# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) the Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Zuo, Jing-Lin' _publ_contact_author_email zuojl@nju.edu.cn _publ_section_title ; Structures and Physical Properties of Oligomeric and Polymeric Metal Complexes Based on Bis(pyridyl)-substituted TTF Ligands and Its Inorganic Analogue ; loop_ _publ_author_name 'Ru Wang' 'Ling-Chen Kang' 'Jing Xiong' 'Xiao-Wei Dou' 'Xiao-Yu Chen' ; Jing-Lin Zuo ; 'Xiaozeng You' # Attachment '- 1-4-all.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 782320' #TrackingRef '- 1-4-all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C110 H84 B2 Co2 N14 O4 S4' _chemical_formula_sum 'C110 H84 B2 Co2 N14 O4 S4' _chemical_formula_weight 1933.67 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' B B 0.0013 0.0007 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.272(7) _cell_length_b 25.084(15) _cell_length_c 20.103(10) _cell_angle_alpha 90.00 _cell_angle_beta 116.91(3) _cell_angle_gamma 90.00 _cell_volume 4619(5) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 0.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9315 _exptl_absorpt_correction_T_max 0.9361 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 '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 24239 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9052 _reflns_number_gt 6229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0400P)^2^+0.6600P] 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 9052 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 B1 B 0.8603(3) 0.84422(12) 0.21261(18) 0.0400(7) Uani 1 1 d . . . H1A H 0.8752 0.8813 0.2022 0.048 Uiso 1 1 d R . . C1 C 0.1050(3) 0.62019(12) 0.00632(17) 0.0492(8) Uani 1 1 d . . . H1 H 0.1024 0.6564 -0.0044 0.059 Uiso 1 1 calc R . . C2 C 0.2211(3) 0.59948(12) 0.05887(16) 0.0485(8) Uani 1 1 d . . . C3 C 0.3597(3) 0.62879(12) 0.10170(16) 0.0438(7) Uani 1 1 d . . . C4 C 0.3749(3) 0.67987(11) 0.09152(15) 0.0428(7) Uani 1 1 d . . . H4 H 0.2961 0.6995 0.0574 0.051 Uiso 1 1 calc R . . C5 C 0.5094(3) 0.70427(12) 0.13214(17) 0.0443(7) Uani 1 1 d . . . H5 H 0.5172 0.7398 0.1212 0.053 Uiso 1 1 calc R . . C6 C 0.4807(3) 0.60254(11) 0.15647(16) 0.0425(7) Uani 1 1 d . . . H6 H 0.4769 0.5665 0.1663 0.051 Uiso 1 1 calc R . . C7 C 0.6044(3) 0.63156(11) 0.19497(17) 0.0491(8) Uani 1 1 d . . . H7 H 0.6827 0.6142 0.2331 0.059 Uiso 1 1 calc R . . C8 C 1.3057(3) 0.71225(11) 0.45986(17) 0.0486(7) Uani 1 1 d . . . H8 H 1.3658 0.7192 0.4375 0.058 Uiso 1 1 calc R . . C9 C 1.3547(3) 0.67787(11) 0.51948(16) 0.0478(7) Uani 1 1 d . . . H9 H 1.4452 0.6615 0.5355 0.057 Uiso 1 1 calc R . . C10 C 1.2738(3) 0.66754(12) 0.55494(18) 0.0491(7) Uani 1 1 d . . . H10 H 1.3064 0.6437 0.5947 0.059 Uiso 1 1 calc R . . C11 C 1.1365(3) 0.69396(11) 0.53030(16) 0.0449(7) Uani 1 1 d . . . H11 H 1.0806 0.6893 0.5556 0.054 Uiso 1 1 calc R . . C12 C 1.0881(3) 0.72662(11) 0.46799(16) 0.0453(7) Uani 1 1 d . . . H12 H 0.9961 0.7421 0.4502 0.054 Uiso 1 1 calc R . . C13 C 1.1704(3) 0.73705(11) 0.43160(17) 0.0446(7) Uani 1 1 d . . . C14 C 1.1299(3) 0.77636(11) 0.37346(16) 0.0435(7) Uani 1 1 d . . . C15 C 1.2144(3) 0.81865(11) 0.37422(15) 0.0420(7) Uani 1 1 d . . . H15 H 1.3091 0.8258 0.4102 0.050 Uiso 1 1 calc R . . C16 C 1.1339(3) 0.84832(11) 0.31233(16) 0.0412(6) Uani 1 1 d . . . C17 C 1.1680(3) 0.89654(10) 0.28440(15) 0.0368(6) Uani 1 1 d . . . C18 C 1.2456(3) 0.93638(12) 0.33487(18) 0.0491(7) Uani 1 1 d . . . H18 H 1.2695 0.9325 0.3851 0.059 Uiso 1 1 calc R . . C19 C 1.2875(3) 0.98201(12) 0.31026(17) 0.0474(7) Uani 1 1 d . . . H19 H 1.3394 1.0087 0.3440 0.057 Uiso 1 1 calc R . . C20 C 1.2517(3) 0.98778(12) 0.23518(17) 0.0455(7) Uani 1 1 d . . . H20 H 1.2797 1.0183 0.2187 0.055 Uiso 1 1 calc R . . C21 C 1.1741(3) 0.94794(11) 0.18471(18) 0.0468(7) Uani 1 1 d . . . H21 H 1.1501 0.9518 0.1345 0.056 Uiso 1 1 calc R . . C22 C 1.1322(3) 0.90231(12) 0.20932(17) 0.0460(7) Uani 1 1 d . . . H22 H 1.0802 0.8757 0.1755 0.055 Uiso 1 1 calc R . . C23 C 0.8315(3) 0.64424(12) 0.10414(17) 0.0478(8) Uani 1 1 d . . . H23 H 0.9111 0.6522 0.1495 0.057 Uiso 1 1 calc R . . C24 C 0.7906(3) 0.59218(11) 0.08063(17) 0.0456(7) Uani 1 1 d . . . H24 H 