? C41 C38 C39 C34 -179.3(6) . . . . ? C37 C38 C41 N13 144.9(7) . . . . ? C39 C38 C41 N13 -35.9(10) . . . . ? C37 C38 C41 C40 -35.3(9) . . . . ? C39 C38 C41 C40 144.0(6) . . . . ? N15 C43 C44 C45 -178.3(6) . . . . ? C48 C43 C44 C45 0.0(10) . . . . ? C43 C44 C45 C46 -1.0(10) . . . . ? C44 C45 C46 C47 1.9(11) . . . . ? C44 C45 C46 N16 179.2(6) . . . . ? C45 C46 C47 C48 -1.6(11) . . . . ? N16 C46 C47 C48 -179.0(6) . . . . ? C46 C47 C48 C43 0.6(11) . . . . ? C44 C43 C48 C47 0.2(10) . . . . ? N15 C43 C48 C47 178.7(6) . . . . ? C2 C1 N1 O2 -173.5(6) . . . . ? C6 C1 N1 O2 8.2(9) . . . . ? C2 C1 N1 O1 4.1(9) . . . . ? C6 C1 N1 O1 -174.2(6) . . . . ? N3 C7 N2 C4 -2.7(11) . . . . ? S1 C7 N2 C4 178.9(6) . . . . ? C3 C4 N2 C7 158.4(7) . . . . ? C5 C4 N2 C7 -24.9(11) . . . . ? N2 C7 N3 N4 -176.0(6) . . . . ? S1 C7 N3 N4 2.0(9) . . . . ? C10 C9 N4 N3 1.5(10) . . . . ? C8 C9 N4 N3 179.9(6) . . . . ? C10 C9 N4 Zn1 -172.8(5) . . . . ? C8 C9 N4 Zn1 5.6(9) . . . . ? C7 N3 N4 C9 -179.6(6) . . . . ? C7 N3 N4 Zn1 -4.8(7) . . . . ? C14 C17 N5 N6 173.6(5) . . . . ? C16 C17 N5 N6 -7.9(9) . . . . ? C14 C17 N5 Zn1 -20.8(9) . . . 2_666 ? C16 C17 N5 Zn1 157.7(5) . . . 2_666 ? N7 C18 N6 N5 175.1(6) . . . . ? S2 C18 N6 N5 -8.9(9) . . . . ? C17 N5 N6 C18 164.4(6) . . . . ? Zn1 N5 N6 C18 -2.7(7) 2_666 . . . ? N6 C18 N7 C19 -11.9(11) . . . . ? S2 C18 N7 C19 171.5(6) . . . . ? C20 C19 N7 C18 11.6(11) . . . . ? C24 C19 N7 C18 -170.0(6) . . . . ? C21 C22 N8 O3 -175.8(6) . . . . ? C23 C22 N8 O3 3.4(9) . . . . ? C21 C22 N8 O4 2.7(9) . . . . ? C23 C22 N8 O4 -178.1(6) . . . . ? C30 C25 N9 O6 175.8(6) . . . . ? C26 C25 N9 O6 -6.0(10) . . . . ? C30 C25 N9 O5 -7.2(10) . . . . ? C26 C25 N9 O5 170.9(6) . . . . ? N11 C31 N10 C28 -0.4(11) . . . . ? S3 C31 N10 C28 -178.3(6) . . . . ? C29 C28 N10 C31 -3.7(11) . . . . ? C27 C28 N10 C31 176.5(7) . . . . ? N10 C31 N11 N12 177.9(5) . . . . ? S3 C31 N11 N12 -4.4(9) . . . . ? C34 C33 N12 N11 170.6(5) . . . . ? C32 C33 N12 N11 -9.9(9) . . . . ? C34 C33 N12 Zn2 -24.3(8) . . . . ? C32 C33 N12 Zn2 155.3(5) . . . . ? C31 N11 N12 C33 159.4(6) . . . . ? C31 N11 N12 Zn2 -7.1(7) . . . . ? C38 C41 N13 N14 -0.8(10) . . . . ? C40 C41 N13 N14 179.3(5) . . . . ? C38 C41 N13 Zn2 -172.9(5) . . . 2_655 ? C40 C41 N13 Zn2 7.2(8) . . . 2_655 ? N15 C42 N14 N13 -177.0(5) . . . . ? S4 C42 N14 N13 2.3(9) . . . . ? C41 N13 N14 C42 -178.2(6) . . . . ? Zn2 N13 N14 C42 -5.2(7) 2_655 . . . ? N14 C42 N15 C43 -6.6(11) . . . . ? S4 C42 N15 C43 174.0(6) . . . . ? C44 C43 N15 C42 -15.4(11) . . . . ? C48 C43 N15 C42 166.2(7) . . . . ? C47 C46 N16 O8 178.3(7) . . . . ? C45 C46 N16 O8 0.9(10) . . . . ? C47 C46 N16 O7 -1.2(10) . . . . ? C45 C46 N16 O7 -178.5(6) . . . . ? N3 C7 S1 Zn1 1.5(7) . . . . ? N2 C7 S1 Zn1 179.6(5) . . . . ? N6 C18 S2 Zn1 13.5(6) . . . 2_666 ? N7 C18 S2 Zn1 -170.3(5) . . . 2_666 ? N11 C31 S3 Zn2 11.4(6) . . . . ? N10 C31 S3 Zn2 -170.9(5) . . . . ? N14 C42 S4 Zn2 1.4(7) . . . 2_655 ? N15 C42 S4 Zn2 -179.3(5) . . . 2_655 ? C9 N4 Zn1 N5 -51.9(6) . . . 2_666 ? N3 N4 Zn1 N5 133.8(4) . . . 2_666 ? C9 N4 Zn1 S1 179.0(6) . . . . ? N3 N4 Zn1 S1 4.7(4) . . . . ? C9 N4 Zn1 S2 53.0(6) . . . 2_666 ? N3 N4 Zn1 S2 -121.4(4) . . . 2_666 ? C7 S1 Zn1 N5 -131.1(3) . . . 2_666 ? C7 S1 Zn1 N4 -2.8(3) . . . . ? C7 S1 Zn1 S2 119.2(2) . . . 2_666 ? C33 N12 Zn2 N13 87.0(6) . . . 2_655 ? N11 N12 Zn2 N13 -108.0(4) . . . 2_655 ? C33 N12 Zn2 S4 -24.2(6) . . . 2_655 ? N11 N12 Zn2 S4 140.8(4) . . . 2_655 ? C33 N12 Zn2 S3 -153.8(6) . . . . ? N11 N12 Zn2 S3 11.3(4) . . . . ? C31 S3 Zn2 N12 -9.8(3) . . . . ? C31 S3 Zn2 N13 114.5(3) . . . 2_655 ? C31 S3 Zn2 S4 -138.5(2) . . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O10 0.88 2.06 2.928(8) 169.1 . N7 H7 O11 0.88 2.26 2.988(13) 140.5 . N7 H7 S3 0.88 2.72 3.405(6) 135.2 . N10 H10 S2 0.88 2.64 3.493(6) 162.7 . N15 H15A O9 0.88 2.02 2.873(7) 161.8 2_656 # END of CIF # Attachment '- 5.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-07-11 at 11:23:09 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : 5 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_15ZnLPhOMe _database_code_depnum_ccdc_archive 'CCDC 893872' #TrackingRef '- 5.cif' _audit_creation_date 2012-07-11T11:23:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H52 N12 O4 S4 Zn2' _chemical_formula_sum 'C52 H52 N12 O4 S4 Zn2' _chemical_formula_weight 1168.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9413(3) _cell_length_b 12.1646(4) _cell_length_c 13.6340(5) _cell_angle_alpha 65.614(2) _cell_angle_beta 76.570(2) _cell_angle_gamma 70.636(2) _cell_volume 1266.36(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1988 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 0.975 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_unetI/netI 0.0613 _diffrn_reflns_number 18926 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4981 _reflns_number_gt 3694 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.8262P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4981 _refine_ls_number_parameters 353 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.08 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.73 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2905(4) 1.2252(3) 0.4821(3) 0.0331(9) Uani 1 1 d . . . H1A H -0.312 1.207 0.4255 0.05 Uiso 1 1 calc R . . H1B H -0.2422 1.2936 0.4508 0.05 Uiso 1 1 calc R . . H1C H -0.3885 1.2474 0.5252 0.05 Uiso 1 1 calc R . . C2 C -0.2334(4) 1.0086(3) 0.5961(2) 0.0208(7) Uani 1 1 d . . . C3 C -0.1208(4) 0.9021(3) 0.6505(2) 0.0223(7) Uani 1 1 d . . . H3 H -0.0198 0.9079 0.6507 0.027 Uiso 1 1 calc R . . C4 C -0.1555(4) 0.7879(3) 0.7041(2) 0.0200(7) Uani 1 1 d . . . H4 H -0.0787 0.718 0.7406 0.024 Uiso 1 1 calc R . . C5 C -0.3061(4) 0.7774(3) 0.7036(2) 0.0161(7) Uani 1 1 d . . . C6 C -0.4164(4) 0.8840(3) 0.6474(2) 0.0204(7) Uani 1 1 d . . . H6 H -0.5167 0.8783 0.6452 0.024 Uiso 1 1 calc R . . C7 C -0.3816(4) 0.9989(3) 0.5943(2) 0.0203(7) Uani 1 1 d . . . H7 H -0.458 1.0691 0.5577 0.024 Uiso 1 1 calc R . . C8 C -0.2812(4) 0.5494(3) 0.8217(2) 0.0167(7) Uani 1 1 d . . . C9 C 0.1706(4) 0.4941(3) 0.8369(3) 0.0229(7) Uani 1 1 d . . . H9A H 0.1554 0.5258 0.7617 0.034 Uiso 1 1 calc R . . H9B H 0.2826 0.4636 0.8444 0.034 Uiso 1 1 calc R . . H9C H 0.1236 0.56 0.865 0.034 Uiso 1 1 calc R . . C10 C 0.0925(4) 0.3892(3) 0.8989(2) 0.0175(7) Uani 1 1 d . . . C11 C 0.1856(3) 0.2669(3) 0.9678(2) 0.0152(6) Uani 1 1 d . . . C12 C 0.3094(4) 0.2617(3) 1.0181(2) 0.0168(7) Uani 1 1 d . . . H12 H 0.3329 0.3352 1.0072 0.02 Uiso 1 1 calc R . . C13 C 0.3962(4) 0.1483(3) 1.0836(2) 0.0192(7) Uani 1 1 d . . . H13 H 0.4787 0.1456 1.116 0.023 Uiso 1 1 calc R . . C14 C 0.3615(4) 0.0386(3) 1.1014(2) 0.0184(7) Uani 1 1 d . . . H14 H 0.4174 -0.037 1.1486 0.022 Uiso 1 1 calc R . . C15 C 0.2431(3) 0.0404(3) 1.0492(2) 0.0143(6) Uani 1 1 d . . . C16 C 0.1577(3) 0.1550(3) 0.9817(2) 0.0151(6) Uani 1 1 d . . . H16 H 0.0804 0.157 0.9452 0.018 Uiso 1 1 calc R . . C17 C 0.2082(4) -0.1713(3) 1.1839(2) 0.0213(7) Uani 1 1 d . . . H17A H 0.1531 -0.2306 1.1916 0.032 Uiso 1 1 calc R . . H17B H 0.1528 -0.1264 1.2311 0.032 Uiso 1 1 calc R . . H17C H 0.3148 -0.2149 1.2027 0.032 Uiso 1 1 calc R . . C18 C 0.2142(4) -0.0813(3) 1.0691(2) 0.0162(7) Uani 1 1 d . . . C19 C 0.1968(3) -0.0680(3) 0.8152(2) 0.0150(6) Uani 1 1 d . A . C20 C 0.2038(4) 0.1406(3) 0.6658(2) 0.0169(7) Uani 1 1 d . A . C21 C 0.1599(4) 0.2128(3) 0.5627(3) 0.0265(8) Uani 1 1 d . . . H21 H 0.1162 0.1807 0.5283 0.032 Uiso 1 1 calc R . . C22 C 0.1804(5) 0.3328(3) 0.5098(3) 0.0377(10) Uani 1 1 d . A . H22 H 0.15 0.3808 0.4405 0.045 Uiso 1 1 calc R . . C23 C 0.2462(5) 0.3806(3) 0.5609(3) 0.0352(9) Uani 1 1 d U . . C24 C 0.2891(4) 0.3088(3) 0.6638(3) 0.0291(8) Uani 1 1 d . A . H24 H 0.3326 0.3411 0.6983 0.035 Uiso 1 1 calc R . . C26 C 