Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_section_title ; Hierarchical regulated assembly of new metallosupramolecular networks on the basis of metal thiocyanate and trans-1-(2-pyridyl)-2-(4-pyridyl)ethylene (bpe) via multiple interactions ; _publ_contact_author 'Miao Du' _publ_contact_author_address ; College of Chemistry and Life Science, Tianjin Normal University, Tianjin 300074, P. R. China ; _publ_contact_author_email dumiao@public.tpt.tj.cn _publ_contact_author_name 'Miao Du' loop_ _publ_author_name 'Miao Du.' 'Cheng-Peng Li.' 'Xiao-Jun Zhao.' data_1 _database_code_depnum_ccdc_archive 'CCDC 284287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Co N6 O2 S2' _chemical_formula_weight 589.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.139(3) _cell_length_b 10.665(4) _cell_length_c 14.968(6) _cell_angle_alpha 103.458(6) _cell_angle_beta 96.406(7) _cell_angle_gamma 97.493(7) _cell_volume 1391.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 704 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 24.18 _exptl_crystal_description Block _exptl_crystal_colour Pale-red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.672783 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7283 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4889 _reflns_number_gt 3258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.0402P)^2^+0.7574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4889 _refine_ls_number_parameters 423 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.70985(6) 0.79967(5) 0.74278(4) 0.03553(17) Uani 1 1 d . . . S1 S 1.07324(15) 1.17888(14) 0.88752(10) 0.0718(4) Uani 1 1 d . A . S2 S 0.36786(16) 0.40077(14) 0.60130(10) 0.0734(4) Uani 1 1 d . A . O1 O 0.6461(3) 0.7981(3) 0.8756(2) 0.0472(8) Uani 1 1 d . A . H1 H 0.6243 0.7154 0.8859 0.057 Uiso 1 1 calc R . . N1 N 0.8394(4) 0.9850(4) 0.7944(3) 0.0467(9) Uani 1 1 d . A . N2 N 0.5794(4) 0.6178(4) 0.6889(3) 0.0495(10) Uani 1 1 d . A . N3 N 0.5184(4) 0.8882(3) 0.7059(2) 0.0417(9) Uani 1 1 d . A . N4 N -0.0123(4) 1.2478(3) 0.4908(3) 0.0466(9) Uani 1 1 d . . . C1 C 0.9342(5) 1.0638(4) 0.8334(3) 0.0439(11) Uani 1 1 d . . . C2 C 0.4924(5) 0.5278(4) 0.6511(3) 0.0411(10) Uani 1 1 d . . . C3 C 0.5215(5) 0.9697(4) 0.6505(3) 0.0502(12) Uani 1 1 d . . . H3 H 0.6087 0.9878 0.6259 0.060 Uiso 1 1 calc R A . C4 C 0.4015(5) 1.0285(4) 0.6278(3) 0.0545(12) Uani 1 1 d . A . H4 H 0.4090 1.0841 0.5885 0.065 Uiso 1 1 calc R . . C5 C 0.2692(5) 1.0050(4) 0.6635(3) 0.0441(11) Uani 1 1 d . . . C6 C 0.2685(5) 0.9213(5) 0.7208(3) 0.0555(13) Uani 1 1 d . A . H6 H 0.1837 0.9027 0.7474 0.067 Uiso 1 1 calc R . . C7 C 0.3908(5) 0.8651(5) 0.7393(3) 0.0514(12) Uani 1 1 d . . . H7 H 0.3848 0.8075 0.7773 0.062 Uiso 1 1 calc R A . C8 C 0.1365(5) 1.0653(4) 0.6440(3) 0.0539(12) Uani 1 1 d . A . H8 H 0.0622 1.0580 0.6810 0.065 Uiso 1 1 calc R . . C9 C 0.1139(5) 1.1271(4) 0.5804(3) 0.0490(11) Uani 1 1 d . . . H9 H 0.1868 1.1311 0.5421 0.059 Uiso 1 1 calc R A . C10 C -0.0153(5) 1.1921(4) 0.5622(3) 0.0426(10) Uani 1 1 d . A . C11 C -0.1299(5) 1.2008(5) 0.6158(4) 0.0572(13) Uani 1 1 d . . . H11 H -0.1302 1.1620 0.6654 0.069 Uiso 1 1 calc R A . C12 C -0.2424(5) 1.2670(5) 0.5951(4) 0.0612(14) Uani 1 1 d . A . H12 H -0.3205 1.2724 0.6299 0.073 Uiso 1 1 calc R . . C13 C -0.2394(5) 1.3254(5) 0.5229(4) 0.0587(13) Uani 1 1 d . . . H13 H -0.3141 1.3717 0.5081 0.070 Uiso 1 1 calc R A . C14 C -0.1224(5) 1.3133(4) 0.4730(3) 0.0538(12) Uani 1 1 d . A . H14 H -0.1197 1.3530 0.4240 0.065 Uiso 1 1 calc R . . N5 N 0.9071(11) 0.7248(12) 0.7905(10) 0.042(4) Uani 0.518(11) 1 d PGU A 1 C15 C 0.9976(13) 0.7907(10) 0.8734(9) 0.072(5) Uani 0.518(11) 1 d PG A 1 H15A H 0.9722 0.8656 0.9101 0.086 Uiso 0.518(11) 1 calc PR A 1 C16 C 1.1261(11) 0.7448(8) 0.9016(6) 0.043(3) Uani 0.518(11) 1 d PG A 1 H16A H 1.1867 0.7889 0.9570 0.052 Uiso 0.518(11) 1 calc PR A 1 C17 C 1.1641(8) 0.6329(8) 0.8468(6) 0.035(3) Uani 0.518(11) 1 d PGD A 1 C18 C 1.0736(10) 0.5670(8) 0.7639(6) 0.043(3) Uani 0.518(11) 1 d PGD A 1 H18A H 1.0990 0.4921 0.7272 0.052 Uiso 0.518(11) 1 calc PR A 1 C19 C 0.9451(11) 0.6129(10) 0.7357(7) 0.039(3) Uani 0.518(11) 1 d PG A 1 H19A H 0.8845 0.5688 0.6802 0.047 Uiso 0.518(11) 1 calc PR A 1 C20 C 1.2995(7) 0.5846(8) 0.8689(6) 0.039(3) Uani 0.518(11) 1 d PD A 1 H20A H 1.3683 0.6442 0.9146 0.047 Uiso 0.518(11) 1 calc PR A 1 C21 C 1.3450(9) 0.4755(8) 0.8382(6) 0.037(3) Uani 0.518(11) 1 d PD A 1 H21A H 1.2743 0.4116 0.7969 0.045 Uiso 0.518(11) 1 calc PR A 1 C22 C 1.4889(9) 0.4366(11) 0.8579(7) 0.039(3) Uani 0.518(11) 1 d PGDU A 1 C23 C 1.5203(10) 0.3098(9) 0.8398(11) 0.066(5) Uani 0.518(11) 1 d PGD A 1 H23A H 1.4448 0.2397 0.8118 0.079 Uiso 0.518(11) 1 calc PR A 1 C24 C 1.6644(12) 0.2878(9) 0.8636(14) 0.074(6) Uani 0.518(11) 1 d PG A 1 H24A H 1.6854 0.2030 0.8514 0.088 Uiso 0.518(11) 1 calc PR A 1 C25 C 1.7772(9) 0.3926(13) 0.9054(12) 0.050(5) Uani 0.518(11) 1 d PG A 1 H25A H 1.8736 0.3778 0.9213 0.060 Uiso 0.518(11) 1 calc PR A 1 C26 C 1.7457(11) 0.5193(10) 0.9235(9) 0.028(3) Uani 0.518(11) 1 d PGU A 1 H26A H 1.8212 0.5894 0.9516 0.034 Uiso 0.518(11) 1 calc PR A 1 N6 N 1.6016(13) 0.5414(8) 0.8998(8) 0.035(3) Uani 0.518(11) 1 d PGU A 1 N5' N 0.8934(10) 0.7021(11) 0.7768(9) 0.031(3) Uani 0.482(11) 1 d PG A 2 C15' C 0.9972(10) 0.7575(9) 0.8560(7) 0.019(2) Uani 0.482(11) 1 d PG A 2 H15B H 0.9861 0.8358 0.8958 0.022 Uiso 0.482(11) 1 calc PR A 2 C16' C 1.1175(9) 0.6961(10) 0.8758(6) 0.033(3) Uani 0.482(11) 1 d PGU A 2 H16B H 1.1869 0.7332 0.9288 0.039 Uiso 0.482(11) 1 calc PR A 2 C17' C 1.1340(7) 0.5792(10) 0.8164(7) 0.033(3) Uani 0.482(11) 1 d PGDU A 2 C18' C 1.0302(10) 0.5237(10) 0.7371(7) 0.053(4) Uani 0.482(11) 1 d PGD A 2 H18B H 1.0413 0.4455 0.6973 0.063 Uiso 0.482(11) 1 calc PR A 2 C19' C 0.9099(11) 0.5852(11) 0.7173(8) 0.054(4) Uani 0.482(11) 1 d PGU A 2 H19B H 0.8405 0.5480 0.6643 0.065 Uiso 0.482(11) 1 calc PR A 2 C20' C 1.2552(8) 0.5015(11) 0.8264(7) 0.052(3) Uani 0.482(11) 1 d PDU A 2 H20B H 1.2400 0.4139 0.7944 0.062 Uiso 0.482(11) 1 calc PR A 2 C21' C 1.3842(8) 0.5530(11) 0.8796(7) 0.054(4) Uani 0.482(11) 1 d PD A 2 H21B H 1.3949 0.6381 0.9160 0.064 Uiso 0.482(11) 1 calc PR A 2 C22' C 1.5122(8) 0.4822(11) 0.8840(8) 0.031(3) Uani 0.482(11) 1 d PGDU A 2 C23' C 1.5018(12) 0.3473(11) 0.8550(12) 0.056(4) Uani 0.482(11) 1 d PGD A 2 H23B H 1.4089 0.2950 0.8347 0.067 Uiso 0.482(11) 1 calc PR A 2 C24' C 1.6303(18) 0.2905(9) 0.8564(15) 0.065(5) Uani 0.482(11) 1 d PG A 2 H24B H 1.6234 0.2003 0.8371 0.078 Uiso 0.482(11) 1 calc PR A 2 C25' C 1.7693(13) 0.3687(15) 0.8868(15) 0.069(7) Uani 0.482(11) 1 d PG A 2 H25B H 1.8553 0.3307 0.8878 0.082 Uiso 0.482(11) 1 calc PR A 2 C26' C 1.7796(8) 0.5036(14) 0.9158(12) 0.074(6) Uani 0.482(11) 1 d PG A 2 H26B H 1.8726 0.5559 0.9361 0.088 Uiso 0.482(11) 1 calc PR A 2 N6' N 1.6511(12) 0.5604(9) 0.9143(9) 0.041(3) Uani 0.482(11) 1 d PGU A 2 O2 O 0.7644(3) 0.7827(3) 0.60513(19) 0.0522(8) Uani 1 1 d . A . H2A H 0.7044 0.7196 0.5684 0.063 Uiso 1 1 d R . . H2B H 0.8554 0.7892 0.5968 0.063 Uiso 1 1 d R . . C27 C 0.6316(7) 0.9012(5) 0.9497(4) 0.0775(17) Uani 1 1 d . . . H27A H 0.7237 0.9269 0.9919 0.116 Uiso 1 1 calc R A . H27B H 0.5529 0.8734 0.9817 0.116 Uiso 1 1 calc R . . H27C H 0.6084 0.9740 0.9264 0.116 Uiso 1 1 calc R . . 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 0.0324(3) 0.0380(3) 0.0380(3) 0.0117(2) 0.0055(2) 0.0079(2) S1 0.0556(8) 0.0675(9) 0.0740(10) -0.0087(7) -0.0043(7) 0.0036(7) S2 0.0771(10) 0.0686(9) 0.0561(9) -0.0012(7) 0.0109(8) -0.0248(8) O1 0.062(2) 0.0457(17) 0.0436(18) 0.0170(14) 0.0210(16) 0.0221(15) N1 0.038(2) 0.045(2) 0.058(3) 0.016(2) 0.0040(19) 0.0055(18) N2 0.047(2) 0.045(2) 0.053(3) 0.010(2) 0.006(2) 0.0018(19) N3 0.037(2) 0.046(2) 0.046(2) 0.0200(18) 0.0054(17) 0.0065(16) N4 0.043(2) 0.048(2) 0.052(2) 0.0160(19) 0.0072(19) 0.0100(17) C1 0.054(3) 0.046(3) 0.040(3) 0.016(2) 0.014(2) 0.021(2) C2 0.045(3) 0.044(3) 0.038(3) 0.013(2) 0.011(2) 0.011(2) C3 0.041(3) 0.056(3) 0.064(3) 0.031(3) 0.014(2) 0.012(2) C4 0.060(3) 0.052(3) 0.062(3) 0.033(2) 0.005(3) 0.014(2) C5 0.038(2) 0.045(3) 0.048(3) 0.007(2) 0.006(2) 0.010(2) C6 0.042(3) 0.077(3) 0.059(3) 0.032(3) 0.014(2) 0.019(2) C7 0.041(3) 0.070(3) 0.055(3) 0.035(3) 0.011(2) 0.014(2) C8 0.053(3) 0.062(3) 0.052(3) 0.019(3) 0.014(3) 0.016(2) C9 0.048(3) 0.048(3) 0.051(3) 0.012(2) 0.005(2) 0.007(2) C10 0.039(2) 0.037(2) 0.049(3) 0.006(2) 0.003(2) 0.0092(19) C11 0.055(3) 0.068(3) 0.064(3) 0.034(3) 0.018(3) 0.022(3) C12 0.049(3) 0.077(4) 0.070(4) 0.027(3) 0.024(3) 0.026(3) C13 0.054(3) 0.059(3) 0.071(4) 0.021(3) 0.011(3) 0.027(2) C14 0.058(3) 0.055(3) 0.052(3) 0.022(2) 0.004(3) 0.013(2) N5 0.044(7) 0.027(5) 0.056(7) 0.004(5) 0.026(6) 0.004(4) C15 0.082(11) 0.072(9) 0.063(10) 0.011(7) 0.010(8) 0.030(8) C16 0.059(7) 0.036(7) 0.032(6) -0.006(5) 0.009(5) 0.026(5) C17 0.045(6) 0.031(6) 0.021(6) -0.006(5) 0.004(4) -0.002(5) C18 0.058(8) 0.021(6) 0.043(8) -0.015(6) 0.021(7) 0.009(6) C19 0.038(6) 0.032(6) 0.036(6) 0.001(5) -0.004(5) -0.008(5) C20 0.026(5) 0.053(6) 0.037(6) 0.011(5) 0.000(5) 0.008(5) C21 0.026(6) 0.053(6) 0.035(6) 0.016(5) -0.003(4) 0.009(5) C22 0.053(6) 0.038(6) 0.024(6) -0.003(5) 0.011(4) 0.009(5) C23 0.092(11) 0.044(7) 0.070(10) 0.014(7) 0.017(8) 0.037(7) C24 0.072(10) 0.086(14) 0.060(11) 0.001(10) -0.008(8) 0.052(9) C25 0.051(9) 0.061(9) 0.053(10) 0.023(7) 0.021(7) 0.036(7) C26 0.013(4) 0.041(4) 0.036(4) 0.014(3) 0.007(3) 0.016(3) N6 0.021(6) 0.053(6) 0.042(5) 0.023(4) 0.006(4) 0.020(4) N5' 0.028(6) 0.034(6) 0.030(6) 0.005(5) -0.002(5) 0.012(5) C15' 0.012(5) 0.026(4) 0.016(5) 0.000(4) 0.001(4) 0.005(3) C16' 0.038(5) 0.035(7) 0.019(5) -0.009(5) 0.008(4) 0.011(5) C17' 0.037(6) 0.042(6) 0.023(6) 0.007(6) 0.006(5) 0.019(5) C18' 0.060(8) 0.028(7) 0.069(10) 0.000(6) 0.017(7) 0.016(6) C19' 0.037(6) 0.053(7) 0.066(7) -0.003(5) 0.007(5) 0.012(6) C20' 0.058(6) 0.043(6) 0.052(6) 0.005(5) 0.010(5) 0.012(5) C21' 0.035(6) 0.086(10) 0.030(6) 0.018(6) -0.008(5) -0.020(6) C22' 0.025(5) 0.036(6) 0.031(6) 0.010(5) -0.006(4) 0.005(5) C23' 0.052(7) 0.042(8) 0.070(10) 0.011(8) -0.007(7) 0.016(7) C24' 0.093(11) 0.047(10) 0.071(13) 0.030(9) 0.011(10) 0.041(8) C25' 0.078(15) 0.091(14) 0.042(9) 0.010(9) 0.001(9) 0.051(11) C26' 0.067(9) 0.106(13) 0.081(11) 0.043(8) 0.043(9) 0.070(9) N6' 0.020(6) 0.060(6) 0.047(6) 0.023(4) 0.003(5) 0.008(4) O2 0.0408(17) 0.073(2) 0.0401(19) 0.0114(16) 0.0088(15) 0.0016(15) C27 0.097(4) 0.084(4) 0.055(4) 0.009(3) 0.019(3) 0.036(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 2.071(4) . ? Co1 N1 2.093(4) . ? Co1 O1 2.137(3) . ? Co1 O2 2.146(3) . ? Co1 N5' 2.160(5) . ? Co1 N3 2.172(3) . ? Co1 N5 2.180(6) . ? S1 C1 1.637(5) . ? S2 C2 1.620(5) . ? O1 C27 1.399(5) . ? O1 H1 0.9300 . ? N1 C1 1.125(5) . ? N2 C2 1.149(5) . ? N3 C3 1.334(5) . ? N3 C7 1.335(5) . ? N4 C14 1.334(5) . ? N4 C10 1.339(5) . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 C5 1.391(6) . ? C4 H4 0.9300 . ? C5 C6 1.374(6) . ? C5 C8 1.477(6) . ? C6 C7 1.366(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.291(6) . ? C8 H8 0.9300 . ? C9 C10 1.476(6) . ? C9 H9 0.9300 . ? C10 C11 1.389(6) . ? C11 C12 1.368(6) . ? C11 H11 0.9300 . ? C12 C13 1.368(6) . ? C12 H12 0.9300 . ? C13 C14 1.374(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? N5 C15 1.3900 . ? N5 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C17 C18 1.3900 . ? C17 C20 1.435(6) . ? C18 C19 1.3900 . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.287(8) . ? C20 H20A 0.9300 . ? C21 C22 1.449(6) . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 N6 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 H25A 0.9300 . ? C26 N6 1.3900 . ? C26 H26A 0.9300 . ? N5' C15' 1.3900 . ? N5' C19' 1.3900 . ? C15' C16' 1.3900 . ? C15' H15B 0.9300 . ? C16' C17' 1.3900 . ? C16' H16B 0.9300 . ? C17' C18' 1.3900 . ? C17' C20' 1.482(9) . ? C18' C19' 1.3900 . ? C18' H18B 0.9300 . ? C19' H19B 0.9300 . ? C20' C21' 1.320(9) . ? C20' H20B 0.9300 . ? C21' C22' 1.476(7) . ? C21' H21B 0.9300 . ? C22' C23' 1.3900 . ? C22' N6' 1.3900 . ? C23' C24' 1.3900 . ? C23' H23B 0.9300 . ? C24' C25' 1.3900 . ? C24' H24B 0.9300 . ? C25' C26' 1.3900 . ? C25' H25B 0.9300 . ? C26' N6' 1.3900 . ? C26' H26B 0.9300 . ? O2 H2A 0.8483 . ? O2 H2B 0.8509 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N1 178.57(16) . . ? N2 Co1 O1 88.95(13) . . ? N1 Co1 O1 92.02(13) . . ? N2 Co1 O2 85.84(13) . . ? N1 Co1 O2 93.20(13) . . ? O1 Co1 O2 174.72(12) . . ? N2 Co1 N5' 88.4(3) . . ? N1 Co1 N5' 92.7(3) . . ? O1 Co1 N5' 88.5(4) . . ? O2 Co1 N5' 90.5(4) . . ? N2 Co1 N3 88.71(14) . . ? N1 Co1 N3 90.22(13) . . ? O1 Co1 N3 91.39(12) . . ? O2 Co1 N3 89.40(12) . . ? N5' Co1 N3 177.1(3) . . ? N2 Co1 N5 95.3(4) . . ? N1 Co1 N5 85.8(4) . . ? O1 Co1 N5 85.8(4) . . ? O2 Co1 N5 93.8(4) . . ? N5' Co1 N5 7.4(5) . . ? N3 Co1 N5 175.0(4) . . ? C27 O1 Co1 130.6(3) . . ? C27 O1 H1 114.7 . . ? Co1 O1 H1 114.7 . . ? C1 N1 Co1 160.0(4) . . ? C2 N2 Co1 168.6(4) . . ? C3 N3 C7 116.3(4) . . ? C3 N3 Co1 122.5(3) . . ? C7 N3 Co1 121.2(3) . . ? C14 N4 C10 118.0(4) . . ? N1 C1 S1 178.5(4) . . ? N2 C2 S2 178.0(4) . . ? N3 C3 C4 123.1(4) . . ? N3 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 115.6(4) . . ? C6 C5 C8 120.5(4) . . ? C4 C5 C8 123.9(4) . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? N3 C7 C6 123.7(4) . . ? N3 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? C9 C8 C5 126.2(4) . . ? C9 C8 H8 116.9 . . ? C5 C8 H8 116.9 . . ? C8 C9 C10 126.9(4) . . ? C8 C9 H9 116.5 . . ? C10 C9 H9 116.5 . . ? N4 C10 C11 121.3(4) . . ? N4 C10 C9 114.8(4) . . ? C11 C10 C9 123.8(4) . . ? C12 C11 C10 119.4(4) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 117.8(4) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? N4 C14 C13 123.8(4) . . ? N4 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C15 N5 C19 120.0 . . ? C15 N5 Co1 120.5(6) . . ? C19 N5 Co1 119.5(6) . . ? C16 C15 N5 120.0 . . ? C16 C15 H15A 120.0 . . ? N5 C15 H15A 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 C20 122.9(6) . . ? C18 C17 C20 117.0(6) . . ? C19 C18 C17 120.0 . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 N5 120.0 . . ? C18 C19 H19A 120.0 . . ? N5 C19 H19A 120.0 . . ? C21 C20 C17 133.0(8) . . ? C21 C20 H20A 113.5 . . ? C17 C20 H20A 113.5 . . ? C20 C21 C22 130.3(9) . . ? C20 C21 H21A 114.9 . . ? C22 C21 H21A 114.9 . . ? C23 C22 N6 120.0 . . ? C23 C22 C21 126.7(8) . . ? N6 C22 C21 113.3(8) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? N6 C26 C25 120.0 . . ? N6 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 N6 C22 120.0 . . ? C15' N5' C19' 120.0 . . ? C15' N5' Co1 120.4(5) . . ? C19' N5' Co1 119.6(5) . . ? N5' C15' C16' 120.0 . . ? N5' C15' H15B 120.0 . . ? C16' C15' H15B 120.0 . . ? C17' C16' C15' 120.0 . . ? C17' C16' H16B 120.0 . . ? C15' C16' H16B 120.0 . . ? C18' C17' C16' 120.0 . . ? C18' C17' C20' 112.9(6) . . ? C16' C17' C20' 127.1(6) . . ? C17' C18' C19' 120.0 . . ? C17' C18' H18B 120.0 . . ? C19' C18' H18B 120.0 . . ? C18' C19' N5' 120.0 . . ? C18' C19' H19B 120.0 . . ? N5' C19' H19B 120.0 . . ? C21' C20' C17' 121.9(9) . . ? C21' C20' H20B 119.1 . . ? C17' C20' H20B 119.0 . . ? C20' C21' C22' 123.2(9) . . ? C20' C21' H21B 118.4 . . ? C22' C21' H21B 118.4 . . ? C23' C22' N6' 120.0 . . ? C23' C22' C21' 124.4(8) . . ? N6' C22' C21' 115.4(8) . . ? C22' C23' C24' 120.0 . . ? C22' C23' H23B 120.0 . . ? C24' C23' H23B 120.0 . . ? C23' C24' C25' 120.0 . . ? C23' C24' H24B 120.0 . . ? C25' C24' H24B 120.0 . . ? C26' C25' C24' 120.0 . . ? C26' C25' H25B 120.0 . . ? C24' C25' H25B 120.0 . . ? C25' C26' N6' 120.0 . . ? C25' C26' H26B 120.0 . . ? N6' C26' H26B 120.0 . . ? C26' N6' C22' 120.0 . . ? Co1 O2 H2A 108.3 . . ? Co1 O2 H2B 119.6 . . ? H2A O2 H2B 116.6 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 N2 Co1 O1 C27 -150.9(4) . . . . ? N1 Co1 O1 C27 28.1(4) . . . . ? N5' Co1 O1 C27 120.7(5) . . . . ? N3 Co1 O1 C27 -62.2(4) . . . . ? N5 Co1 O1 C27 113.8(5) . . . . ? O1 Co1 N1 C1 72.6(11) . . . . ? O2 Co1 N1 C1 -106.6(11) . . . . ? N5' Co1 N1 C1 -16.0(12) . . . . ? N3 Co1 N1 C1 164.0(11) . . . . ? N5 Co1 N1 C1 -13.0(12) . . . . ? O1 Co1 N2 C2 112.1(18) . . . . ? O2 Co1 N2 C2 -68.8(18) . . . . ? N5' Co1 N2 C2 -159.4(19) . . . . ? N3 Co1 N2 C2 20.7(18) . . . . ? N5 Co1 N2 C2 -162.3(19) . . . . ? N2 Co1 N3 C3 -122.8(4) . . . . ? N1 Co1 N3 C3 56.2(4) . . . . ? O1 Co1 N3 C3 148.3(4) . . . . ? O2 Co1 N3 C3 -37.0(4) . . . . ? N2 Co1 N3 C7 58.3(4) . . . . ? N1 Co1 N3 C7 -122.6(4) . . . . ? O1 Co1 N3 C7 -30.6(3) . . . . ? O2 Co1 N3 C7 144.2(3) . . . . ? C7 N3 C3 C4 0.1(7) . . . . ? Co1 N3 C3 C4 -178.8(4) . . . . ? N3 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C3 C4 C5 C8 179.0(4) . . . . ? C4 C5 C6 C7 -0.8(7) . . . . ? C8 C5 C6 C7 -180.0(4) . . . . ? C3 N3 C7 C6 -1.1(7) . . . . ? Co1 N3 C7 C6 177.8(4) . . . . ? C5 C6 C7 N3 1.5(8) . . . . ? C6 C5 C8 C9 -167.7(5) . . . . ? C4 C5 C8 C9 13.2(8) . . . . ? C5 C8 C9 C10 -177.6(4) . . . . ? C14 N4 C10 C11 0.6(6) . . . . ? C14 N4 C10 C9 -177.1(4) . . . . ? C8 C9 C10 N4 -179.1(5) . . . . ? C8 C9 C10 C11 3.3(8) . . . . ? N4 C10 C11 C12 0.3(7) . . . . ? C9 C10 C11 C12 177.8(4) . . . . ? C10 C11 C12 C13 -1.0(8) . . . . ? C11 C12 C13 C14 0.7(8) . . . . ? C10 N4 C14 C13 -0.9(7) . . . . ? C12 C13 C14 N4 0.2(8) . . . . ? N2 Co1 N5 C15 -142.7(6) . . . . ? N1 Co1 N5 C15 38.2(6) . . . . ? O1 Co1 N5 C15 -54.2(6) . . . . ? O2 Co1 N5 C15 131.1(6) . . . . ? N5' Co1 N5 C15 -166(7) . . . . ? N2 Co1 N5 C19 39.6(7) . . . . ? N1 Co1 N5 C19 -139.5(7) . . . . ? O1 Co1 N5 C19 128.2(7) . . . . ? O2 Co1 N5 C19 -46.6(7) . . . . ? Co1 N5 C15 C16 -177.7(9) . . . . ? N5 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C15 C16 C17 C20 176.2(10) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C20 C17 C18 C19 -176.4(9) . . . . ? C17 C18 C19 N5 0.0 . . . . ? C15 N5 C19 C18 0.0 . . . . ? Co1 N5 C19 C18 177.7(9) . . . . ? C16 C17 C20 C21 166.8(10) . . . . ? C18 C17 C20 C21 -17.0(14) . . . . ? C17 C20 C21 C22 174.1(10) . . . . ? C20 C21 C22 C23 163.9(11) . . . . ? C20 C21 C22 N6 -15.5(14) . . . . ? N6 C22 C23 C24 0.0 . . . . ? C21 C22 C23 C24 -179.4(11) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 N6 0.0 . . . . ? C25 C26 N6 C22 0.0 . . . . ? C23 C22 N6 C26 0.0 . . . . ? C21 C22 N6 C26 179.5(10) . . . . ? N2 Co1 N5' C15' -145.8(7) . . . . ? N1 Co1 N5' C15' 35.1(7) . . . . ? O1 Co1 N5' C15' -56.8(7) . . . . ? O2 Co1 N5' C15' 128.3(7) . . . . ? N2 Co1 N5' C19' 36.2(5) . . . . ? N1 Co1 N5' C19' -142.9(5) . . . . ? O1 Co1 N5' C19' 125.2(6) . . . . ? O2 Co1 N5' C19' -49.7(5) . . . . ? Co1 N5' C15' C16' -178.0(9) . . . . ? C15' C16' C17' C20' 179.6(10) . . . . ? C20' C17' C18' C19' -179.6(9) . . . . ? Co1 N5' C19' C18' 178.0(9) . . . . ? C18' C17' C20' C21' 160.1(9) . . . . ? C16' C17' C20' C21' -19.5(15) . . . . ? C17' C20' C21' C22' -173.8(10) . . . . ? C20' C21' C22' C23' -18.6(16) . . . . ? C20' C21' C22' N6' 157.4(11) . . . . ? N6' C22' C23' C24' 0.0 . . . . ? C21' C22' C23' C24' 175.8(12) . . . . ? C21' C22' N6' C26' -176.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.357 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.059 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 284288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 N6 Ni O2 S2' _chemical_formula_weight 589.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0804(12) _cell_length_b 10.6630(13) _cell_length_c 14.8873(19) _cell_angle_alpha 103.457(2) _cell_angle_beta 96.601(2) _cell_angle_gamma 97.377(2) _cell_volume 1374.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1561 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 21.92 _exptl_crystal_description Block _exptl_crystal_colour Pale-Green _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.777317 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8020 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4805 _reflns_number_gt 3376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.0606P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4805 _refine_ls_number_parameters 423 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ni1 Ni 0.70848(4) 0.79890(4) 0.74143(3) 0.03798(15) Uani 1 1 d . . . S1 S 1.06945(12) 1.17646(10) 0.88706(8) 0.0726(3) Uani 1 1 d . A . S2 S 0.36867(13) 0.40157(11) 0.60092(7) 0.0743(3) Uani 1 1 d . A . O1 O 0.6468(2) 0.7989(2) 0.87301(15) 0.0503(6) Uani 1 1 d . A . H1 H 0.6236 0.7165 0.8836 0.060 Uiso 1 1 calc R . . N1 N 0.8372(3) 0.9789(3) 0.7907(2) 0.0496(7) Uani 1 1 d . A . N2 N 0.5790(3) 0.6208(3) 0.6890(2) 0.0519(7) Uani 1 1 d . A . N3 N 0.5209(3) 0.8855(3) 0.70527(18) 0.0436(6) Uani 1 1 d . A . N4 N -0.0114(3) 1.2485(3) 0.48980(19) 0.0481(7) Uani 1 1 d . . . C1 C 0.9316(4) 1.0614(3) 0.8321(2) 0.0441(8) Uani 1 1 d . . . C2 C 0.4914(4) 0.5294(3) 0.6513(2) 0.0438(8) Uani 1 1 d . . . C3 C 0.5247(4) 0.9689(3) 0.6514(2) 0.0516(9) Uani 1 1 d . . . H3 H 0.6130 0.9882 0.6278 0.062 Uiso 1 1 calc R A . C4 C 0.4046(4) 1.0282(3) 0.6285(3) 0.0559(9) Uani 1 1 d . A . H4 H 0.4129 1.0845 0.5895 0.067 Uiso 1 1 calc R . . C5 C 0.2718(4) 1.0048(3) 0.6633(2) 0.0466(8) Uani 1 1 d . . . C6 C 0.2692(4) 0.9191(4) 0.7201(2) 0.0560(9) Uani 1 1 d . A . H6 H 0.1834 0.9004 0.7462 0.067 Uiso 1 1 calc R . . C7 C 0.3912(4) 0.8619(3) 0.7383(2) 0.0535(9) Uani 1 1 d . . . H7 H 0.3844 0.8033 0.7757 0.064 Uiso 1 1 calc R A . C8 C 0.1392(4) 1.0646(3) 0.6444(2) 0.0538(9) Uani 1 1 d . A . H8 H 0.0645 1.0573 0.6816 0.065 Uiso 1 1 calc R . . C9 C 0.1169(4) 1.1273(3) 0.5798(2) 0.0494(8) Uani 1 1 d . . . H9 H 0.1903 1.1312 0.5414 0.059 Uiso 1 1 calc R A . C10 C -0.0127(4) 1.1926(3) 0.5616(2) 0.0450(8) Uani 1 1 d . A . C11 C -0.1273(4) 1.2005(4) 0.6156(3) 0.0611(10) Uani 1 1 d . . . H11 H -0.1267 1.1620 0.6656 0.073 Uiso 1 1 calc R A . C12 C -0.2426(4) 1.2664(4) 0.5941(3) 0.0669(11) Uani 1 1 d . A . H12 H -0.3215 1.2711 0.6287 0.080 Uiso 1 1 calc R . . C13 C -0.2396(4) 1.3245(4) 0.5219(3) 0.0602(10) Uani 1 1 d . . . H13 H -0.3151 1.3706 0.5068 0.072 Uiso 1 1 calc R A . C14 C -0.1218(4) 1.3130(3) 0.4721(3) 0.0574(9) Uani 1 1 d . A . H14 H -0.1195 1.3529 0.4229 0.069 Uiso 1 1 calc R . . N5 N 0.9010(9) 0.7246(10) 0.7858(7) 0.038(3) Uani 0.508(9) 1 d PG A 1 C15 C 0.9936(11) 0.7907(8) 0.8687(7) 0.058(3) Uani 0.508(9) 1 d PG A 1 H15A H 0.9702 0.8670 0.9048 0.070 Uiso 0.508(9) 1 calc PR A 1 C16 C 1.1213(9) 0.7426(7) 0.8975(5) 0.040(2) Uani 0.508(9) 1 d PG A 1 H16A H 1.1833 0.7868 0.9530 0.048 Uiso 0.508(9) 1 calc PR A 1 C17 C 1.1563(7) 0.6284(7) 0.8435(5) 0.037(2) Uani 0.508(9) 1 d PGD A 1 C18 C 1.0636(8) 0.5623(7) 0.7606(5) 0.047(3) Uani 0.508(9) 1 d PGD A 1 H18A H 1.0871 0.4859 0.7245 0.056 Uiso 0.508(9) 1 calc PR A 1 C19 C 0.9360(8) 0.6104(9) 0.7318(6) 0.036(2) Uani 0.508(9) 1 d PG A 1 H19A H 0.8739 0.5662 0.6763 0.044 Uiso 0.508(9) 1 calc PR A 1 C20 C 1.2961(7) 0.5846(8) 0.8665(5) 0.049(2) Uani 0.508(9) 1 d PD A 1 H20A H 1.3642 0.6467 0.9117 0.059 Uiso 0.508(9) 1 calc PR A 1 C21 C 1.3457(8) 0.4774(8) 0.8374(5) 0.046(2) Uani 0.508(9) 1 d PD A 1 H21A H 1.2765 0.4135 0.7943 0.056 Uiso 0.508(9) 1 calc PR A 1 C22 C 1.4881(7) 0.4371(9) 0.8588(6) 0.041(2) Uani 0.508(9) 1 d PGDU A 1 C23 C 1.5198(8) 0.3104(8) 0.8403(9) 0.067(4) Uani 0.508(9) 1 d PGD A 1 H23A H 1.4437 0.2403 0.8126 0.081 Uiso 0.508(9) 1 calc PR A 1 C24 C 1.6654(10) 0.2883(7) 0.8631(12) 0.075(4) Uani 0.508(9) 1 d PG A 1 H24A H 1.6867 0.2035 0.8507 0.091 Uiso 0.508(9) 1 calc PR A 1 C25 C 1.7792(7) 0.3931(10) 0.9045(11) 0.060(4) Uani 0.508(9) 1 d PG A 1 H25A H 1.8766 0.3783 0.9198 0.072 Uiso 0.508(9) 1 calc PR A 1 C26 C 1.7475(9) 0.5199(8) 0.9231(7) 0.029(2) Uani 0.508(9) 1 d PGU A 1 H26A H 1.8236 0.5900 0.9508 0.035 Uiso 0.508(9) 1 calc PR A 1 N6 N 1.6019(11) 0.5419(6) 0.9002(7) 0.036(2) Uani 0.508(9) 1 d PGU A 1 N5' N 0.8880(10) 0.7022(10) 0.7735(8) 0.044(4) Uani 0.492(9) 1 d PG A 2 C15' C 0.9917(10) 0.7539(8) 0.8542(7) 0.028(2) Uani 0.492(9) 1 d PG A 2 H15B H 0.9802 0.8305 0.8959 0.033 Uiso 0.492(9) 1 calc PR A 2 C16' C 1.1126(8) 0.6912(8) 0.8725(5) 0.036(2) Uani 0.492(9) 1 d PGU A 2 H16B H 1.1820 0.7258 0.9265 0.043 Uiso 0.492(9) 1 calc PR A 2 C17' C 1.1298(6) 0.5766(8) 0.8102(6) 0.040(2) Uani 0.492(9) 1 d PGDU A 2 C18' C 1.0261(9) 0.5249(9) 0.7295(6) 0.061(3) Uani 0.492(9) 1 d PGD A 2 H18B H 1.0376 0.4482 0.6878 0.073 Uiso 0.492(9) 1 calc PR A 2 C19' C 0.9052(10) 0.5876(11) 0.7112(6) 0.072(4) Uani 0.492(9) 1 d PGU A 2 H19B H 0.8358 0.5530 0.6572 0.087 Uiso 0.492(9) 1 calc PR A 2 C20' C 1.2512(7) 0.5008(8) 0.8243(6) 0.055(2) Uani 0.492(9) 1 d PDU A 2 H20B H 1.2374 0.4125 0.7939 0.065 Uiso 0.492(9) 1 calc PR A 2 C21' C 1.3803(7) 0.5556(8) 0.8794(6) 0.052(3) Uani 0.492(9) 1 d PD A 2 H21B H 1.3887 0.6402 0.9164 0.062 Uiso 0.492(9) 1 calc PR A 2 C22' C 1.5113(7) 0.4860(9) 0.8838(6) 0.035(2) Uani 0.492(9) 1 d PGDU A 2 C23' C 1.4993(9) 0.3508(9) 0.8563(8) 0.052(3) Uani 0.492(9) 1 d PGD A 2 H23B H 1.4053 0.2992 0.8368 0.062 Uiso 0.492(9) 1 calc PR A 2 C24' C 1.6279(14) 0.2929(7) 0.8580(11) 0.068(4) Uani 0.492(9) 1 d PG A 2 H24B H 1.6199 0.2024 0.8396 0.082 Uiso 0.492(9) 1 calc PR A 2 C25' C 1.7685(10) 0.3701(12) 0.8872(12) 0.072(5) Uani 0.492(9) 1 d PG A 2 H25B H 1.8545 0.3313 0.8883 0.087 Uiso 0.492(9) 1 calc PR A 2 C26' C 1.7805(6) 0.5052(11) 0.9147(10) 0.085(5) Uani 0.492(9) 1 d PG A 2 H26B H 1.8745 0.5569 0.9342 0.102 Uiso 0.492(9) 1 calc PR A 2 N6' N 1.6519(10) 0.5632(7) 0.9130(7) 0.043(3) Uani 0.492(9) 1 d PGU A 2 O2 O 0.7606(2) 0.7833(2) 0.60551(14) 0.0532(6) Uani 1 1 d . A . H2A H 0.7006 0.7203 0.5688 0.064 Uiso 1 1 d R . . H2B H 0.8516 0.7899 0.5971 0.064 Uiso 1 1 d R . . C27 C 0.6351(5) 0.9034(4) 0.9477(3) 0.0777(13) Uani 1 1 d . . . H27A H 0.7337 0.9465 0.9778 0.116 Uiso 1 1 calc R A . H27B H 0.5816 0.8709 0.9917 0.116 Uiso 1 1 calc R . . H27C H 0.5817 0.9643 0.9245 0.116 Uiso 1 1 calc R . . 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 Ni1 0.0347(2) 0.0423(3) 0.0394(2) 0.01295(17) 0.00592(17) 0.00975(18) S1 0.0576(7) 0.0681(7) 0.0744(7) -0.0069(5) -0.0043(5) 0.0042(5) S2 0.0782(8) 0.0702(7) 0.0577(6) -0.0003(5) 0.0123(5) -0.0218(6) O1 0.0624(16) 0.0506(14) 0.0477(13) 0.0196(11) 0.0178(11) 0.0230(12) N1 0.0419(17) 0.0495(18) 0.0557(18) 0.0126(14) 0.0027(14) 0.0067(14) N2 0.0498(19) 0.0496(18) 0.0555(18) 0.0138(15) 0.0097(15) 0.0025(15) N3 0.0373(16) 0.0527(17) 0.0453(15) 0.0210(13) 0.0045(12) 0.0096(13) N4 0.0438(17) 0.0514(17) 0.0524(17) 0.0171(14) 0.0080(13) 0.0112(14) C1 0.044(2) 0.051(2) 0.0426(19) 0.0141(16) 0.0087(16) 0.0206(17) C2 0.049(2) 0.048(2) 0.0413(19) 0.0179(16) 0.0144(16) 0.0126(18) C3 0.042(2) 0.062(2) 0.061(2) 0.0318(19) 0.0146(17) 0.0110(17) C4 0.058(2) 0.055(2) 0.065(2) 0.0354(19) 0.0051(19) 0.0143(18) C5 0.039(2) 0.056(2) 0.0474(19) 0.0137(17) 0.0060(15) 0.0144(16) C6 0.042(2) 0.077(3) 0.060(2) 0.032(2) 0.0121(17) 0.0202(19) C7 0.040(2) 0.075(3) 0.059(2) 0.0369(19) 0.0121(17) 0.0175(18) C8 0.047(2) 0.067(2) 0.055(2) 0.0242(19) 0.0139(17) 0.0168(18) C9 0.043(2) 0.050(2) 0.055(2) 0.0139(17) 0.0066(16) 0.0067(17) C10 0.0409(19) 0.0390(18) 0.054(2) 0.0094(16) 0.0022(16) 0.0101(15) C11 0.061(3) 0.072(3) 0.066(2) 0.035(2) 0.020(2) 0.023(2) C12 0.054(3) 0.084(3) 0.077(3) 0.030(2) 0.027(2) 0.032(2) C13 0.055(2) 0.064(2) 0.070(3) 0.023(2) 0.009(2) 0.031(2) C14 0.059(2) 0.062(2) 0.056(2) 0.0231(18) 0.0053(19) 0.018(2) N5 0.021(5) 0.033(4) 0.060(7) 0.006(4) 0.017(5) 0.009(4) C15 0.072(8) 0.048(6) 0.062(7) 0.021(5) 0.007(5) 0.025(5) C16 0.048(5) 0.034(6) 0.037(5) 0.001(4) 0.008(4) 0.019(4) C17 0.059(5) 0.030(5) 0.022(5) -0.003(4) 0.014(3) 0.019(4) C18 0.084(7) 0.033(5) 0.021(6) -0.008(4) 0.011(5) 0.023(5) C19 0.040(5) 0.030(4) 0.033(4) -0.006(3) 0.005(3) 0.006(4) C20 0.044(6) 0.063(6) 0.050(5) 0.027(4) 0.008(4) 0.019(5) C21 0.039(5) 0.063(6) 0.046(5) 0.023(4) 0.003(4) 0.023(4) C22 0.057(5) 0.035(6) 0.031(4) 0.005(4) 0.013(3) 0.010(4) C23 0.102(9) 0.042(6) 0.069(7) 0.010(5) 0.026(6) 0.047(6) C24 0.049(7) 0.106(12) 0.084(9) 0.032(8) 0.005(6) 0.050(7) C25 0.076(10) 0.055(7) 0.058(7) 0.018(5) 0.025(6) 0.027(6) C26 0.010(3) 0.045(4) 0.040(3) 0.018(3) 0.006(3) 0.014(3) N6 0.021(5) 0.046(4) 0.051(4) 0.025(3) 0.009(4) 0.014(3) N5' 0.055(7) 0.045(6) 0.030(4) 0.014(4) -0.002(4) 0.003(5) C15' 0.023(5) 0.025(4) 0.032(4) 0.000(3) 0.004(4) 0.004(3) C16' 0.046(4) 0.029(6) 0.026(4) -0.006(4) -0.001(3) 0.010(4) C17' 0.059(6) 0.036(5) 0.028(6) -0.001(5) 0.025(4) 0.019(4) C18' 0.068(6) 0.068(7) 0.039(6) -0.011(5) 0.005(4) 0.032(6) C19' 0.061(6) 0.067(7) 0.085(7) 0.007(5) 0.006(5) 0.024(5) C20' 0.058(5) 0.045(5) 0.063(5) 0.011(4) 0.018(4) 0.016(4) C21' 0.056(6) 0.056(7) 0.038(5) 0.010(4) 0.003(4) -0.005(5) C22' 0.035(5) 0.031(5) 0.039(5) 0.012(4) -0.001(4) 0.005(4) C23' 0.057(6) 0.038(7) 0.059(7) 0.011(6) -0.006(5) 0.016(5) C24' 0.093(9) 0.053(7) 0.072(8) 0.019(6) 0.010(8) 0.056(7) C25' 0.049(10) 0.131(14) 0.060(8) 0.042(9) 0.010(6) 0.064(9) C26' 0.072(8) 0.112(11) 0.100(9) 0.043(7) 0.041(7) 0.068(7) N6' 0.017(5) 0.062(5) 0.053(4) 0.023(3) 0.004(4) 0.005(3) O2 0.0446(14) 0.0731(16) 0.0407(13) 0.0134(11) 0.0078(10) 0.0056(12) C27 0.099(3) 0.088(3) 0.052(2) 0.011(2) 0.021(2) 0.039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.031(3) . ? Ni1 N1 2.040(3) . ? Ni1 O1 2.098(2) . ? Ni1 N5' 2.105(4) . ? Ni1 O2 2.105(2) . ? Ni1 N3 2.114(2) . ? Ni1 N5 2.110(4) . ? S1 C1 1.627(4) . ? S2 C2 1.614(4) . ? O1 C27 1.404(4) . ? O1 H1 0.9300 . ? N1 C1 1.149(4) . ? N2 C2 1.158(4) . ? N3 C3 1.329(4) . ? N3 C7 1.344(4) . ? N4 C14 1.323(4) . ? N4 C10 1.339(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.383(5) . ? C4 H4 0.9300 . ? C5 C6 1.382(4) . ? C5 C8 1.462(4) . ? C6 C7 1.361(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.305(4) . ? C8 H8 0.9300 . ? C9 C10 1.472(4) . ? C9 H9 0.9300 . ? C10 C11 1.386(5) . ? C11 C12 1.381(4) . ? C11 H11 0.9300 . ? C12 C13 1.361(5) . ? C12 H12 0.9300 . ? C13 C14 1.372(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? N5 C15 1.3900 . ? N5 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C17 C18 1.3900 . ? C17 C20 1.440(5) . ? C18 C19 1.3900 . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.283(8) . ? C20 H20A 0.9300 . ? C21 C22 1.438(6) . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 N6 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 H25A 0.9300 . ? C26 N6 1.3900 . ? C26 H26A 0.9300 . ? N5' C15' 1.3900 . ? N5' C19' 1.3900 . ? C15' C16' 1.3900 . ? C15' H15B 0.9300 . ? C16' C17' 1.3900 . ? C16' H16B 0.9300 . ? C17' C18' 1.3900 . ? C17' C20' 1.473(7) . ? C18' C19' 1.3900 . ? C18' H18B 0.9300 . ? C19' H19B 0.9300 . ? C20' C21' 1.329(8) . ? C20' H20B 0.9300 . ? C21' C22' 1.484(6) . ? C21' H21B 0.9300 . ? C22' C23' 1.3900 . ? C22' N6' 1.3900 . ? C23' C24' 1.3900 . ? C23' H23B 0.9300 . ? C24' C25' 1.3900 . ? C24' H24B 0.9300 . ? C25' C26' 1.3900 . ? C25' H25B 0.9300 . ? C26' N6' 1.3900 . ? C26' H26B 0.9300 . ? O2 H2A 0.8452 . ? O2 H2B 0.8461 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 178.46(11) . . ? N2 Ni1 O1 89.01(10) . . ? N1 Ni1 O1 92.29(10) . . ? N2 Ni1 N5' 88.0(3) . . ? N1 Ni1 N5' 92.8(3) . . ? O1 Ni1 N5' 88.9(3) . . ? N2 Ni1 O2 86.35(10) . . ? N1 Ni1 O2 92.35(10) . . ? O1 Ni1 O2 175.35(9) . . ? N5' Ni1 O2 90.5(3) . . ? N2 Ni1 N3 88.70(11) . . ? N1 Ni1 N3 90.45(11) . . ? O1 Ni1 N3 91.38(9) . . ? N5' Ni1 N3 176.7(3) . . ? O2 Ni1 N3 88.92(9) . . ? N2 Ni1 N5 94.9(3) . . ? N1 Ni1 N5 86.0(3) . . ? O1 Ni1 N5 86.5(3) . . ? N5' Ni1 N5 7.3(5) . . ? O2 Ni1 N5 93.5(3) . . ? N3 Ni1 N5 175.8(3) . . ? C27 O1 Ni1 130.3(2) . . ? C27 O1 H1 114.9 . . ? Ni1 O1 H1 114.9 . . ? C1 N1 Ni1 161.2(3) . . ? C2 N2 Ni1 169.3(3) . . ? C3 N3 C7 116.0(3) . . ? C3 N3 Ni1 122.6(2) . . ? C7 N3 Ni1 121.4(2) . . ? C14 N4 C10 118.3(3) . . ? N1 C1 S1 177.5(3) . . ? N2 C2 S2 178.7(3) . . ? N3 C3 C4 123.4(3) . . ? N3 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 115.8(3) . . ? C6 C5 C8 119.7(3) . . ? C4 C5 C8 124.5(3) . . ? C7 C6 C5 120.7(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? N3 C7 C6 123.7(3) . . ? N3 C7 H7 118.2 . . ? C6 C7 H7 118.2 . . ? C9 C8 C5 125.5(3) . . ? C9 C8 H8 117.2 . . ? C5 C8 H8 117.2 . . ? C8 C9 C10 126.7(3) . . ? C8 C9 H9 116.7 . . ? C10 C9 H9 116.7 . . ? N4 C10 C11 121.2(3) . . ? N4 C10 C9 115.4(3) . . ? C11 C10 C9 123.3(3) . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 118.0(3) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? N4 C14 C13 124.0(3) . . ? N4 C14 H14 118.0 . . ? C13 C14 H14 118.0 . . ? C15 N5 C19 120.0 . . ? C15 N5 Ni1 119.9(5) . . ? C19 N5 Ni1 120.1(5) . . ? C16 C15 N5 120.0 . . ? C16 C15 H15A 120.0 . . ? N5 C15 H15A 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 C20 118.7(5) . . ? C16 C17 C20 120.9(5) . . ? C19 C18 C17 120.0 . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 N5 120.0 . . ? C18 C19 H19A 120.0 . . ? N5 C19 H19A 120.0 . . ? C21 C20 C17 133.1(7) . . ? C21 C20 H20A 113.5 . . ? C17 C20 H20A 113.5 . . ? C20 C21 C22 132.2(8) . . ? C20 C21 H21A 113.9 . . ? C22 C21 H21A 113.9 . . ? C23 C22 N6 120.0 . . ? C23 C22 C21 127.2(7) . . ? N6 C22 C21 112.8(7) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 N6 120.0 . . ? C25 C26 H26A 120.0 . . ? N6 C26 H26A 120.0 . . ? C26 N6 C22 120.0 . . ? C15' N5' C19' 120.0 . . ? C15' N5' Ni1 120.8(5) . . ? C19' N5' Ni1 119.2(5) . . ? C16' C15' N5' 120.0 . . ? C16' C15' H15B 120.0 . . ? N5' C15' H15B 120.0 . . ? C15' C16' C17' 120.0 . . ? C15' C16' H16B 120.0 . . ? C17' C16' H16B 120.0 . . ? C18' C17' C16' 120.0 . . ? C18' C17' C20' 115.7(5) . . ? C16' C17' C20' 124.3(5) . . ? C17' C18' C19' 120.0 . . ? C17' C18' H18B 120.0 . . ? C19' C18' H18B 120.0 . . ? C18' C19' N5' 120.0 . . ? C18' C19' H19B 120.0 . . ? N5' C19' H19B 120.0 . . ? C21' C20' C17' 121.6(8) . . ? C21' C20' H20B 119.2 . . ? C17' C20' H20B 119.2 . . ? C20' C21' C22' 122.1(7) . . ? C20' C21' H21B 118.9 . . ? C22' C21' H21B 118.9 . . ? C23' C22' N6' 120.0 . . ? C23' C22' C21' 123.3(7) . . ? N6' C22' C21' 116.7(7) . . ? C22' C23' C24' 120.0 . . ? C22' C23' H23B 120.0 . . ? C24' C23' H23B 120.0 . . ? C25' C24' C23' 120.0 . . ? C25' C24' H24B 120.0 . . ? C23' C24' H24B 120.0 . . ? C24' C25' C26' 120.0 . . ? C24' C25' H25B 120.0 . . ? C26' C25' H25B 120.0 . . ? N6' C26' C25' 120.0 . . ? N6' C26' H26B 120.0 . . ? C25' C26' H26B 120.0 . . ? C26' N6' C22' 120.0 . . ? Ni1 O2 H2A 108.2 . . ? Ni1 O2 H2B 119.3 . . ? H2A O2 H2B 116.5 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 N2 Ni1 O1 C27 -151.7(3) . . . . ? N1 Ni1 O1 C27 27.5(3) . . . . ? N5' Ni1 O1 C27 120.3(4) . . . . ? N3 Ni1 O1 C27 -63.0(3) . . . . ? N5 Ni1 O1 C27 113.4(4) . . . . ? O1 Ni1 N1 C1 65.1(9) . . . . ? N5' Ni1 N1 C1 -24.0(9) . . . . ? O2 Ni1 N1 C1 -114.6(9) . . . . ? N3 Ni1 N1 C1 156.5(9) . . . . ? N5 Ni1 N1 C1 -21.3(9) . . . . ? O1 Ni1 N2 C2 113.4(15) . . . . ? N5' Ni1 N2 C2 -157.7(15) . . . . ? O2 Ni1 N2 C2 -67.0(15) . . . . ? N3 Ni1 N2 C2 22.0(15) . . . . ? N5 Ni1 N2 C2 -160.2(15) . . . . ? N2 Ni1 N3 C3 -124.6(3) . . . . ? N1 Ni1 N3 C3 54.1(3) . . . . ? O1 Ni1 N3 C3 146.4(3) . . . . ? O2 Ni1 N3 C3 -38.3(3) . . . . ? N2 Ni1 N3 C7 57.5(3) . . . . ? N1 Ni1 N3 C7 -123.8(3) . . . . ? O1 Ni1 N3 C7 -31.5(3) . . . . ? O2 Ni1 N3 C7 143.8(3) . . . . ? C7 N3 C3 C4 -0.7(5) . . . . ? Ni1 N3 C3 C4 -178.7(3) . . . . ? N3 C3 C4 C5 1.3(6) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C3 C4 C5 C8 179.0(3) . . . . ? C4 C5 C6 C7 -0.8(5) . . . . ? C8 C5 C6 C7 179.7(3) . . . . ? C3 N3 C7 C6 -0.7(5) . . . . ? Ni1 N3 C7 C6 177.3(3) . . . . ? C5 C6 C7 N3 1.5(6) . . . . ? C6 C5 C8 C9 -166.9(4) . . . . ? C4 C5 C8 C9 13.7(6) . . . . ? C5 C8 C9 C10 -177.6(3) . . . . ? C14 N4 C10 C11 0.7(5) . . . . ? C14 N4 C10 C9 -177.4(3) . . . . ? C8 C9 C10 N4 -178.8(3) . . . . ? C8 C9 C10 C11 3.2(6) . . . . ? N4 C10 C11 C12 0.6(6) . . . . ? C9 C10 C11 C12 178.5(3) . . . . ? C10 C11 C12 C13 -1.4(6) . . . . ? C11 C12 C13 C14 1.0(6) . . . . ? C10 N4 C14 C13 -1.1(5) . . . . ? C12 C13 C14 N4 0.3(6) . . . . ? N2 Ni1 N5 C15 -142.9(5) . . . . ? N1 Ni1 N5 C15 38.4(5) . . . . ? O1 Ni1 N5 C15 -54.2(5) . . . . ? N5' Ni1 N5 C15 -163(6) . . . . ? O2 Ni1 N5 C15 130.5(5) . . . . ? N2 Ni1 N5 C19 37.8(6) . . . . ? N1 Ni1 N5 C19 -141.0(6) . . . . ? O1 Ni1 N5 C19 126.5(6) . . . . ? N5' Ni1 N5 C19 17(5) . . . . ? O2 Ni1 N5 C19 -48.8(6) . . . . ? Ni1 N5 C15 C16 -179.3(8) . . . . ? N5 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C15 C16 C17 C20 173.1(7) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C20 C17 C18 C19 -173.3(7) . . . . ? C17 C18 C19 N5 0.0 . . . . ? C15 N5 C19 C18 0.0 . . . . ? Ni1 N5 C19 C18 179.3(8) . . . . ? C18 C17 C20 C21 -18.1(12) . . . . ? C16 C17 C20 C21 168.7(8) . . . . ? C17 C20 C21 C22 177.3(9) . . . . ? C20 C21 C22 C23 164.0(9) . . . . ? C20 C21 C22 N6 -17.8(12) . . . . ? C21 C22 C23 C24 178.0(10) . . . . ? C21 C22 N6 C26 -178.3(8) . . . . ? N2 Ni1 N5' C15' -143.6(6) . . . . ? N1 Ni1 N5' C15' 37.7(6) . . . . ? O1 Ni1 N5' C15' -54.6(6) . . . . ? O2 Ni1 N5' C15' 130.0(6) . . . . ? N2 Ni1 N5' C19' 38.7(5) . . . . ? N1 Ni1 N5' C19' -140.0(5) . . . . ? O1 Ni1 N5' C19' 127.7(5) . . . . ? O2 Ni1 N5' C19' -47.6(5) . . . . ? Ni1 N5' C15' C16' -177.7(8) . . . . ? C15' C16' C17' C20' -178.3(8) . . . . ? C16' C17' C18' C19' 0.0 . . . . ? C20' C17' C18' C19' 178.4(7) . . . . ? Ni1 N5' C19' C18' 177.7(8) . . . . ? C18' C17' C20' C21' 158.4(8) . . . . ? C16' C17' C20' C21' -23.3(11) . . . . ? C17' C20' C21' C22' -171.1(8) . . . . ? C20' C21' C22' C23' -20.9(12) . . . . ? C20' C21' C22' N6' 155.9(8) . . . . ? N6' C22' C23' C24' 0.0 . . . . ? C21' C22' C23' C24' 176.7(10) . . . . ? C21' C22' N6' C26' -176.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.336 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.055 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 284289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H68 Cu3 N18 O2 S6' _chemical_formula_weight 1696.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4775(18) _cell_length_b 13.038(3) _cell_length_c 17.523(3) _cell_angle_alpha 75.595(2) _cell_angle_beta 75.360(2) _cell_angle_gamma 71.835(2) _cell_volume 1956.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1876 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.87 _exptl_crystal_description Lamellar _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 873 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.925796 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11269 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6812 _reflns_number_gt 4424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.0413P)^2^+1.6354P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6812 _refine_ls_number_parameters 572 _refine_ls_number_restraints 209 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.5000 1.0000 1.0000 0.0466(2) Uani 1 2 d S . . Cu2 Cu 0.12363(6) 0.78403(4) 0.28169(3) 0.04377(17) Uani 1 1 d . . . S1 S 0.2789(2) 0.42341(12) 0.41413(11) 0.1035(6) Uani 1 1 d . A . S2 S 0.18744(13) 1.09793(9) 0.09156(7) 0.0532(3) Uani 1 1 d . A . S3 S 0.46583(15) 0.69641(10) 1.20509(8) 0.0651(4) Uani 1 1 d . . . O1 O -0.1267(3) 0.8383(2) 0.35983(17) 0.0576(8) Uani 1 1 d D A . H1A H -0.2044 0.8889 0.3490 0.086 Uiso 1 1 d RD . . N3 N 0.1969(4) 0.8232(3) 0.36722(19) 0.0452(8) Uani 1 1 d . A . N4 N 0.4061(4) 1.0133(3) 0.6596(2) 0.0525(9) Uani 1 1 d . . . N5 N 0.0970(6) 0.7416(4) 0.6872(3) 0.0851(14) Uani 1 1 d . . . N6 N 0.4022(4) 0.9292(3) 0.94383(19) 0.0455(8) Uani 1 1 d . . . N7 N 0.5226(4) 0.8694(3) 1.0834(2) 0.0520(9) Uani 1 1 d . . . N8 N 0.1537(4) 0.6330(3) 0.3384(2) 0.0511(9) Uani 1 1 d . A . N9 N 0.1253(4) 0.9280(3) 0.2147(2) 0.0478(9) Uani 1 1 d . A . C1 C -0.1583(10) 0.6094(7) -0.1267(5) 0.051(3) Uani 0.586(9) 1 d PGDU A 1 H1B H -0.0915 0.6532 -0.1396 0.062 Uiso 0.586(9) 1 calc PR A 1 C2 C -0.1970(15) 0.5781(11) -0.1873(4) 0.059(4) Uani 0.586(9) 1 d PGU A 1 H2A H -0.1561 0.6010 -0.2407 0.071 Uiso 0.586(9) 1 calc PR A 1 C3 C -0.2967(17) 0.5127(12) -0.1680(5) 0.073(8) Uani 0.586(9) 1 d PGU A 1 H3A H -0.3226 0.4918 -0.2085 0.087 Uiso 0.586(9) 1 calc PR A 1 C4 C -0.3577(13) 0.4786(10) -0.0881(6) 0.092(5) Uani 0.586(9) 1 d PGU A 1 H4A H -0.4244 0.4348 -0.0752 0.110 Uiso 0.586(9) 1 calc PR A 1 N1 N -0.3190(9) 0.5099(7) -0.0276(4) 0.064(3) Uani 0.586(9) 1 d PGDU A 1 C5 C -0.2193(9) 0.5753(6) -0.0469(4) 0.044(3) Uani 0.586(9) 1 d PGDU A 1 C6 C -0.1851(8) 0.6065(6) 0.0190(5) 0.045(2) Uani 0.586(9) 1 d PDU A 1 H6A H -0.2443 0.5923 0.0695 0.054 Uiso 0.586(9) 1 calc PR A 1 C7 C -0.0768(9) 0.6534(6) 0.0131(5) 0.047(2) Uani 0.586(9) 1 d PDU A 1 H7A H -0.0164 0.6647 -0.0375 0.056 Uiso 0.586(9) 1 calc PR A 1 C8 C -0.0406(8) 0.6899(6) 0.0772(4) 0.035(2) Uani 0.586(9) 1 d PGDU A 1 C9 C -0.1073(8) 0.6649(7) 0.1574(4) 0.044(2) Uani 0.586(9) 1 d PGDU A 1 H9A H -0.1833 0.6288 0.1717 0.053 Uiso 0.586(9) 1 calc PR A 1 C10 C -0.0606(11) 0.6940(9) 0.2162(3) 0.038(2) Uani 0.586(9) 1 d PGU A 1 H10A H -0.1052 0.6773 0.2698 0.046 Uiso 0.586(9) 1 calc PR A 1 N2 N 0.0530(12) 0.7480(10) 0.1948(5) 0.039(3) Uani 0.586(9) 1 d PGU A 1 C11 C 0.1197(11) 0.7730(9) 0.1146(6) 0.057(3) Uani 0.586(9) 1 d PGU A 1 H11A H 0.1957 0.8092 0.1003 0.069 Uiso 0.586(9) 1 calc PR A 1 C12 C 0.0730(9) 0.7439(7) 0.0558(4) 0.046(3) Uani 0.586(9) 1 d PGDU A 1 H12A H 0.1176 0.7607 0.0022 0.055 Uiso 0.586(9) 1 calc PR A 1 C6' C -0.1038(12) 0.6351(9) -0.0254(5) 0.051(3) Uani 0.414(9) 1 d PDU A 2 H6'A H -0.0235 0.6657 -0.0506 0.062 Uiso 0.414(9) 1 calc PR A 2 C1' C -0.1269(14) 0.6096(11) -0.1571(5) 0.056(4) Uani 0.414(9) 1 d PGDU A 2 H1'A H -0.0551 0.6481 -0.1830 0.068 Uiso 0.414(9) 1 calc PR A 2 C2' C -0.190(2) 0.5666(15) -0.2014(4) 0.061(6) Uani 0.414(9) 1 d PGU A 2 H2'A H -0.1600 0.5763 -0.2570 0.073 Uiso 0.414(9) 1 calc PR A 2 C3' C -0.2971(19) 0.5090(15) -0.1628(7) 0.043(8) Uani 0.414(9) 1 d PGU A 2 H3'A H -0.3392 0.4802 -0.1924 0.051 Uiso 0.414(9) 1 calc PR A 2 C4' C -0.3416(13) 0.4944(10) -0.0798(7) 0.033(3) Uani 0.414(9) 1 d PGU A 2 H4'A H -0.4134 0.4559 -0.0539 0.040 Uiso 0.414(9) 1 calc PR A 2 N1' N -0.2787(11) 0.5375(8) -0.0354(4) 0.038(3) Uani 0.414(9) 1 d PGDU A 2 C5' C -0.1714(11) 0.5950(8) -0.0741(5) 0.040(3) Uani 0.414(9) 1 d PGDU A 2 C7' C -0.1507(12) 0.6301(9) 0.0527(5) 0.044(3) Uani 0.414(9) 1 d PDU A 2 H7'A H -0.2303 0.5986 0.0776 0.053 Uiso 0.414(9) 1 calc PR A 2 C8' C -0.0851(11) 0.6713(8) 0.1033(5) 0.035(3) Uani 0.414(9) 1 d PGDU A 2 C9' C -0.1349(13) 0.6496(11) 0.1859(5) 0.051(4) Uani 0.414(9) 1 d PGDU A 2 H9'A H -0.2070 0.6101 0.2075 0.061 Uiso 0.414(9) 1 calc PR A 2 C10' C -0.0771(19) 0.6867(15) 0.2361(5) 0.075(6) Uani 0.414(9) 1 d PGU A 2 H10B H -0.1105 0.6721 0.2914 0.090 Uiso 0.414(9) 1 calc PR A 2 N2' N 0.0306(19) 0.7456(15) 0.2038(7) 0.042(5) Uani 0.414(9) 1 d PGU A 2 C11' C 0.0804(14) 0.7673(11) 0.1212(7) 0.030(3) Uani 0.414(9) 1 d PGU A 2 H11B H 0.1525 0.8067 0.0996 0.036 Uiso 0.414(9) 1 calc PR A 2 C12' C 0.0226(12) 0.7302(9) 0.0709(5) 0.035(3) Uani 0.414(9) 1 d PGDU A 2 H12B H 0.0560 0.7447 0.0157 0.042 Uiso 0.414(9) 1 calc PR A 2 C13 C 0.3545(5) 0.7834(4) 0.4634(3) 0.0557(12) Uani 1 1 d . A . H13 H 0.4310 0.7338 0.4885 0.067 Uiso 1 1 calc R . . C14 C 0.3058(5) 0.7543(4) 0.4058(2) 0.0521(11) Uani 1 1 d . . . H14 H 0.3500 0.6845 0.3934 0.063 Uiso 1 1 calc R A . C15 C 0.1356(5) 0.9221(4) 0.3873(3) 0.0518(11) Uani 1 1 d . . . H15 H 0.0595 0.9709 0.3615 0.062 Uiso 1 1 calc R A . C16 C 0.1785(5) 0.9555(4) 0.4439(3) 0.0553(12) Uani 1 1 d . A . H16 H 0.1319 1.0256 0.4555 0.066 Uiso 1 1 calc R . . C17 C 0.2896(5) 0.8866(4) 0.4838(2) 0.0513(11) Uani 1 1 d . . . C18 C 0.3364(5) 0.9246(4) 0.5430(3) 0.0575(12) Uani 1 1 d . A . H18 H 0.2894 0.9969 0.5493 0.069 Uiso 1 1 calc R . . C19 C 0.4343(5) 0.8702(4) 0.5873(3) 0.0582(12) Uani 1 1 d . . . H19 H 0.4798 0.7970 0.5828 0.070 Uiso 1 1 calc R A . C20 C 0.4814(5) 0.9123(4) 0.6442(2) 0.0498(11) Uani 1 1 d . A . C21 C 0.4551(5) 1.0519(4) 0.7087(3) 0.0546(11) Uani 1 1 d . . . H21 H 0.4040 1.1220 0.7190 0.066 Uiso 1 1 calc R . . C22 C 0.5765(5) 0.9945(4) 0.7449(3) 0.0543(12) Uani 1 1 d . . . H22 H 0.6071 1.0248 0.7787 0.065 Uiso 1 1 calc R . . C23 C 0.6508(5) 0.8913(4) 0.7299(3) 0.0606(13) Uani 1 1 d . A . H23 H 0.7328 0.8496 0.7539 0.073 Uiso 1 1 calc R . . C24 C 0.6035(5) 0.8499(4) 0.6791(3) 0.0587(12) Uani 1 1 d . . . H24 H 0.6536 0.7799 0.6682 0.070 Uiso 1 1 calc R A . C25 C 0.2978(8) 0.5808(6) 0.6878(4) 0.099(2) Uani 1 1 d . . . H25 H 0.3845 0.5376 0.7072 0.118 Uiso 1 1 calc R . . C26 C 0.2492(8) 0.5479(6) 0.6337(4) 0.104(2) Uani 1 1 d . . . H26 H 0.3028 0.4826 0.6157 0.124 Uiso 1 1 calc R . . C27 C 0.1234(8) 0.6101(6) 0.6062(3) 0.0858(18) Uani 1 1 d . . . H27 H 0.0869 0.5881 0.5701 0.103 Uiso 1 1 calc R . . C28 C 0.0502(7) 0.7073(6) 0.6329(4) 0.0901(18) Uani 1 1 d . . . H28 H -0.0354 0.7517 0.6130 0.108 Uiso 1 1 calc R . . C29 C 0.2205(7) 0.6764(5) 0.7140(3) 0.0711(15) Uani 1 1 d . . . C30 C 0.2791(7) 0.7110(5) 0.7735(4) 0.0845(17) Uani 1 1 d . . . H30 H 0.3632 0.6631 0.7932 0.101 Uiso 1 1 calc R . . C31 C 0.2208(6) 0.8007(5) 0.7980(3) 0.0755(15) Uani 1 1 d . . . H31 H 0.1329 0.8459 0.7808 0.091 Uiso 1 1 calc R . . C32 C 0.2822(5) 0.8399(4) 0.8525(3) 0.0585(12) Uani 1 1 d . . . C33 C 0.2229(5) 0.9455(4) 0.8643(3) 0.0594(12) Uani 1 1 d . . . H33 H 0.1405 0.9899 0.8415 0.071 Uiso 1 1 calc R . . C34 C 0.2829(5) 0.9872(4) 0.9091(3) 0.0520(11) Uani 1 1 d . . . H34 H 0.2388 1.0596 0.9160 0.062 Uiso 1 1 calc R . . C35 C 0.4589(5) 0.8247(4) 0.9343(3) 0.0546(11) Uani 1 1 d . . . H35 H 0.5398 0.7814 0.9588 0.065 Uiso 1 1 calc R . . C36 C 0.4033(6) 0.7783(4) 0.8902(3) 0.0637(13) Uani 1 1 d . . . H36 H 0.4467 0.7051 0.8854 0.076 Uiso 1 1 calc R . . C37 C 0.4994(4) 0.7975(4) 1.1342(3) 0.0425(10) Uani 1 1 d . . . C38 C 0.2055(5) 0.5455(4) 0.3693(3) 0.0477(10) Uani 1 1 d . . . C39 C 0.1530(4) 0.9972(3) 0.1628(3) 0.0403(9) Uani 1 1 d . . . C40 C -0.1700(7) 0.7693(5) 0.4321(3) 0.0850(17) Uani 1 1 d . . . H40A H -0.2132 0.7182 0.4213 0.127 Uiso 1 1 d R A . H40B H -0.2433 0.8128 0.4685 0.127 Uiso 1 1 d R . . H40C H -0.0828 0.7298 0.4558 0.127 Uiso 1 1 d R . . 