0.8416 0.5646 0.1128 0.055 Uiso 1 1 calc R . . C25 C 0.6809(3) 0.57966(13) 0.01366(18) 0.0515(8) Uani 1 1 d . . . H25 H 0.6581 0.5440 0.0009 0.062 Uiso 1 1 calc R . . C26 C 0.6041(3) 0.61772(12) -0.03494(17) 0.0474(7) Uani 1 1 d . . . H26 H 0.5294 0.6086 -0.0814 0.057 Uiso 1 1 calc R . . C27 C 0.6366(3) 0.67068(11) -0.01548(16) 0.0435(7) Uani 1 1 d . . . H27 H 0.5862 0.6974 -0.0495 0.052 Uiso 1 1 calc R . . C28 C 0.7454(3) 0.68386(12) 0.05537(16) 0.0454(7) Uani 1 1 d . . . C29 C 0.7685(3) 0.74022(13) 0.07644(18) 0.0507(7) Uani 1 1 d . . . C30 C 0.7506(3) 0.78241(11) 0.02900(18) 0.0486(7) Uani 1 1 d . . . H30 H 0.7262 0.7800 -0.0215 0.058 Uiso 1 1 calc R . . C31 C 0.7749(3) 0.82814(11) 0.06934(16) 0.0422(7) Uani 1 1 d . . . C32 C 0.7644(3) 0.88310(12) 0.04476(16) 0.0446(7) Uani 1 1 d . . . C33 C 0.8215(3) 0.89609(11) -0.00402(17) 0.0461(7) Uani 1 1 d . . . H33 H 0.8644 0.8698 -0.0203 0.055 Uiso 1 1 calc R . . C34 C 0.8145(3) 0.94832(11) -0.02850(16) 0.0443(7) Uani 1 1 d . . . H34 H 0.8527 0.9570 -0.0611 0.053 Uiso 1 1 calc R . . C35 C 0.7504(3) 0.98757(12) -0.00421(17) 0.0496(8) Uani 1 1 d . . . H35 H 0.7457 1.0225 -0.0206 0.060 Uiso 1 1 calc R . . C36 C 0.6933(3) 0.97457(11) 0.04456(17) 0.0444(7) Uani 1 1 d . . . H36 H 0.6504 1.0008 0.0608 0.053 Uiso 1 1 calc R . . C37 C 0.7003(3) 0.92234(11) 0.06905(15) 0.0421(7) Uani 1 1 d . . . H37 H 0.6621 0.9136 0.1017 0.051 Uiso 1 1 calc R . . C38 C 0.5425(3) 0.71914(11) 0.31232(16) 0.0456(7) Uani 1 1 d . . . H38 H 0.6426 0.7130 0.3351 0.055 Uiso 1 1 calc R . . C39 C 0.4493(3) 0.68265(11) 0.32089(16) 0.0418(7) Uani 1 1 d . . . H39 H 0.4872 0.6521 0.3494 0.050 Uiso 1 1 calc R . . C40 C 0.2997(3) 0.69180(11) 0.28682(16) 0.0435(7) Uani 1 1 d . . . H40 H 0.2374 0.6674 0.2926 0.052 Uiso 1 1 calc R . . C41 C 0.2432(3) 0.73744(12) 0.24417(17) 0.0454(7) Uani 1 1 d . . . H41 H 0.1430 0.7436 0.2214 0.054 Uiso 1 1 calc R . . C42 C 0.3363(3) 0.77392(11) 0.23559(16) 0.0419(6) Uani 1 1 d . . . H42 H 0.2985 0.8045 0.2071 0.050 Uiso 1 1 calc R . . C43 C 0.4860(3) 0.76477(12) 0.26966(17) 0.0483(7) Uani 1 1 d . . . C44 C 0.5731(3) 0.80568(12) 0.26020(18) 0.0476(7) Uani 1 1 d . . . C45 C 0.5529(3) 0.85960(12) 0.25849(16) 0.0453(7) Uani 1 1 d . . . H45 H 0.4796 0.8770 0.2650 0.054 Uiso 1 1 calc R . . C46 C 0.6569(3) 0.88327(11) 0.24571(17) 0.0452(7) Uani 1 1 d . . . C47 C 0.6893(3) 0.93850(11) 0.23958(16) 0.0427(7) Uani 1 1 d . . . C48 C 0.5682(3) 0.97094(11) 0.20182(16) 0.0417(7) Uani 1 1 d . . . H48 H 0.4749 0.9563 0.1813 0.050 Uiso 1 1 calc R . . C49 C 0.5865(3) 1.02520(12) 0.19473(17) 0.0485(7) Uani 1 1 d . . . H49 H 0.5054 1.0469 0.1695 0.058 Uiso 1 1 calc R . . C50 C 0.7259(3) 1.04702(12) 0.22539(17) 0.0498(8) Uani 1 1 d . . . H50 H 0.7381 1.0833 0.2206 0.060 Uiso 1 1 calc R . . C51 C 0.8471(3) 1.01458(11) 0.26316(16) 0.0444(7) Uani 1 1 d . . . H51 H 0.9404 1.0292 0.2837 0.053 Uiso 1 1 calc R . . C52 C 0.8288(3) 0.96032(12) 0.27025(18) 0.0508(8) Uani 1 1 d . . . H52 H 0.9098 0.9386 0.2955 0.061 Uiso 1 1 calc R . . C53 C 0.9435(3) 0.64786(12) 0.32511(17) 0.0438(7) Uani 1 1 d . . . C54 C 1.0268(3) 0.60188(11) 0.36880(17) 0.0485(7) Uani 1 1 d . . . H54A H 1.0175 0.5729 0.3358 0.073 Uiso 1 1 calc R . . H54B H 0.9896 0.5912 0.4028 0.073 Uiso 1 1 calc R . . H54C H 1.1278 0.6115 0.3964 0.073 Uiso 1 1 calc R . . C55 C 0.0350(3) 0.52328(11) 0.00520(15) 0.0385(6) Uani 1 1 d . . . Co1 Co 0.81521(4) 0.727582(14) 0.24670(2) 0.03865(11) Uani 1 1 d . . . N1 N 0.9982(2) 0.77901(9) 0.31285(14) 0.0471(6) Uani 1 1 d . . . N2 N 1.0005(2) 0.82360(8) 0.27475(12) 0.0330(5) Uani 1 1 d . . . N3 N 0.8061(2) 0.75891(9) 0.14583(13) 0.0424(6) Uani 1 1 d . . . N4 N 0.8116(2) 0.81232(9) 0.14142(13) 0.0425(6) Uani 1 1 d . . . N5 N 0.6894(2) 0.79536(9) 0.24790(12) 0.0384(5) Uani 1 1 d . . . N6 N 0.7400(2) 0.84346(9) 0.23908(13) 0.0379(5) Uani 1 1 d . . . N7 N 0.6234(2) 0.68255(9) 0.18301(13) 0.0400(5) Uani 1 1 d . . . O1 O 0.8557(2) 0.67319(7) 0.34034(10) 0.0408(4) Uani 1 1 d . . . O2 O 0.9634(2) 0.66465(7) 0.27249(11) 0.0453(5) Uani 1 1 d . . . S1 S -0.04518(8) 0.58079(3) -0.04395(4) 0.0580(2) Uani 1 1 d . . . S2 S 0.21437(8) 0.53228(3) 0.07293(4) 0.0501(2) 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 