0.234(3) 0.5721(16) 0.4055(11) 0.047(3) Uani 0.58(3) 1 d PU A 1 H26A H 0.2929 0.5352 0.3532 0.07 Uiso 0.58(3) 1 calc PR A 1 H26B H 0.2475 0.6543 0.3834 0.07 Uiso 0.58(3) 1 calc PR A 1 H26C H 0.1226 0.578 0.4105 0.07 Uiso 0.58(3) 1 calc PR A 1 C25 C 0.2689(4) 0.1898(3) 0.7166(3) 0.0226(7) Uani 1 1 d . . . H25 H 0.2987 0.1425 0.786 0.027 Uiso 1 1 calc R A . N1 N -0.3591(3) 0.6672(2) 0.7603(2) 0.0179(6) Uani 1 1 d . . . N2 N -0.1288(3) 0.5258(2) 0.8263(2) 0.0167(6) Uani 1 1 d . . . N3 N -0.0570(3) 0.4053(2) 0.89419(19) 0.0155(5) Uani 1 1 d . . . N4 N 0.1958(3) -0.1156(2) 0.99543(19) 0.0152(5) Uani 1 1 d . . . N5 N 0.1927(3) -0.0264(2) 0.89004(19) 0.0157(6) Uani 1 1 d . . . N6 N 0.1894(3) 0.0161(2) 0.7105(2) 0.0187(6) Uani 1 1 d . . . O1 O -0.1850(3) 1.11771(19) 0.54867(18) 0.0297(6) Uani 1 1 d . . . O2 O 0.2937(19) 0.4912(12) 0.5152(10) 0.0380(17) Uani 0.58(3) 1 d PU A 1 S1 S -0.40349(9) 0.44722(7) 0.88519(6) 0.01944(19) Uani 1 1 d . . . S2 S 0.21386(9) -0.22163(7) 0.82865(6) 0.01789(18) Uani 1 1 d . . . Zn1 Zn -0.21014(4) 0.29625(3) 0.98708(3) 0.01571(11) Uani 1 1 d . . . O2B O 0.240(2) 0.5067(18) 0.5183(13) 0.0380(17) Uani 0.42(3) 1 d PD A 2 C26B C 0.299(3) 0.550(2) 0.4003(15) 0.047(3) Uani 0.42(3) 1 d PD A 2 H26D H 0.3852 0.484 0.3857 0.07 Uiso 0.42(3) 1 calc PR A 2 H26E H 0.3371 0.6221 0.381 0.07 Uiso 0.42(3) 1 calc PR A 2 H26F H 0.2143 0.5708 0.3585 0.07 Uiso 0.42(3) 1 calc PR A 2 H1N H -0.463(5) 0.682(4) 0.764(3) 0.056 Uiso 1 1 d . . . H6N H 0.177(4) -0.007(3) 0.665(3) 0.024(9) Uiso 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 C1 0.051(3) 0.0177(18) 0.031(2) -0.0037(16) -0.0060(18) -0.0150(17) C2 0.0256(19) 0.0177(17) 0.0195(17) -0.0040(14) -0.0016(14) -0.0104(14) C3 0.0201(19) 0.0227(18) 0.0232(18) -0.0022(15) -0.0041(15) -0.0116(14) C4 0.0189(18) 0.0170(16) 0.0228(18) -0.0029(14) -0.0073(14) -0.0054(13) C5 0.0187(17) 0.0149(16) 0.0160(16) -0.0051(13) -0.0032(13) -0.0057(13) C6 0.0174(18) 0.0190(17) 0.0236(18) -0.0038(14) -0.0061(14) -0.0062(14) C7 0.0243(19) 0.0126(16) 0.0197(17) -0.0021(13) -0.0052(14) -0.0025(13) C8 0.0225(19) 0.0125(16) 0.0158(16) -0.0038(13) -0.0060(14) -0.0047(13) C9 0.0180(18) 0.0147(16) 0.034(2) -0.0022(15) -0.0074(15) -0.0070(14) C10 0.0202(18) 0.0132(16) 0.0224(17) -0.0065(14) -0.0054(14) -0.0065(13) C11 0.0125(16) 0.0157(16) 0.0166(16) -0.0055(13) -0.0016(13) -0.0031(12) C12 0.0178(17) 0.0157(16) 0.0199(17) -0.0074(13) 0.0001(13) -0.0086(13) C13 0.0165(17) 0.0243(18) 0.0215(17) -0.0112(15) -0.0045(14) -0.0061(14) C14 0.0183(18) 0.0164(16) 0.0172(16) -0.0044(13) -0.0064(14) 0.0002(13) C15 0.0145(17) 0.0118(15) 0.0143(15) -0.0040(13) -0.0009(13) -0.0022(12) C16 0.0117(16) 0.0153(16) 0.0186(16) -0.0051(13) -0.0036(13) -0.0039(12) C17 0.0265(19) 0.0168(16) 0.0188(17) -0.0040(14) -0.0044(14) -0.0055(14) C18 0.0119(17) 0.0135(15) 0.0205(17) -0.0051(13) -0.0030(13) -0.0007(12) C19 0.0117(16) 0.0108(15) 0.0209(17) -0.0018(13) -0.0059(13) -0.0032(12) C20 0.0218(18) 0.0114(15) 0.0134(16) -0.0015(13) 0.0001(13) -0.0047(13) C21 0.042(2) 0.0188(18) 0.0209(18) -0.0071(15) -0.0065(16) -0.0099(16) C22 0.071(3) 0.0205(19) 0.0196(19) -0.0023(16) -0.0105(19) -0.0130(19) C23 0.070(3) 0.0192(18) 0.0184(17) -0.0036(14) 0.0028(18) -0.0237(18) C24 0.048(2) 0.0245(19) 0.0222(18) -0.0087(15) 0.0020(17) -0.0220(17) C26 0.095(9) 0.026(5) 0.018(2) -0.002(3) 0.006(5) -0.030(6) C25 0.031(2) 0.0184(17) 0.0162(17) -0.0005(14) -0.0028(15) -0.0114(15) N1 0.0145(14) 0.0126(13) 0.0240(15) -0.0020(11) -0.0046(12) -0.0045(11) N2 0.0166(15) 0.0088(13) 0.0207(14) 0.0014(11) -0.0085(11) -0.0027(11) N3 0.0147(14) 0.0115(13) 0.0202(14) -0.0041(11) -0.0042(11) -0.0037(11) N4 0.0144(14) 0.0114(13) 0.0168(13) -0.0016(11) -0.0027(11) -0.0038(10) N5 0.0174(15) 0.0121(13) 0.0171(14) -0.0034(11) -0.0051(11) -0.0037(11) N6 0.0280(17) 0.0142(14) 0.0151(14) -0.0029(12) -0.0084(12) -0.0063(12) O1 0.0375(15) 0.0150(12) 0.0344(14) 0.0009(10) -0.0089(12) -0.0139(11) O2 0.077(5) 0.020(3) 0.0184(14) -0.0015(16) 0.003(3) -0.027(4) S1 0.0155(4) 0.0139(4) 0.0259(4) -0.0004(3) -0.0057(3) -0.0068(3) S2 0.0234(5) 0.0117(4) 0.0198(4) -0.0040(3) -0.0048(3) -0.0068(3) Zn1 0.0170(2) 0.01094(19) 0.0184(2) -0.00218(15) -0.00413(15) -0.00540(14) O2B 0.077(5) 0.020(3) 0.0184(14) -0.0015(16) 0.003(3) -0.027(4) C26B 0.095(9) 0.026(5) 0.018(2) -0.002(3) 0.006(5) -0.030(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.422(4) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 C7 1.375(4) . ? C2 O1 1.382(3) . ? C2 C3 1.389(4) . ? C3 C4 1.379(4) . ? C3 H3 0.93 . ? C4 C5 1.396(4) . ? C4 H4 0.93 . ? C5 C6 1.387(4) . ? C5 N1 1.419(4) . ? C6 C7 1.386(4) . ? C6 H6 0.93 . ? C7 H7 0.93 . ? C8 N2 1.306(4) . ? C8 N1 1.364(4) . ? C8 S1 1.750(3) . ? C9 C10 1.502(4) . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 N3 1.298(4) . ? C10 C11 1.476(4) . ? C11 C16 1.393(4) . ? C11 C12 1.403(4) . ? C12 C13 1.377(4) . ? C12 H12 0.93 . ? C13 C14 1.381(4) . ? C13 H13 0.93 . ? C14 C15 1.397(4) . ? C14 H14 0.93 . ? C15 C16 1.391(4) . ? C15 C18 1.490(4) . ? C16 H16 0.93 . ? C17 C18 1.496(4) . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C17 H17C 0.96 . ? C18 N4 1.296(4) . ? C19 N5 1.302(4) . ? C19 N6 1.371(4) . ? C19 S2 1.758(3) . ? C20 C21 1.382(4) . ? C20 C25 1.392(4) . ? C20 N6 1.419(4) . ? C21 C22 1.390(4) . ? C21 H21 0.93 . ? C22 C23 1.387(5) . ? C22 H22 0.93 . ? C23 C24 1.377(5) . ? C23 O2B 1.38(2) . ? C23 O2 1.394(14) . ? C24 C25 1.377(4) . ? C24 H24 0.93 . ? C26 O2 1.517(17) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C25 H25 0.93 . ? N1 H1N 0.88(4) . ? N2 N3 1.396(3) . ? N3 Zn1 2.061(2) . ? N4 N5 1.398(3) . ? N4 Zn1 2.073(2) 2_557 ? N6 H6N 0.82(3) . ? S1 Zn1 2.2793(8) . ? S2 Zn1 2.2880(8) 2_557 ? Zn1 N4 2.073(2) 2_557 ? Zn1 S2 2.2880(8) 2_557 ? O2B C26B 1.496(18) . ? C26B H26D 0.96 . ? C26B H26E 0.96 . ? C26B H26F 0.96 . ? 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 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 O1 125.3(3) . . ? C7 C2 C3 119.0(3) . . ? O1 C2 C3 115.6(3) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120 . . ? C5 C4 H4 120 . . ? C6 C5 C4 118.0(3) . . ? C6 C5 N1 116.7(3) . . ? C4 C5 N1 125.3(3) . . ? C7 C6 C5 121.9(3) . . ? C7 C6 H6 119 . . ? C5 C6 H6 119 . . ? C2 C7 C6 119.7(3) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? N2 C8 N1 118.1(3) . . ? N2 C8 S1 128.2(2) . . ? N1 C8 S1 113.8(2) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 C11 119.4(3) . . ? N3 C10 C9 120.9(3) . . ? C11 C10 C9 119.7(3) . . ? C16 C11 C12 118.6(3) . . ? C16 C11 C10 121.7(3) . . ? C12 C11 C10 119.7(3) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.5(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.7(3) . . ? C16 C15 C18 123.2(3) . . ? C14 C15 C18 118.1(3) . . ? C15 C16 C11 121.3(3) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C15 125.5(3) . . ? N4 C18 C17 117.7(3) . . ? C15 C18 C17 116.8(2) . . ? N5 C19 N6 117.8(3) . . ? N5 C19 S2 128.6(2) . . ? N6 C19 S2 113.6(2) . . ? C21 C20 C25 119.0(3) . . ? C21 C20 N6 117.0(3) . . ? C25 C20 N6 123.8(3) . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 O2B 119.5(9) . . ? C24 C23 C22 119.4(3) . . ? O2B C23 C22 119.9(10) . . ? C24 C23 O2 113.1(6) . . ? C22 C23 O2 127.0(6) . . ? C23 C24 C25 121.1(3) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C20 119.9(3) . . ? C24 C25 H25 120 . . ? C20 C25 H25 120 . . ? C8 N1 C5 130.9(3) . . ? C8 N1 H1N 116(3) . . ? C5 N1 H1N 113(3) . . ? C8 N2 N3 115.5(2) . . ? C10 N3 N2 112.6(2) . . ? C10 N3 Zn1 130.9(2) . . ? N2 N3 Zn1 115.54(18) . . ? C18 N4 N5 116.2(2) . . ? C18 N4 Zn1 126.3(2) . 2_557 ? N5 N4 Zn1 116.59(17) . 2_557 ? C19 N5 N4 115.1(2) . . ? C19 N6 C20 129.4(3) . . ? C19 N6 H6N 118(2) . . ? C20 N6 H6N 113(2) . . ? C2 O1 C1 117.0(2) . . ? C23 O2 C26 111.5(14) . . ? C8 S1 Zn1 92.48(10) . . ? C19 S2 Zn1 92.97(10) . 