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 Cu1 0.0546(5) 0.0453(4) 0.0431(4) -0.0046(3) -0.0195(4) -0.0124(4) Cu2 0.0574(3) 0.0406(3) 0.0425(3) -0.0051(2) -0.0236(2) -0.0165(2) S1 0.1304(15) 0.0530(9) 0.1151(14) 0.0116(9) -0.0520(12) -0.0063(9) S2 0.0526(7) 0.0487(7) 0.0505(7) 0.0008(5) -0.0112(5) -0.0093(5) S3 0.0636(8) 0.0522(7) 0.0673(8) 0.0031(6) -0.0059(7) -0.0145(6) O1 0.0493(18) 0.065(2) 0.0527(19) -0.0073(16) -0.0072(15) -0.0126(16) N3 0.049(2) 0.046(2) 0.046(2) -0.0099(16) -0.0162(17) -0.0134(17) N4 0.048(2) 0.071(3) 0.048(2) -0.0125(19) -0.0191(17) -0.019(2) N5 0.083(3) 0.098(4) 0.090(3) -0.039(3) -0.004(3) -0.037(3) N6 0.043(2) 0.051(2) 0.043(2) -0.0111(17) -0.0119(16) -0.0073(17) N7 0.055(2) 0.052(2) 0.049(2) -0.0060(19) -0.0178(19) -0.0119(19) N8 0.065(2) 0.045(2) 0.050(2) -0.0072(18) -0.0228(19) -0.0154(19) N9 0.053(2) 0.045(2) 0.051(2) -0.0028(18) -0.0223(18) -0.0165(18) C1 0.059(5) 0.056(5) 0.047(6) -0.019(5) -0.016(5) -0.015(4) C2 0.072(7) 0.052(6) 0.048(5) -0.015(5) -0.009(5) -0.007(5) C3 0.073(11) 0.075(11) 0.070(10) -0.025(7) -0.019(7) -0.007(7) C4 0.099(8) 0.103(8) 0.103(8) -0.062(6) -0.031(6) -0.024(6) N1 0.063(5) 0.073(6) 0.079(5) -0.030(4) -0.018(4) -0.037(4) C5 0.039(5) 0.043(5) 0.058(5) -0.014(4) -0.016(5) -0.014(4) C6 0.051(5) 0.039(4) 0.048(5) -0.014(3) -0.023(4) 0.000(3) C7 0.053(5) 0.051(5) 0.042(5) -0.015(4) -0.017(4) -0.009(4) C8 0.039(5) 0.035(4) 0.029(4) 0.001(4) -0.006(4) -0.015(4) C9 0.039(4) 0.054(5) 0.039(6) -0.002(4) -0.001(4) -0.023(4) C10 0.035(4) 0.055(5) 0.027(4) -0.011(3) -0.002(3) -0.017(4) N2 0.035(5) 0.036(5) 0.051(6) -0.012(4) -0.009(4) -0.013(4) C11 0.048(6) 0.076(6) 0.057(6) -0.013(5) -0.015(5) -0.024(5) C12 0.043(5) 0.058(5) 0.041(5) -0.003(4) -0.010(4) -0.025(4) C6' 0.049(6) 0.047(6) 0.055(6) -0.009(5) -0.010(5) -0.006(5) C1' 0.069(8) 0.065(7) 0.047(7) -0.024(6) -0.016(6) -0.018(6) C2' 0.076(10) 0.066(9) 0.059(7) -0.026(7) -0.032(7) -0.018(7) C3' 0.046(11) 0.055(11) 0.043(10) -0.027(7) -0.024(7) -0.009(7) C4' 0.035(4) 0.039(4) 0.039(5) -0.019(3) -0.013(3) -0.014(3) N1' 0.043(6) 0.045(6) 0.040(5) -0.024(4) -0.013(4) -0.016(5) C5' 0.046(7) 0.034(6) 0.040(7) -0.008(5) -0.007(6) -0.009(5) C7' 0.045(6) 0.053(6) 0.048(6) -0.020(5) -0.017(5) -0.015(5) C8' 0.032(6) 0.031(5) 0.039(7) 0.007(5) -0.003(6) -0.018(4) C9' 0.055(7) 0.063(7) 0.045(7) -0.018(6) -0.013(5) -0.019(5) C10' 0.081(9) 0.079(9) 0.083(8) -0.029(7) -0.023(7) -0.031(7) N2' 0.042(7) 0.052(8) 0.032(6) -0.005(6) -0.017(5) -0.009(6) C11' 0.023(5) 0.034(6) 0.033(6) -0.002(5) -0.002(4) -0.015(4) C12' 0.032(7) 0.046(6) 0.021(5) -0.001(5) 0.010(5) -0.019(5) C13 0.059(3) 0.065(3) 0.052(3) -0.003(2) -0.030(2) -0.020(2) C14 0.061(3) 0.050(3) 0.053(3) -0.010(2) -0.023(2) -0.016(2) C15 0.055(3) 0.054(3) 0.054(3) -0.016(2) -0.021(2) -0.011(2) C16 0.057(3) 0.062(3) 0.056(3) -0.026(2) -0.015(2) -0.013(2) C17 0.063(3) 0.063(3) 0.041(2) -0.018(2) -0.007(2) -0.030(3) C18 0.068(3) 0.062(3) 0.052(3) -0.015(2) -0.022(2) -0.018(3) C19 0.061(3) 0.070(3) 0.051(3) -0.012(2) -0.014(2) -0.026(3) C20 0.052(3) 0.066(3) 0.040(2) -0.017(2) -0.007(2) -0.023(2) C21 0.050(3) 0.068(3) 0.054(3) -0.022(2) -0.013(2) -0.016(2) C22 0.048(3) 0.077(3) 0.049(3) -0.025(2) -0.012(2) -0.020(3) C23 0.049(3) 0.080(4) 0.060(3) -0.016(3) -0.023(2) -0.014(3) C24 0.063(3) 0.061(3) 0.061(3) -0.018(2) -0.023(3) -0.015(2) C25 0.105(5) 0.096(5) 0.113(5) -0.028(4) -0.039(4) -0.031(4) C26 0.113(6) 0.093(5) 0.122(6) -0.037(4) -0.032(5) -0.031(4) C27 0.103(5) 0.102(5) 0.078(4) -0.026(4) -0.024(4) -0.050(4) C28 0.083(4) 0.110(5) 0.088(4) -0.019(4) -0.022(3) -0.035(4) C29 0.069(4) 0.095(4) 0.066(3) -0.022(3) -0.010(3) -0.043(3) C30 0.076(4) 0.087(4) 0.093(4) -0.012(4) -0.016(3) -0.029(3) C31 0.062(3) 0.084(4) 0.082(4) -0.031(3) 0.007(3) -0.028(3) C32 0.051(3) 0.082(4) 0.053(3) -0.017(3) -0.008(2) -0.031(3) C33 0.046(3) 0.073(4) 0.065(3) -0.015(3) -0.019(2) -0.015(3) C34 0.044(3) 0.058(3) 0.056(3) -0.013(2) -0.016(2) -0.009(2) C35 0.052(3) 0.056(3) 0.055(3) -0.013(2) -0.017(2) -0.006(2) C36 0.069(3) 0.060(3) 0.066(3) -0.028(3) -0.004(3) -0.017(3) C37 0.034(2) 0.046(3) 0.049(3) -0.016(2) -0.014(2) -0.002(2) C38 0.049(3) 0.051(3) 0.048(3) -0.016(2) -0.009(2) -0.016(2) C39 0.033(2) 0.043(2) 0.050(3) -0.016(2) -0.0179(19) -0.0044(19) C40 0.089(4) 0.080(4) 0.068(4) -0.005(3) 0.004(3) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N7 1.943(4) 2_677 ? Cu1 N7 1.943(4) . ? Cu1 N6 2.032(3) . ? Cu1 N6 2.032(3) 2_677 ? Cu2 N8 1.940(4) . ? Cu2 N9 1.953(4) . ? Cu2 N2 2.013(5) . ? Cu2 N2' 2.029(7) . ? Cu2 N3 2.029(3) . ? Cu2 O1 2.408(3) . ? S1 C38 1.612(5) . ? S2 C39 1.623(5) . ? S3 C37 1.621(5) . ? O1 C40 1.408(5) . ? O1 H1A 0.8477 . ? N3 C15 1.334(5) . ? N3 C14 1.342(5) . ? N4 C21 1.332(5) . ? N4 C20 1.344(5) . ? N5 C29 1.332(7) . ? N5 C28 1.360(7) . ? N6 C35 1.336(5) . ? N6 C34 1.344(5) . ? N7 C37 1.154(5) . ? N8 C38 1.146(5) . ? N9 C39 1.153(5) . ? C1 C2 1.3900 . ? C1 C5 1.3900 . ? C1 H1B 0.9300 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 N1 1.3900 . ? C4 H4A 0.9300 . ? N1 C5 1.3900 . ? C5 C6 1.452(6) . ? C6 C7 1.320(8) . ? C6 H6A 0.9300 . ? C7 C8 1.473(6) . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 C12 1.3900 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 N2 1.3900 . ? C10 H10A 0.9300 . ? N2 C11 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C6' C7' 1.321(9) . ? C6' C5' 1.455(7) . ? C6' H6'A 0.9300 . ? C1' C2' 1.3900 . ? C1' C5' 1.3900 . ? C1' H1'A 0.9300 . ? C2' C3' 1.3900 . ? C2' H2'A 0.9300 . ? C3' C4' 1.3900 . ? C3' H3'A 0.9300 . ? C4' N1' 1.3900 . ? C4' H4'A 0.9300 . ? N1' C5' 1.3900 . ? C7' C8' 1.478(7) . ? C7' H7'A 0.9300 . ? C8' C9' 1.3900 . ? C8' C12' 1.3900 . ? C9' C10' 1.3900 . ? C9' H9'A 0.9300 . ? C10' N2' 1.3900 . ? C10' H10B 0.9300 . ? N2' C11' 1.3900 . ? C11' C12' 1.3900 . ? C11' H11B 0.9300 . ? C12' H12B 0.9300 . ? C13 C14 1.383(5) . ? C13 C17 1.388(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.367(5) . ? C15 H15 0.9300 . ? C16 C17 1.369(6) . ? C16 H16 0.9300 . ? C17 C18 1.465(5) . ? C18 C19 1.283(6) . ? C18 H18 0.9300 . ? C19 C20 1.466(5) . ? C19 H19 0.9300 . ? C20 C24 1.378(6) . ? C21 C22 1.372(6) . ? C21 H21 0.9300 . ? C22 C23 1.366(6) . ? C22 H22 0.9300 . ? C23 C24 1.370(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.357(8) . ? C25 C29 1.358(8) . ? C25 H25 0.9300 . ? C26 C27 1.344(8) . ? C26 H26 0.9300 . ? C27 C28 1.374(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.511(7) . ? C30 C31 1.260(7) . ? C30 H30 0.9300 . ? C31 C32 1.490(6) . ? C31 H31 0.9300 . ? C32 C33 1.362(6) . ? C32 C36 1.394(6) . ? C33 C34 1.366(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.371(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Cu1 N7 180.000(2) 2_677 . ? N7 Cu1 N6 90.74(14) 2_677 . ? N7 Cu1 N6 89.26(14) . . ? N7 Cu1 N6 89.26(14) 2_677 2_677 ? N7 Cu1 N6 90.74(14) . 2_677 ? N6 Cu1 N6 180.00(14) . 2_677 ? N8 Cu2 N9 170.94(16) . . ? N8 Cu2 N2 90.8(4) . . ? N9 Cu2 N2 88.3(4) . . ? N8 Cu2 N2' 88.5(5) . . ? N9 Cu2 N2' 91.5(5) . . ? N2 Cu2 N2' 6.7(7) . . ? N8 Cu2 N3 90.39(13) . . ? N9 Cu2 N3 90.43(13) . . ? N2 Cu2 N3 178.6(3) . . ? N2' Cu2 N3 174.4(4) . . ? N8 Cu2 O1 92.24(13) . . ? N9 Cu2 O1 96.82(13) . . ? N2 Cu2 O1 94.4(3) . . ? N2' Cu2 O1 88.3(5) . . ? N3 Cu2 O1 86.23(12) . . ? C40 O1 Cu2 119.3(3) . . ? C40 O1 H1A 108.3 . . ? Cu2 O1 H1A 131.6 . . ? C15 N3 C14 117.0(3) . . ? C15 N3 Cu2 119.6(3) . . ? C14 N3 Cu2 123.4(3) . . ? C21 N4 C20 117.8(4) . . ? C29 N5 C28 116.8(5) . . ? C35 N6 C34 116.1(4) . . ? C35 N6 Cu1 122.1(3) . . ? C34 N6 Cu1 121.7(3) . . ? C37 N7 Cu1 163.7(3) . . ? C38 N8 Cu2 163.8(4) . . ? C39 N9 Cu2 163.1(4) . . ? C2 C1 C5 120.0 . . ? C2 C1 H1B 120.0 . . ? C5 C1 H1B 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? N1 C4 C3 120.0 . . ? N1 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 N1 C4 120.0 . . ? N1 C5 C1 120.0 . . ? N1 C5 C6 117.4(5) . . ? C1 C5 C6 122.6(5) . . ? C7 C6 C5 125.4(7) . . ? C7 C6 H6A 117.3 . . ? C5 C6 H6A 117.3 . . ? C6 C7 C8 127.6(8) . . ? C6 C7 H7A 116.2 . . ? C8 C7 H7A 116.2 . . ? C9 C8 C12 120.0 . . ? C9 C8 C7 122.3(5) . . ? C12 C8 C7 117.5(5) . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? N2 C10 C9 120.0 . . ? N2 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C11 N2 C10 120.0 . . ? C11 N2 Cu2 120.9(5) . . ? C10 N2 Cu2 119.1(5) . . ? N2 C11 C12 120.0 . . ? N2 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C8 120.0 . . ? C11 C12 H12A 120.0 . . ? C8 C12 H12A 120.0 . . ? C7' C6' C5' 123.3(9) . . ? C7' C6' H6'A 118.4 . . ? C5' C6' H6'A 118.4 . . ? C2' C1' C5' 120.0 . . ? C2' C1' H1'A 120.0 . . ? C5' C1' H1'A 120.0 . . ? C3' C2' C1' 120.0 . . ? C3' C2' H2'A 120.0 . . ? C1' C2' H2'A 120.0 . . ? C2' C3' C4' 120.0 . . ? C2' C3' H3'A 120.0 . . ? C4' C3' H3'A 120.0 . . ? N1' C4' C3' 120.0 . . ? N1' C4' H4'A 120.0 . . ? C3' C4' H4'A 120.0 . . ? C4' N1' C5' 120.0 . . ? N1' C5' C1' 120.0 . . ? N1' C5' C6' 118.4(6) . . ? C1' C5' C6' 121.6(6) . . ? C6' C7' C8' 124.3(9) . . ? C6' C7' H7'A 117.9 . . ? C8' C7' H7'A 117.9 . . ? C9' C8' C12' 120.0 . . ? C9' C8' C7' 117.7(6) . . ? C12' C8' C7' 122.3(6) . . ? C8' C9' C10' 120.0 . . ? C8' C9' H9'A 120.0 . . ? C10' C9' H9'A 120.0 . . ? C9' C10' N2' 120.0 . . ? C9' C10' H10B 120.0 . . ? N2' C10' H10B 120.0 . . ? C11' N2' C10' 120.0 . . ? C11' N2' Cu2 122.3(7) . . ? C10' N2' Cu2 117.4(7) . . ? N2' C11' C12' 120.0 . . ? N2' C11' H11B 120.0 . . ? C12' C11' H11B 120.0 . . ? C11' C12' C8' 120.0 . . ? C11' C12' H12B 120.0 . . ? C8' C12' H12B 120.0 . . ? C14 C13 C17 120.2(4) . . ? C14 C13 H13 119.9 . . ? C17 C13 H13 119.9 . . ? N3 C14 C13 122.3(4) . . ? N3 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? N3 C15 C16 123.5(4) . . ? N3 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C13 116.7(4) . . ? C16 C17 C18 119.7(4) . . ? C13 C17 C18 123.6(4) . . ? C19 C18 C17 127.8(5) . . ? C19 C18 H18 116.1 . . ? C17 C18 H18 116.1 . . ? C18 C19 C20 126.1(5) . . ? C18 C19 H19 116.9 . . ? C20 C19 H19 116.9 . . ? N4 C20 C24 121.3(4) . . ? N4 C20 C19 118.8(4) . . ? C24 C20 C19 119.8(4) . . ? N4 C21 C22 123.9(4) . . ? N4 C21 H21 118.0 . . ? C22 C21 H21 118.0 . . ? C23 C22 C21 117.9(4) . . ? C23 C22 H22 121.1 . . ? C21 C22 H22 121.1 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C20 119.7(4) . . ? C23 C24 H24 120.2 . . ? C20 C24 H24 120.2 . . ? C26 C25 C29 120.4(6) . . ? C26 C25 H25 119.8 . . ? C29 C25 H25 119.8 . . ? C27 C26 C25 119.7(7) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 118.1(6) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? N5 C28 C27 123.1(6) . . ? N5 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? N5 C29 C25 121.9(5) . . ? N5 C29 C30 119.2(5) . . ? C25 C29 C30 118.9(6) . . ? C31 C30 C29 123.9(6) . . ? C31 C30 H30 118.1 . . ? C29 C30 H30 118.1 . . ? C30 C31 C32 124.9(6) . . ? C30 C31 H31 117.6 . . ? C32 C31 H31 117.6 . . ? C33 C32 C36 116.0(4) . . ? C33 C32 C31 118.9(5) . . ? C36 C32 C31 125.0(5) . . ? C32 C33 C34 120.9(4) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? N6 C34 C33 123.5(4) . . ? N6 C34 H34 118.3 . . ? C33 C34 H34 118.3 . . ? N6 C35 C36 123.0(4) . . ? N6 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C32 120.5(4) . . ? C35 C36 H36 119.7 . . ? C32 C36 H36 119.7 . . ? N7 C37 S3 179.5(4) . . ? N8 C38 S1 179.0(4) . . ? N9 C39 S2 177.9(4) . . ? O1 C40 H40A 109.4 . . ? O1 C40 H40B 109.6 . . ? H40A C40 H40B 109.5 . . ? O1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 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 N8 Cu2 O1 C40 16.5(3) . . . . ? N9 Cu2 O1 C40 -163.8(3) . . . . ? N2 Cu2 O1 C40 107.5(5) . . . . ? N2' Cu2 O1 C40 104.9(6) . . . . ? N3 Cu2 O1 C40 -73.8(3) . . . . ? N8 Cu2 N3 C15 -145.2(3) . . . . ? N9 Cu2 N3 C15 43.8(3) . . . . ? O1 Cu2 N3 C15 -53.0(3) . . . . ? N8 Cu2 N3 C14 34.8(3) . . . . ? N9 Cu2 N3 C14 -136.2(3) . . . . ? O1 Cu2 N3 C14 127.0(3) . . . . ? N7 Cu1 N6 C35 135.3(3) 2_677 . . . ? N7 Cu1 N6 C35 -44.7(3) . . . . ? N7 Cu1 N6 C34 -39.9(3) 2_677 . . . ? N7 Cu1 N6 C34 140.1(3) . . . . ? N6 Cu1 N7 C37 -55.7(12) . . . . ? N6 Cu1 N7 C37 124.3(12) 2_677 . . . ? N2 Cu2 N8 C38 121.3(13) . . . . ? N2' Cu2 N8 C38 127.5(13) . . . . ? N3 Cu2 N8 C38 -58.0(13) . . . . ? O1 Cu2 N8 C38 -144.2(13) . . . . ? N2 Cu2 N9 C39 -62.9(11) . . . . ? N2' Cu2 N9 C39 -68.8(12) . . . . ? N3 Cu2 N9 C39 116.5(11) . . . . ? O1 Cu2 N9 C39 -157.2(10) . . . . ? C4 N1 C5 C6 179.1(8) . . . . ? C2 C1 C5 N1 0.0 . . . . ? C2 C1 C5 C6 -179.1(9) . . . . ? N1 C5 C6 C7 169.0(7) . . . . ? C1 C5 C6 C7 -11.8(11) . . . . ? C5 C6 C7 C8 177.8(7) . . . . ? C6 C7 C8 C9 9.0(11) . . . . ? C6 C7 C8 C12 -175.9(7) . . . . ? C12 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C10 175.0(8) . . . . ? C8 C9 C10 N2 0.0 . . . . ? C9 C10 N2 C11 0.0 . . . . ? C9 C10 N2 Cu2 -177.7(8) . . . . ? N8 Cu2 N2 C11 -126.3(5) . . . . ? N9 Cu2 N2 C11 44.7(5) . . . . ? O1 Cu2 N2 C11 141.4(5) . . . . ? N8 Cu2 N2 C10 51.4(6) . . . . ? N9 Cu2 N2 C10 -137.6(6) . . . . ? O1 Cu2 N2 C10 -40.9(6) . . . . ? Cu2 N2 C11 C12 177.7(8) . . . . ? C7 C8 C12 C11 -175.2(7) . . . . ? C4' N1' C5' C6' -177.6(11) . . . . ? C2' C1' C5' N1' 0.0 . . . . ? C2' C1' C5' C6' 177.5(11) . . . . ? C7' C6' C5' N1' -7.6(15) . . . . ? C7' C6' C5' C1' 174.8(10) . . . . ? C5' C6' C7' C8' -179.3(10) . . . . ? C6' C7' C8' C9' -173.1(10) . . . . ? C6' C7' C8' C12' 7.1(16) . . . . ? C12' C8' C9' C10' 0.0 . . . . ? C7' C8' C9' C10' -179.8(11) . . . . ? C8' C9' C10' N2' 0.0 . . . . ? C9' C10' N2' C11' 0.0 . . . . ? C9' C10' N2' Cu2 -174.3(12) . . . . ? N8 Cu2 N2' C11' -127.0(9) . . . . ? N9 Cu2 N2' C11' 44.0(9) . . . . ? O1 Cu2 N2' C11' 140.7(9) . . . . ? N8 Cu2 N2' C10' 47.2(7) . . . . ? N9 Cu2 N2' C10' -141.9(7) . . . . ? O1 Cu2 N2' C10' -45.1(7) . . . . ? C10' N2' C11' C12' 0.0 . . . . ? Cu2 N2' C11' C12' 174.0(12) . . . . ? C7' C8' C12' C11' 179.8(11) . . . . ? C15 N3 C14 C13 -0.6(6) . . . . ? Cu2 N3 C14 C13 179.4(3) . . . . ? C17 C13 C14 N3 0.6(7) . . . . ? C14 N3 C15 C16 0.3(6) . . . . ? Cu2 N3 C15 C16 -179.7(3) . . . . ? N3 C15 C16 C17 -0.2(7) . . . . ? C15 C16 C17 C13 0.2(7) . . . . ? C15 C16 C17 C18 178.7(4) . . . . ? C14 C13 C17 C16 -0.4(6) . . . . ? C14 C13 C17 C18 -178.9(4) . . . . ? C16 C17 C18 C19 177.6(5) . . . . ? C13 C17 C18 C19 -4.0(8) . . . . ? C17 C18 C19 C20 178.0(4) . . . . ? C21 N4 C20 C24 1.1(6) . . . . ? C21 N4 C20 C19 -177.0(4) . . . . ? C18 C19 C20 N4 7.7(7) . . . . ? C18 C19 C20 C24 -170.4(5) . . . . ? C20 N4 C21 C22 -0.6(6) . . . . ? N4 C21 C22 C23 -0.3(7) . . . . ? C21 C22 C23 C24 0.8(7) . . . . ? C22 C23 C24 C20 -0.4(7) . . . . ? N4 C20 C24 C23 -0.6(7) . . . . ? C19 C20 C24 C23 177.4(4) . . . . ? C29 C25 C26 C27 -0.4(10) . . . . ? C25 C26 C27 C28 1.7(10) . . . . ? C29 N5 C28 C27 0.5(9) . . . . ? C26 C27 C28 N5 -1.8(9) . . . . ? C28 N5 C29 C25 0.9(8) . . . . ? C28 N5 C29 C30 179.2(5) . . . . ? C26 C25 C29 N5 -0.9(10) . . . . ? C26 C25 C29 C30 -179.3(6) . . . . ? N5 C29 C30 C31 -2.5(9) . . . . ? C25 C29 C30 C31 175.9(6) . . . . ? C29 C30 C31 C32 -175.8(5) . . . . ? C30 C31 C32 C33 169.6(5) . . . . ? C30 C31 C32 C36 -6.8(9) . . . . ? C36 C32 C33 C34 1.4(7) . . . . ? C31 C32 C33 C34 -175.3(4) . . . . ? C35 N6 C34 C33 -1.9(6) . . . . ? Cu1 N6 C34 C33 173.5(3) . . . . ? C32 C33 C34 N6 0.3(7) . . . . ? C34 N6 C35 C36 1.7(6) . . . . ? Cu1 N6 C35 C36 -173.7(3) . . . . ? N6 C35 C36 C32 0.0(7) . . . . ? C33 C32 C36 C35 -1.6(7) . . . . ? C31 C32 C36 C35 174.