B1 0.0349(15) 0.0309(17) 0.0440(19) 0.0052(13) 0.0090(14) -0.0093(12) C1 0.0370(15) 0.0385(16) 0.0509(19) -0.0008(13) 0.0014(14) -0.0127(12) C2 0.0448(16) 0.0411(17) 0.0405(17) -0.0124(13) 0.0026(13) -0.0174(13) C3 0.0400(15) 0.0471(18) 0.0408(17) -0.0128(13) 0.0152(13) -0.0163(13) C4 0.0400(15) 0.0465(18) 0.0355(16) -0.0037(12) 0.0116(12) -0.0073(13) C5 0.0377(15) 0.0439(17) 0.0464(17) -0.0003(13) 0.0146(14) -0.0054(12) C6 0.0378(15) 0.0386(16) 0.0451(17) 0.0018(12) 0.0134(13) -0.0151(12) C7 0.0340(14) 0.0386(16) 0.0461(18) 0.0008(13) -0.0069(13) -0.0088(12) C8 0.0504(17) 0.0427(16) 0.0406(16) 0.0083(13) 0.0100(14) -0.0054(13) C9 0.0491(16) 0.0416(17) 0.0386(16) 0.0126(13) 0.0076(14) -0.0070(13) C10 0.0442(16) 0.0415(16) 0.0505(19) 0.0044(13) 0.0116(14) -0.0100(13) C11 0.0386(15) 0.0427(16) 0.0458(17) -0.0031(13) 0.0125(13) -0.0133(12) C12 0.0409(15) 0.0443(17) 0.0419(16) -0.0025(13) 0.0111(13) -0.0124(13) C13 0.0405(15) 0.0375(16) 0.0492(18) 0.0017(13) 0.0145(14) -0.0111(12) C14 0.0386(14) 0.0411(16) 0.0406(16) 0.0001(13) 0.0088(12) -0.0062(12) C15 0.0344(14) 0.0438(16) 0.0383(16) -0.0125(12) 0.0081(12) -0.0200(12) C16 0.0353(14) 0.0416(16) 0.0398(16) -0.0066(12) 0.0111(13) -0.0101(12) C17 0.0255(12) 0.0386(15) 0.0421(16) -0.0050(12) 0.0118(12) -0.0086(11) C18 0.0416(16) 0.0463(17) 0.0505(19) -0.0049(14) 0.0130(14) -0.0117(13) C19 0.0408(15) 0.0502(18) 0.0479(18) -0.0098(14) 0.0172(14) -0.0124(13) C20 0.0438(16) 0.0412(16) 0.0477(18) 0.0127(13) 0.0174(14) -0.0012(13) C21 0.0424(16) 0.0372(16) 0.0540(19) 0.0123(13) 0.0158(15) 0.0014(13) C22 0.0456(16) 0.0407(16) 0.0448(18) 0.0053(13) 0.0144(14) -0.0008(13) C23 0.0505(17) 0.0503(18) 0.0469(18) -0.0144(14) 0.0258(15) 0.0171(14) C24 0.0515(17) 0.0412(17) 0.0443(17) -0.0042(13) 0.0218(14) 0.0133(13) C25 0.0513(18) 0.0427(17) 0.0518(19) -0.0160(14) 0.0156(15) -0.0111(14) C26 0.0459(16) 0.0524(18) 0.0418(17) -0.0218(14) 0.0180(14) -0.0150(14) C27 0.0432(15) 0.0364(15) 0.0464(17) -0.0158(13) 0.0164(13) 0.0043(12) C28 0.0353(14) 0.0475(17) 0.0455(17) -0.0154(13) 0.0113(13) -0.0063(12) C29 0.0440(16) 0.0538(19) 0.0465(18) -0.0049(14) 0.0136(14) -0.0003(14) C30 0.0440(16) 0.0426(17) 0.0527(19) 0.0058(14) 0.0160(14) 0.0159(13) C31 0.0420(15) 0.0334(14) 0.0396(16) 0.0033(12) 0.0084(13) 0.0023(12) C32 0.0457(16) 0.0468(17) 0.0355(16) 0.0137(13) 0.0133(13) 0.0075(13) C33 0.0481(17) 0.0407(16) 0.0497(18) 0.0156(13) 0.0222(15) 0.0183(13) C34 0.0494(16) 0.0449(17) 0.0365(16) 0.0156(12) 0.0175(13) 0.0130(13) C35 0.0520(18) 0.0422(17) 0.0521(19) 0.0202(14) 0.0214(15) 0.0180(13) C36 0.0387(14) 0.0404(16) 0.0459(17) 0.0128(13) 0.0118(13) 0.0112(12) C37 0.0359(14) 0.0433(16) 0.0352(15) 0.0208(12) 0.0056(12) 0.0115(12) C38 0.0438(15) 0.0455(17) 0.0464(18) -0.0047(13) 0.0195(14) -0.0106(13) C39 0.0384(15) 0.0467(17) 0.0433(17) -0.0143(13) 0.0211(13) -0.0154(12) C40 0.0404(15) 0.0456(16) 0.0482(17) -0.0188(14) 0.0232(13) -0.0166(13) C41 0.0353(14) 0.0469(18) 0.0524(18) -0.0097(14) 0.0185(13) -0.0062(12) C42 0.0361(14) 0.0450(16) 0.0416(16) -0.0043(13) 0.0150(12) 0.0006(12) C43 0.0398(15) 0.0459(18) 0.0498(18) -0.0096(14) 0.0120(14) -0.0084(13) C44 0.0349(15) 0.0459(18) 0.0562(19) -0.0073(14) 0.0155(14) -0.0034(13) C45 0.0443(16) 0.0504(19) 0.0357(16) -0.0064(13) 0.0133(13) 0.0041(13) C46 0.0455(16) 0.0427(16) 0.0432(18) -0.0107(13) 0.0165(14) -0.0022(13) C47 0.0458(16) 0.0412(16) 0.0395(17) -0.0058(12) 0.0177(13) -0.0008(13) C48 0.0427(15) 0.0419(16) 0.0456(17) 0.0070(13) 0.0244(14) 0.0072(13) C49 0.0466(17) 0.0448(17) 0.0438(18) 0.0148(13) 0.0114(14) 0.0159(14) C50 0.065(2) 0.0362(16) 0.0464(19) 0.0026(13) 0.0242(17) -0.0041(14) C51 0.0447(16) 0.0388(16) 0.0473(18) -0.0146(13) 0.0188(14) -0.0109(13) C52 0.0522(17) 0.0486(18) 0.0520(19) -0.0143(14) 0.0238(15) -0.0166(14) C53 0.0409(16) 0.0398(16) 0.0435(18) -0.0032(13) 0.0126(14) -0.0094(13) C54 0.0492(17) 0.0433(17) 0.0457(18) 0.0015(13) 0.0151(14) 0.0011(14) C55 0.0367(14) 0.0391(15) 0.0367(15) -0.0054(12) 0.0138(12) -0.0099(11) Co1 0.03044(18) 0.0346(2) 0.0488(2) -0.00225(16) 0.01615(17) -0.01030(15) N1 0.0367(12) 0.0416(14) 0.0507(15) 0.0081(11) 0.0091(11) -0.0131(10) N2 0.0341(11) 0.0304(12) 0.0383(13) -0.0028(9) 