2_557 ? N3 Zn1 N4 128.57(10) . 2_557 ? N3 Zn1 S1 86.98(7) . . ? N4 Zn1 S1 114.33(7) 2_557 . ? N3 Zn1 S2 117.79(7) . 2_557 ? N4 Zn1 S2 86.63(7) 2_557 2_557 ? S1 Zn1 S2 127.46(3) . 2_557 ? C23 O2B C26B 111.9(19) . . ? O2B C26B H26D 109.5 . . ? O2B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O2B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 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 C7 C2 C3 C4 -1.2(5) . . . . ? O1 C2 C3 C4 178.0(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C3 C4 C5 N1 -176.5(3) . . . . ? C4 C5 C6 C7 -1.1(5) . . . . ? N1 C5 C6 C7 176.1(3) . . . . ? O1 C2 C7 C6 -178.5(3) . . . . ? C3 C2 C7 C6 0.7(5) . . . . ? C5 C6 C7 C2 0.5(5) . . . . ? N3 C10 C11 C16 34.5(4) . . . . ? C9 C10 C11 C16 -146.7(3) . . . . ? N3 C10 C11 C12 -147.7(3) . . . . ? C9 C10 C11 C12 31.1(4) . . . . ? C16 C11 C12 C13 -2.8(4) . . . . ? C10 C11 C12 C13 179.3(3) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? C12 C13 C14 C15 3.1(5) . . . . ? C13 C14 C15 C16 -2.0(4) . . . . ? C13 C14 C15 C18 178.3(3) . . . . ? C14 C15 C16 C11 -1.6(4) . . . . ? C18 C15 C16 C11 178.1(3) . . . . ? C12 C11 C16 C15 4.0(4) . . . . ? C10 C11 C16 C15 -178.2(3) . . . . ? C16 C15 C18 N4 45.3(5) . . . . ? C14 C15 C18 N4 -135.0(3) . . . . ? C16 C15 C18 C17 -135.6(3) . . . . ? C14 C15 C18 C17 44.2(4) . . . . ? C25 C20 C21 C22 0.1(5) . . . . ? N6 C20 C21 C22 -175.6(3) . . . . ? C20 C21 C22 C23 0.3(6) . . . . ? C21 C22 C23 C24 -0.6(6) . . . . ? C21 C22 C23 O2B -167.9(9) . . . . ? C21 C22 C23 O2 171.1(9) . . . . ? O2B C23 C24 C25 167.9(9) . . . . ? C22 C23 C24 C25 0.5(6) . . . . ? O2 C23 C24 C25 -172.3(8) . . . . ? C23 C24 C25 C20 -0.1(5) . . . . ? C21 C20 C25 C24 -0.2(5) . . . . ? N6 C20 C25 C24 175.2(3) . . . . ? N2 C8 N1 C5 -5.5(5) . . . . ? S1 C8 N1 C5 174.7(3) . . . . ? C6 C5 N1 C8 179.7(3) . . . . ? C4 C5 N1 C8 -3.2(5) . . . . ? N1 C8 N2 N3 177.2(2) . . . . ? S1 C8 N2 N3 -3.0(4) . . . . ? C11 C10 N3 N2 179.6(2) . . . . ? C9 C10 N3 N2 0.8(4) . . . . ? C11 C10 N3 Zn1 11.3(4) . . . . ? C9 C10 N3 Zn1 -167.5(2) . . . . ? C8 N2 N3 C10 -177.2(3) . . . . ? C8 N2 N3 Zn1 -7.0(3) . . . . ? C15 C18 N4 N5 -4.5(4) . . . . ? C17 C18 N4 N5 176.4(2) . . . . ? C15 C18 N4 Zn1 164.1(2) . . . 2_557 ? C17 C18 N4 Zn1 -15.0(4) . . . 2_557 ? N6 C19 N5 N4 178.1(2) . . . . ? S2 C19 N5 N4 -2.9(4) . . . . ? C18 N4 N5 C19 170.7(3) . . . . ? Zn1 N4 N5 C19 1.0(3) 2_557 . . . ? N5 C19 N6 C20 11.6(5) . . . . ? S2 C19 N6 C20 -167.6(3) . . . . ? C21 C20 N6 C19 -167.3(3) . . . . ? C25 C20 N6 C19 17.2(5) . . . . ? C7 C2 O1 C1 -7.8(5) . . . . ? C3 C2 O1 C1 173.0(3) . . . . ? C24 C23 O2 C26 -175.8(14) . . . . ? O2B C23 O2 C26 -62(4) . . . . ? C22 C23 O2 C26 12(2) . . . . ? N2 C8 S1 Zn1 9.5(3) . . . . ? N1 C8 S1 Zn1 -170.7(2) . . . . ? N5 C19 S2 Zn1 2.8(3) . . . 2_557 ? N6 C19 S2 Zn1 -178.2(2) . . . 2_557 ? C10 N3 Zn1 N4 -62.6(3) . . . 2_557 ? N2 N3 Zn1 N4 129.34(18) . . . 2_557 ? C10 N3 Zn1 S1 178.3(3) . . . . ? N2 N3 Zn1 S1 10.29(17) . . . . ? C10 N3 Zn1 S2 47.0(3) . . . 2_557 ? N2 N3 Zn1 S2 -121.07(17) . . . 2_557 ? C8 S1 Zn1 N3 -8.69(12) . . . . ? C8 S1 Zn1 N4 -140.10(12) . . . 2_557 ? C8 S1 Zn1 S2 114.53(10) . . . 2_557 ? C24 C23 O2B C26B 141.8(19) . . . . ? C22 C23 O2B C26B -51(3) . . . . ? O2 C23 O2B C26B 67(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N S2 0.88(4) 2.82(4) 3.639(3) 156(3) 1_465 # END of CIF # Attachment '- 6.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-06 at 10:56:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : e:\xprogs\wingx\files\archive.reqdat # CIF files read : 6 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_18CdPhNO2 _database_code_depnum_ccdc_archive 'CCDC 893873' #TrackingRef '- 6.cif' _audit_creation_date 2010-08-06T10:56:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H40 Cd2 N16 O8 S4, 4(C2 H6 O S)' _chemical_formula_sum 'C56 H64 Cd2 N16 O12 S8 ' _chemical_formula_weight 1634.51 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 30.0597(13) _cell_length_b 8.3317(4) _cell_length_c 27.4037(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6863.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1898 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.18 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.8572 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 108959 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 13806 _reflns_number_gt 12050 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR-97 (Giacovazzo et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+7.2442P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 13806 _refine_ls_number_parameters 872 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.455(15) _refine_diff_density_max 1.218 _refine_diff_density_min -0.44 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.14253(13) 0.3619(6) 0.00062(15) 0.0237(10) Uani 1 1 d . . . C2 C -0.11563(13) 0.2439(5) -0.01869(14) 0.0234(10) Uani 1 1 d . . . H2 H -0.1249 0.184 -0.0464 0.028 Uiso 1 1 calc R . . C3 C -0.07494(13) 0.2142(6) 0.00290(14) 0.0230(9) Uani 1 1 d . . . H3 H -0.0556 0.1368 -0.0111 0.028 Uiso 1 1 calc R . . C4 C -0.06185(13) 0.2959(5) 0.04485(14) 0.0181(8) Uani 1 1 d . . . C5 C -0.08970(13) 0.4155(5) 0.06387(15) 0.0230(9) Uani 1 1 d . . . H5 H -0.0811 0.473 0.0923 0.028 Uiso 1 1 calc R . . C6 C -0.12992(15) 0.4499(6) 0.04108(16) 0.0250(11) Uani 1 1 d . . . H6 H -0.1485 0.533 0.0532 0.03 Uiso 1 1 calc R . . C7 C -0.00135(12) 0.2898(5) 0.10911(13) 0.0162(8) Uani 1 1 d . . . C8 C -0.07966(11) 0.5238(5) 0.19974(18) 0.0215(8) Uani 1 1 d . . . H8A H -0.0943 0.4258 0.1882 0.032 Uiso 1 1 calc R . . H8B H -0.0805 0.6053 0.174 0.032 Uiso 1 1 calc R . . H8C H -0.0952 0.5641 0.2287 0.032 Uiso 1 1 calc R . . C9 C -0.03212(12) 0.4873(5) 0.21262(13) 0.0160(9) Uani 1 1 d . . . C10 C -0.01402(13) 0.5447(5) 0.25997(14) 0.0171(9) Uani 1 1 d . . . C11 C -0.04053(13) 0.5541(5) 0.30197(14) 0.0210(9) Uani 1 1 d . . . H11 H -0.0705 0.5183 0.3012 0.025 Uiso 1 1 calc R . . C12 C -0.02263(14) 0.6162(5) 0.34467(15) 0.0248(10) Uani 1 1 d . . . H12 H -0.0406 0.6216 0.3731 0.03 Uiso 1 1 calc R . . C13 C 0.02058(13) 0.6701(5) 0.34677(15) 0.0220(9) Uani 1 1 d . . . H13 H 0.032 0.7115 0.3765 0.026 Uiso 1 1 calc R . . C14 C 0.04777(13) 0.6643(5) 0.30536(14) 0.0162(8) Uani 1 1 d . . . C15 C 0.02973(12) 0.5988(5) 0.26279(13) 0.0150(8) Uani 1 1 d . . . H15 H 0.048 0.5909 0.2346 0.018 Uiso 1 1 calc R . . C16 C 0.12246(14) 0.7094(6) 0.35002(15) 0.0244(10) Uani 1 1 d . . . H16A H 0.1325 0.8164 0.36 0.037 Uiso 1 1 calc R . . H16B H 0.1484 0.6421 0.3427 0.037 Uiso 1 1 calc R . . H16C H 0.1052 0.6605 0.3765 0.037 Uiso 1 1 calc R . . C17 C 0.09395(13) 0.7234(5) 0.30545(15) 0.0176(9) Uani 1 1 d . . . C18 C 0.16821(12) 0.9153(5) 0.23070(15) 0.0184(9) Uani 1 1 d . . . C19 C 0.24325(12) 0.9517(5) 0.26989(15) 0.0176(9) Uani 1 1 d . . . C20 C 0.23627(14) 0.8761(6) 0.31522(16) 0.0270(10) Uani 1 1 d . . . H20 H 0.209 0.8214 0.3209 0.032 Uiso 1 1 calc R . . C21 C 0.26795(13) 0.8798(5) 0.35134(16) 0.0252(10) Uani 1 1 d . . . H21 H 0.2628 0.8288 0.3818 0.03 Uiso 1 1 calc R . . C22 C 0.30792(12) 0.9602(5) 0.34226(15) 0.0205(9) Uani 1 1 d . . . C23 C 0.31631(12) 1.0318(5) 0.29755(15) 0.0227(9) Uani 1 1 d . . . H23 H 0.3441 1.0829 0.2917 0.027 Uiso 1 1 calc R . . C24 C 0.28446(12) 1.0285(5) 0.26183(15) 0.0216(9) Uani 1 1 d . . . H24 H 0.2901 1.0785 0.2313 0.026 Uiso 1 1 calc R . . C25 C 0.27300(13) 0.3625(5) 0.39493(15) 0.0211(9) Uani 1 1 d . . . C26 C 0.25958(14) 0.4445(6) 0.35319(15) 0.0216(10) Uani 1 1 d . . . H26 H 0.2774 0.5287 0.3403 0.026 Uiso 1 1 calc R . . C27 C 0.22032(13) 0.4025(5) 0.33077(15) 0.0226(9) Uani 1 1 d . . . H27 H 0.2114 0.4556 0.3017 0.027 Uiso 1 1 calc R . . C28 C 0.19345(12) 