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.589 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.063 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 284290' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H64 Cu3 N18 O2 S6' _chemical_formula_weight 1668.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.708(3) _cell_length_b 12.900(4) _cell_length_c 17.142(6) _cell_angle_alpha 71.910(5) _cell_angle_beta 75.596(5) _cell_angle_gamma 71.955(5) _cell_volume 1912.4(11) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1615 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 20.52 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 857 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.582398 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10419 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6678 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6678 _refine_ls_number_parameters 643 _refine_ls_number_restraints 237 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.0000 0.0000 0.5000 0.0488(2) Uani 1 2 d S . . Cu2 Cu 0.38090(6) 0.23895(4) 0.20390(3) 0.04639(18) Uani 1 1 d . . . S1 S 0.24208(18) 0.61780(12) 0.05345(11) 0.1019(5) Uani 1 1 d . . . S2 S 0.30628(13) -0.09086(10) 0.40458(7) 0.0583(3) Uani 1 1 d . . . S3 S -0.03260(15) -0.32489(10) 0.71264(8) 0.0685(4) Uani 1 1 d . . . O1 O 0.6131(3) 0.2015(3) 0.11977(18) 0.0680(9) Uani 1 1 d . A . H1A H 0.6948 0.1536 0.1267 0.102 Uiso 1 1 d R . . H1B H 0.6121 0.2552 0.0759 0.102 Uiso 1 1 d R . . N7 N 0.3469(4) 0.3987(3) 0.1406(2) 0.0575(10) Uani 1 1 d . A . N8 N 0.3765(4) 0.0898(3) 0.2767(2) 0.0556(10) Uani 1 1 d . A . N9 N 0.0268(4) -0.1402(3) 0.5871(2) 0.0539(9) Uani 1 1 d . . . C1 C 0.0598(14) -0.0998(7) -0.2071(7) 0.086(5) Uani 0.584(10) 1 d PG A 1 H1C H 0.0991 -0.1694 -0.2197 0.103 Uiso 0.584(10) 1 calc PR A 1 C2 C -0.0611(15) -0.0249(10) -0.2408(8) 0.080(7) Uani 0.584(10) 1 d PG A 1 H2A H -0.1025 -0.0443 -0.2759 0.096 Uiso 0.584(10) 1 calc PR A 1 C3 C -0.1199(13) 0.0791(9) -0.2220(8) 0.061(5) Uani 0.584(10) 1 d PG A 1 H3A H -0.2007 0.1292 -0.2446 0.073 Uiso 0.584(10) 1 calc PR A 1 C4 C -0.0579(11) 0.1081(7) -0.1695(7) 0.051(3) Uani 0.584(10) 1 d PG A 1 H4A H -0.0973 0.1777 -0.1569 0.061 Uiso 0.584(10) 1 calc PR A 1 C5 C 0.0629(10) 0.0332(8) -0.1358(5) 0.031(2) Uani 0.584(10) 1 d PGD A 1 N1 N 0.1217(9) -0.0708(7) -0.1546(6) 0.047(2) Uani 0.584(10) 1 d PG A 1 C6 C 0.1389(9) 0.0530(7) -0.0802(5) 0.048(2) Uani 0.584(10) 1 d PD A 1 H6A H 0.2229 -0.0020 -0.0654 0.057 Uiso 0.584(10) 1 calc PR A 1 C7 C 0.1000(8) 0.1413(7) -0.0490(4) 0.052(2) Uani 0.584(10) 1 d PD A 1 H7A H 0.0181 0.1967 -0.0662 0.063 Uiso 0.584(10) 1 calc PR A 1 C8 C 0.1681(8) 0.1640(6) 0.0090(4) 0.043(2) Uani 0.584(10) 1 d PGD A 1 C9 C 0.1079(7) 0.2637(6) 0.0341(5) 0.053(2) Uani 0.584(10) 1 d PGD A 1 H9A H 0.0243 0.3143 0.0148 0.064 Uiso 0.584(10) 1 calc PR A 1 C10 C 0.1727(10) 0.2877(6) 0.0879(6) 0.073(3) Uani 0.584(10) 1 d PG A 1 H10A H 0.1324 0.3544 0.1047 0.088 Uiso 0.584(10) 1 calc PR A 1 N2 N 0.2976(10) 0.2121(7) 0.1168(5) 0.043(3) Uani 0.584(10) 1 d PG A 1 C11 C 0.3577(8) 0.1124(7) 0.0917(5) 0.043(2) Uani 0.584(10) 1 d PG A 1 H11A H 0.4413 0.0618 0.1110 0.052 Uiso 0.584(10) 1 calc PR A 1 C12 C 0.2930(8) 0.0884(6) 0.0378(4) 0.047(2) Uani 0.584(10) 1 d PGD A 1 H12A H 0.3332 0.0217 0.0210 0.057 Uiso 0.584(10) 1 calc PR A 1 C18 C 0.5824(7) 0.3510(6) 0.4810(4) 0.047(2) Uani 0.654(9) 1 d PD A 1 H18A H 0.5253 0.3339 0.5333 0.056 Uiso 0.654(9) 1 calc PR A 1 C13 C 0.4321(7) 0.2648(6) 0.4369(3) 0.047(2) Uani 0.654(9) 1 d PGD A 1 H13A H 0.3889 0.2439 0.4924 0.057 Uiso 0.654(9) 1 calc PR A 1 C14 C 0.3859(9) 0.2402(8) 0.3757(4) 0.062(3) Uani 0.654(9) 1 d PG A 1 H14A H 0.3118 0.2027 0.3903 0.074 Uiso 0.654(9) 1 calc PR A 1 N3 N 0.4505(10) 0.2716(9) 0.2929(4) 0.041(3) Uani 0.654(9) 1 d PG A 1 C15 C 0.5612(8) 0.3276(7) 0.2712(3) 0.0353(19) Uani 0.654(9) 1 d PG A 1 H15A H 0.6044 0.3485 0.2157 0.042 Uiso 0.654(9) 1 calc PR A 1 C16 C 0.6074(6) 0.3522(5) 0.3324(3) 0.0442(19) Uani 0.654(9) 1 d PGD A 1 H16A H 0.6816 0.3896 0.3179 0.053 Uiso 0.654(9) 1 calc PR A 1 C17 C 0.5429(7) 0.3208(5) 0.4153(3) 0.0345(18) Uani 0.654(9) 1 d PGD A 1 C19 C 0.6858(7) 0.3983(5) 0.4772(4) 0.047(2) Uani 0.654(9) 1 d PD A 1 H19A H 0.7435 0.4168 0.4253 0.056 Uiso 0.654(9) 1 calc PR A 1 C20 C 0.7199(6) 0.4248(5) 0.5449(3) 0.0409(19) Uani 0.654(9) 1 d PGD A 1 N4 N 0.8193(7) 0.4908(6) 0.5239(3) 0.059(2) Uani 0.654(9) 1 d PGD A 1 C21 C 0.8639(9) 0.5145(7) 0.5861(5) 0.0626(18) Uani 0.654(9) 1 d PGU A 1 H21A H 0.9304 0.5587 0.5721 0.075 Uiso 0.654(9) 1 calc PR A 1 C22 C 0.8092(12) 0.4721(9) 0.6693(4) 0.061(4) Uani 0.654(9) 1 d PG A 1 H22A H 0.8391 0.4880 0.7109 0.073 Uiso 0.654(9) 1 calc PR A 1 C23 C 0.7099(11) 0.4061(8) 0.6902(3) 0.063(3) Uani 0.654(9) 1 d PG A 1 H23A H 0.6732 0.3778 0.7459 0.075 Uiso 0.654(9) 1 calc PR A 1 C24 C 0.6652(7) 0.3824(6) 0.6280(4) 0.0480(19) Uani 0.654(9) 1 d PGD A 1 H24A H 0.5987 0.3383 0.6420 0.058 Uiso 0.654(9) 1 calc PR A 1 C37 C 0.3459(4) 0.0157(4) 0.3304(3) 0.0432(10) Uani 1 1 d . A 1 C38 C 0.3031(5) 0.4907(4) 0.1040(3) 0.0528(11) Uani 1 1 d . A 1 C39 C 0.0016(4) -0.2171(4) 0.6396(3) 0.0451(10) Uani 1 1 d . B 1 C1' C 0.0628(13) -0.0806(8) -0.2000(8) 0.023(3) Uani 0.416(10) 1 d PGU A 2 H1'A H 0.1164 -0.1504 -0.2094 0.027 Uiso 0.416(10) 1 calc PR A 2 C2' C -0.0627(16) -0.0228(10) -0.2354(9) 0.027(4) Uani 0.416(10) 1 d PGU A 2 H2'A H -0.0931 -0.0539 -0.2684 0.032 Uiso 0.416(10) 1 calc PR A 2 C3' C -0.1429(15) 0.0815(11) -0.2214(12) 0.060(6) Uani 0.416(10) 1 d PGU A 2 H3'A H -0.2268 0.1202 -0.2451 0.072 Uiso 0.416(10) 1 calc PR A 2 C4' C -0.0975(15) 0.1280(10) -0.1721(11) 0.067(5) Uani 0.416(10) 1 d PGU A 2 H4'A H -0.1511 0.1978 -0.1628 0.080 Uiso 0.416(10) 1 calc PR A 2 C5' C 0.0281(14) 0.0702(10) -0.1368(8) 0.052(5) Uani 0.416(10) 1 d PGDU A 2 N1' N 0.1082(11) -0.0341(10) -0.1507(7) 0.034(3) Uani 0.416(10) 1 d PGU A 2 C6' C 0.0763(12) 0.1131(10) -0.0825(6) 0.048(4) Uani 0.416(10) 1 d PDU A 2 H6'A H 0.0253 0.1850 -0.0767 0.057 Uiso 0.416(10) 1 calc PR A 2 C7' C 0.1851(11) 0.0604(9) -0.0407(6) 0.052(3) Uani 0.416(10) 1 d PDU A 2 H7'A H 0.2397 -0.0113 -0.0456 0.063 Uiso 0.416(10) 1 calc PR A 2 C8' C 0.2228(11) 0.1128(8) 0.0144(5) 0.037(3) Uani 0.416(10) 1 d PGDU A 2 C9' C 0.1465(10) 0.2166(8) 0.0306(6) 0.040(3) Uani 0.416(10) 1 d PGU A 2 H9'A H 0.0679 0.2610 0.0036 0.048 Uiso 0.416(10) 1 calc PR A 2 C10' C 0.1876(12) 0.2539(7) 0.0871(6) 0.023(3) Uani 0.416(10) 1 d PGU A 2 H10B H 0.1365 0.3233 0.0980 0.028 Uiso 0.416(10) 1 calc PR A 2 N2' N 0.3051(14) 0.1875(9) 0.1274(7) 0.039(4) Uani 0.416(10) 1 d PGU A 2 C11' C 0.3814(11) 0.0837(9) 0.1112(7) 0.053(4) Uani 0.416(10) 1 d PGU A 2 H11B H 0.4600 0.0392 0.1382 0.063 Uiso 0.416(10) 1 calc PR A 2 C12' C 0.3403(10) 0.0464(7) 0.0547(6) 0.038(3) Uani 0.416(10) 1 d PGU A 2 H12B H 0.3914 -0.0231 0.0439 0.046 Uiso 0.416(10) 1 calc PR A 2 C18' C 0.6533(15) 0.3743(12) 0.4421(6) 0.054(4) Uani 0.346(9) 1 d PDU A 2 H18B H 0.7337 0.4047 0.4171 0.064 Uiso 0.346(9) 1 calc PR A 2 C13' C 0.4823(12) 0.2775(10) 0.4221(6) 0.031(4) Uani 0.346(9) 1 d PGDU A 2 H13B H 0.4506 0.2579 0.4793 0.037 Uiso 0.346(9) 1 calc PR A 2 C14' C 0.4240(15) 0.2455(14) 0.3696(8) 0.021(3) Uani 0.346(9) 1 d PGU A 2 H14B H 0.3533 0.2045 0.3916 0.026 Uiso 0.346(9) 1 calc PR A 2 N3' N 0.471(2) 0.2747(18) 0.2840(8) 0.044(6) Uani 0.346(9) 1 d PGU A 2 C15' C 0.577(2) 0.3359(17) 0.2510(5) 0.096(8) Uani 0.346(9) 1 d PGU A 2 H15B H 0.6087 0.3555 0.1938 0.115 Uiso 0.346(9) 1 calc PR A 2 C16' C 0.6353(14) 0.3680(11) 0.3036(6) 0.044(4) Uani 0.346(9) 1 d PGDU A 2 H16B H 0.7060 0.4089 0.2815 0.053 Uiso 0.346(9) 1 calc PR A 2 C17' C 0.5879(11) 0.3388(9) 0.3891(6) 0.027(3) Uani 0.346(9) 1 d PGDU A 2 C19' C 0.6073(14) 0.3664(11) 0.5216(6) 0.051(4) Uani 0.346(9) 1 d PDU A 2 H19B H 0.5230 0.3410 0.5467 0.061 Uiso 0.346(9) 1 calc PR A 2 C20' C 0.6821(13) 0.3958(10) 0.5730(6) 0.048(5) Uani 0.346(9) 1 d PGDU A 2 N4' N 0.7778(13) 0.4645(11) 0.5334(5) 0.040(3) Uani 0.346(9) 1 d PGDU A 2 C21' C 0.8319(18) 0.5097(14) 0.5797(8) 0.055(2) Uani 0.346(9) 1 d PGU A 2 H21B H 0.8959 0.5557 0.5532 0.066 Uiso 0.346(9) 1 calc PR A 2 C22' C 0.790(2) 0.4862(18) 0.6658(8) 0.046(6) Uani 0.346(9) 1 d PGU A 2 H22B H 0.8265 0.5164 0.6968 0.055 Uiso 0.346(9) 1 calc PR A 2 C23' C 0.695(2) 0.4174(17) 0.7055(5) 0.053(5) Uani 0.346(9) 1 d PGU A 2 H23B H 0.6669 0.4017 0.7630 0.064 Uiso 0.346(9) 1 calc PR A 2 C24' C 0.6406(16) 0.3723(12) 0.6591(6) 0.064(6) Uani 0.346(9) 1 d PGDU A 2 H24B H 0.5766 0.3263 0.6856 0.076 Uiso 0.346(9) 1 calc PR A 2 C25 C 0.2171(8) 0.3997(5) 0.8125(4) 0.103(2) Uani 1 1 d . . . H25A H 0.1300 0.4419 0.7931 0.124 Uiso 1 1 calc R . . C26 C 0.2662(8) 0.4331(5) 0.8664(4) 0.097(2) Uani 1 1 d . . . H26A H 0.2134 0.4984 0.8833 0.117 Uiso 1 1 calc R . . C27 C 0.3923(8) 0.3706(6) 0.8952(3) 0.0888(19) Uani 1 1 d . . . H27A H 0.4278 0.3922 0.9319 0.107 Uiso 1 1 calc R . . C28 C 0.4660(7) 0.2754(6) 0.8691(4) 0.0908(18) Uani 1 1 d . . . H28A H 0.5523 0.2320 0.8889 0.109 Uiso 1 1 calc R . . N5 N 0.4180(6) 0.2411(4) 0.8147(3) 0.0882(15) Uani 1 1 d . . . C29 C 0.2930(8) 0.3070(6) 0.7874(3) 0.0824(17) Uani 1 1 d D . . C30 C 0.2323(7) 0.2753(5) 0.7287(3) 0.0930(18) Uani 1 1 d D . . H30A H 0.1472 0.3244 0.7104 0.112 Uiso 1 1 calc R . . C31 C 0.2846(6) 0.1895(5) 0.7018(3) 0.0818(17) Uani 1 1 d D . . H31A H 0.3730 0.1431 0.7177 0.098 Uiso 1 1 calc R . . C32 C 0.2214(5) 0.1530(5) 0.6472(3) 0.0597(13) Uani 1 1 d D B . C33 C 0.1009(5) 0.2179(4) 0.6087(3) 0.0623(13) Uani 1 1 d . . . H33A H 0.0600 0.2920 0.6123 0.075 Uiso 1 1 calc R . . C34 C 0.0425(5) 0.1734(4) 0.5655(3) 0.0561(11) Uani 1 1 d . B . H34A H -0.0392 0.2179 0.5413 0.067 Uiso 1 1 calc R . . N5' N 0.0996(4) 0.0666(3) 0.55704(19) 0.0461(8) Uani 1 1 d . . . C35 C 0.2177(5) 0.0067(4) 0.5924(3) 0.0543(11) Uani 1 1 d . B . H35A H 0.2596 -0.0665 0.5867 0.065 Uiso 1 1 calc R . . C36 C 0.2804(5) 0.0463(4) 0.6360(3) 0.0633(13) Uani 1 1 d . . . H36A H 0.3637 0.0009 0.6584 0.076 Uiso 1 1 calc R B . 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 Cu1 0.0657(5) 0.0432(4) 0.0421(4) -0.0061(3) -0.0226(3) -0.0141(4) Cu2 0.0605(4) 0.0432(3) 0.0453(3) -0.0095(2) -0.0245(2) -0.0161(2) S1 0.0913(12) 0.0636(10) 0.1216(13) 0.0163(9) -0.0331(10) -0.0069(8) S2 0.0625(8) 0.0492(7) 0.0547(7) -0.0052(5) -0.0120(6) -0.0088(6) S3 0.0780(9) 0.0520(7) 0.0678(8) -0.0025(6) -0.0084(7) -0.0215(7) O1 0.060(2) 0.074(2) 0.065(2) -0.0126(17) -0.0107(16) -0.0155(17) N7 0.075(3) 0.050(2) 0.053(2) -0.007(2) -0.020(2) -0.020(2) N8 0.069(3) 0.047(2) 0.061(2) -0.006(2) -0.033(2) -0.019(2) N9 0.070(3) 0.048(2) 0.045(2) -0.0081(18) -0.0185(18) -0.0140(19) C1 0.087(10) 0.116(11) 0.090(9) -0.049(8) -0.013(7) -0.055(9) C2 0.074(11) 0.117(13) 0.067(10) -0.046(9) -0.005(7) -0.031(9) C3 0.044(6) 0.100(10) 0.046(6) -0.019(6) -0.021(5) -0.018(6) C4 0.047(6) 0.055(6) 0.063(6) -0.034(5) -0.006(5) -0.013(5) C5 0.044(5) 0.027(5) 0.031(4) -0.017(3) -0.003(3) -0.014(5) N1 0.056(5) 0.042(5) 0.052(5) -0.021(4) -0.003(4) -0.021(4) C6 0.050(6) 0.049(5) 0.051(5) -0.016(4) -0.017(4) -0.011(4) C7 0.051(5) 0.072(6) 0.049(5) -0.026(4) -0.016(4) -0.021(4) C8 0.038(5) 0.047(6) 0.046(5) -0.014(4) -0.010(4) -0.008(5) C9 0.058(6) 0.049(6) 0.057(5) -0.017(5) -0.023(4) -0.007(5) C10 0.099(9) 0.060(7) 0.079(7) -0.005(6) -0.047(6) -0.035(6) N2 0.068(7) 0.037(4) 0.030(4) 0.000(4) -0.012(4) -0.025(4) C11 0.052(5) 0.041(5) 0.038(5) -0.004(4) -0.022(4) -0.010(4) C12 0.055(6) 0.031(5) 0.052(5) -0.013(4) -0.023(5) 0.008(5) C18 0.052(5) 0.053(4) 0.039(4) -0.018(4) -0.011(4) -0.010(3) C13 0.044(5) 0.068(5) 0.038(4) -0.014(4) -0.002(3) -0.028(4) C14 0.058(7) 0.078(6) 0.061(6) -0.017(5) -0.018(5) -0.028(5) N3 0.045(5) 0.044(5) 0.042(5) -0.013(4) -0.013(3) -0.014(4) C15 0.039(4) 0.051(4) 0.027(3) -0.013(3) -0.005(3) -0.025(3) C16 0.053(5) 0.053(5) 0.030(5) -0.001(4) -0.004(4) -0.031(4) C17 0.036(4) 0.033(4) 0.029(4) 0.002(3) -0.001(3) -0.014(3) C19 0.051(5) 0.049(4) 0.045(4) -0.024(3) -0.015(3) -0.002(3) C20 0.045(5) 0.035(4) 0.057(5) -0.017(4) -0.015(4) -0.019(4) N4 0.060(5) 0.074(5) 0.063(4) -0.029(4) -0.009(3) -0.034(4) C21 0.063(4) 0.075(4) 0.064(4) -0.026(3) -0.021(3) -0.020(3) C22 0.066(7) 0.065(7) 0.069(7) -0.035(5) -0.028(5) -0.007(6) C23 0.091(8) 0.060(6) 0.037(4) -0.023(4) -0.006(4) -0.012(5) C24 0.052(5) 0.056(5) 0.046(6) -0.021(4) -0.006(4) -0.021(4) C37 0.038(2) 0.046(3) 0.054(3) -0.024(2) -0.022(2) 0.000(2) C38 0.061(3) 0.062(3) 0.047(3) -0.016(2) -0.008(2) -0.029(3) C39 0.049(3) 0.048(3) 0.045(3) -0.020(2) -0.014(2) -0.008(2) C1' 0.026(5) 0.025(4) 0.026(4) -0.019(4) -0.007(4) -0.006(3) C2' 0.031(7) 0.038(6) 0.025(6) -0.017(4) -0.014(4) -0.012(5) C3' 0.061(7) 0.062(8) 0.062(8) -0.018(5) -0.014(5) -0.018(5) C4' 0.069(7) 0.067(7) 0.067(7) -0.018(5) -0.014(5) -0.016(4) C5' 0.052(6) 0.050(7) 0.052(6) -0.016(4) -0.010(4) -0.006(4) N1' 0.039(5) 0.038(5) 0.037(4) -0.011(4) -0.017(3) -0.018(4) C6' 0.049(5) 0.047(5) 0.047(5) -0.011(4) -0.009(4) -0.014(4) C7' 0.054(5) 0.051(5) 0.052(5) -0.012(4) -0.015(4) -0.011(4) C8' 0.034(5) 0.038(5) 0.038(5) -0.011(4) -0.005(4) -0.005(4) C9' 0.039(5) 0.034(5) 0.041(5) -0.004(4) -0.016(4) -0.001(4) C10' 0.027(4) 0.018(4) 0.026(4) -0.006(3) -0.008(3) -0.003(3) N2' 0.035(5) 0.039(5) 0.046(6) -0.003(4) -0.018(4) -0.014(4) C11' 0.060(6) 0.056(6) 0.044(6) -0.016(4) -0.011(4) -0.013(4) C12' 0.041(5) 0.038(5) 0.041(5) -0.013(4) -0.015(4) -0.008(4) C18' 0.056(6) 0.057(6) 0.051(6) -0.015(4) -0.014(4) -0.013(4) C13' 0.025(6) 0.033(5) 0.025(5) 0.000(4) 0.008(4) -0.014(4) C14' 0.018(4) 0.024(5) 0.025(5) -0.006(4) 0.002(3) -0.013(4) N3' 0.045(7) 0.044(7) 0.039(7) -0.008(5) -0.011(4) -0.007(5) C15' 0.098(10) 0.096(9) 0.103(9) -0.028(5) -0.020(5) -0.031(5) C16' 0.048(6) 0.049(6) 0.036(6) -0.012(4) -0.007(4) -0.015(4) C17' 0.027(5) 0.024(5) 0.031(6) -0.001(4) -0.004(4) -0.016(4) C19' 0.051(6) 0.050(6) 0.050(6) -0.013(4) -0.010(4) -0.006(4) C20' 0.050(6) 0.047(6) 0.044(6) -0.008(5) -0.006(5) -0.013(4) N4' 0.047(6) 0.049(5) 0.032(5) -0.022(4) -0.007(4) -0.012(4) C21' 0.055(3) 0.056(3) 0.056(3) -0.0151(11) -0.0105(11) -0.0157(11) C22' 0.044(7) 0.050(7) 0.046(8) -0.014(5) -0.014(5) -0.011(5) C23' 0.059(7) 0.053(7) 0.055(6) -0.025(5) -0.011(4) -0.011(5) C24' 0.070(7) 0.068(7) 0.055(7) -0.021(5) -0.012(5) -0.014(5) C25 0.157(7) 0.083(4) 0.092(4) -0.009(4) -0.057(4) -0.046(4) C26 0.138(6) 0.076(4) 0.095(5) -0.020(4) -0.022(4) -0.053(4) C27 0.118(6) 0.110(5) 0.072(4) -0.022(4) -0.018(4) -0.076(5) C28 0.084(4) 0.119(5) 0.084(4) -0.018(4) -0.012(3) -0.054(4) N5 0.097(4) 0.105(4) 0.083(3) -0.042(3) 0.012(3) -0.057(3) C29 0.101(5) 0.107(5) 0.061(3) -0.016(3) -0.014(3) -0.063(4) C30 0.117(5) 0.093(5) 0.084(4) -0.016(4) -0.019(4) -0.051(4) C31 0.082(4) 0.105(5) 0.076(4) -0.042(3) 0.011(3) -0.048(4) C32 0.054(3) 0.087(4) 0.052(3) -0.025(3) 0.000(2) -0.038(3) C33 0.076(4) 0.054(3) 0.063(3) -0.027(2) -0.003(3) -0.020(3) C34 0.064(3) 0.052(3) 0.054(3) -0.018(2) -0.018(2) -0.007(2) N5 0.052(2) 0.048(2) 0.0392(19) -0.0107(16) -0.0131(16) -0.0108(18) C35 0.048(3) 0.060(3) 0.055(3) -0.018(2) -0.013(2) -0.006(2) C36 0.051(3) 0.082(4) 0.067(3) -0.020(3) -0.022(2) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N9 1.947(4) . ? Cu1 N9 1.947(4) 2_556 ? Cu1 N5 2.034(3) . ? Cu1 N5 2.034(3) 2_556 ? Cu2 N8 1.948(4) . ? Cu2 N7 1.975(4) . ? Cu2 N2' 2.006(6) . ? Cu2 N3 2.011(4) . ? Cu2 N2 2.025(4) . ? Cu2 N3' 2.028(8) . ? Cu2 O1 2.353(3) . ? S1 C38 1.600(5) . ? S2 C37 1.629(5) . ? S3 C39 1.615(5) . ? O1 H1A 0.8499 . ? O1 H1B 0.8499 . ? N7 C38 1.158(5) . ? N8 C37 1.159(5) . ? N9 C39 1.158(5) . ? C1 C2 1.3900 . ? C1 N1 1.3900 . ? C1 H1C 0.9300 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 N1 1.3900 . ? C5 C6 1.462(7) . ? C6 C7 1.318(7) . ? C6 H6A 0.9300 . ? C7 C8 1.461(6) . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 C12 1.3900 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 N2 1.3900 . ? C10 H10A 0.9300 . ? N2 C11 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C18 C19 1.305(7) . ? C18 C17 1.466(5) . ? C18 H18A 0.9300 . ? C13 C14 1.3900 . ? C13 C17 1.3900 . ? C13 H13A 0.9300 . ? C14 N3 1.3900 . ? C14 H14A 0.9300 . ? N3 C15 1.3900 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C19 C20 1.443(5) . ? C19 H19A 0.9300 . ? C20 N4 1.3900 . ? C20 C24 1.3900 . ? N4 C21 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C1' C2' 1.3900 . ? C1' N1' 1.3900 . ? C1' H1'A 0.9300 . ? C2' C3' 1.3900 . ? C2' H2'A 0.9300 . ? C3' C4' 1.3900 . ? C3' H3'A 0.9300 . ? C4' C5' 1.3900 . ? C4' H4'A 0.9300 . ? C5' N1' 1.3900 . ? C5' C6' 1.444(8) . ? C6' C7' 1.313(9) . ? C6' H6'A 0.9300 . ? C7' C8' 1.484(8) . ? C7' H7'A 0.9300 . ? C8' C9' 1.3900 . ? C8' C12' 1.3900 . ? C9' C10' 1.3900 . ? C9' H9'A 0.9300 . ? C10' N2' 1.3900 . ? C10' H10B 0.9300 . ? N2' C11' 1.3900 . ? C11' C12' 1.3900 . ? C11' H11B 0.9300 . ? C12' H12B 0.9300 . ? C18' C19' 1.307(9) . ? C18' C17' 1.471(8) . ? C18' H18B 0.9300 . ? C13' C14' 1.3900 . ? C13' C17' 1.3900 . ? C13' H13B 0.9300 . ? C14' N3' 1.3900 . ? C14' H14B 0.9300 . ? N3' C15' 1.3900 . ? C15' C16' 1.3900 . ? C15' H15B 0.9300 . ? C16' C17' 1.3900 . ? C16' H16B 0.9300 . ? C19' C20' 1.465(8) . ? C19' H19B 0.9300 . ? C20' N4' 1.3900 . ? C20' C24' 1.3900 . ? N4' C21' 1.3900 . ? C21' C22' 1.3900 . ? C21' H21B 0.9300 . ? C22' C23' 1.3900 . ? C22' H22B 0.9300 . ? C23' C24' 1.3900 . ? C23' H23B 0.9300 . ? C24' H24B 0.9300 . ? C25 C29 1.331(8) . ? C25 C26 1.364(7) . ? C25 H25A 0.9300 . ? C26 C27 1.355(8) . ? C26 H26A 0.9300 . ? C27 C28 1.363(8) . ? C27 H27A 0.9300 . ? C28 N5 1.371(6) . ? C28 H28A 0.9300 . ? N5 C29 1.346(7) . ? C29 C30 1.494(6) . ? C30 C31 1.243(6) . ? C30 H30A 0.9300 . ? C31 C32 1.489(5) . ? C31 H31A 0.9300 . ? C32 C36 1.370(6) . ? C32 C33 1.392(6) . ? C33 C34 1.368(5) . ? C33 H33A 0.9300 . ? C34 N5 1.356(5) . ? C34 H34A 0.9300 . ? N5 C35 1.336(5) . ? C35 C36 1.360(5) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? 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 N9 Cu1 N9 180.00(19) . 2_556 ? N9 Cu1 N5 90.61(13) . . ? N9 Cu1 N5 89.39(13) 2_556 . ? N9 Cu1 N5 89.39(13) . 2_556 ? N9 Cu1 N5 90.61(13) 2_556 2_556 ? N5 Cu1 N5 180.0 . 2_556 ? N8 Cu2 N7 169.22(15) . . ? N8 Cu2 N2' 83.7(4) . . ? N7 Cu2 N2' 96.0(4) . . ? N8 Cu2 N3 88.5(3) . . ? N7 Cu2 N3 91.4(3) . . ? N2' Cu2 N3 172.0(5) . . ? N8 Cu2 N2 92.2(3) . . ? N7 Cu2 N2 87.2(3) . . ? N2' Cu2 N2 8.8(5) . . ? N3 Cu2 N2 176.3(4) . . ? N8 Cu2 N3' 91.8(6) . . ? N7 Cu2 N3' 89.2(6) . . ? N2' Cu2 N3' 174.1(7) . . ? N3 Cu2 N3' 6.4(6) . . ? N2 Cu2 N3' 175.6(5) . . ? N8 Cu2 O1 101.51(14) . . ? N7 Cu2 O1 89.22(13) . . ? N2' Cu2 O1 87.3(4) . . ? N3 Cu2 O1 96.0(3) . . ? N2 Cu2 O1 87.5(3) . . ? N3' Cu2 O1 89.9(5) . . ? Cu2 O1 H1A 134.6 . . ? Cu2 O1 H1B 107.4 . . ? H1A O1 H1B 117.4 . . ? C38 N7 Cu2 168.3(4) . . ? C37 N8 Cu2 163.9(4) . . ? C39 N9 Cu1 161.2(4) . . ? C2 C1 N1 120.0 . . ? C2 C1 H1C 120.0 . . ? N1 C1 H1C 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 C6 125.7(7) . . ? N1 C5 C6 114.3(7) . . ? C5 N1 C1 120.0 . . ? C7 C6 C5 126.3(8) . . ? C7 C6 H6A 116.8 . . ? C5 C6 H6A 116.8 . . ? C6 C7 C8 128.9(7) . . ? C6 C7 H7A 115.6 . . ? C8 C7 H7A 115.6 . . ? C9 C8 C12 120.0 . . ? C9 C8 C7 119.2(5) . . ? C12 C8 C7 120.8(5) . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 H10A 120.0 . . ? N2 C10 H10A 120.0 . . ? C11 N2 C10 120.0 . . ? C11 N2 Cu2 119.5(4) . . ? C10 N2 Cu2 120.2(4) . . ? N2 C11 C12 120.0 . . ? N2 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C8 120.0 . . ? C11 C12 H12A 120.0 . . ? C8 C12 H12A 120.0 . . ? C19 C18 C17 129.7(6) . . ? C19 C18 H18A 115.2 . . ? C17 C18 H18A 115.2 . . ? C14 C13 C17 120.0 . . ? C14 C13 H13A 120.0 . . ? C17 C13 H13A 120.0 . . ? C13 C14 N3 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C14 H14A 120.0 . . ? C14 N3 C15 120.0 . . ? C14 N3 Cu2 120.1(4) . . ? C15 N3 Cu2 119.9(4) . . ? C16 C15 N3 120.0 . . ? C16 C15 H15A 120.0 . . ? N3 C15 H15A 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C13 120.0 . . ? C16 C17 C18 121.7(4) . . ? C13 C17 C18 118.3(4) . . ? C18 C19 C20 126.9(6) . . ? C18 C19 H19A 116.6 . . ? C20 C19 H19A 116.6 . . ? N4 C20 C24 120.0 . . ? N4 C20 C19 116.7(4) . . ? C24 C20 C19 123.2(4) . . ? C21 N4 C20 120.0 . . ? N4 C21 C22 120.0 . . ? N4 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C20 120.0 . . ? C23 C24 H24A 120.0 . . ? C20 C24 H24A 120.0 . . ? N8 C37 S2 178.4(4) . . ? N7 C38 S1 179.8(4) . . ? N9 C39 S3 179.6(5) . . ? C2' C1' N1' 120.0 . . ? C2' C1' H1'A 120.0 . . ? N1' C1' H1'A 120.0 . . ? C1' C2' C3' 120.0 . . ? C1' C2' H2'A 120.0 . . ? C3' C2' H2'A 120.0 . . ? C2' C3' C4' 120.0 . . ? C2' C3' H3'A 120.0 . . ? C4' C3' H3'A 120.0 . . ? C5' C4' C3' 120.0 . . ? C5' C4' H4'A 120.0 . . ? C3' C4' H4'A 120.0 . . ? N1' C5' C4' 120.0 . . ? N1' C5' C6' 118.0(9) . . ? C4' C5' C6' 122.0(9) . . ? C5' N1' C1' 120.0 . . ? C7' C6' C5' 126.3(11) . . ? C7' C6' H6'A 116.8 . . ? C5' C6' H6'A 116.8 . . ? C6' C7' C8' 121.3(10) . . ? C6' C7' H7'A 119.3 . . ? C8' C7' H7'A 119.3 . . ? C9' C8' C12' 120.0 . . ? C9' C8' C7' 125.4(7) . . ? C12' C8' C7' 114.5(7) . . ? C10' C9' C8' 120.0 . . ? C10' C9' H9'A 120.0 . . ? C8' C9' H9'A 120.0 . . ? C9' C10' N2' 120.0 . . ? C9' C10' H10B 120.0 . . ? N2' C10' H10B 120.0 . . ? C10' N2' C11' 120.0 . . ? C10' N2' Cu2 122.7(5) . . ? C11' N2' Cu2 117.1(5) . . ? N2' C11' C12' 120.0 . . ? N2' C11' H11B 120.0 . . ? C12' C11' H11B 120.0 . . ? C11' C12' C8' 120.0 . . ? C11' C12' H12B 120.0 . . ? C8' C12' H12B 120.0 . . ? C19' C18' C17' 125.1(11) . . ? C19' C18' H18B 117.5 . . ? C17' C18' H18B 117.5 . . ? C14' C13' C17' 120.0 . . ? C14' C13' H13B 120.0 . . ? C17' C13' H13B 120.0 . . ? C13' C14' N3' 120.0 . . ? C13' C14' H14B 120.0 . . ? N3' C14' H14B 120.0 . . ? C15' N3' C14' 120.0 . . ? C15' N3' Cu2 118.2(7) . . ? C14' N3' Cu2 121.7(7) . . ? N3' C15' C16' 120.0 . . ? N3' C15' H15B 120.0 . . ? C16' C15' H15B 120.0 . . ? C17' C16' C15' 120.0 . . ? C17' C16' H16B 120.0 . . ? C15' C16' H16B 120.0 . . ? C16' C17' C13' 120.0 . . ? C16' C17' C18' 117.9(6) . . ? C13' C17' C18' 122.1(6) . . ? C18' C19' C20' 123.1(10) . . ? C18' C19' H19B 118.5 . . ? C20' C19' H19B 118.5 . . ? N4' C20' C24' 120.0 . . ? N4' C20' C19' 118.2(6) . . ? C24' C20' C19' 120.9(6) . . ? C20' N4' C21' 120.0 . . ? C22' C21' N4' 120.0 . . ? C22' C21' H21B 120.0 . . ? N4' C21' H21B 120.0 . . ? C21' C22' C23' 120.0 . . ? C21' C22' H22B 120.0 . . ? C23' C22' H22B 120.0 . . ? C22' C23' C24' 120.0 . . ? C22' C23' H23B 120.0 . . ? C24' C23' H23B 120.0 . . ? C23' C24' C20' 120.0 . . ? C23' C24' H24B 120.0 . . ? C20' C24' H24B 120.0 . . ? C29 C25 C26 120.5(6) . . ? C29 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C27 C26 C25 119.5(6) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 118.3(5) . . ? C26 C27 H27A 120.9 . . ? C28 C27 H27A 120.9 . . ? C27 C28 N5 122.7(6) . . ? C27 C28 H28A 118.6 . . ? N5 C28 H28A 118.6 . . ? C29 N5 C28 116.5(5) . . ? C25 C29 N5 122.5(5) . . ? C25 C29 C30 117.5(6) . . ? N5 C29 C30 120.0(6) . . ? C31 C30 C29 126.3(6) . . ? C31 C30 H30A 116.8 . . ? C29 C30 H30A 116.8 . . ? C30 C31 C32 127.2(6) . . ? C30 C31 H31A 116.4 . . ? C32 C31 H31A 116.4 . . ? C36 C32 C33 116.6(4) . . ? C36 C32 C31 118.6(5) . . ? C33 C32 C31 124.7(5) . . ? C34 C33 C32 120.5(4) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? N5 C34 C33 122.2(4) . . ? N5 C34 H34A 118.9 . . ? C33 C34 H34A 118.9 . . ? C35 N5 C34 116.5(3) . . ? C35 N5 Cu1 122.6(3) . . ? C34 N5 Cu1 120.8(3) . . ? N5 C35 C36 123.9(4) . . ? N5 C35 H35A 118.0 . . ? C36 C35 H35A 118.0 . . ? C35 C36 C32 120.2(4) . . ? C35 C36 H36A 119.9 . . ? C32 C36 H36A 119.9 . . ? 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 N8 Cu2 N7 C38 -37(2) . . . . ? N2' Cu2 N7 C38 50.5(18) . . . . ? N3 Cu2 N7 C38 -126.4(18) . . . . ? N2 Cu2 N7 C38 50.2(18) . . . . ? N3' Cu2 N7 C38 -132.4(18) . . . . ? O1 Cu2 N7 C38 137.7(18) . . . . ? N7 Cu2 N8 C37 -18.7(16) . . . . ? N2' Cu2 N8 C37 -107.5(12) . . . . ? N3 Cu2 N8 C37 70.8(12) . . . . ? N2 Cu2 N8 C37 -105.5(12) . . . . ? N3' Cu2 N8 C37 76.4(12) . . . . ? O1 Cu2 N8 C37 166.6(11) . . . . ? N5 Cu1 N9 C39 126.2(10) . . . . ? N5 Cu1 N9 C39 -53.8(10) 2_556 . . . ? C3 C4 C5 C6 179.8(9) . . . . ? C6 C5 N1 C1 -179.8(8) . . . . ? C4 C5 C6 C7 4.6(12) . . . . ? N1 C5 C6 C7 -175.6(7) . . . . ? C5 C6 C7 C8 177.6(8) . . . . ? C6 C7 C8 C9 -179.9(7) . . . . ? C6 C7 C8 C12 1.3(11) . . . . ? C7 C8 C9 C10 -178.8(7) . . . . ? C9 C10 N2 Cu2 -174.0(7) . . . . ? N8 Cu2 N2 C11 -47.9(5) . . . . ? N7 Cu2 N2 C11 142.8(5) . . . . ? O1 Cu2 N2 C11 53.5(5) . . . . ? N8 Cu2 N2 C10 126.1(4) . . . . ? N7 Cu2 N2 C10 -43.1(4) . . . . ? O1 Cu2 N2 C10 -132.5(4) . . . . ? C10 N2 C11 C12 0.0 . . . . ? Cu2 N2 C11 C12 174.0(7) . . . . ? C7 C8 C12 C11 178.8(7) . . . . ? C17 C13 C14 N3 0.0 . . . . ? C13 C14 N3 C15 0.0 . . . . ? C13 C14 N3 Cu2 -178.7(7) . . . . ? N8 Cu2 N3 C14 -43.2(4) . . . . ? N7 Cu2 N3 C14 126.0(4) . . . . ? O1 Cu2 N3 C14 -144.6(4) . . . . ? N8 Cu2 N3 C15 138.1(5) . . . . ? N7 Cu2 N3 C15 -52.7(5) . . . . ? O1 Cu2 N3 C15 36.6(5) . . . . ? C14 N3 C15 C16 0.0 . . . . ? Cu2 N3 C15 C16 178.7(7) . . . . ? N3 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C13 0.0 . . . . ? C15 C16 C17 C18 -176.4(7) . . . . ? C14 C13 C17 C16 0.0 . . . . ? C14 C13 C17 C18 176.5(6) . . . . ? C19 C18 C17 C16 -7.1(10) . . . . ? C19 C18 C17 C13 176.4(7) . . . . ? C17 C18 C19 C20 -179.4(6) . . . . ? C18 C19 C20 N4 -170.2(6) . . . . ? C18 C19 C20 C24 13.6(10) . . . . ? C24 C20 N4 C21 0.0 . . . . ? C19 C20 N4 C21 -176.3(7) . . . . ? C19 C20 C24 C23 176.1(7) . . . . ? C3' C4' C5' C6' -177.6(13) . . . . ? C4' C5' N1' C1' 0.0 . . . . ? C6' C5' N1' C1' 177.7(12) . . . . ? C2' C1' N1' C5' 0.0 . . . . ? N1' C5' C6' C7' -4.0(18) . . . . ? C4' C5' C6' C7' 173.6(11) . . . . ? C5' C6' C7' C8' -179.0(11) . . . . ? C6' C7' C8' C9' 3.3(14) . . . . ? C6' C7' C8' C12' 179.8(9) . . . . ? C12' C8' C9' C10' 0.0 . . . . ? C7' C8' C9' C10' 176.3(10) . . . . ? C9' C10' N2' Cu2 175.7(10) . . . . ? N8 Cu2 N2' C10' 133.5(7) . . . . ? N7 Cu2 N2' C10' -35.7(7) . . . . ? O1 Cu2 N2' C10' -124.6(7) . . . . ? N8 Cu2 N2' C11' -50.7(5) . . . . ? N7 Cu2 N2' C11' 140.1(5) . . . . ? O1 Cu2 N2' C11' 51.2(5) . . . . ? C10' N2' C11' C12' 0.0 . . . . ? Cu2 N2' C11' C12' -175.9(9) . . . . ? N2' C11' C12' C8' 0.0 . . . . ? C9' C8' C12' C11' 0.0 . . . . ? C7' C8' C12' C11' -176.7(9) . . . . ? C17' C13' C14' N3' 0.0 . . . . ? C13' C14' N3' C15' 0.0 . . . . ? C13' C14' N3' Cu2 -176.0(15) . . . . ? N8 Cu2 N3' C15' 142.2(8) . . . . ? N7 Cu2 N3' C15' -48.6(8) . . . . ? O1 Cu2 N3' C15' 40.6(8) . . . . ? N8 Cu2 N3' C14' -41.8(10) . . . . ? N7 Cu2 N3' C14' 127.5(10) . . . . ? O1 Cu2 N3' C14' -143.3(10) . . . . ? C14' N3' C15' C16' 0.0 . . . . ? Cu2 N3' C15' C16' 176.2(14) . . . . ? C15' C16' C17' C18' 179.8(13) . . . . ? C14' C13' C17' C16' 0.0 . . . . ? C14' C13' C17' C18' -179.8(13) . . . . ? C19' C18' C17' C16' 170.6(13) . . . . ? C19' C18' C17' C13' -9.7(19) . . . . ? C17' C18' C19' C20' 175.7(12) . . . . ? C18' C19' C20' N4' 19.3(18) . . . . ? C18' C19' C20' C24' -171.5(12) . . . . ? C24' C20' N4' C21' 0.0 . . . . ? C19' C20' N4' C21' 169.3(13) . . . . ? C19' C20' C24' C23' -169.0(14) . . . . ? C29 C25 C26 C27 -0.7(9) . . . . ? C25 C26 C27 C28 -0.2(9) . . . . ? C26 C27 C28 N5 0.4(8) . . . . ? C27 C28 N5 C29 0.3(8) . . . . ? C26 C25 C29 N5 1.5(9) . . . . ? C26 C25 C29 C30 179.8(5) . . . . ? C28 N5 C29 C25 -1.2(8) . . . . ? C28 N5 C29 C30 -179.5(4) . . . . ? C25 C29 C30 C31 -176.6(6) . . . . ? N5 C29 C30 C31 1.7(9) . . . . ? C29 C30 C31 C32 176.2(5) . . . . ? C30 C31 C32 C36 -168.5(5) . . . . ? C30 C31 C32 C33 8.6(8) . . . . ? C36 C32 C33 C34 3.0(6) . . . . ? C31 C32 C33 C34 -174.1(4) . . . . ? C32 C33 C34 N5 -1.3(7) . . . . ? C33 C34 N5 C35 -0.7(6) . . . . ? C33 C34 N5 Cu1 175.3(3) . . . . ? N9 Cu1 N5 C35 40.1(3) . . . . ? N9 Cu1 N5 C35 -139.9(3) 2_556 . . . ? N9 Cu1 N5 C34 -135.6(3) . . . . ? N9 Cu1 N5 C34 44.4(3) 2_556 . . . ? C34 N5 C35 C36 0.8(6) . . . . ? Cu1 N5 C35 C36 -175.1(3) . . . . ? N5 C35 C36 C32 1.1(7) . . . . ? C33 C32 C36 C35 -2.9(6) . . . . ? C31 C32 C36 C35 174.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.773 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.063 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 284291' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H24 Fe N6 O2 S2' _chemical_formula_weight 572.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.845(4) _cell_length_b 10.255(4) _cell_length_c 17.677(7) _cell_angle_alpha 78.625(6) _cell_angle_beta 83.681(6) _cell_angle_gamma 78.665(4) _cell_volume 1363.