0.0199(10) -0.0137(9) N3 0.0419(13) 0.0347(13) 0.0438(14) -0.0021(10) 0.0135(11) -0.0015(10) N4 0.0351(12) 0.0407(14) 0.0424(14) 0.0006(11) 0.0095(11) -0.0072(10) N5 0.0346(11) 0.0393(12) 0.0356(13) -0.0055(10) 0.0111(10) -0.0086(10) N6 0.0326(11) 0.0345(13) 0.0393(13) -0.0036(9) 0.0098(10) -0.0090(9) N7 0.0347(12) 0.0345(13) 0.0428(14) -0.0032(10) 0.0104(11) -0.0090(10) O1 0.0448(11) 0.0367(10) 0.0360(11) -0.0074(8) 0.0138(9) -0.0104(9) O2 0.0388(10) 0.0429(11) 0.0418(12) 0.0022(9) 0.0073(9) -0.0032(8) S1 0.0456(4) 0.0478(5) 0.0443(4) 0.0122(3) -0.0115(3) -0.0184(3) S2 0.0434(4) 0.0415(4) 0.0440(4) 0.0031(3) 0.0008(3) -0.0159(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 B1 N2 1.508(4) . ? B1 N4 1.513(4) . ? B1 N6 1.551(4) . ? B1 H1A 0.9800 . ? C1 C2 1.292(4) . ? C1 S1 1.722(3) . ? C1 H1 0.9300 . ? C2 C3 1.483(4) . ? C2 S2 1.716(3) . ? C3 C4 1.318(4) . ? C3 C6 1.397(4) . ? C4 C5 1.389(4) . ? C4 H4 0.9300 . ? C5 N7 1.277(4) . ? C5 H5 0.9300 . ? C6 C7 1.361(4) . ? C6 H6 0.9300 . ? C7 N7 1.332(4) . ? C7 H7 0.9300 . ? C8 C9 1.374(4) . ? C8 C13 1.389(4) . ? C8 H8 0.9300 . ? C9 C10 1.342(4) . ? C9 H9 0.9300 . ? C10 C11 1.429(4) . ? C10 H10 0.9300 . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 C13 1.370(4) . ? C12 H12 0.9300 . ? C13 C14 1.439(4) . ? C14 N1 1.352(4) . ? C14 C15 1.366(4) . ? C15 C16 1.362(4) . ? C15 H15 0.9300 . ? C16 N2 1.377(3) . ? C16 C17 1.442(4) . ? C17 C18 1.390(4) . ? C17 C22 1.390(4) . ? C18 C19 1.390(4) . ? C18 H18 0.9300 . ? C19 C20 1.390(4) . ? C19 H19 0.9300 . ? C20 C21 1.390(4) . ? C20 H20 0.9300 . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.387(4) . ? C23 C28 1.395(4) . ? C23 H23 0.9300 . ? C24 C25 1.345(4) . ? C24 H24 0.9300 . ? C25 C26 1.338(4) . ? C25 H25 0.9300 . ? C26 C27 1.383(4) . ? C26 H26 0.9300 . ? C27 C28 1.395(4) . ? C27 H27 0.9300 . ? C28 C29 1.464(4) . ? C29 N3 1.352(4) . ? C29 C30 1.380(4) . ? C30 C31 1.361(4) . ? C30 H30 0.9300 . ? C31 N4 1.380(4) . ? C31 C32 1.452(4) . ? C32 C33 1.390(4) . ? C32 C37 1.390(4) . ? C33 C34 1.390(4) . ? C33 H33 0.9300 . ? C34 C35 1.390(4) . ? C34 H34 0.9300 . ? C35 C36 1.390(4) . ? C35 H35 0.9300 . ? C36 C37 1.390(4) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.390(4) . ? C38 C43 1.390(4) . ? C38 H38 0.9300 . ? C39 C40 1.390(4) . ? C39 H39 0.9300 . ? C40 C41 1.390(4) . ? C40 H40 0.9300 . ? C41 C42 1.390(4) . ? C41 H41 0.9300 . ? C42 C43 1.390(4) . ? C42 H42 0.9300 . ? C43 C44 1.430(4) . ? C44 N5 1.349(4) . ? C44 C45 1.366(4) . ? C45 C46 1.345(4) . ? C45 H45 0.9300 . ? C46 N6 1.359(4) . ? C46 C47 1.443(4) . ? C47 C48 1.390(4) . ? C47 C52 1.390(4) . ? C48 C49 1.390(4) . ? C48 H48 0.9300 . ? C49 C50 1.390(4) . ? C49 H49 0.9300 . ? C50 C51 1.390(4) . ? C50 H50 0.9300 . ? C51 C52 1.390(4) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 O2 1.238(4) . ? C53 O1 1.249(3) . ? C53 C54 1.468(4) . ? C53 Co1 2.518(3) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C55 1.338(5) 3_565 ? C55 S1 1.732(3) . ? C55 S2 1.740(3) . ? Co1 O2 2.089(2) . ? Co1 N7 2.124(2) . ? Co1 N3 2.137(3) . ? Co1 N5 2.142(3) . ? Co1 N1 2.169(2) . ? Co1 O1 2.207(2) . ? N1 N2 1.362(3) . ? N3 N4 1.346(3) . ? N5 N6 1.357(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 B1 N4 112.7(2) . . ? N2 B1 N6 108.8(2) . . ? N4 B1 N6 110.1(2) . . ? N2 B1 H1A 108.6 . . ? N4 B1 H1A 108.5 . . ? N6 B1 H1A 108.1 . . ? C2 C1 S1 120.0(2) . . ? C2 C1 H1 120.0 . . ? S1 C1 H1 120.0 . . ? C1 C2 C3 124.3(3) . . ? C1 C2 S2 116.0(2) . . ? C3 C2 S2 119.4(2) . . ? C4 C3 C6 117.1(2) . . ? C4 C3 C2 122.8(3) . . ? C6 C3 C2 120.1(3) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N7 C5 C4 126.2(3) . . ? N7 C5 H5 116.9 . . ? C4 C5 H5 116.9 . . ? C7 C6 C3 117.7(3) . . ? C7 C6 H6 121.2 . . ? C3 C6 H6 121.2 . . ? N7 C7 C6 125.9(3) . . ? N7 C7 H7 117.1 . . ? C6 C7 H7 117.1 . . ? C9 C8 C13 122.8(3) . . ? C9 C8 H8 118.6 . . ? C13 C8 H8 118.6 . . ? C10 C9 C8 121.0(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 118.5(3) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 118.8(3) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 122.6(3) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C8 116.2(3) . . ? C12 C13 C14 122.9(3) . . ? C8 C13 C14 120.4(3) . . ? N1 C14 C15 110.1(3) . . ? N1 C14 C13 124.7(2) . . ? C15 C14 C13 125.1(3) . . ? C16 C15 C14 107.1(2) . . ? C16 C15 H15 126.5 . . ? C14 C15 H15 126.5 . . ? C15 C16 N2 107.3(2) . . ? C15 C16 C17 131.3(2) . . ? N2 C16 C17 121.4(2) . . ? C18 C17 C22 120.0(3) . . ? C18 C17 C16 118.6(3) . . ? C22 C17 C16 121.3(2) . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.0(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C17 120.0(3) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C24 C23 C28 115.7(3) . . ? C24 C23 H23 122.2 . . ? C28 C23 H23 122.2 . . ? C25 C24 C23 123.2(3) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 119.5(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 119.7(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 120.6(3) . . ? C27 C28 C29 118.3(3) . . ? C23 C28 C29 121.1(3) . . ? N3 C29 C30 109.5(3) . . ? N3 C29 C28 124.5(3) . . ? C30 C29 C28 126.0(3) . . ? C31 C30 C29 107.7(3) . . ? C31 C30 H30 126.2 . . ? C29 C30 H30 126.2 . . ? C30 C31 N4 105.8(2) . . ? C30 C31 C32 129.2(3) . . ? N4 C31 C32 125.0(3) . . ? C33 C32 C37 120.0(3) . . ? C33 C32 C31 118.2(3) . . ? C37 C32 C31 121.8(3) . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0(3) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 120.0(3) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C32 120.0(3) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C39 C38 C43 120.0(3) . . ? C39 C38 H38 120.0 . . ? C43 C38 H38 120.0 . . ? C38 C39 C40 120.0(3) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.0(3) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.0(3) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C38 120.0(3) . . ? C42 C43 C44 115.8(3) . . ? C38 C43 C44 124.1(3) . . ? N5 C44 C45 108.8(3) . . ? N5 C44 C43 123.1(3) . . ? C45 C44 C43 128.0(3) . . ? C46 C45 C44 108.5(3) . . ? C46 C45 H45 125.8 . . ? C44 C45 H45 125.8 . . ? C45 C46 N6 106.4(3) . . ? C45 C46 C47 132.4(3) . . ? N6 C46 C47 121.2(3) . . ? C48 C47 C52 120.0(3) . . ? C48 C47 C46 115.1(3) . . ? C52 C47 C46 124.8(3) . . ? C49 C48 C47 120.0(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.0(3) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C51 120.0(3) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.0(3) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C47 120.0(3) . . ? C51 C52 H52 120.0 . . ? C47 C52 H52 120.0 . . ? O2 C53 O1 116.9(3) . . ? O2 C53 C54 120.1(3) . . ? O1 C53 C54 122.9(3) . . ? O2 C53 Co1 55.75(15) . . ? O1 C53 Co1 61.20(15) . . ? C54 C53 Co1 175.6(2) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C55 C55 S1 123.7(3) 3_565 . ? C55 C55 S2 122.7(3) 3_565 . ? S1 C55 S2 113.58(15) . . ? O2 Co1 N7 96.92(9) . . ? O2 Co1 N3 103.16(9) . . ? N7 Co1 N3 89.60(10) . . ? O2 Co1 N5 166.53(8) . . ? N7 Co1 N5 91.66(10) . . ? N3 Co1 N5 87.20(9) . . ? O2 Co1 N1 88.01(10) . . ? N7 Co1 N1 174.77(10) . . ? N3 Co1 N1 90.96(10) . . ? N5 Co1 N1 83.17(10) . . ? O2 Co1 O1 59.08(8) . . ? N7 Co1 O1 87.18(9) . . ? N3 Co1 O1 161.31(8) . . ? N5 Co1 O1 111.28(9) . . ? N1 Co1 O1 93.91(9) . . ? O2 Co1 C53 29.35(9) . . ? N7 Co1 C53 92.00(10) . . ? N3 Co1 C53 132.22(10) . . ? N5 Co1 C53 140.41(10) . . ? N1 Co1 C53 91.48(10) . . ? O1 Co1 C53 29.73(8) . . ? C14 N1 N2 106.4(2) . . ? C14 N1 Co1 139.42(19) . . ? N2 N1 Co1 111.99(16) . . ? N1 N2 C16 109.1(2) . . ? N1 N2 B1 119.7(2) . . ? C16 N2 B1 129.8(2) . . ? N4 N3 C29 106.1(2) . . ? N4 N3 Co1 116.35(17) . . ? C29 N3 Co1 136.2(2) . . ? N3 N4 C31 110.8(2) . . ? N3 N4 B1 118.0(2) . . ? C31 N4 B1 131.1(2) . . ? C44 N5 N6 106.1(2) . . ? C44 N5 Co1 137.96(19) . . ? N6 N5 Co1 115.80(17) . . ? N5 N6 C46 110.2(2) . . ? N5 N6 B1 117.9(2) . . ? C46 N6 B1 131.1(2) . . ? C5 N7 C7 113.5(2) . . ? C5 N7 Co1 121.34(19) . . ? C7 N7 Co1 124.99(18) . . ? C53 O1 Co1 89.07(18) . . ? C53 O2 Co1 94.90(19) . . ? C1 S1 C55 94.29(14) . . ? C2 S2 C55 96.07(13) . . ? 