0.2824(5) 0.35047(14) 0.0188(9) Uani 1 1 d . . . C29 C 0.20788(13) 0.2018(5) 0.39315(14) 0.0234(10) Uani 1 1 d . . . H29 H 0.19 0.1192 0.4068 0.028 Uiso 1 1 calc R . . C30 C 0.24768(13) 0.2423(5) 0.41499(15) 0.0233(10) Uani 1 1 d . . . H30 H 0.2574 0.1879 0.4435 0.028 Uiso 1 1 calc R . . C31 C 0.13141(12) 0.2780(5) 0.28893(14) 0.0158(8) Uani 1 1 d . . . C32 C 0.20872(12) 0.4902(5) 0.19340(16) 0.0232(10) Uani 1 1 d . . . H32A H 0.2213 0.3868 0.2034 0.035 Uiso 1 1 calc R . . H32B H 0.213 0.5689 0.2195 0.035 Uiso 1 1 calc R . . H32C H 0.2237 0.5275 0.1637 0.035 Uiso 1 1 calc R . . C33 C 0.16005(13) 0.4707(5) 0.18347(14) 0.0169(9) Uani 1 1 d . . . C34 C 0.14092(12) 0.5353(5) 0.13753(14) 0.0149(8) Uani 1 1 d . . . C35 C 0.16544(13) 0.5398(5) 0.09447(14) 0.0201(9) Uani 1 1 d . . . H35 H 0.1944 0.4942 0.0937 0.024 Uiso 1 1 calc R . . C36 C 0.14825(13) 0.6094(5) 0.05302(15) 0.0237(10) Uani 1 1 d . . . H36 H 0.1653 0.6101 0.0238 0.028 Uiso 1 1 calc R . . C37 C 0.10591(13) 0.6793(5) 0.05357(15) 0.0203(10) Uani 1 1 d . . . H37 H 0.0947 0.7308 0.0252 0.024 Uiso 1 1 calc R . . C38 C 0.08025(13) 0.6728(5) 0.09612(14) 0.0144(8) Uani 1 1 d . . . C39 C 0.09822(12) 0.5999(5) 0.13718(14) 0.0158(8) Uani 1 1 d . . . H39 H 0.0808 0.5938 0.166 0.019 Uiso 1 1 calc R . . C40 C 0.00587(13) 0.7399(5) 0.05366(14) 0.0219(10) Uani 1 1 d . . . H40A H -0.0041 0.8492 0.0463 0.033 Uiso 1 1 calc R . . H40B H -0.02 0.6713 0.0597 0.033 Uiso 1 1 calc R . . H40C H 0.0228 0.6976 0.0259 0.033 Uiso 1 1 calc R . . C41 C 0.03492(12) 0.7423(5) 0.09806(14) 0.0167(9) Uani 1 1 d . . . C42 C -0.03458(13) 0.9416(5) 0.17630(14) 0.0174(9) Uani 1 1 d . . . C43 C -0.11008(12) 0.9943(5) 0.14060(14) 0.0173(9) Uani 1 1 d . . . C44 C -0.10567(14) 0.9162(6) 0.09611(16) 0.0272(11) Uani 1 1 d . . . H44 H -0.0796 0.8562 0.0891 0.033 Uiso 1 1 calc R . . C45 C -0.13965(13) 0.9266(5) 0.06203(15) 0.0254(10) Uani 1 1 d . . . H45 H -0.1368 0.8732 0.0315 0.03 Uiso 1 1 calc R . . C46 C -0.17751(12) 1.0137(5) 0.07212(14) 0.0201(9) Uani 1 1 d . . . C47 C -0.18321(13) 1.0894(5) 0.11715(14) 0.0209(9) Uani 1 1 d . . . H47 H -0.2097 1.1467 0.1243 0.025 Uiso 1 1 calc R . . C48 C -0.14946(13) 1.0790(5) 0.15081(14) 0.0207(9) Uani 1 1 d . . . H48 H -0.1528 1.1301 0.1816 0.025 Uiso 1 1 calc R . . C49 C 0.55836(15) 0.1114(6) 0.97809(18) 0.0313(11) Uani 1 1 d . . . H49A H 0.5307 0.0744 0.963 0.047 Uiso 1 1 calc R . . H49B H 0.5563 0.099 1.0136 0.047 Uiso 1 1 calc R . . H49C H 0.5833 0.0475 0.9657 0.047 Uiso 1 1 calc R . . C50 C 0.61570(14) 0.3496(7) 0.99949(16) 0.0312(11) Uani 1 1 d . . . H50A H 0.6091 0.3234 1.0336 0.047 Uiso 1 1 calc R . . H50B H 0.625 0.4621 0.9971 0.047 Uiso 1 1 calc R . . H50C H 0.6396 0.28 0.9876 0.047 Uiso 1 1 calc R . . C51 C 0.5856(2) 0.1268(6) 0.4241(2) 0.0476(14) Uani 1 1 d . . . H51A H 0.6173 0.1075 0.4301 0.071 Uiso 1 1 calc R . . H51B H 0.579 0.1087 0.3895 0.071 Uiso 1 1 calc R . . H51C H 0.5678 0.0532 0.4441 0.071 Uiso 1 1 calc R . . C52 C 0.51882(15) 0.3317(7) 0.4122(2) 0.0428(14) Uani 1 1 d . . . H52A H 0.5219 0.3118 0.3771 0.064 Uiso 1 1 calc R . . H52B H 0.5049 0.4367 0.4174 0.064 Uiso 1 1 calc R . . H52C H 0.5002 0.2479 0.4268 0.064 Uiso 1 1 calc R . . C53 C 0.42573(15) 0.3936(6) 0.34318(17) 0.0350(11) Uani 1 1 d . . . H53A H 0.4512 0.4318 0.3241 0.053 Uiso 1 1 calc R . . H53B H 0.4311 0.2829 0.3537 0.053 Uiso 1 1 calc R . . H53C H 0.4218 0.4623 0.3719 0.053 Uiso 1 1 calc R . . C54 C 0.37744(18) 0.6142(6) 0.29482(19) 0.0407(13) Uani 1 1 d . . . H54A H 0.3525 0.6428 0.2735 0.061 Uiso 1 1 calc R . . H54B H 0.4055 0.6434 0.279 0.061 Uiso 1 1 calc R . . H54C H 0.3747 0.6722 0.3258 0.061 Uiso 1 1 calc R . . C55 C 0.70764(14) 0.4433(6) 0.06561(16) 0.0330(11) Uani 1 1 d . . . H55A H 0.6839 0.4949 0.0844 0.05 Uiso 1 1 calc R . . H55B H 0.6998 0.3309 0.0595 0.05 Uiso 1 1 calc R . . H55C H 0.7114 0.4993 0.0344 0.05 Uiso 1 1 calc R . . C56 C 0.75938(18) 0.6628(6) 0.1069(2) 0.0478(14) Uani 1 1 d . . . H56A H 0.7848 0.6926 0.1274 0.072 Uiso 1 1 calc R . . H56B H 0.7317 0.6978 0.1226 0.072 Uiso 1 1 calc R . . H56C H 0.7622 0.7147 0.075 0.072 Uiso 1 1 calc R . . N1 N -0.18526(12) 0.3981(5) -0.02330(13) 0.0300(9) Uani 1 1 d . . . N2 N -0.02042(11) 0.2529(4) 0.06416(12) 0.0201(8) Uani 1 1 d . . . H2N H -0.0057(15) 0.188(6) 0.0485(17) 0.03 Uiso 1 1 d . . . N3 N -0.02499(10) 0.3776(4) 0.13867(11) 0.0193(8) Uani 1 1 d . . . N4 N -0.00552(11) 0.4145(4) 0.18353(11) 0.0171(7) Uani 1 1 d . . . N5 N 0.10876(10) 0.7859(4) 0.26496(11) 0.0164(7) Uani 1 1 d . . . N6 N 0.15314(10) 0.8309(4) 0.26746(12) 0.0179(7) Uani 1 1 d . . . N7 N 0.21235(11) 0.9633(4) 0.23237(13) 0.0199(8) Uani 1 1 d . . . H7N H 0.2198(13) 1.020(5) 0.2062(18) 0.03 Uiso 1 1 d . . . N8 N 0.34113(11) 0.9717(5) 0.38144(13) 0.0274(9) Uani 1 1 d . . . N9 N 0.31490(11) 0.4082(5) 0.41805(13) 0.0257(8) Uani 1 1 d . . . N10 N 0.15200(11) 0.2343(4) 0.33227(12) 0.0196(8) Uani 1 1 d . . . H10N H 0.1353(14) 0.172(6) 0.3518(16) 0.029 Uiso 1 1 d . . . N11 N 0.15426(11) 0.3599(4) 0.25780(11) 0.0176(7) Uani 1 1 d . . . N12 N 0.13275(10) 0.4040(4) 0.21473(10) 0.0167(8) Uani 1 1 d . . . N13 N 0.02196(10) 0.8028(4) 0.13939(11) 0.0158(7) Uani 1 1 d . . . N14 N -0.02159(10) 0.8573(4) 0.13867(11) 0.0171(7) Uani 1 1 d . . . N15 N -0.07761(11) 0.9978(4) 0.17683(12) 0.0198(8) Uani 1 1 d D . . H15N H -0.0822(13) 1.049(5) 0.2035(11) 0.03 Uiso 1 1 d D . . N16 N -0.21170(11) 1.0289(5) 0.03518(13) 0.0251(8) Uani 1 1 d . . . O1 O -0.19658(11) 0.3173(5) -0.05837(13) 0.0483(10) Uani 1 1 d . . . O2 O -0.20755(10) 0.5090(5) -0.00714(11) 0.0386(9) Uani 1 1 d . . . O3 O 0.37703(10) 1.0356(5) 0.37186(12) 0.0397(9) Uani 1 1 d . . . O4 O 0.33157(11) 0.9182(4) 0.42207(12) 0.0428(9) Uani 1 1 d . . . O5 O 0.32801(11) 0.3274(4) 0.45269(12) 0.0407(9) Uani 1 1 d . . . O6 O 0.33531(9) 0.5250(4) 0.40222(10) 0.0302(7) Uani 1 1 d . . . O7 O -0.20579(11) 0.9634(5) -0.00420(12) 0.0556(12) Uani 1 1 d . . . O8 O -0.24515(10) 1.1089(4) 0.04406(12) 0.0337(9) Uani 1 1 d . . . O9 O 0.52997(10) 0.4109(4) 0.98727(11) 0.0292(8) Uani 1 1 d . . . O10 O 0.60135(10) 0.4351(4) 0.40903(12) 0.0314(8) Uani 1 1 d . . . O11 O 0.38841(9) 0.3206(4) 0.25879(10) 0.0270(7) Uani 1 1 d . . . O12 O 0.74953(10) 0.3807(4) 0.14886(10) 0.0273(7) Uani 1 1 d . . . S1 S 0.05197(3) 0.20781(13) 0.11572(4) 0.0181(2) Uani 1 1 d . . . S2 S 0.14143(3) 0.98258(13) 0.17772(4) 0.0194(2) Uani 1 1 d . . . S3 S 0.07650(3) 0.20616(14) 0.28575(4) 0.0196(2) Uani 1 1 d . . . S4 S -0.00558(3) 0.99397(13) 0.22940(4) 0.0188(2) Uani 1 1 d . . . S5 S 0.56716(4) 0.31939(17) 0.96338(4) 0.0249(3) Uani 1 1 d . . . S6 S 0.57217(4) 0.32950(18) 0.43989(5) 0.0313(3) Uani 1 1 d . . . S7 S 0.37664(3) 0.40089(14) 0.30632(4) 0.0251(2) Uani 1 1 d . . . S8 S 0.75839(3) 0.45190(14) 0.09920(4) 0.0253(2) Uani 1 1 d . . . Cd1 Cd 0.062305(8) 0.29132(3) 0.201274(13) 0.01748(6) Uani 1 1 d . . . Cd2 Cd 0.067088(8) 0.89332(3) 0.202235(16) 0.01768(6) 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 C1 0.019(2) 0.035(3) 0.017(2) 0.0107(19) 0.0021(17) -0.0026(19) C2 0.030(2) 0.025(3) 0.015(2) -0.0020(18) -0.0043(17) -0.0065(19) C3 0.022(2) 0.027(3) 0.020(2) -0.0042(19) -0.0018(17) -0.0015(19) C4 0.0213(19) 0.020(2) 0.0133(19) 0.0013(17) -0.0021(15) -0.0043(17) C5 0.024(2) 0.029(3) 0.015(2) 0.0013(19) -0.0004(17) -0.0005(19) C6 0.022(2) 0.031(3) 0.021(2) 0.003(2) 0.0015(18) 0.002(2) C7 0.0180(18) 0.015(2) 0.015(2) -0.0017(17) 0.0014(15) -0.0050(16) C8 0.0191(17) 0.028(2) 0.0173(19) 0.000(2) 0.004(2) -0.0004(15) C9 0.0181(18) 0.013(2) 0.017(2) 0.0050(16) 0.0018(15) -0.0032(15) C10 0.023(2) 0.015(2) 0.0133(19) 0.0025(17) 0.0010(16) 0.0005(16) C11 0.0181(19) 0.030(3) 0.015(2) -0.0001(18) 0.0015(16) 0.0003(17) C12 0.026(2) 0.035(3) 0.014(2) -0.0043(19) 0.0058(17) 0.002(2) C13 0.026(2) 0.028(3) 