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1564 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 24.16 _exptl_crystal_description Lamellar _exptl_crystal_colour Dark-red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.824184 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7437 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4751 _reflns_number_gt 3379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4751 _refine_ls_number_parameters 492 _refine_ls_number_restraints 497 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1329 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Fe1 Fe 0.20176(6) 0.49894(5) 0.22567(3) 0.0494(2) Uani 1 1 d . . . S1 S 0.69714(15) 0.29289(13) 0.37812(7) 0.0858(4) Uani 1 1 d . A . S2 S -0.37425(13) 0.75335(11) 0.19112(7) 0.0729(3) Uani 1 1 d . A . N5 N -0.0422(4) 0.5993(3) 0.1812(2) 0.0684(9) Uani 1 1 d . A . N6 N 0.4260(4) 0.3965(3) 0.28260(19) 0.0616(8) Uani 1 1 d . A . C25 C -0.1818(5) 0.6625(3) 0.1849(2) 0.0497(9) Uani 1 1 d . . . C26 C 0.5383(5) 0.3527(3) 0.3226(2) 0.0521(8) Uani 1 1 d . . . O1 O 0.3527(3) 0.6027(2) 0.13537(14) 0.0651(7) Uani 1 1 d . A . H1A H 0.4388 0.6252 0.1517 0.098 Uiso 1 1 d R . . H1B H 0.3264 0.6411 0.0899 0.098 Uiso 1 1 d R . . O2 O 0.0621(3) 0.3907(3) 0.31828(15) 0.0716(7) Uani 1 1 d . A . H2A H 0.1027 0.3505 0.3611 0.107 Uiso 1 1 d R . . H2B H -0.0477 0.3998 0.3168 0.107 Uiso 1 1 d R . . C1 C 0.2305(11) -0.1042(5) -0.1180(4) 0.056(2) Uani 0.671(8) 1 d PGDU A 1 H1C H 0.2054 -0.0115 -0.1361 0.068 Uiso 0.671(8) 1 calc PR A 1 C2 C 0.2288(14) -0.1941(7) -0.1673(3) 0.060(3) Uani 0.671(8) 1 d PGU A 1 H2C H 0.2025 -0.1615 -0.2184 0.072 Uiso 0.671(8) 1 calc PR A 1 C3 C 0.2664(14) -0.3326(6) -0.1402(4) 0.0586(18) Uani 0.671(8) 1 d PGU A 1 H3A H 0.2652 -0.3927 -0.1732 0.070 Uiso 0.671(8) 1 calc PR A 1 C4 C 0.3057(11) -0.3813(4) -0.0639(4) 0.0611(19) Uani 0.671(8) 1 d PGU A 1 H4A H 0.3308 -0.4740 -0.0457 0.073 Uiso 0.671(8) 1 calc PR A 1 N1 N 0.3074(9) -0.2914(6) -0.0146(3) 0.0535(18) Uani 0.671(8) 1 d PGU A 1 C5 C 0.2698(9) -0.1529(5) -0.0417(3) 0.0416(16) Uani 0.671(8) 1 d PGDU A 1 C6 C 0.2750(8) -0.0674(5) 0.0141(3) 0.0509(16) Uani 0.671(8) 1 d PDU A 1 H6A H 0.3154 -0.1091 0.0621 0.061 Uiso 0.671(8) 1 calc PR A 1 C7 C 0.2268(8) 0.0643(5) 0.0017(3) 0.0520(16) Uani 0.671(8) 1 d PDU A 1 H7A H 0.1844 0.1033 -0.0462 0.062 Uiso 0.671(8) 1 calc PR A 1 C8 C 0.2314(7) 0.1585(5) 0.0546(3) 0.0420(16) Uani 0.671(8) 1 d PGDU A 1 C9 C 0.3044(7) 0.1182(4) 0.1256(3) 0.0550(19) Uani 0.671(8) 1 d PGDU A 1 H9A H 0.3573 0.0287 0.1409 0.066 Uiso 0.671(8) 1 calc PR A 1 C10 C 0.2983(9) 0.2116(5) 0.1735(3) 0.0493(16) Uani 0.671(8) 1 d PGU A 1 H10A H 0.3472 0.1846 0.2210 0.059 Uiso 0.671(8) 1 calc PR A 1 N2 N 0.2193(11) 0.3454(5) 0.1505(4) 0.048(2) Uani 0.671(8) 1 d PGU A 1 C11 C 0.1463(11) 0.3857(4) 0.0796(4) 0.065(3) Uani 0.671(8) 1 d PGU A 1 H11A H 0.0934 0.4752 0.0642 0.078 Uiso 0.671(8) 1 calc PR A 1 C12 C 0.1523(8) 0.2923(5) 0.0316(3) 0.0540(18) Uani 0.671(8) 1 d PGDU A 1 H12A H 0.1035 0.3193 -0.0158 0.065 Uiso 0.671(8) 1 calc PR A 1 C18 C 0.1737(7) 1.0140(5) 0.3937(3) 0.0608(16) Uani 0.758(8) 1 d PDU A 1 H18A H 0.1200 1.0976 0.3680 0.073 Uiso 0.758(8) 1 calc PR A 1 C13 C 0.1071(7) 0.9153(4) 0.2872(3) 0.0648(18) Uani 0.758(8) 1 d PGU A 1 H13A H 0.0541 1.0015 0.2648 0.078 Uiso 0.758(8) 1 calc PR A 1 C14 C 0.1148(9) 0.8068(5) 0.2498(3) 0.076(2) Uani 0.758(8) 1 d PGU A 1 H14A H 0.0668 0.8204 0.2024 0.091 Uiso 0.758(8) 1 calc PR A 1 N3 N 0.1941(9) 0.6780(5) 0.2833(3) 0.0532(19) Uani 0.758(8) 1 d PGU A 1 C15 C 0.2657(8) 0.6576(4) 0.3541(3) 0.0572(14) Uani 0.758(8) 1 d PGU A 1 H15A H 0.3188 0.5714 0.3764 0.069 Uiso 0.758(8) 1 calc PR A 1 C16 C 0.2581(7) 0.7661(5) 0.3914(2) 0.0622(15) Uani 0.758(8) 1 d PGDU A 1 H16A H 0.3060 0.7525 0.4388 0.075 Uiso 0.758(8) 1 calc PR A 1 C17 C 0.1788(6) 0.8949(4) 0.3580(3) 0.0534(16) Uani 0.758(8) 1 d PGDU A 1 C19 C 0.2392(7) 1.0104(6) 0.4590(3) 0.0592(15) Uani 0.758(8) 1 d PDU A 1 H19A H 0.2922 0.9255 0.4834 0.071 Uiso 0.758(8) 1 calc PR A 1 C20 C 0.2402(8) 1.1213(5) 0.4986(3) 0.0564(18) Uani 0.758(8) 1 d PGDU A 1 C21 C 0.2979(9) 1.1000(4) 0.5724(3) 0.074(2) Uani 0.758(8) 1 d PGDU A 1 H21A H 0.3398 1.0127 0.5974 0.089 Uiso 0.758(8) 1 calc PR A 1 C22 C 0.2930(10) 1.2092(6) 0.6088(3) 0.080(2) Uani 0.758(8) 1 d PGU A 1 H22A H 0.3316 1.1950 0.6581 0.096 Uiso 0.758(8) 1 calc PR A 1 C23 C 0.2304(10) 1.3397(5) 0.5714(4) 0.079(2) Uani 0.758(8) 1 d PGU A 1 H23A H 0.2271 1.4128 0.5958 0.095 Uiso 0.758(8) 1 calc PR A 1 C24 C 0.1727(8) 1.3610(4) 0.4976(3) 0.076(2) Uani 0.758(8) 1 d PGU A 1 H24A H 0.1308 1.4483 0.4726 0.091 Uiso 0.758(8) 1 calc PR A 1 N4 N 0.1776(7) 1.2517(6) 0.4612(2) 0.0598(16) Uani 0.758(8) 1 d PGU A 1 C6' C 0.2146(16) -0.0026(13) -0.0195(6) 0.058(4) Uani 0.329(8) 1 d PDU A 2 H6'A H 0.1547 0.0800 -0.0435 0.070 Uiso 0.329(8) 1 calc PR A 2 C1' C 0.191(2) -0.1030(11) -0.1362(8) 0.062(5) Uani 0.329(8) 1 d PGDU A 2 H1'A H 0.1457 -0.0183 -0.1637 0.075 Uiso 0.329(8) 1 calc PR A 2 C2' C 0.223(3) -0.2154(15) -0.1721(7) 0.071(7) Uani 0.329(8) 1 d PGU A 2 H2'A H 0.1987 -0.2059 -0.2235 0.085 Uiso 0.329(8) 1 calc PR A 2 C3' C 0.290(3) -0.3420(13) -0.1311(10) 0.056(3) Uani 0.329(8) 1 d PGU A 2 H3'A H 0.3111 -0.4172 -0.1551 0.068 Uiso 0.329(8) 1 calc PR A 2 C4' C 0.325(2) -0.3562(10) -0.0543(9) 0.041(2) Uani 0.329(8) 1 d PGU A 2 H4'A H 0.3704 -0.4409 -0.0269 0.049 Uiso 0.329(8) 1 calc PR A 2 N1' N 0.2936(18) -0.2438(13) -0.0185(6) 0.048(4) Uani 0.329(8) 1 d PGU A 2 C5' C 0.2263(18) -0.1172(11) -0.0594(7) 0.055(5) Uani 0.329(8) 1 d PGDU A 2 C7' C 0.2781(15) -0.0029(10) 0.0459(6) 0.058(3) Uani 0.329(8) 1 d PDU A 2 H7'A H 0.3352 -0.0854 0.0714 0.069 Uiso 0.329(8) 1 calc PR A 2 C8' C 0.2672(13) 0.1172(8) 0.0832(6) 0.040(4) Uani 0.329(8) 1 d PGDU A 2 C9' C 0.3259(18) 0.0945(10) 0.1569(6) 0.072(5) Uani 0.329(8) 1 d PGDU A 2 H9'A H 0.3791 0.0082 0.1792 0.086 Uiso 0.329(8) 1 calc PR A 2 C10' C 0.305(2) 0.2006(14) 0.1973(7) 0.116(8) Uani 0.329(8) 1 d PGU A 2 H10B H 0.3445 0.1854 0.2465 0.139 Uiso 0.329(8) 1 calc PR A 2 N2' N 0.226(2) 0.3295(12) 0.1640(8) 0.049(5) Uani 0.329(8) 1 d PGU A 2 C11' C 0.1671(19) 0.3523(8) 0.0903(8) 0.028(3) Uani 0.329(8) 1 d PGU A 2 H11B H 0.1139 0.4385 0.0680 0.034 Uiso 0.329(8) 1 calc PR A 2 C12' C 0.1878(15) 0.2461(9) 0.0499(6) 0.049(4) Uani 0.329(8) 1 d PGDU A 2 H12B H 0.1485 0.2613 0.0006 0.059 Uiso 0.329(8) 1 calc PR A 2 C18' C 0.227(3) 0.9473(12) 0.4345(9) 0.072(6) Uani 0.242(8) 1 d PDU A 2 H18B H 0.2691 0.9066 0.4824 0.087 Uiso 0.242(8) 1 calc PR A 2 C13' C 0.143(2) 0.8896(10) 0.3128(7) 0.051(5) Uani 0.242(8) 1 d PGDU A 2 H13B H 0.1050 0.9804 0.2931 0.061 Uiso 0.242(8) 1 calc PR A 2 C14' C 0.132(2) 0.7915(13) 0.2704(7) 0.023(3) Uani 0.242(8) 1 d PGU A 2 H14B H 0.0851 0.8167 0.2224 0.028 Uiso 0.242(8) 1 calc PR A 2 N3' N 0.189(3) 0.6556(12) 0.2998(9) 0.044(5) Uani 0.242(8) 1 d PGU A 2 C15' C 0.258(3) 0.6179(9) 0.3716(9) 0.077(4) Uani 0.242(8) 1 d PGU A 2 H15B H 0.2967 0.5271 0.3913 0.093 Uiso 0.242(8) 1 calc PR A 2 C16' C 0.270(2) 0.7160(12) 0.4140(8) 0.069(3) Uani 0.242(8) 1 d PGDU A 2 H16B H 0.3165 0.6908 0.4621 0.083 Uiso 0.242(8) 1 calc PR A 2 C17' C 0.2127(19) 0.8518(10) 0.3846(7) 0.047(5) Uani 0.242(8) 1 d PGDU A 2 C19' C 0.192(2) 1.0791(12) 0.4237(8) 0.062(5) Uani 0.242(8) 1 d PDU A 2 H19B H 0.1564 1.1256 0.3757 0.074 Uiso 0.242(8) 1 calc PR A 2 C20' C 0.205(2) 1.1592(13) 0.4836(8) 0.032(4) Uani 0.242(8) 1 d PGDU A 2 C21' C 0.262(2) 1.0922(9) 0.5551(10) 0.048(5) Uani 0.242(8) 1 d PGDU A 2 H21B H 0.2797 0.9983 0.5669 0.058 Uiso 0.242(8) 1 calc PR A 2 C22' C 0.292(3) 1.1656(16) 0.6089(8) 0.070(7) Uani 0.242(8) 1 d PGU A 2 H22B H 0.3305 1.1207 0.6568 0.084 Uiso 0.242(8) 1 calc PR A 2 C23' C 0.265(2) 1.3060(16) 0.5913(9) 0.050(5) Uani 0.242(8) 1 d PGU A 2 H23B H 0.2858 1.3550 0.6273 0.060 Uiso 0.242(8) 1 calc PR A 2 C24' C 0.208(2) 1.3730(9) 0.5198(10) 0.069(7) Uani 0.242(8) 1 d PGU A 2 H24B H 0.1903 1.4669 0.5079 0.082 Uiso 0.242(8) 1 calc PR A 2 N4' N 0.178(2) 1.2996(14) 0.4659(7) 0.050(5) Uani 0.242(8) 1 d PGU A 2 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 Fe1 0.0540(3) 0.0465(3) 0.0521(3) -0.0193(2) -0.0148(2) -0.0030(2) S1 0.0726(7) 0.1016(9) 0.0775(8) 0.0160(7) -0.0330(6) -0.0190(6) S2 0.0574(6) 0.0732(7) 0.0931(9) -0.0287(6) -0.0181(6) -0.0030(5) N5 0.067(2) 0.063(2) 0.080(2) -0.0290(18) -0.0246(18) 0.0006(17) N6 0.0587(19) 0.068(2) 0.059(2) -0.0179(16) -0.0157(16) -0.0021(16) C25 0.064(2) 0.0438(18) 0.048(2) -0.0140(16) -0.0180(17) -0.0129(17) C26 0.056(2) 0.0494(19) 0.053(2) -0.0126(17) -0.0043(18) -0.0113(17) O1 0.0765(17) 0.0700(16) 0.0575(16) -0.0156(13) -0.0171(13) -0.0225(14) O2 0.0602(16) 0.0899(19) 0.0643(17) -0.0049(15) -0.0135(13) -0.0168(14) C1 0.072(5) 0.051(4) 0.053(4) -0.021(3) -0.014(4) -0.013(3) C2 0.085(6) 0.054(4) 0.046(4) -0.023(3) -0.005(4) -0.006(4) C3 0.065(4) 0.059(3) 0.058(3) -0.030(3) -0.006(3) -0.006(3) C4 0.071(4) 0.061(3) 0.064(4) -0.037(3) -0.007(3) -0.016(3) N1 0.066(3) 0.042(4) 0.056(4) -0.014(3) -0.004(3) -0.012(3) C5 0.043(4) 0.037(4) 0.047(3) -0.016(3) -0.008(3) -0.002(3) C6 0.063(4) 0.048(3) 0.044(3) -0.016(3) -0.008(3) -0.005(3) C7 0.067(4) 0.051(3) 0.043(3) -0.019(3) -0.009(3) -0.008(3) C8 0.049(3) 0.040(4) 0.036(3) -0.004(3) -0.012(3) -0.004(3) C9 0.073(4) 0.041(3) 0.049(5) -0.008(3) -0.016(4) 0.004(3) C10 0.062(4) 0.031(3) 0.058(3) -0.014(2) -0.020(3) -0.001(2) N2 0.059(4) 0.035(3) 0.053(4) -0.015(3) -0.009(3) 0.000(3) C11 0.080(5) 0.049(4) 0.063(5) -0.012(4) -0.017(4) 0.007(4) C12 0.068(4) 0.047(4) 0.046(4) -0.013(3) -0.026(3) 0.008(3) C18 0.074(3) 0.044(3) 0.068(4) -0.018(3) -0.022(3) -0.001(2) C13 0.075(4) 0.045(3) 0.075(4) -0.012(3) -0.033(3) 0.000(3) C14 0.094(5) 0.071(4) 0.067(4) -0.015(4) -0.035(4) -0.007(4) N3 0.069(4) 0.057(4) 0.041(3) -0.011(3) -0.010(3) -0.023(3) C15 0.086(3) 0.048(3) 0.041(3) -0.012(2) -0.012(3) -0.012(3) C16 0.088(3) 0.058(4) 0.042(3) -0.013(3) -0.014(3) -0.008(3) C17 0.064(3) 0.041(3) 0.054(4) -0.009(3) -0.010(3) -0.001(3) C19 0.081(4) 0.048(3) 0.052(3) -0.018(3) -0.010(3) -0.008(3) C20 0.059(4) 0.053(3) 0.057(4) -0.013(3) -0.014(3) -0.001(3) C21 0.103(5) 0.070(4) 0.064(4) -0.031(3) -0.030(4) -0.019(3) C22 0.113(5) 0.077(5) 0.065(4) -0.039(4) -0.014(4) -0.020(4) C23 0.106(6) 0.068(4) 0.071(5) -0.027(4) -0.018(4) -0.012(4) C24 0.099(5) 0.061(4) 0.081(5) -0.043(3) -0.009(4) -0.012(3) N4 0.073(3) 0.053(4) 0.063(3) -0.034(3) 0.000(2) -0.013(3) C6' 0.061(7) 0.054(7) 0.061(7) -0.019(6) -0.004(6) -0.004(6) C1' 0.064(8) 0.068(8) 0.065(8) -0.021(6) -0.018(7) -0.018(6) C2' 0.086(11) 0.068(9) 0.071(10) -0.043(8) -0.004(7) -0.016(7) C3' 0.060(4) 0.055(4) 0.058(4) -0.018(3) -0.007(3) -0.010(3) C4' 0.051(4) 0.033(3) 0.051(4) -0.025(3) -0.006(3) -0.018(3) N1' 0.056(6) 0.051(8) 0.047(7) -0.028(5) -0.002(5) -0.010(6) C5' 0.050(8) 0.054(7) 0.061(9) -0.008(6) -0.024(6) -0.003(6) C7' 0.066(7) 0.048(6) 0.062(7) -0.020(6) -0.013(5) -0.002(5) C8' 0.045(6) 0.026(5) 0.039(7) 0.009(5) -0.003(6) 0.004(4) C9' 0.083(8) 0.070(8) 0.066(9) -0.013(6) -0.017(7) -0.015(6) C10' 0.128(12) 0.107(11) 0.127(11) -0.046(9) -0.010(9) -0.027(9) N2' 0.053(8) 0.062(9) 0.038(6) -0.006(5) -0.014(5) -0.022(6) C11' 0.041(6) 0.013(4) 0.029(6) -0.003(4) -0.020(4) 0.008(4) C12' 0.047(6) 0.057(8) 0.033(6) 0.003(6) -0.026(5) 0.016(6) C18' 0.084(9) 0.068(9) 0.072(10) -0.035(8) -0.012(8) -0.005(7) C13' 0.057(8) 0.026(6) 0.055(9) 0.015(7) -0.023(8) 0.017(6) C14' 0.039(6) 0.009(5) 0.021(5) 0.000(4) -0.026(4) 0.005(4) N3' 0.056(8) 0.025(6) 0.043(8) -0.005(6) 0.015(6) 0.001(6) C15' 0.095(5) 0.074(6) 0.066(6) -0.019(5) -0.007(5) -0.017(5) C16' 0.091(5) 0.063(6) 0.055(6) -0.015(5) -0.007(5) -0.014(5) C17' 0.054(8) 0.050(9) 0.042(8) -0.013(7) -0.021(6) -0.009(7) C19' 0.071(9) 0.053(8) 0.062(9) -0.009(7) -0.009(7) -0.012(7) C20' 0.043(7) 0.017(6) 0.038(6) -0.015(5) -0.009(5) 0.006(5) C21' 0.059(8) 0.053(8) 0.041(9) -0.022(7) -0.028(7) -0.003(6) C22' 0.084(10) 0.064(10) 0.073(11) -0.018(7) -0.023(8) -0.024(8) C23' 0.065(9) 0.042(8) 0.047(8) -0.022(7) -0.025(7) 0.005(7) C24' 0.068(9) 0.074(10) 0.071(11) -0.019(8) -0.035(8) -0.009(7) N4' 0.054(7) 0.040(8) 0.054(8) -0.008(6) -0.007(6) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 2.111(3) . ? Fe1 O2 2.116(3) . ? Fe1 O1 2.119(3) . ? Fe1 N5 2.140(3) . ? Fe1 N2' 2.195(7) . ? Fe1 N2 2.228(3) . ? Fe1 N3' 2.247(8) . ? Fe1 N3 2.256(3) . ? S1 C26 1.620(4) . ? S2 C25 1.616(4) . ? N5 C25 1.159(4) . ? N6 C26 1.155(4) . ? O1 H1A 0.8500 . ? O1 H1B 0.8500 . ? O2 H2A 0.8502 . ? O2 H2B 0.8501 . ? C1 C2 1.3900 . ? C1 C5 1.3900 . ? C1 H1C 0.9300 . ? C2 C3 1.3900 . ? C2 H2C 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 N1 1.3900 . ? C4 H4A 0.9300 . ? N1 C5 1.3900 . ? C5 C6 1.452(5) . ? C6 C7 1.309(6) . ? C6 H6A 0.9300 . ? C7 C8 1.479(5) . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 C12 1.3900 . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 N2 1.3900 . ? C10 H10A 0.9300 . ? N2 C11 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C18 C19 1.306(6) . ? C18 C17 1.474(5) . ? C18 H18A 0.9300 . ? C13 C14 1.3900 . ? C13 C17 1.3900 . ? C13 H13A 0.9300 . ? C14 N3 1.3900 . ? C14 H14A 0.9300 . ? N3 C15 1.3900 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C19 C20 1.449(5) . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 N4 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 N4 1.3900 . ? C24 H24A 0.9300 . ? C6' C7' 1.306(9) . ? C6' C5' 1.469(8) . ? C6' H6'A 0.9300 . ? C1' C2' 1.3900 . ? C1' C5' 1.3900 . ? C1' H1'A 0.9300 . ? C2' C3' 1.3900 . ? C2' H2'A 0.9300 . ? C3' C4' 1.3900 . ? C3' H3'A 0.9300 . ? C4' N1' 1.3900 . ? C4' H4'A 0.9300 . ? N1' C5' 1.3900 . ? C7' C8' 1.492(7) . ? C7' H7'A 0.9300 . ? C8' C9' 1.3900 . ? C8' C12' 1.3900 . ? C9' C10' 1.3900 . ? C9' H9'A 0.9300 . ? C10' N2' 1.3900 . ? C10' H10B 0.9300 . ? N2' C11' 1.3900 . ? C11' C12' 1.3900 . ? C11' H11B 0.9300 . ? C12' H12B 0.9300 . ? C18' C19' 1.305(10) . ? C18' C17' 1.469(8) . ? C18' H18B 0.9300 . ? C13' C14' 1.3900 . ? C13' C17' 1.3900 . ? C13' H13B 0.9300 . ? C14' N3' 1.3900 . ? C14' H14B 0.9300 . ? N3' C15' 1.3900 . ? C15' C16' 1.3900 . ? C15' H15B 0.9300 . ? C16' C17' 1.3900 . ? C16' H16B 0.9300 . ? C19' C20' 1.484(8) . ? C19' H19B 0.9300 . ? C20' C21' 1.3900 . ? C20' N4' 1.3900 . ? C21' C22' 1.3900 . ? C21' H21B 0.9300 . ? C22' C23' 1.3900 . ? C22' H22B 0.9300 . ? C23' C24' 1.3900 . ? C23' H23B 0.9300 . ? C24' N4' 1.3900 . ? C24' H24B 0.9300 . ? 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 N6 Fe1 O2 85.32(12) . . ? N6 Fe1 O1 91.98(12) . . ? O2 Fe1 O1 177.30(9) . . ? N6 Fe1 N5 173.16(13) . . ? O2 Fe1 N5 88.49(13) . . ? O1 Fe1 N5 94.20(12) . . ? N6 Fe1 N2' 88.6(4) . . ? O2 Fe1 N2' 88.6(5) . . ? O1 Fe1 N2' 91.3(5) . . ? N5 Fe1 N2' 94.1(4) . . ? N6 Fe1 N2 93.56(19) . . ? O2 Fe1 N2 93.7(2) . . ? O1 Fe1 N2 86.5(2) . . ? N5 Fe1 N2 89.7(2) . . ? N2' Fe1 N2 6.8(5) . . ? N6 Fe1 N3' 86.1(4) . . ? O2 Fe1 N3' 87.5(5) . . ? O1 Fe1 N3' 92.3(5) . . ? N5 Fe1 N3' 90.7(5) . . ? N2' Fe1 N3' 173.7(5) . . ? N2 Fe1 N3' 178.7(6) . . ? N6 Fe1 N3 90.23(17) . . ? O2 Fe1 N3 95.42(19) . . ? O1 Fe1 N3 84.58(19) . . ? N5 Fe1 N3 87.44(17) . . ? N2' Fe1 N3 175.7(6) . . ? N2 Fe1 N3 170.4(3) . . ? N3' Fe1 N3 8.6(5) . . ? C25 N5 Fe1 154.5(3) . . ? C26 N6 Fe1 169.1(3) . . ? N5 C25 S2 178.5(3) . . ? N6 C26 S1 179.3(4) . . ? Fe1 O1 H1A 112.4 . . ? Fe1 O1 H1B 129.4 . . ? H1A O1 H1B 116.1 . . ? Fe1 O2 H2A 125.1 . . ? Fe1 O2 H2B 118.1 . . ? H2A O2 H2B 115.7 . . ? C2 C1 C5 120.0 . . ? C2 C1 H1C 120.0 . . ? C5 C1 H1C 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2C 120.0 . . ? C3 C2 H2C 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 N1 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C4 H4A 120.0 . . ? C5 N1 C4 120.0 . . ? N1 C5 C1 120.0 . . ? N1 C5 C6 115.9(5) . . ? C1 C5 C6 124.1(5) . . ? C7 C6 C5 124.7(6) . . ? C7 C6 H6A 117.7 . . ? C5 C6 H6A 117.7 . . ? C6 C7 C8 128.0(5) . . ? C6 C7 H7A 116.0 . . ? C8 C7 H7A 116.0 . . ? C9 C8 C12 120.0 . . ? C9 C8 C7 123.2(4) . . ? C12 C8 C7 116.8(4) . . ? C10 C9 C8 120.0 . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 H10A 120.0 . . ? N2 C10 H10A 120.0 . . ? C10 N2 C11 120.0 . . ? C10 N2 Fe1 121.7(3) . . ? C11 N2 Fe1 118.3(3) . . ? N2 C11 C12 120.0 . . ? N2 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C8 120.0 . . ? C11 C12 H12A 120.0 . . ? C8 C12 H12A 120.0 . . ? C19 C18 C17 124.6(5) . . ? C19 C18 H18A 117.7 . . ? C17 C18 H18A 117.7 . . ? C14 C13 C17 120.0 . . ? C14 C13 H13A 120.0 . . ? C17 C13 H13A 120.0 . . ? C13 C14 N3 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C14 H14A 120.0 . . ? C15 N3 C14 120.0 . . ? C15 N3 Fe1 119.2(2) . . ? C14 N3 Fe1 120.8(2) . . ? C16 C15 N3 120.0 . . ? C16 C15 H15A 120.0 . . ? N3 C15 H15A 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C13 120.0 . . ? C16 C17 C18 122.0(3) . . ? C13 C17 C18 117.9(3) . . ? C18 C19 C20 128.5(5) . . ? C18 C19 H19A 115.7 . . ? C20 C19 H19A 115.7 . . ? C21 C20 N4 120.0 . . ? C21 C20 C19 122.0(4) . . ? N4 C20 C19 118.0(4) . . ? C20 C21 C22 120.0 . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? N4 C24 C23 120.0 . . ? N4 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 N4 C20 120.0 . . ? C7' C6' C5' 127.8(11) . . ? C7' C6' H6'A 116.1 . . ? C5' C6' H6'A 116.1 . . ? C2' C1' C5' 120.0 . . ? C2' C1' H1'A 120.0 . . ? C5' C1' H1'A 120.0 . . ? C3' C2' C1' 120.0 . . ? C3' C2' H2'A 120.0 . . ? C1' C2' H2'A 120.0 . . ? C2' C3' C4' 120.0 . . ? C2' C3' H3'A 120.0 . . ? C4' C3' H3'A 120.0 . . ? N1' C4' C3' 120.0 . . ? N1' C4' H4'A 120.0 . . ? C3' C4' H4'A 120.0 . . ? C4' N1' C5' 120.0 . . ? N1' C5' C1' 120.0 . . ? N1' C5' C6' 116.0(9) . . ? C1' C5' C6' 123.7(9) . . ? C6' C7' C8' 125.9(10) . . ? C6' C7' H7'A 117.0 . . ? C8' C7' H7'A 117.0 . . ? C9' C8' C12' 120.0 . . ? C9' C8' C7' 117.5(6) . . ? C12' C8' C7' 122.3(6) . . ? C10' C9' C8' 120.0 . . ? C10' C9' H9'A 120.0 . . ? C8' C9' H9'A 120.0 . . ? C9' C10' N2' 120.0 . . ? C9' C10' H10B 120.0 . . ? N2' C10' H10B 120.0 . . ? C11' N2' C10' 120.0 . . ? C11' N2' Fe1 119.9(6) . . ? C10' N2' Fe1 120.1(6) . . ? C12' C11' N2' 120.0 . . ? C12' C11' H11B 120.0 . . ? N2' C11' H11B 120.0 . . ? C11' C12' C8' 120.0 . . ? C11' C12' H12B 120.0 . . ? C8' C12' H12B 120.0 . . ? C19' C18' C17' 131.4(12) . . ? C19' C18' H18B 114.3 . . ? C17' C18' H18B 114.3 . . ? C14' C13' C17' 120.0 . . ? C14' C13' H13B 120.0 . . ? C17' C13' H13B 120.0 . . ? N3' C14' C13' 120.0 . . ? N3' C14' H14B 120.0 . . ? C13' C14' H14B 120.0 . . ? C14' N3' C15' 120.0 . . ? C14' N3' Fe1 120.1(7) . . ? C15' N3' Fe1 119.4(7) . . ? N3' C15' C16' 120.0 . . ? N3' C15' H15B 120.0 . . ? C16' C15' H15B 120.0 . . ? C17' C16' C15' 120.0 . . ? C17' C16' H16B 120.0 . . ? C15' C16' H16B 120.0 . . ? C16' C17' C13' 120.0 . . ? C16' C17' C18' 115.8(7) . . ? C13' C17' C18' 124.2(7) . . ? C18' C19' C20' 123.8(11) . . ? C18' C19' H19B 118.1 . . ? C20' C19' H19B 118.1 . . ? C21' C20' N4' 120.0 . . ? C21' C20' C19' 119.1(10) . . ? N4' C20' C19' 120.5(10) . . ? C20' C21' C22' 120.0 . . ? C20' C21' H21B 120.0 . . ? C22' C21' H21B 120.0 . . ? C23' C22' C21' 120.0 . . ? C23' C22' H22B 120.0 . . ? C21' C22' H22B 120.0 . . ? C24' C23' C22' 120.0 . . ? C24' C23' H23B 120.0 . . ? C22' C23' H23B 120.0 . . ? C23' C24' N4' 120.0 . . ? C23' C24' H24B 120.0 . . ? N4' C24' H24B 120.0 . . ? C24' N4' C20' 120.0 . . ? 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 O2 Fe1 N5 C25 54.2(7) . . . . ? O1 Fe1 N5 C25 -125.7(7) . . . . ? N2' Fe1 N5 C25 142.7(9) . . . . ? N2 Fe1 N5 C25 147.8(7) . . . . ? N3' Fe1 N5 C25 -33.4(8) . . . . ? N3 Fe1 N5 C25 -41.3(7) . . . . ? O2 Fe1 N6 C26 -68.0(17) . . . . ? O1 Fe1 N6 C26 112.0(17) . . . . ? N2' Fe1 N6 C26 -156.8(18) . . . . ? N2 Fe1 N6 C26 -161.4(17) . . . . ? N3' Fe1 N6 C26 19.8(18) . . . . ? N3 Fe1 N6 C26 27.4(17) . . . . ? C5 C1 C2 C3 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 N1 0.0 . . . . ? C3 C4 N1 C5 0.0 . . . . ? C4 N1 C5 C1 0.0 . . . . ? C4 N1 C5 C6 -180.0(6) . . . . ? C2 C1 C5 N1 0.0 . . . . ? C2 C1 C5 C6 180.0(7) . . . . ? N1 C5 C6 C7 -172.9(6) . . . . ? C1 C5 C6 C7 7.2(9) . . . . ? C5 C6 C7 C8 -178.6(6) . . . . ? C6 C7 C8 C9 5.6(9) . . . . ? C6 C7 C8 C12 -172.1(6) . . . . ? C12 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C10 -177.6(6) . . . . ? C8 C9 C10 N2 0.0 . . . . ? C9 C10 N2 C11 0.0 . . . . ? C9 C10 N2 Fe1 179.0(6) . . . . ? N6 Fe1 N2 C10 26.8(5) . . . . ? O2 Fe1 N2 C10 -58.7(5) . . . . ? O1 Fe1 N2 C10 118.6(4) . . . . ? N5 Fe1 N2 C10 -147.2(5) . . . . ? O2 Fe1 N2 C11 120.3(3) . . . . ? O1 Fe1 N2 C11 -62.4(3) . . . . ? N5 Fe1 N2 C11 31.8(3) . . . . ? C10 N2 C11 C12 0.0 . . . . ? Fe1 N2 C11 C12 -179.0(6) . . . . ? N2 C11 C12 C8 0.0 . . . . ? C9 C8 C12 C11 0.0 . . . . ? C7 C8 C12 C11 177.8(5) . . . . ? C17 C13 C14 N3 0.0 . . . . ? C13 C14 N3 C15 0.0 . . . . ? C13 C14 N3 Fe1 178.2(4) . . . . ? N6 Fe1 N3 C15 -26.7(3) . . . . ? O2 Fe1 N3 C15 58.6(3) . . . . ? O1 Fe1 N3 C15 -118.7(3) . . . . ? N5 Fe1 N3 C15 146.9(3) . . . . ? O2 Fe1 N3 C14 -119.6(3) . . . . ? O1 Fe1 N3 C14 63.1(3) . . . . ? N5 Fe1 N3 C14 -31.4(3) . . . . ? C14 N3 C15 C16 0.0 . . . . ? Fe1 N3 C15 C16 -178.3(4) . . . . ? N3 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C13 0.0 . . . . ? C15 C16 C17 C18 -177.5(5) . . . . ? C14 C13 C17 C16 0.0 . . . . ? C14 C13 C17 C18 177.6(5) . . . . ? C19 C18 C17 C16 -0.9(8) . . . . ? C19 C18 C17 C13 -178.4(5) . . . . ? C17 C18 C19 C20 -179.8(6) . . . . ? C18 C19 C20 C21 172.7(6) . . . . ? C18 C19 C20 N4 -6.0(9) . . . . ? N4 C20 C21 C22 0.0 . . . . ? C19 C20 C21 C22 -178.6(6) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 N4 0.0 . . . . ? C23 C24 N4 C20 0.0 . . . . ? C21 C20 N4 C24 0.0 . . . . ? C19 C20 N4 C24 178.7(6) . . . . ? C5' C1' C2' C3' 0.0 . . . . ? C1' C2' C3' C4' 0.0 . . . . ? C2' C3' C4' N1' 0.0 . . . . ? C3' C4' N1' C5' 0.0 . . . . ? C4' N1' C5' C1' 0.0 . . . . ? C4' N1' C5' C6' -173.7(14) . . . . ? C2' C1' C5' N1' 0.0 . . . . ? C2' C1' C5' C6' 173.2(14) . . . . ? C7' C6' C5' N1' 8.8(19) . . . . ? C7' C6' C5' C1' -164.7(13) . . . . ? C5' C6' C7' C8' 178.1(12) . . . . ? C6' C7' C8' C9' 173.1(12) . . . . ? C6' C7' C8' C12' -1.2(18) . . . . ? C12' C8' C9' C10' 0.0 . . . . ? C7' C8' C9' C10' -174.4(11) . . . . ? C8' C9' C10' N2' 0.0 . . . . ? C9' C10' N2' C11' 0.0 . . . . ? C9' C10' N2' Fe1 -177.7(12) . . . . ? N6 Fe1 N2' C11' -150.4(9) . . . . ? O2 Fe1 N2' C11' 124.3(9) . . . . ? O1 Fe1 N2' C11' -58.4(9) . . . . ? N5 Fe1 N2' C11' 35.9(9) . . . . ? N6 Fe1 N2' C10' 27.3(7) . . . . ? O2 Fe1 N2' C10' -58.0(7) . . . . ? O1 Fe1 N2' C10' 119.3(7) . . . . ? N5 Fe1 N2' C10' -146.4(7) . . . . ? C10' N2' C11' C12' 0.0 . . . . ? Fe1 N2' C11' C12' 177.7(12) . . . . ? N2' C11' C12' C8' 0.0 . . . . ? C9' C8' C12' C11' 0.0 . . . . ? C7' C8' C12' C11' 174.2(11) . . . . ? C17' C13' C14' N3' 0.0 . . . . ? C13' C14' N3' C15' 0.0 . . . . ? C13' C14' N3' Fe1 -172.2(13) . . . . ? N6 Fe1 N3' C14' 144.8(10) . . . . ? O2 Fe1 N3' C14' -129.7(10) . . . . ? O1 Fe1 N3' C14' 53.0(10) . . . . ? N5 Fe1 N3' C14' -41.2(10) . . . . ? N6 Fe1 N3' C15' -27.5(8) . . . . ? O2 Fe1 N3' C15' 58.0(8) . . . . ? O1 Fe1 N3' C15' -119.3(8) . . . . ? N5 Fe1 N3' C15' 146.5(8) . . . . ? C14' N3' C15' C16' 0.0 . . . . ? Fe1 N3' C15' C16' 172.3(13) . . . . ? N3' C15' C16' C17' 0.0 . . . . ? C15' C16' C17' C13' 0.0 . . . . ? C15' C16' C17' C18' 178.7(15) . . . . ? C14' C13' C17' C16' 0.0 . . . . ? C14' C13' C17' C18' -178.6(17) . . . . ? C17' C18' C19' C20' 176.0(18) . . . . ? C18' C19' C20' N4' 175.0(17) . . . . ? N4' C20' C21' C22' 0.0 . . . . ? C19' C20' C21' C22' 173.2(16) . . . . ? C20' C21' C22' C23' 0.0 . . . . ? C21' C22' C23' C24' 0.0 . . . . ? C22' C23' C24' N4' 0.0 . . . . ? C23' C24' N4' C20' 0.0 . . . . ? C21' C20' N4' C24' 0.0 . . . . ? C19' C20' N4' C24' -173.1(16) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.351 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.056 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 284292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 N4 Pb S2' _chemical_formula_weight 505.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.976(6) _cell_length_b 7.232(3) _cell_length_c 13.109(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.374(4) _cell_angle_gamma 90.00 _cell_volume 1507.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4771 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.73 _exptl_crystal_description Block _exptl_crystal_colour Pale-Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 2.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 11.463 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.688759 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6959 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2619 _reflns_number_gt 2290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2sigma(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^)+(0.1322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2619 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Pb1 Pb 0.05266(2) 0.27425(6) 0.60801(3) 0.0279(3) Uani 1 1 d . . . S1 S 0.12208(19) 0.5430(4) 0.9566(2) 0.0378(7) Uani 1 1 d . . . S2 S 0.08736(18) 0.9068(4) 0.7308(2) 0.0341(7) Uani 1 1 d . . . N1 N 0.1967(6) 0.3543(14) 0.5606(7) 0.034(2) Uani 1 1 d . . . N2 N 0.5539(10) 0.406(2) 0.2281(14) 0.094(5) Uani 1 1 d . . . N3 N 0.1334(6) 0.3518(16) 0.7753(7) 0.038(2) Uani 1 1 d . . . N4 N 0.0332(7) 0.6303(14) 0.5928(7) 0.040(2) Uani 1 1 d . . . C1 C 0.6042(13) 0.2602(19) 0.3824(15) 0.061(5) Uani 1 1 d . . . H1 H 0.5943 0.2149 0.4466 0.073 Uiso 1 1 calc R . . C2 C 0.6814(12) 0.247(2) 0.346(2) 0.073(7) Uani 1 1 d . . . H2 H 0.7249 0.1888 0.3862 0.088 Uiso 1 1 calc R . . C3 C 0.6962(10) 0.315(2) 0.2529(18) 0.068(5) Uani 1 1 d . . . H3 H 0.7497 0.3099 0.2304 0.081 Uiso 1 1 calc R . . C4 C 0.6330(13) 0.390(3) 0.1952(15) 0.086(6) Uani 1 1 d . . . H4 H 0.6421 0.4324 0.1302 0.103 Uiso 1 1 calc R . . C5 C 0.5427(8) 0.343(2) 0.3202(13) 0.052(4) Uani 1 1 d . . . C6 C 0.4578(9) 0.370(3) 0.3560(14) 0.065(4) Uani 1 1 d . . . H6 H 0.4173 0.4313 0.3127 0.078 Uiso 1 1 calc R . . C7 C 0.4375(10) 0.315(2) 0.4429(13) 0.057(4) Uani 1 1 d . . . H7 H 0.4788 0.2550 0.4856 0.068 Uiso 1 1 calc R . . C8 C 0.3530(8) 0.337(2) 0.4817(11) 0.047(3) Uani 1 1 d . . . C9 C 0.2847(9) 0.4300(19) 0.4317(10) 0.054(3) Uani 1 1 d . . . H9 H 0.2905 0.4890 0.3697 0.064 Uiso 1 1 calc R . . C10 C 0.2076(8) 0.4352(19) 0.4733(9) 0.043(3) Uani 1 1 d . . . H10 H 0.1628 0.4976 0.4384 0.051 Uiso 1 1 calc R . . C11 C 0.2632(10) 0.2696(18) 0.6119(12) 0.047(3) Uani 1 1 d . . . H11 H 0.2571 0.2165 0.6754 0.057 Uiso 1 1 calc R . . C12 C 0.3388(9) 0.2604(18) 0.5729(15) 0.053(4) Uani 1 1 d . . . H12 H 0.3827 0.1988 0.6102 0.064 Uiso 1 1 calc R . . C13 C 0.1297(6) 0.4309(15) 0.8507(8) 0.028(2) Uani 1 1 d . . . C14 C 0.0546(7) 0.7442(14) 0.6499(11) 0.028(3) 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 Pb1 0.0293(4) 0.0235(4) 0.0312(4) 0.00032(13) 0.0053(2) -0.00080(14) S1 0.0466(18) 0.0340(14) 0.0332(15) -0.0058(12) 0.0054(12) 0.0030(13) S2 0.0336(16) 0.0329(15) 0.0360(15) -0.0017(12) 0.0039(11) 0.0013(12) N1 0.025(5) 0.038(6) 0.038(5) -0.003(4) 0.008(4) 0.002(4) N2 0.081(11) 0.086(12) 0.117(13) -0.011(11) 0.016(9) 0.013(9) N3 0.041(6) 0.049(6) 0.025(5) -0.004(5) 0.002(4) 0.000(5) N4 0.067(7) 0.019(5) 0.036(6) 0.000(4) 0.007(5) 0.002(5) C1 0.070(13) 0.052(9) 0.062(11) -0.008(7) 0.012(9) -0.012(7) C2 0.042(11) 0.047(8) 0.13(2) -0.020(9) -0.021(11) 0.008(7) C3 0.030(8) 0.049(8) 0.129(17) -0.002(11) 0.033(9) 0.007(7) C4 0.095(15) 0.064(11) 0.105(14) -0.001(11) 0.048(12) 0.006(11) C5 0.026(7) 0.052(9) 0.079(11) -0.020(8) 0.014(7) -0.013(6) C6 0.045(9) 0.062(11) 0.087(11) -0.016(10) 0.008(8) -0.013(8) C7 0.045(9) 0.066(10) 0.062(10) -0.004(8) 0.015(7) -0.013(8) C8 0.029(7) 0.054(8) 0.060(9) -0.014(7) 0.008(6) -0.006(6) C9 0.059(9) 0.050(8) 0.055(8) 0.000(6) 0.023(7) -0.015(7) C10 0.036(7) 0.050(8) 0.044(7) 0.000(6) 0.012(5) 0.003(6) C11 0.041(9) 0.058(9) 0.042(8) 0.002(6) 0.002(6) -0.002(6) C12 0.021(8) 0.063(9) 0.077(12) 0.002(7) 0.012(7) 0.009(6) C13 0.017(5) 0.033(6) 0.035(6) 0.003(5) -0.002(4) -0.005(4) C14 0.021(6) 0.023(5) 0.041(8) 0.008(5) 0.010(5) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N3 2.502(9) . ? Pb1 N1 2.506(9) . ? Pb1 N4 2.599(10) . ? Pb1 S2 3.130(3) 1_545 ? S1 C13 1.622(11) . ? S2 C14 1.636(13) . ? S2 Pb1 3.130(3) 1_565 ? N1 C10 1.311(15) . ? N1 C11 1.351(18) . ? N2 C5 1.32(2) . ? N2 C4 1.38(2) . ? N3 C13 1.148(13) . ? N4 C14 1.144(17) . ? C1 C5 1.36(3) . ? C1 C2 1.37(3) . ? C1 H1 0.9300 . ? C2 C3 1.36(3) . ? C2 H2 0.9300 . ? C3 C4 1.32(3) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.49(2) . ? C6 C7 1.28(3) . ? C6 H6 0.9300 . ? C7 C8 1.50(2) . ? C7 H7 0.9300 . ? C8 C12 1.36(2) . ? C8 C9 1.39(2) . ? C9 C10 1.393(17) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.36(2) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 Pb1 N1 75.9(3) . . ? N3 Pb1 N4 83.9(3) . . ? N1 Pb1 N4 81.8(3) . . ? N3 Pb1 S2 71.8(3) . 1_545 ? N1 Pb1 S2 101.6(2) . 1_545 ? N4 Pb1 S2 153.5(2) . 1_545 ? C14 S2 Pb1 104.3(4) . 1_565 ? C10 N1 C11 118.3(11) . . ? C10 N1 Pb1 121.3(8) . . ? C11 N1 Pb1 118.0(9) . . ? C5 N2 C4 117.7(17) . . ? C13 N3 Pb1 143.4(8) . . ? C14 N4 Pb1 129.5(9) . . ? C5 C1 C2 116.6(18) . . ? C5 C1 H1 121.7 . . ? C2 C1 H1 121.7 . . ? C3 C2 C1 121.7(18) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 118.4(16) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 N2 122.0(18) . . ? C3 C4 H4 119.0 . . ? N2 C4 H4 119.0 . . ? N2 C5 C1 123.4(15) . . ? N2 C5 C6 116.7(16) . . ? C1 C5 C6 119.9(16) . . ? C7 C6 C5 123.6(18) . . ? C7 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C6 C7 C8 125.5(18) . . ? C6 C7 H7 117.3 . . ? C8 C7 H7 117.3 . . ? C12 C8 C9 115.1(12) . . ? C12 C8 C7 119.0(14) . . ? C9 C8 C7 125.9(14) . . ? C8 C9 C10 120.8(12) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? N1 C10 C9 121.6(12) . . ? N1 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? N1 C11 C12 121.4(14) . . ? N1 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C8 122.7(14) . . ? C11 C12 H12 118.7 . . ? C8 C12 H12 118.7 . . ? N3 C13 S1 178.6(9) . . ? N4 C14 S2 178.7(12) . . ? 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 Pb1 N1 C10 -146.6(10) . . . . ? N4 Pb1 N1 C10 -60.9(9) . . . . ? S2 Pb1 N1 C10 145.7(9) 1_545 . . . ? N3 Pb1 N1 C11 51.1(9) . . . . ? N4 Pb1 N1 C11 136.8(9) . . . . ? S2 Pb1 N1 C11 -16.6(9) 1_545 . . . ? N1 Pb1 N3 C13 136.1(16) . . . . ? N4 Pb1 N3 C13 53.0(15) . . . . ? S2 Pb1 N3 C13 -116.4(15) 1_545 . . . ? N3 Pb1 N4 C14 -3.0(12) . . . . ? N1 Pb1 N4 C14 -79.6(12) . . . . ? S2 Pb1 N4 C14 20.1(16) 1_545 . . . ? C5 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 -3(3) . . . . ? C2 C3 C4 N2 3(3) . . . . ? C5 N2 C4 C3 0(3) . . . . ? C4 N2 C5 C1 -2(3) . . . . ? C4 N2 C5 C6 177.2(16) . . . . ? C2 C1 C5 N2 1(2) . . . . ? C2 C1 C5 C6 -177.5(14) . . . . ? N2 C5 C6 C7 179.1(17) . . . . ? C1 C5 C6 C7 -2(2) . . . . ? C5 C6 C7 C8 -179.4(16) . . . . ? C6 C7 C8 C12 175.7(17) . . . . ? C6 C7 C8 C9 -3(3) . . . . ? C12 C8 C9 C10 -2(2) . . . . ? C7 C8 C9 C10 177.1(14) . . . . ? C11 N1 C10 C9 2.2(19) . . . . ? Pb1 N1 C10 C9 -160.0(10) . . . . ? C8 C9 C10 N1 0(2) . . . . ? C10 N1 C11 C12 -2.9(19) . . . . ? Pb1 N1 C11 C12 159.9(11) . . . . ? N1 C11 C12 C8 1(2) . . . . ? C9 C8 C12 C11 1(2) . . . . ? C7 C8 C12 C11 -177.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.864 _refine_diff_density_min -4.274 _refine_diff_density_rms 0.413 #===END