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 S1 C1 C2 C3 175.3(2) . . . . ? S1 C1 C2 S2 0.8(4) . . . . ? C1 C2 C3 C4 2.6(5) . . . . ? S2 C2 C3 C4 176.9(2) . . . . ? C1 C2 C3 C6 -178.5(3) . . . . ? S2 C2 C3 C6 -4.2(4) . . . . ? C6 C3 C4 C5 3.0(4) . . . . ? C2 C3 C4 C5 -178.1(3) . . . . ? C3 C4 C5 N7 -3.7(5) . . . . ? C4 C3 C6 C7 0.1(4) . . . . ? C2 C3 C6 C7 -178.9(3) . . . . ? C3 C6 C7 N7 -3.3(5) . . . . ? C13 C8 C9 C10 -1.7(5) . . . . ? C8 C9 C10 C11 -1.3(4) . . . . ? C9 C10 C11 C12 3.9(4) . . . . ? C10 C11 C12 C13 -3.9(4) . . . . ? C11 C12 C13 C8 1.0(4) . . . . ? C11 C12 C13 C14 -171.3(3) . . . . ? C9 C8 C13 C12 1.8(4) . . . . ? C9 C8 C13 C14 174.4(3) . . . . ? C12 C13 C14 N1 -51.9(5) . . . . ? C8 C13 C14 N1 136.1(3) . . . . ? C12 C13 C14 C15 122.8(3) . . . . ? C8 C13 C14 C15 -49.2(5) . . . . ? N1 C14 C15 C16 -0.4(4) . . . . ? C13 C14 C15 C16 -175.7(3) . . . . ? C14 C15 C16 N2 0.2(3) . . . . ? C14 C15 C16 C17 -179.2(3) . . . . ? C15 C16 C17 C18 -40.6(5) . . . . ? N2 C16 C17 C18 140.1(3) . . . . ? C15 C16 C17 C22 135.7(3) . . . . ? N2 C16 C17 C22 -43.7(4) . . . . ? C22 C17 C18 C19 0.0(4) . . . . ? C16 C17 C18 C19 176.3(3) . . . . ? C17 C18 C19 C20 0.0(4) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C19 C20 C21 C22 0.0(4) . . . . ? C20 C21 C22 C17 0.0(4) . . . . ? C18 C17 C22 C21 0.0(4) . . . . ? C16 C17 C22 C21 -176.2(3) . . . . ? C28 C23 C24 C25 3.7(4) . . . . ? C23 C24 C25 C26 0.2(5) . . . . ? C24 C25 C26 C27 -1.0(5) . . . . ? C25 C26 C27 C28 -2.2(4) . . . . ? C26 C27 C28 C23 6.3(4) . . . . ? C26 C27 C28 C29 -174.8(3) . . . . ? C24 C23 C28 C27 -6.9(4) . . . . ? C24 C23 C28 C29 174.4(3) . . . . ? C27 C28 C29 N3 144.3(3) . . . . ? C23 C28 C29 N3 -36.8(5) . . . . ? C27 C28 C29 C30 -33.1(5) . . . . ? C23 C28 C29 C30 145.7(3) . . . . ? N3 C29 C30 C31 -1.0(4) . . . . ? C28 C29 C30 C31 176.7(3) . . . . ? C29 C30 C31 N4 1.7(3) . . . . ? C29 C30 C31 C32 -177.5(3) . . . . ? C30 C31 C32 C33 -43.1(5) . . . . ? N4 C31 C32 C33 137.8(3) . . . . ? C30 C31 C32 C37 137.4(3) . . . . ? N4 C31 C32 C37 -41.7(4) . . . . ? C37 C32 C33 C34 0.0(4) . . . . ? C31 C32 C33 C34 -179.6(3) . . . . ? C32 C33 C34 C35 0.0(5) . . . . ? C33 C34 C35 C36 0.0(5) . . . . ? C34 C35 C36 C37 0.0(5) . . . . ? C35 C36 C37 C32 0.0(4) . . . . ? C33 C32 C37 C36 0.0(4) . . . . ? C31 C32 C37 C36 179.6(3) . . . . ? C43 C38 C39 C40 0.0(4) . . . . ? C38 C39 C40 C41 0.0(4) . . . . ? C39 C40 C41 C42 0.0(4) . . . . ? C40 C41 C42 C43 0.0(4) . . . . ? C41 C42 C43 C38 0.0(4) . . . . ? C41 C42 C43 C44 -177.4(3) . . . . ? C39 C38 C43 C42 0.0(4) . . . . ? C39 C38 C43 C44 177.2(3) . . . . ? C42 C43 C44 N5 -139.9(3) . . . . ? C38 C43 C44 N5 42.8(5) . . . . ? C42 C43 C44 C45 37.0(5) . . . . ? C38 C43 C44 C45 -140.3(3) . . . . ? N5 C44 C45 C46 -0.5(4) . . . . ? C43 C44 C45 C46 -177.7(3) . . . . ? C44 C45 C46 N6 0.4(3) . . . . ? C44 C45 C46 C47 -178.9(3) . . . . ? C45 C46 C47 C48 -39.5(5) . . . . ? N6 C46 C47 C48 141.2(3) . . . . ? C45 C46 C47 C52 138.3(4) . . . . ? N6 C46 C47 C52 -41.0(4) . . . . ? C52 C47 C48 C49 0.0(4) . . . . ? C46 C47 C48 C49 177.9(3) . . . . ? C47 C48 C49 C50 0.0(5) . . . . ? C48 C49 C50 C51 0.0(5) . . . . ? C49 C50 C51 C52 0.0(5) . . . . ? C50 C51 C52 C47 0.0(5) . . . . ? C48 C47 C52 C51 0.0(4) . . . . ? C46 C47 C52 C51 -177.7(3) . . . . ? O1 C53 Co1 O2 178.6(3) . . . . ? C54 C53 Co1 O2 20(3) . . . . ? O2 C53 Co1 N7 100.60(17) . . . . ? O1 C53 Co1 N7 -80.78(16) . . . . ? C54 C53 Co1 N7 120(3) . . . . ? O2 C53 Co1 N3 9.3(2) . . . . ? O1 C53 Co1 N3 -172.05(13) . . . . ? C54 C53 Co1 N3 29(3) . . . . ? O2 C53 Co1 N5 -164.36(14) . . . . ? O1 C53 Co1 N5 14.3(2) . . . . ? C54 C53 Co1 N5 -145(3) . . . . ? O2 C53 Co1 N1 -83.31(17) . . . . ? O1 C53 Co1 N1 95.31(16) . . . . ? C54 C53 Co1 N1 -64(3) . . . . ? O2 C53 Co1 O1 -178.6(3) . . . . ? C54 C53 Co1 O1 -159(3) . . . . ? C15 C14 N1 N2 0.3(3) . . . . ? C13 C14 N1 N2 175.7(3) . . . . ? C15 C14 N1 Co1 161.1(2) . . . . ? C13 C14 N1 Co1 -23.6(5) . . . . ? O2 Co1 N1 C14 -31.5(3) . . . . ? N7 Co1 N1 C14 129.3(9) . . . . ? N3 Co1 N1 C14 -134.6(3) . . . . ? N5 Co1 N1 C14 138.3(3) . . . . ? O1 Co1 N1 C14 27.3(3) . . . . ? C53 Co1 N1 C14 -2.4(3) . . . . ? O2 Co1 N1 N2 128.53(19) . . . . ? N7 Co1 N1 N2 -70.7(11) . . . . ? N3 Co1 N1 N2 25.40(19) . . . . ? N5 Co1 N1 N2 -61.67(19) . . . . ? O1 Co1 N1 N2 -172.65(18) . . . . ? C53 Co1 N1 N2 157.68(19) . . . . ? C14 N1 N2 C16 -0.2(3) . . . . ? Co1 N1 N2 C16 -166.78(18) . . . . ? C14 N1 N2 B1 -167.8(3) . . . . ? Co1 N1 N2 B1 25.6(3) . . . . ? C15 C16 N2 N1 -0.1(3) . . . . ? C17 C16 N2 N1 179.4(3) . . . . ? C15 