0.012(2) -0.0062(19) 0.0020(17) -0.0023(19) C14 0.023(2) 0.010(2) 0.016(2) -0.0010(17) 0.0012(17) 0.0025(17) C15 0.0210(19) 0.013(2) 0.0111(18) 0.0015(16) 0.0003(15) 0.0017(16) C16 0.024(2) 0.032(3) 0.017(2) 0.0027(19) -0.0038(18) -0.003(2) C17 0.021(2) 0.015(2) 0.017(2) -0.0073(18) 0.0005(17) 0.0022(17) C18 0.0145(19) 0.015(2) 0.026(2) -0.0016(19) -0.0020(16) 0.0024(16) C19 0.0168(19) 0.014(2) 0.022(2) -0.0003(17) -0.0010(16) 0.0013(16) C20 0.019(2) 0.030(3) 0.032(3) 0.007(2) -0.0043(18) -0.0036(19) C21 0.025(2) 0.026(3) 0.024(2) 0.0033(19) -0.0031(18) -0.0014(19) C22 0.0164(19) 0.021(2) 0.024(2) -0.0007(18) -0.0065(16) 0.0048(17) C23 0.0128(19) 0.024(2) 0.031(2) -0.0056(19) -0.0008(17) 0.0002(17) C24 0.0175(19) 0.025(2) 0.022(2) -0.0015(19) -0.0008(17) 0.0003(17) C25 0.019(2) 0.022(3) 0.022(2) -0.0048(18) -0.0042(17) 0.0027(18) C26 0.024(2) 0.024(3) 0.018(2) -0.0035(19) -0.0002(17) -0.0030(19) C27 0.024(2) 0.026(3) 0.017(2) 0.0063(19) -0.0025(17) -0.0011(19) C28 0.0186(19) 0.022(2) 0.0157(19) 0.0014(18) -0.0037(16) -0.0015(17) C29 0.026(2) 0.026(3) 0.018(2) 0.0044(19) 0.0024(17) -0.0005(19) C30 0.022(2) 0.031(3) 0.017(2) 0.0005(19) -0.0045(17) 0.0021(18) C31 0.0206(19) 0.012(2) 0.0147(19) 0.0010(16) -0.0034(16) -0.0017(16) C32 0.0208(19) 0.024(2) 0.025(3) 0.0083(19) -0.0032(17) -0.0014(16) C33 0.0198(19) 0.012(2) 0.018(2) -0.0018(16) -0.0014(16) -0.0013(16) C34 0.0182(19) 0.009(2) 0.017(2) -0.0008(16) 0.0046(16) 0.0001(16) C35 0.0177(19) 0.019(2) 0.023(2) -0.0027(19) 0.0054(17) 0.0014(17) C36 0.024(2) 0.031(3) 0.017(2) 0.0039(19) 0.0055(17) 0.0019(19) C37 0.025(2) 0.018(2) 0.018(2) 0.0016(18) -0.0011(17) 0.0020(18) C38 0.018(2) 0.012(2) 0.013(2) 0.0002(17) 0.0017(16) -0.0041(17) C39 0.0203(19) 0.013(2) 0.0141(19) -0.0017(17) 0.0042(16) -0.0044(16) C40 0.023(2) 0.026(3) 0.017(2) -0.0010(18) -0.0007(17) 0.0033(18) C41 0.0175(19) 0.014(2) 0.019(2) 0.0020(18) -0.0025(16) -0.0016(16) C42 0.019(2) 0.016(2) 0.017(2) 0.0020(17) -0.0003(16) -0.0022(16) C43 0.0178(19) 0.016(2) 0.018(2) -0.0012(17) -0.0001(16) -0.0012(16) C44 0.018(2) 0.034(3) 0.029(2) -0.005(2) -0.0014(18) 0.0067(19) C45 0.022(2) 0.033(3) 0.021(2) -0.0078(19) -0.0026(17) 0.0027(19) C46 0.0147(18) 0.023(2) 0.023(2) -0.0007(18) -0.0022(16) -0.0061(17) C47 0.020(2) 0.021(2) 0.022(2) 0.0052(19) 0.0043(16) 0.0016(17) C48 0.023(2) 0.022(2) 0.017(2) 0.0012(18) -0.0005(16) 0.0007(18) C49 0.035(3) 0.032(3) 0.027(2) 0.005(2) 0.001(2) -0.003(2) C50 0.027(2) 0.046(3) 0.021(2) 0.002(2) 0.0018(19) -0.009(2) C51 0.069(4) 0.028(3) 0.046(3) 0.012(3) 0.001(3) 0.005(3) C52 0.028(3) 0.055(4) 0.045(3) -0.014(3) 0.001(2) 0.006(3) C53 0.031(2) 0.042(3) 0.033(3) -0.003(2) -0.002(2) -0.002(2) C54 0.047(3) 0.030(3) 0.045(3) 0.001(2) 0.009(3) -0.002(2) C55 0.027(2) 0.043(3) 0.029(3) 0.001(2) -0.0025(19) 0.005(2) C56 0.056(3) 0.029(3) 0.058(4) 0.003(3) -0.002(3) 0.000(3) N1 0.0233(19) 0.047(3) 0.0193(19) 0.0120(19) -0.0022(16) -0.0025(19) N2 0.0198(17) 0.023(2) 0.0177(18) -0.0052(16) -0.0036(14) 0.0012(15) N3 0.0194(17) 0.025(2) 0.0137(17) -0.0031(15) -0.0025(14) -0.0013(15) N4 0.0232(17) 0.0177(19) 0.0104(15) -0.0014(14) -0.0014(13) 0.0001(14) N5 0.0154(15) 0.0163(19) 0.0176(17) 0.0009(15) -0.0016(13) -0.0002(14) N6 0.0139(15) 0.0170(19) 0.0228(18) 0.0034(15) 0.0007(14) -0.0062(14) N7 0.0191(17) 0.022(2) 0.0189(19) 0.0047(16) -0.0007(14) -0.0023(15) N8 0.0192(18) 0.033(2) 0.030(2) -0.0099(18) -0.0063(15) 0.0039(17) N9 0.0209(18) 0.032(2) 0.025(2) -0.0091(18) -0.0037(15) -0.0025(17) N10 0.0209(17) 0.023(2) 0.0154(17) 0.0078(15) -0.0011(14) -0.0063(15) N11 0.0216(17) 0.020(2) 0.0116(16) 0.0028(14) -0.0036(13) -0.0013(14) N12 0.0171(15) 0.0183(18) 0.0147(19) 0.0011(14) -0.0024(12) 0.0012(14) N13 0.0129(15) 0.0166(19) 0.0179(17) -0.0005(15) 0.0024(13) 0.0024(13) N14 0.0153(15) 0.0182(19) 0.0176(17) -0.0031(14) -0.0020(13) 0.0025(14) N15 0.0169(16) 0.025(2) 0.0172(17) -0.0035(16) -0.0001(14) 0.0049(15) N16 0.0209(19) 0.029(2) 0.025(2) -0.0042(17) -0.0052(15) -0.0031(16) O1 0.0349(18) 0.072(3) 0.038(2) -0.010(2) -0.0215(16) 0.0051(19) O2 0.0305(17) 0.059(3) 0.0265(18) 0.0088(17) -0.0027(14) 0.0152(18) O3 0.0144(15) 0.072(3) 0.0331(19) -0.0085(19) -0.0022(14) -0.0063(17) O4 0.0402(19) 0.058(3) 0.0304(19) 0.0143(18) -0.0125(15) -0.0095(17) O5 0.0419(19) 0.045(2) 0.0350(19) 0.0117(17) -0.0212(16) -0.0023(17) O6 0.0267(16) 0.042(2) 0.0221(16) -0.0022(15) -0.0031(13) -0.0132(15) O7 0.039(2) 0.091(3) 0.037(2) -0.035(2) -0.0198(17) 0.024(2) O8 0.0215(16) 0.047(2) 0.0331(19) -0.0048(17) -0.0033(14) 0.0086(15) O9 0.0308(17) 0.030(2) 0.0269(17) 0.0091(14) -0.0013(13) 0.0004(14) O10 0.0352(18) 0.025(2) 0.0339(18) -0.0095(14) 0.0029(14) -0.0045(14) O11 0.0334(16) 0.0279(19) 0.0198(15) -0.0028(13) 0.0006(13) -0.0096(14) O12 0.0305(16) 0.0300(19) 0.0214(15) 0.0029(13) 0.0033(12) 0.0107(14) S1 0.0176(5) 0.0228(6) 0.0138(5) -0.0011(4) 0.0000(4) 0.0013(4) S2 0.0169(5) 0.0234(6) 0.0180(5) 0.0034(5) 0.0006(4) -0.0018(4) S3 0.0179(5) 0.0244(6) 0.0163(5) 0.0021(4) -0.0023(4) -0.0035(5) S4 0.0169(5) 0.0238(6) 0.0156(5) -0.0013(4) -0.0005(4) 0.0007(4) S5 0.0284(6) 0.0299(8) 0.0165(6) 0.0058(5) -0.0006(4) -0.0067(5) S6 0.0360(7) 0.0351(8) 0.0229(7) -0.0067(6) -0.0016(5) 0.0016(6) S7 0.0254(5) 0.0288(6) 0.0210(5) 0.0006(5) 0.0031(4) -0.0046(5) S8 0.0216(5) 0.0290(6) 0.0252(6) 0.0016(5) 0.0011(4) 0.0032(5) Cd1 0.01908(12) 0.01932(14) 0.01404(12) 0.00002(18) -0.00303(13) -0.00108(11) Cd2 0.01460(11) 0.01993(14) 0.01851(12) 0.00058(18) -0.00112(13) -0.00023(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(6) . ? C1 C6 1.382(6) . ? C1 N1 1.473(5) . ? C2 C3 1.381(5) . ? C2 H2 0.95 . ? C3 C4 1.393(6) . ? C3 H3 0.95 . ? C4 N2 1.400(5) . ? C4 C5 1.402(6) . ? C5 C6 1.391(6) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 N3 1.303(5) . ? C7 N2 1.393(5) . ? C7 S1 1.752(4) . ? C8 C9 1.503(5) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 N4 1.282(5) . ? C9 C10 1.486(5) . ? C10 C15 1.392(5) . ? C10 C11 1.402(5) . ? C11 C12 1.388(6) . ? C11 H11 0.95 . ? C12 C13 1.376(6) . ? C12 H12 0.95 . ? C13 C14 1.399(5) . ? C13 H13 0.95 . ? C14 C15 1.397(5) . ? C14 C17 1.473(5) . ? C15 H15 0.95 . ? C16 C17 1.497(5) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 N5 1.304(5) . ? C18 N6 1.309(5) . ? C18 N7 1.387(5) . ? C18 S2 1.752(4) . ? C19 N7 1.389(5) . ? C19 C20 1.408(6) . ? C19 C24 1.412(5) . ? C20 C21 1.374(6) . ? C20 H20 0.95 . ? C21 C22 1.398(6) . ? C21 H21 0.95 . ? C22 C23 1.386(6) . ? C22 N8 1.469(5) . ? C23 C24 1.370(5) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C30 1.372(6) . ? C25 C26 1.392(6) . ? C25 N9 1.460(5) . ? C26 C27 1.376(6) . ? C26 H26 0.95 . ? C27 C28 1.394(6) . ? C27 H27 0.95 . ? C28 N10 1.401(5) . ? C28 C29 1.417(6) . ? C29 C30 1.380(6) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 N11 1.290(5) . ? C31 N10 1.388(5) . ? C31 S3 1.758(4) . ? C32 C33 1.497(5) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 N12 1.310(5) . ? C33 C34 1.485(5) . ? C34 C35 1.392(5) . ? C34 C39 1.392(5) . ? C35 C36 1.376(6) . ? C35 H35 0.95 . ? C36 C37 1.400(6) . ? C36 H36 0.95 . ? C37 C38 1.399(5) . ? C37 H37 0.95 . ? C38 C39 1.388(5) . ? C38 C41 1.481(5) . ? C39 H39 0.95 . ? C40 C41 1.498(5) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 N13 1.300(5) . ? C42 N14 1.308(5) . ? C42 N15 1.375(5) . ? C42 S4 1.751(4) . ? C43 C44 1.388(6) . ? C43 N15 1.393(5) . ? C43 C48 1.406(5) . ? C44 C45 1.387(6) . ? C44 H44 0.95 . ? C45 C46 1.378(6) . ? C45 H45 0.95 . ? C46 C47 1.397(6) . ? C46 N16 1.448(5) . ? C47 C48 1.374(5) . ? C47 H47 0.95 . ? C48 H48 0.95 . ? C49 S5 1.798(5) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 S5 1.781(4) . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 S6 1.789(5) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 S6 1.774(5) . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 S7 1.789(4) . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? C54 S7 1.805(5) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 S8 1.783(4) . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C56 S8 1.770(5) . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? N1 O1 1.222(5) . ? N1 O2 1.224(5) . ? N2 H2N 0.82(5) . ? N3 N4 1.396(4) . ? N4 Cd1 2.334(3) . ? N5 N6 1.387(4) . ? N5 Cd2 2.307(3) . ? N7 H7N 0.89(5) . ? N8 O3 1.232(5) . ? N8 O4 1.233(5) . ? N9 O5 1.229(5) . ? N9 O6 1.230(5) . ? N10 H10N 0.90(5) . ? N11 N12 1.395(4) . ? N12 Cd1 2.346(3) . ? N13 N14 1.385(4) . ? N13 Cd2 2.318(3) . ? N15 H15N 0.858(19) . ? N16 O7 1.223(5) . ? N16 O8 1.230(4) . ? O9 S5 1.503(3) . ? O10 S6 1.503(3) . ? O11 S7 1.506(3) . ? O12 S8 1.508(3) . ? S1 Cd1 2.4653(10) . ? S2 Cd2 2.4490(10) . ? S3 Cd1 2.4586(11) . ? S4 Cd2 2.4552(10) . ? Cd1 Cd2 3.3192(4) 1_545 ? Cd2 Cd1 3.3192(4) 1_565 ? 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 C2 C1 C6 121.7(4) . . ? C2 C1 N1 119.1(4) . . ? C6 C1 N1 119.2(4) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 N2 116.0(4) . . ? C3 C4 C5 119.0(4) . . ? N2 C4 C5 124.9(4) . . ? C6 C5 C4 119.9(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C1 C6 C5 119.3(4) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N3 C7 N2 116.7(3) . . ? N3 C7 S1 130.8(3) . . ? N2 C7 S1 112.5(3) . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 117.8(3) . . ? N4 C9 C8 122.9(3) . . ? C10 C9 C8 119.2(3) . . ? C15 C10 C11 118.2(4) . . ? C15 C10 C9 119.9(3) . . ? C11 C10 C9 121.8(3) . . ? C12 C11 C10 119.5(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 121.5(4) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 117.6(4) . . ? C15 C14 C17 119.9(3) . . ? C13 C14 C17 122.5(4) . . ? C10 C15 C14 122.6(4) . . ? C10 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 C14 117.0(3) . . ? N5 C17 C16 122.0(4) . . ? C14 C17 C16 121.0(4) . . ? N6 C18 N7 117.4(3) . . ? N6 C18 S2 130.6(3) . . ? N7 C18 S2 112.0(3) . . ? N7 C19 C20 125.8(4) . . ? N7 C19 C24 116.1(4) . . ? C20 C19 C24 118.1(4) . . ? C21 C20 C19 121.5(4) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 118.6(4) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 121.3(4) . . ? C23 C22 N8 119.6(4) . . ? C21 C22 N8 119.0(4) . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.7(4) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C30 C25 C26 121.8(4) . . ? C30 C25 N9 119.6(4) . . ? C26 C25 N9 118.6(4) . . ? C27 C26 C25 119.4(4) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 N10 125.6(4) . . ? C27 C28 C29 118.9(4) . . ? N10 C28 C29 115.5(4) . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C25 C30 C29 119.1(4) . . ? C25 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? N11 C31 N10 117.8(3) . . ? N11 C31 S3 130.3(3) . . ? N10 C31 S3 111.8(3) . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N12 C33 C34 117.7(3) . . ? N12 C33 C32 122.6(3) . . ? C34 C33 C32 119.6(3) . . ? C35 C34 C39 118.2(4) . . ? C35 C34 C33 121.6(3) . . ? C39 C34 C33 120.2(3) . . ? C36 C35 C34 120.8(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 120.5(4) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 119.6(4) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C37 118.5(4) . . ? C39 C38 C41 120.0(3) . . ? C37 C38 C41 121.5(3) . . ? C38 C39 C34 122.3(4) . . ? C38 C39 H39 118.9 . . ? C34 C39 H39 118.9 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N13 C41 C38 117.3(3) . . ? N13 C41 C40 122.6(3) . . ? C38 C41 C40 120.1(3) . . ? N14 C42 N15 118.2(4) . . ? N14 C42 S4 129.8(3) . . ? N15 C42 S4 112.0(3) . . ? C44 C43 N15 124.7(4) . . ? C44 C43 C48 119.4(4) . . ? N15 C43 C48 116.0(3) . . ? C45 C44 C43 119.5(4) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C44 120.4(4) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 121.1(4) . . ? C45 C46 N16 119.5(4) . . ? C47 C46 N16 119.4(4) . . ? C48 C47 C46 118.3(4) . . ? C48 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? C47 C48 C43 121.3(4) . . ? C47 C48 H48 119.4 . . ? C43 C48 H48 119.4 . . ? S5 C49 H49A 109.5 . . ? S5 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? S5 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? S5 C50 H50A 109.5 . . ? S5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? S5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? S6 C51 H51A 109.5 . . ? S6 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S6 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S6 C52 H52A 109.5 . . ? S6 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S6 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? S7 C53 H53A 109.5 . . ? S7 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? S7 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? S7 C54 H54A 109.5 . . ? S7 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? S7 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? S8 C55 H55A 109.5 . . ? S8 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? S8 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? S8 C56 H56A 109.5 . . ? S8 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? S8 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O1 N1 O2 123.2(4) . . ? O1 N1 C1 118.7(4) . . ? O2 N1 C1 118.1(4) . . ? C7 N2 C4 130.1(3) . . ? C7 N2 H2N 113(3) . . ? C4 N2 H2N 117(3) . . ? C7 N3 N4 116.3(3) . . ? C9 N4 N3 113.0(3) . . ? C9 N4 Cd1 128.6(2) . . ? N3 N4 Cd1 116.9(2) . . ? C17 N5 N6 113.2(3) . . ? C17 N5 Cd2 127.1(3) . . ? N6 N5 Cd2 117.0(2) . . ? C18 N6 N5 116.1(3) . . ? C18 N7 C19 130.1(3) . . ? C18 N7 H7N 112(3) . . ? C19 N7 H7N 118(3) . . ? O3 N8 O4 123.6(4) . . ? O3 N8 C22 117.9(4) . . ? O4 N8 C22 118.6(3) . . ? O5 N9 O6 123.1(3) . . ? O5 N9 C25 118.0(4) . . ? O6 N9 C25 118.9(4) . . ? C31 N10 C28 128.8(3) . . ? C31 N10 H10N 114(3) . . ? C28 N10 H10N 117(3) . . ? C31 N11 N12 116.9(3) . . ? C33 N12 N11 112.0(3) . . ? C33 N12 Cd1 129.2(2) . . ? N11 N12 Cd1 116.5(2) . . ? C41 N13 N14 113.5(3) . . ? C41 N13 Cd2 126.7(2) . . ? N14 N13 Cd2 117.2(2) . . ? C42 N14 N13 116.6(3) . . ? C42 N15 C43 130.1(3) . . ? C42 N15 H15N 109(3) . . ? C43 N15 H15N 120(3) . . ? O7 N16 O8 122.4(4) . . ? O7 N16 C46 118.3(4) . . ? O8 N16 C46 119.3(4) . . ? C7 S1 Cd1 95.94(13) . . ? C18 S2 Cd2 95.45(13) . . ? C31 S3 Cd1 96.39(13) . . ? C42 S4 Cd2 96.08(13) . . ? O9 S5 C50 107.2(2) . . ? O9 S5 C49 106.3(2) . . ? C50 S5 C49 97.6(2) . . ? O10 S6 C52 106.3(2) . . ? O10 S6 C51 106.6(2) . . ? C52 S6 C51 96.3(3) . . ? O11 S7 C53 106.2(2) . . ? O11 S7 C54 106.5(2) . . ? C53 S7 C54 96.9(2) . . ? O12 S8 C56 106.6(2) . . ? O12 S8 C55 107.4(2) . . ? C56 S8 C55 96.7(2) . . ? N4 Cd1 N12 130.19(10) . . ? N4 Cd1 S3 118.34(8) . . ? N12 Cd1 S3 79.10(7) . . ? N4 Cd1 S1 79.40(8) . . ? N12 Cd1 S1 112.10(7) . . ? S3 Cd1 S1 146.71(3) . . ? N4 Cd1 Cd2 118.62(8) . 1_545 ? N12 Cd1 Cd2 111.07(8) . 1_545 ? S3 Cd1 Cd2 72.34(3) . 1_545 ? S1 Cd1 Cd2 74.40(3) . 1_545 ? N5 Cd2 N13 138.16(10) . . ? N5 Cd2 S2 80.02(8) . . ? N13 Cd2 S2 115.40(8) . . ? N5 Cd2 S4 112.93(8) . . ? N13 Cd2 S4 79.38(8) . . ? S2 Cd2 S4 142.30(4) . . ? N5 Cd2 Cd1 114.63(8) . 1_565 ? N13 Cd2 Cd1 107.07(8) . 1_565 ? S2 Cd2 Cd1 74.57(3) . 1_565 ? S4 Cd2 Cd1 67.83(3) . 1_565 ? 