C16 N2 B1 166.0(3) . . . . ? C17 C16 N2 B1 -14.5(5) . . . . ? N4 B1 N2 N1 -77.4(3) . . . . ? N6 B1 N2 N1 45.0(3) . . . . ? N4 B1 N2 C16 117.9(3) . . . . ? N6 B1 N2 C16 -119.7(3) . . . . ? C30 C29 N3 N4 -0.2(3) . . . . ? C28 C29 N3 N4 -177.9(3) . . . . ? C30 C29 N3 Co1 165.4(2) . . . . ? C28 C29 N3 Co1 -12.4(5) . . . . ? O2 Co1 N3 N4 -135.26(18) . . . . ? N7 Co1 N3 N4 127.73(19) . . . . ? N5 Co1 N3 N4 36.04(18) . . . . ? N1 Co1 N3 N4 -47.07(19) . . . . ? O1 Co1 N3 N4 -152.3(2) . . . . ? C53 Co1 N3 N4 -139.94(17) . . . . ? O2 Co1 N3 C29 60.2(3) . . . . ? N7 Co1 N3 C29 -36.8(3) . . . . ? N5 Co1 N3 C29 -128.5(3) . . . . ? N1 Co1 N3 C29 148.4(3) . . . . ? O1 Co1 N3 C29 43.2(4) . . . . ? C53 Co1 N3 C29 55.6(3) . . . . ? C29 N3 N4 C31 1.3(3) . . . . ? Co1 N3 N4 C31 -167.61(18) . . . . ? C29 N3 N4 B1 -176.4(2) . . . . ? Co1 N3 N4 B1 14.7(3) . . . . ? C30 C31 N4 N3 -1.9(3) . . . . ? C32 C31 N4 N3 177.4(3) . . . . ? C30 C31 N4 B1 175.4(3) . . . . ? C32 C31 N4 B1 -5.3(5) . . . . ? N2 B1 N4 N3 50.0(3) . . . . ? N6 B1 N4 N3 -71.7(3) . . . . ? N2 B1 N4 C31 -127.2(3) . . . . ? N6 B1 N4 C31 111.2(3) . . . . ? C45 C44 N5 N6 0.3(3) . . . . ? C43 C44 N5 N6 177.7(3) . . . . ? C45 C44 N5 Co1 174.9(2) . . . . ? C43 C44 N5 Co1 -7.7(5) . . . . ? O2 Co1 N5 C44 -83.8(4) . . . . ? N7 Co1 N5 C44 46.0(3) . . . . ? N3 Co1 N5 C44 135.5(3) . . . . ? N1 Co1 N5 C44 -133.2(3) . . . . ? O1 Co1 N5 C44 -41.6(3) . . . . ? C53 Co1 N5 C44 -49.2(3) . . . . ? O2 Co1 N5 N6 90.5(4) . . . . ? N7 Co1 N5 N6 -139.78(18) . . . . ? N3 Co1 N5 N6 -50.26(18) . . . . ? N1 Co1 N5 N6 41.05(18) . . . . ? O1 Co1 N5 N6 132.60(17) . . . . ? C53 Co1 N5 N6 125.07(19) . . . . ? C44 N5 N6 C46 0.0(3) . . . . ? Co1 N5 N6 C46 -176.02(18) . . . . ? C44 N5 N6 B1 -171.3(2) . . . . ? Co1 N5 N6 B1 12.8(3) . . . . ? C45 C46 N6 N5 -0.3(3) . . . . ? C47 C46 N6 N5 179.2(2) . . . . ? C45 C46 N6 B1 169.4(3) . . . . ? C47 C46 N6 B1 -11.2(5) . . . . ? N2 B1 N6 N5 -70.1(3) . . . . ? N4 B1 N6 N5 53.8(3) . . . . ? N2 B1 N6 C46 120.9(3) . . . . ? N4 B1 N6 C46 -115.2(3) . . . . ? C4 C5 N7 C7 0.6(5) . . . . ? C4 C5 N7 Co1 -174.3(2) . . . . ? C6 C7 N7 C5 2.9(5) . . . . ? C6 C7 N7 Co1 177.6(2) . . . . ? O2 Co1 N7 C5 -153.6(2) . . . . ? N3 Co1 N7 C5 -50.4(2) . . . . ? N5 Co1 N7 C5 36.8(2) . . . . ? N1 Co1 N7 C5 45.7(11) . . . . ? O1 Co1 N7 C5 148.0(2) . . . . ? C53 Co1 N7 C5 177.3(2) . . . . ? O2 Co1 N7 C7 32.0(3) . . . . ? N3 Co1 N7 C7 135.2(3) . . . . ? N5 Co1 N7 C7 -137.6(3) . . . . ? N1 Co1 N7 C7 -128.6(10) . . . . ? O1 Co1 N7 C7 -26.4(3) . . . . ? C53 Co1 N7 C7 3.0(3) . . . . ? O2 C53 O1 Co1 1.3(2) . . . . ? C54 C53 O1 Co1 178.1(2) . . . . ? O2 Co1 O1 C53 -0.79(15) . . . . ? N7 Co1 O1 C53 99.01(17) . . . . ? N3 Co1 O1 C53 18.6(3) . . . . ? N5 Co1 O1 C53 -170.30(15) . . . . ? N1 Co1 O1 C53 -86.12(17) . . . . ? O1 C53 O2 Co1 -1.4(3) . . . . ? C54 C53 O2 Co1 -178.3(2) . . . . ? N7 Co1 O2 C53 -81.71(18) . . . . ? N3 Co1 O2 C53 -172.92(16) . . . . ? N5 Co1 O2 C53 47.5(4) . . . . ? N1 Co1 O2 C53 96.56(17) . . . . ? O1 Co1 O2 C53 0.80(15) . . . . ? C2 C1 S1 C55 0.8(3) . . . . ? C55 C55 S1 C1 175.2(4) 3_565 . . . ? S2 C55 S1 C1 -2.05(19) . . . . ? C1 C2 S2 C55 -1.9(3) . . . . ? C3 C2 S2 C55 -176.7(2) . . . . ? C55 C55 S2 C2 -174.9(4) 3_565 . . . ? S1 C55 S2 C2 2.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.405 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.045 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 782321' #TrackingRef '- 1-4-all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H84 B2 Co2 N14 Ni O4 S4' _chemical_formula_sum 'C108 H84 B2 Co2 N14 Ni O4 S4' _chemical_formula_weight 1968.34 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.3052(8) _cell_length_b 25.198(2) _cell_length_c 20.1921(13) _cell_angle_alpha 90.00 _cell_angle_beta 117.570(3) _cell_angle_gamma 90.00 _cell_volume 4647.