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 C6 C1 C2 C3 -0.5(6) . . . . ? N1 C1 C2 C3 177.8(4) . . . . ? C1 C2 C3 C4 3.1(6) . . . . ? C2 C3 C4 N2 178.4(4) . . . . ? C2 C3 C4 C5 -3.1(6) . . . . ? C3 C4 C5 C6 0.6(6) . . . . ? N2 C4 C5 C6 178.9(4) . . . . ? C2 C1 C6 C5 -2.0(7) . . . . ? N1 C1 C6 C5 179.7(4) . . . . ? C4 C5 C6 C1 1.9(7) . . . . ? N4 C9 C10 C15 34.2(5) . . . . ? C8 C9 C10 C15 -142.7(4) . . . . ? N4 C9 C10 C11 -149.2(4) . . . . ? C8 C9 C10 C11 33.9(6) . . . . ? C15 C10 C11 C12 -0.1(6) . . . . ? C9 C10 C11 C12 -176.7(4) . . . . ? C10 C11 C12 C13 0.5(7) . . . . ? C11 C12 C13 C14 0.3(7) . . . . ? C12 C13 C14 C15 -1.5(6) . . . . ? C12 C13 C14 C17 178.8(4) . . . . ? C11 C10 C15 C14 -1.2(6) . . . . ? C9 C10 C15 C14 175.6(4) . . . . ? C13 C14 C15 C10 2.0(6) . . . . ? C17 C14 C15 C10 -178.3(4) . . . . ? C15 C14 C17 N5 33.0(6) . . . . ? C13 C14 C17 N5 -147.2(4) . . . . ? C15 C14 C17 C16 -146.0(4) . . . . ? C13 C14 C17 C16 33.7(6) . . . . ? N7 C19 C20 C21 -175.7(4) . . . . ? C24 C19 C20 C21 1.7(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C23 -1.6(7) . . . . ? C20 C21 C22 N8 177.1(4) . . . . ? C21 C22 C23 C24 2.1(6) . . . . ? N8 C22 C23 C24 -176.6(4) . . . . ? C22 C23 C24 C19 -0.6(6) . . . . ? N7 C19 C24 C23 176.4(4) . . . . ? C20 C19 C24 C23 -1.2(6) . . . . ? C30 C25 C26 C27 -1.2(7) . . . . ? N9 C25 C26 C27 179.7(4) . . . . ? C25 C26 C27 C28 2.0(7) . . . . ? C26 C27 C28 N10 177.0(4) . . . . ? C26 C27 C28 C29 -1.6(6) . . . . ? C27 C28 C29 C30 0.4(6) . . . . ? N10 C28 C29 C30 -178.3(4) . . . . ? C26 C25 C30 C29 0.0(6) . . . . ? N9 C25 C30 C29 179.2(4) . . . . ? C28 C29 C30 C25 0.3(6) . . . . ? N12 C33 C34 C35 -150.1(4) . . . . ? C32 C33 C34 C35 32.5(6) . . . . ? N12 C33 C34 C39 32.8(6) . . . . ? C32 C33 C34 C39 -144.6(4) . . . . ? C39 C34 C35 C36 1.4(6) . . . . ? C33 C34 C35 C36 -175.8(4) . . . . ? C34 C35 C36 C37 0.9(7) . . . . ? C35 C36 C37 C38 -2.4(6) . . . . ? C36 C37 C38 C39 1.5(6) . . . . ? C36 C37 C38 C41 -178.8(4) . . . . ? C37 C38 C39 C34 0.9(6) . . . . ? C41 C38 C39 C34 -178.9(4) . . . . ? C35 C34 C39 C38 -2.3(6) . . . . ? C33 C34 C39 C38 174.9(4) . . . . ? C39 C38 C41 N13 32.5(6) . . . . ? C37 C38 C41 N13 -147.2(4) . . . . ? C39 C38 C41 C40 -147.0(4) . . . . ? C37 C38 C41 C40 33.2(6) . . . . ? N15 C43 C44 C45 -177.4(4) . . . . ? C48 C43 C44 C45 1.6(7) . . . . ? C43 C44 C45 C46 0.1(7) . . . . ? C44 C45 C46 C47 -1.9(7) . . . . ? C44 C45 C46 N16 177.2(4) . . . . ? C45 C46 C47 C48 1.9(6) . . . . ? N16 C46 C47 C48 -177.2(4) . . . . ? C46 C47 C48 C43 -0.2(6) . . . . ? C44 C43 C48 C47 -1.6(6) . . . . ? N15 C43 C48 C47 177.5(4) . . . . ? C2 C1 N1 O1 3.3(6) . . . . ? C6 C1 N1 O1 -178.4(4) . . . . ? C2 C1 N1 O2 -176.2(4) . . . . ? C6 C1 N1 O2 2.2(6) . . . . ? N3 C7 N2 C4 0.2(6) . . . . ? S1 C7 N2 C4 -179.5(3) . . . . ? C3 C4 N2 C7 -167.7(4) . . . . ? C5 C4 N2 C7 14.0(7) . . . . ? N2 C7 N3 N4 -179.7(3) . . . . ? S1 C7 N3 N4 -0.1(6) . . . . ? C10 C9 N4 N3 -175.1(3) . . . . ? C8 C9 N4 N3 1.7(5) . . . . ? C10 C9 N4 Cd1 19.6(5) . . . . ? C8 C9 N4 Cd1 -163.6(3) . . . . ? C7 N3 N4 C9 -173.5(3) . . . . ? C7 N3 N4 Cd1 -6.3(4) . . . . ? C14 C17 N5 N6 -176.9(3) . . . . ? C16 C17 N5 N6 2.2(6) . . . . ? C14 C17 N5 Cd2 22.4(5) . . . . ? C16 C17 N5 Cd2 -158.5(3) . . . . ? N7 C18 N6 N5 179.4(3) . . . . ? S2 C18 N6 N5 0.0(6) . . . . ? C17 N5 N6 C18 -170.4(4) . . . . ? Cd2 N5 N6 C18 -7.6(4) . . . . ? N6 C18 N7 C19 -7.9(7) . . . . ? S2 C18 N7 C19 171.6(4) . . . . ? C20 C19 N7 C18 4.2(7) . . . . ? C24 C19 N7 C18 -173.2(4) . . . . ? C23 C22 N8 O3 -5.0(6) . . . . ? C21 C22 N8 O3 176.3(4) . . . . ? C23 C22 N8 O4 174.4(4) . . . . ? C21 C22 N8 O4 -4.3(6) . . . . ? C30 C25 N9 O5 6.1(6) . . . . ? C26 C25 N9 O5 -174.7(4) . . . . ? C30 C25 N9 O6 -173.7(4) . . . . ? C26 C25 N9 O6 5.4(6) . . . . ? N11 C31 N10 C28 8.3(6) . . . . ? S3 C31 N10 C28 -172.5(3) . . . . ? C27 C28 N10 C31 8.8(7) . . . . ? C29 C28 N10 C31 -172.6(4) . . . . ? N10 C31 N11 N12 -179.3(3) . . . . ? S3 C31 N11 N12 1.7(6) . . . . ? C34 C33 N12 N11 -175.3(3) . . . . ? C32 C33 N12 N11 2.0(5) . . . . ? C34 C33 N12 Cd1 22.7(5) . . . . ? C32 C33 N12 Cd1 -160.0(3) . . . . ? C31 N11 N12 C33 -172.9(4) . . . . ? C31 N11 N12 Cd1 -8.4(4) . . . . ? C38 C41 N13 N14 -176.8(3) . . . . ? C40 C41 N13 N14 2.8(6) . . . . ? C38 C41 N13 Cd2 22.3(5) . . . . ? C40 C41 N13 Cd2 -158.2(3) . . . . ? N15 C42 N14 N13 180.0(3) . . . . ? S4 C42 N14 N13 -1.8(6) . . . . ? C41 N13 N14 C42 -169.8(4) . . . . ? Cd2 N13 N14 C42 -6.8(4) . . . . ? N14 C42 N15 C43 -7.5(6) . . . . ? S4 C42 N15 C43 173.9(3) . . . . ? C44 C43 N15 C42 6.2(7) . . . . ? C48 C43 N15 C42 -172.9(4) . . . . ? C45 C46 N16 O7 -0.1(6) . . . . ? C47 C46 N16 O7 179.1(4) . . . . ? C45 C46 N16 O8 -178.9(4) . . . . ? C47 C46 N16 O8 0.3(6) . . . . ? N3 C7 S1 Cd1 5.5(4) . . . . ? N2 C7 S1 Cd1 -174.9(3) . . . . ? N6 C18 S2 Cd2 6.5(4) . . . . ? N7 C18 S2 Cd2 -173.0(3) . . . . ? N11 C31 S3 Cd1 5.0(4) . . . . ? N10 C31 S3 Cd1 -174.0(3) . . . . ? N14 C42 S4 Cd2 8.1(4) . . . . ? N15 C42 S4 Cd2 -173.6(3) . . . . ? C9 N4 Cd1 N12 -77.8(4) . . . . ? N3 N4 Cd1 N12 117.4(2) . . . . ? C9 N4 Cd1 S3 22.2(4) . . . . ? N3 N4 Cd1 S3 -142.6(2) . . . . ? C9 N4 Cd1 S1 172.1(3) . . . . ? N3 N4 Cd1 S1 7.3(2) . . . . ? C9 N4 Cd1 Cd2 106.6(3) . . . 1_545 ? N3 N4 Cd1 Cd2 -58.2(3) . . . 1_545 ? C33 N12 Cd1 N4 -71.9(4) . . . . ? N11 N12 Cd1 N4 126.8(2) . . . . ? C33 N12 Cd1 S3 170.1(3) . . . . ? N11 N12 Cd1 S3 8.7(2) . . . . ? C33 N12 Cd1 S1 22.9(4) . . . . ? N11 N12 Cd1 S1 -138.5(2) . . . . ? C33 N12 Cd1 Cd2 104.0(3) . . . 1_545 ? N11 N12 Cd1 Cd2 -57.4(2) . . . 1_545 ? C31 S3 Cd1 N4 -135.88(16) . . . . ? C31 S3 Cd1 N12 -5.88(15) . . . . ? C31 S3 Cd1 S1 107.99(15) . . . . ? C31 S3 Cd1 Cd2 110.58(14) . . . 1_545 ? C7 S1 Cd1 N4 -5.38(15) . . . . ? C7 S1 Cd1 N12 -134.62(15) . . . . ? C7 S1 Cd1 S3 121.11(14) . . . . ? C7 S1 Cd1 Cd2 118.55(13) . . . 1_545 ? C17 N5 Cd2 N13 -74.0(4) . . . . ? N6 N5 Cd2 N13 126.0(3) . . . . ? C17 N5 Cd2 S2 168.9(3) . . . . ? N6 N5 Cd2 S2 8.8(2) . . . . ? C17 N5 Cd2 S4 26.0(4) . . . . ? N6 N5 Cd2 S4 -134.1(2) . . . . ? C17 N5 Cd2 Cd1 101.1(3) . . . 1_565 ? N6 N5 Cd2 Cd1 -59.0(3) . . . 1_565 ? C41 N13 Cd2 N5 -78.1(4) . . . . ? N14 N13 Cd2 N5 121.5(3) . . . . ? C41 N13 Cd2 S2 25.9(4) . . . . ? N14 N13 Cd2 S2 -134.5(2) . . . . ? C41 N13 Cd2 S4 169.2(3) . . . . ? N14 N13 Cd2 S4 8.9(2) . . . . ? C41 N13 Cd2 Cd1 106.6(3) . . . 1_565 ? N14 N13 Cd2 Cd1 -53.8(3) . . . 1_565 ? C18 S2 Cd2 N5 -6.42(16) . . . . ? C18 S2 Cd2 N13 -145.34(16) . . . . ? C18 S2 Cd2 S4 108.36(14) . . . . ? C18 S2 Cd2 Cd1 112.76(14) . . . 1_565 ? C42 S4 Cd2 N5 -145.12(16) . . . . ? C42 S4 Cd2 N13 -7.08(15) . . . . ? C42 S4 Cd2 S2 111.02(14) . . . . ? C42 S4 Cd2 Cd1 106.44(13) . . . 1_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O9 0.82(5) 2.15(5) 2.932(5) 158(5) 4_454 N7 H7N O12 0.89(5) 1.99(5) 2.859(5) 167(4) 4_465 N10 H10N O10 0.90(5) 2.07(5) 2.956(5) 167(4) 4_455 N15 H15N O11 0.858(19) 2.06(2) 2.895(4) 163(4) 4_465 # END of CIF # Attachment '- H2LMe.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-06-15 at 14:21:50 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : H2LMe struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_Ligand _database_code_depnum_ccdc_archive 'CCDC 893874' #TrackingRef '- H2LMe.cif' _audit_creation_date 2012-06-15T14:21:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H20 N6 S2' _chemical_formula_sum 'C14 H20 N6 S2' _chemical_formula_weight 336.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4234(3) _cell_length_b 10.6842(5) _cell_length_c 14.7858(7) _cell_angle_alpha 77.839(2) _cell_angle_beta 81.951(3) _cell_angle_gamma 87.250(2) _cell_volume 829.13(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5354 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.23 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.87 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.6272 _exptl_absorpt_correction_T_max 0.7454 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_unetI/netI 0.0399 _diffrn_reflns_number 18961 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.54 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 3424 _reflns_number_gt 2620 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.2543P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3424 _refine_ls_number_parameters 219 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.315 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.061 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2040(4) 0.0512(2) 0.56615(15) 0.0260(5) Uani 1 1 d . . . H1A H 1.2197 0.051 0.5007 0.039 Uiso 1 1 calc R . . H1B H 1.1755 -0.0344 0.6014 0.039 Uiso 1 1 calc R . . H1C H 1.3544 0.0822 0.5803 0.039 Uiso 1 1 calc R . . C2 C 0.9779(4) 0.25712(19) 0.55050(13) 0.0178(4) Uani 1 1 d . . . C3 C 0.3641(4) 0.45938(18) 0.65269(14) 0.0223(5) Uani 1 1 d . . . H3A H 0.4231 0.5085 0.6925 0.033 Uiso 1 1 calc R . . H3B H 0.1878 0.4731 0.653 0.033 Uiso 1 1 calc R . . H3C H 0.447 0.4858 0.5902 0.033 Uiso 1 1 calc R . . C4 C 0.4179(4) 0.32013(17) 0.68759(12) 0.0146(4) Uani 1 1 d . . . C5 C 0.2378(3) 0.24246(17) 0.76004(12) 0.0131(4) Uani 1 1 d . . . C6 C 0.2709(4) 0.10858(17) 0.78613(13) 0.0162(4) Uani 1 1 d . . . H6 H 0.4116 0.0689 0.7602 0.019 Uiso 1 1 calc R . . C7 C 0.0965(4) 0.03647(18) 0.84972(13) 0.0171(4) Uani 1 1 d . . . H7 H 0.1184 -0.0519 0.8654 0.021 Uiso 1 1 calc R . . C8 C -0.1127(4) 0.09436(17) 0.89086(13) 0.0160(4) Uani 1 1 d . . . H8 H -0.2294 0.0443 0.9336 0.019 Uiso 1 1 calc R . . C9 C -0.1485(3) 0.22666(17) 0.86845(12) 0.0133(4) Uani 1 1 d . . . C10 C 0.0293(3) 0.29877(17) 0.80264(12) 0.0127(4) Uani 1 1 d . . . H10 H 0.0071 0.3872 0.787 0.015 Uiso 1 1 calc R . . C11 C -0.5443(4) 0.21635(17) 0.98972(12) 0.0156(4) Uani 1 1 d . . . H11A H -0.6017 0.2703 1.033 0.023 Uiso 1 1 calc R . . H11B H -0.4569 0.1431 1.0208 0.023 Uiso 1 1 calc R . . H11C H -0.6843 0.1885 0.9664 0.023 Uiso 1 1 calc R . . C12 C -0.3729(3) 0.28984(17) 0.91014(12) 0.0127(4) Uani 1 1 d . . . C13 C -0.6582(4) 0.59543(17) 0.86413(12) 0.0140(4) Uani 1 1 d . . . C14 C -0.4720(4) 0.78372(18) 0.75484(14) 0.0214(5) Uani 1 1 d . . . H14A H -0.6325 0.8051 0.7348 0.032 Uiso 1 1 calc R . . H14B H -0.3463 0.7946 0.7013 0.032 Uiso 1 1 calc R . . H14C H -0.4392 0.8389 0.7951 0.032 Uiso 1 1 calc R . . S1 S 1.17758(10) 0.33081(5) 0.45994(4) 0.02515(16) Uani 1 1 d . . . S2 S -0.93251(9) 0.66815(4) 0.89128(3) 0.01825(14) Uani 1 1 d . . . N1 N 0.9963(3) 0.13364(16) 0.59039(12) 0.0198(4) Uani 1 1 d D . . H1N H 0.901(4) 0.1089(19) 0.6388(12) 0.019(6) Uiso 1 1 d D . . N2 N 0.7821(3) 0.32357(17) 0.58753(11) 0.0183(4) Uani 1 1 d . . . H2N H 0.770(5) 0.407(3) 0.5640(17) 0.041(7) Uiso 1 1 d . . . N3 N 0.6113(3) 0.25872(15) 0.65695(10) 0.0165(4) Uani 1 1 d . . . N4 N -0.4089(3) 0.40831(14) 0.87194(10) 0.0141(3) Uani 1 1 d . . . N5 N -0.6198(3) 0.47017(15) 0.90423(11) 0.0138(3) Uani 1 1 d . . . H5N H -0.732(4) 0.4370(19) 0.9445(15) 0.015(5) Uiso 1 1 d . . . N6 N -0.4691(3) 0.65184(15) 0.80500(11) 0.0155(4) Uani 1 1 d . . . H6N H -0.335(4) 0.606(2) 0.8030(14) 0.020(6) Uiso 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 C1 0.0222(12) 0.0268(12) 0.0312(12) -0.0124(9) -0.0036(9) 0.0087(9) C2 0.0155(11) 0.0241(11) 0.0155(10) -0.0084(8) -0.0023(8) 0.0008(8) C3 0.0233(12) 0.0169(10) 0.0223(11) -0.0014(8) 0.0080(9) 0.0001(8) C4 0.0150(10) 0.0155(9) 0.0136(9) -0.0044(7) -0.0015(8) 0.0002(8) C5 0.0126(10) 0.0154(9) 0.0121(9) -0.0038(7) -0.0034(7) -0.0001(7) C6 0.0148(11) 0.0160(10) 0.0179(10) -0.0061(7) -0.0002(8) 0.0045(8) C7 0.0199(11) 0.0108(9) 0.0193(10) -0.0022(7) -0.0006(8) 0.0014(8) C8 0.0161(11) 0.0145(9) 0.0160(10) -0.0020(7) 0.0015(8) -0.0015(8) C9 0.0132(10) 0.0154(9) 0.0123(9) -0.0044(7) -0.0032(7) -0.0007(8) C10 0.0143(10) 0.0109(9) 0.0135(9) -0.0031(7) -0.0029(7) -0.0002(7) C11 0.0146(10) 0.0156(9) 0.0154(9) -0.0028(7) 0.0010(8) 0.0002(8) C12 0.0125(10) 0.0128(9) 0.0132(9) -0.0030(7) -0.0019(7) -0.0019(7) C13 0.0153(10) 0.0129(9) 0.0153(9) -0.0058(7) -0.0031(8) -0.0002(7) C14 0.0245(12) 0.0161(10) 0.0198(10) -0.0006(8) 0.0040(9) 0.0028(8) S1 0.0236(3) 0.0286(3) 0.0200(3) -0.0059(2) 0.0091(2) 0.0008(2) S2 0.0124(3) 0.0155(2) 0.0252(3) -0.00310(19) 0.0000(2) 0.00382(19) N1 0.0170(10) 0.0236(9) 0.0182(9) -0.0062(7) 0.0023(7) 0.0015(7) N2 0.0163(9) 0.0200(9) 0.0161(8) -0.0027(7) 0.0039(7) 0.0016(7) N3 0.0144(9) 0.0215(9) 0.0134(8) -0.0049(6) 0.0007(7) -0.0003(7) N4 0.0115(9) 0.0144(8) 0.0170(8) -0.0056(6) -0.0008(6) 0.0011(6) N5 0.0092(9) 0.0145(8) 0.0162(8) -0.0024(6) 0.0020(7) 0.0008(6) N6 0.0128(9) 0.0134(8) 0.0187(8) -0.0028(6) 0.0009(7) 0.0041(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.449(3) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 N1 1.332(3) . ? C2 N2 1.364(2) . ? C2 S1 1.678(2) . ? C3 C4 1.497(3) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 N3 1.290(2) . ? C4 C5 1.483(3) . ? C5 C10 1.390(2) . ? C5 C6 1.410(3) . ? C6 C7 1.374(3) . ? C6 H6 0.93 . ? C7 C8 1.392(3) . ? C7 H7 0.93 . ? C8 C9 1.393(3) . ? C8 H8 0.93 . ? C9 C10 1.401(3) . ? C9 C12 1.484(3) . ? C10 H10 0.93 . ? C11 C12 1.497(2) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N4 1.290(2) . ? C13 N6 1.329(2) . ? C13 N5 1.364(2) . ? C13 S2 1.6827(19) . ? C14 N6 1.448(2) . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? N1 H1N 0.824(15) . ? N2 N3 1.374(2) . ? N2 H2N 0.88(3) . ? N4 N5 1.371(2) . ? N5 H5N 0.82(2) . ? N6 H6N 0.86(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 115.89(17) . . ? N1 C2 S1 123.82(15) . . ? N2 C2 S1 120.29(15) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 115.59(16) . . ? N3 C4 C3 124.45(17) . . ? C5 C4 C3 119.92(16) . . ? C10 C5 C6 118.13(17) . . ? C10 C5 C4 121.15(16) . . ? C6 C5 C4 120.71(16) . . ? C7 C6 C5 120.36(17) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.69(17) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 120.52(18) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 118.14(17) . . ? C8 C9 C12 121.30(17) . . ? C10 C9 C12 120.53(16) . . ? C5 C10 C9 122.13(17) . . ? C5 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C9 115.60(16) . . ? N4 C12 C11 123.90(17) . . ? C9 C12 C11 120.49(16) . . ? N6 C13 N5 115.85(17) . . ? N6 C13 S2 124.48(14) . . ? N5 C13 S2 119.67(14) . . ? N6 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 N1 C1 123.55(18) . . ? C2 N1 H1N 116.3(15) . . ? C1 N1 H1N 118.6(15) . . ? C2 N2 N3 118.96(17) . . ? C2 N2 H2N 117.4(17) . . ? N3 N2 H2N 123.6(17) . . ? C4 N3 N2 118.82(16) . . ? C12 N4 N5 118.38(16) . . ? C13 N5 N4 118.51(16) . . ? C13 N5 H5N 115.9(15) . . ? N4 N5 H5N 125.5(15) . . ? C13 N6 C14 124.57(16) . . ? C13 N6 H6N 114.0(14) . . ? C14 N6 H6N 121.1(15) . . ? 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 N3 C4 C5 C10 176.15(17) . . . . ? C3 C4 C5 C10 -5.8(3) . . . . ? N3 C4 C5 C6 -5.2(3) . . . . ? C3 C4 C5 C6 172.76(17) . . . . ? C10 C5 C6 C7 2.1(3) . . . . ? C4 C5 C6 C7 -176.58(17) . . . . ? C5 C6 C7 C8 -1.4(3) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C7 C8 C9 C10 1.0(3) . . . . ? C7 C8 C9 C12 178.76(17) . . . . ? C6 C5 C10 C9 -1.3(3) . . . . ? C4 C5 C10 C9 177.35(16) . . . . ? C8 C9 C10 C5 -0.2(3) . . . . ? C12 C9 C10 C5 -178.02(16) . . . . ? C8 C9 C12 N4 -167.78(17) . . . . ? C10 C9 C12 N4 10.0(3) . . . . ? C8 C9 C12 C11 10.8(3) . . . . ? C10 C9 C12 C11 -171.48(17) . . . . ? N2 C2 N1 C1 -174.13(17) . . . . ? S1 C2 N1 C1 6.1(3) . . . . ? N1 C2 N2 N3 -4.6(3) . . . . ? S1 C2 N2 N3 175.16(13) . . . . ? C5 C4 N3 N2 177.86(15) . . . . ? C3 C4 N3 N2 0.0(3) . . . . ? C2 N2 N3 C4 -175.53(17) . . . . ? C9 C12 N4 N5 176.74(15) . . . . ? C11 C12 N4 N5 -1.8(3) . . . . ? N6 C13 N5 N4 -8.7(2) . . . . ? S2 C13 N5 N4 171.42(13) . . . . ? C12 N4 N5 C13 179.86(16) . . . . ? N5 C13 N6 C14 179.69(17) . . . . ? S2 C13 N6 C14 -0.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N3 0.824(15) 2.22(2) 2.612(2) 109.5(17) . N6 H6N N4 0.86(2) 2.17(2) 2.604(2) 111.1(17) . C6 H6 N3 0.93 2.46 2.763(3) 98.9 . C10 H10 N4 0.93 2.45 2.761(2) 99.6 . N2 H2N S1 0.88(3) 2.78(3) 3.6220(19) 160(2) 2_766 N5 H5N S2 0.82(2) 2.88(2) 3.6913(18) 169.6(18) 2_367 # END of CIF