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8431 _exptl_absorpt_correction_T_max 0.9014 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 '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 24757 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9102 _reflns_number_gt 6691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0500P)^2^+1.9900P] 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 9102 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 B1 B 0.8489(3) 0.84575(14) 0.20918(19) 0.0330(7) Uani 1 1 d . . . H1A H 0.8632 0.8826 0.1985 0.040 Uiso 1 1 d R . . C1 C 0.0927(4) 0.61235(14) 0.00342(19) 0.0543(10) Uani 1 1 d . . . H1 H 0.0907 0.6484 -0.0072 0.065 Uiso 1 1 calc R . . C2 C 0.2181(4) 0.59185(14) 0.05875(18) 0.0479(9) Uani 1 1 d . . . C3 C 0.3528(3) 0.62330(12) 0.10218(17) 0.0365(7) Uani 1 1 d . . . C4 C 0.3646(3) 0.67433(13) 0.08864(17) 0.0436(8) Uani 1 1 d . . . H4 H 0.2847 0.6917 0.0512 0.052 Uiso 1 1 calc R . . C5 C 0.4929(4) 0.70180(12) 0.12907(17) 0.0409(7) Uani 1 1 d . . . H5 H 0.4957 0.7374 0.1178 0.049 Uiso 1 1 calc R . . C6 C 0.4734(3) 0.60050(13) 0.15861(17) 0.0424(8) Uani 1 1 d . . . H6 H 0.4717 0.5650 0.1709 0.051 Uiso 1 1 calc R . . C7 C 0.5981(4) 0.63078(13) 0.19737(18) 0.0453(8) Uani 1 1 d . . . H7 H 0.6780 0.6148 0.2366 0.054 Uiso 1 1 calc R . . C8 C 1.3001(4) 0.71398(13) 0.45945(18) 0.0443(8) Uani 1 1 d . . . H8 H 1.3597 0.7201 0.4370 0.053 Uiso 1 1 calc R . . C9 C 1.3462(4) 0.67986(13) 0.5200(2) 0.0515(9) Uani 1 1 d . . . H9 H 1.4357 0.6626 0.5368 0.062 Uiso 1 1 calc R . . C10 C 1.2648(4) 0.67123(13) 0.55501(19) 0.0511(9) Uani 1 1 d . . . H10 H 1.2980 0.6486 0.5960 0.061 Uiso 1 1 calc R . . C11 C 1.1308(4) 0.69642(13) 0.52938(18) 0.0442(8) Uani 1 1 d . . . H11 H 1.0742 0.6908 0.5536 0.053 Uiso 1 1 calc R . . C12 C 1.0805(4) 0.72958(13) 0.46844(17) 0.0429(8) Uani 1 1 d . . . H12 H 0.9895 0.7458 0.4512 0.052 Uiso 1 1 calc R . . C13 C 1.1659(3) 0.73887(12) 0.43245(16) 0.0379(7) Uani 1 1 d . . . C14 C 1.1214(3) 0.77830(12) 0.37269(16) 0.0359(7) Uani 1 1 d . . . C15 C 1.2063(4) 0.82067(12) 0.37184(18) 0.0452(8) Uani 1 1 d . . . H15 H 1.3020 0.8279 0.4072 0.054 Uiso 1 1 calc R . . C16 C 1.1238(3) 0.84951(12) 0.30975(18) 0.0376(7) Uani 1 1 d . . . C17 C 1.1614(3) 0.89717(12) 0.28118(17) 0.0368(7) Uani 1 1 d . . . C18 C 1.2385(4) 0.93794(13) 0.33048(19) 0.0468(8) Uani 1 1 d . . . H18 H 1.2620 0.9349 0.3807 0.056 Uiso 1 1 calc R . . C19 C 1.2799(4) 0.98211(13) 0.30647(19) 0.0487(8) Uani 1 1 d . . . H19 H 1.3332 1.0085 0.3404 0.058 Uiso 1 1 calc R . . C20 C 1.2435(4) 0.98793(13) 0.23242(19) 0.0477(8) Uani 1 1 d . . . H20 H 1.2724 1.0181 0.2162 0.057 Uiso 1 1 calc R . . C21 C 1.1663(4) 0.95012(13) 0.18343(18) 0.0452(8) Uani 1 1 d . . . H21 H 1.1386 0.9549 0.1330 0.054 Uiso 1 1 calc R . . C22 C 1.1275(4) 0.90420(13) 0.20664(19) 0.0447(8) Uani 1 1 d . . . H22 H 1.0780 0.8776 0.1721 0.054 Uiso 1 1 calc R . . C23 C 0.8139(4) 0.64398(13) 0.10168(19) 0.0448(8) Uani 1 1 d . . . H23 H 0.8903 0.6522 0.1484 0.054 Uiso 1 1 calc R . . C24 C 0.7796(4) 0.59063(14) 0.08066(18) 0.0465(8) Uani 1 1 d . . . H24 H 0.8313 0.5635 0.1135 0.056 Uiso 1 1 calc R . . C25 C 0.6701(4) 0.57926(14) 0.01176(18) 0.0470(8) Uani 1 1 d . . . H25 H 0.6450 0.5440 -0.0014 0.056 Uiso 1 1 calc R . . C26 C 0.5957(4) 0.61794(13) -0.0387(2) 0.0481(8) Uani 1 1 d . . . H26 H 0.5248 0.6096 -0.0868 0.058 Uiso 1 1 calc R . . C27 C 0.6290(4) 0.66969(13) -0.01614(18) 0.0436(8) Uani 1 1 d . . . H27 H 0.5769 0.6964 -0.0498 0.052 Uiso 1 1 calc R . . C28 C 0.7358(4) 0.68406(13) 0.05392(17) 0.0423(7) Uani 1 1 d . . . C29 C 0.7595(3) 0.73945(13) 0.07389(17) 0.0397(7) Uani 1 1 d . . . C30 C 0.7427(3) 0.78231(13) 0.02715(17) 0.0410(7) Uani 1 1 d . . . H30 H 0.7186 0.7804 -0.0232 0.049 Uiso 1 1 calc R . . C31 C 0.7678(3) 0.82728(12) 0.06798(16) 0.0343(6) Uani 1 1 d . . . C32 C 0.7605(4) 0.88259(15) 0.04289(19) 0.0490(9) Uani 1 1 d . . . C33 C 0.8191(4) 0.89591(14) -0.00407(18) 0.0470(8) Uani 1 1 d . . . H33 H 0.8613 0.8697 -0.0203 0.056 Uiso 1 1 calc R . . C34 C 0.8159(3) 0.94753(12) -0.02734(18) 0.0417(8) Uani 1 1 d . . . H34 H 0.8547 0.9555 -0.0596 0.050 Uiso 1 1 calc R . . C35 C 0.7572(4) 0.98683(14) -0.00404(19) 0.0510(9) Uani 1 1 d . . . H35 H 0.7587 1.0218 -0.0184 0.061 Uiso 1 1 calc R . . C36 C 0.6957(4) 0.97403(13) 0.04114(17) 0.0439(8) Uani 1 1 d . . . H36 H 0.6524 1.0007 0.0561 0.053 Uiso 1 1 calc R . . C37 C 0.6960(4) 0.92310(14) 0.0649(2) 0.0563(9) Uani 1 1 d . . . H37 H 0.6535 0.9155 0.0956 0.068 Uiso 1 1 calc R . . C38 C 0.5348(4) 0.72131(14) 0.3122(2) 0.0513(9) Uani 1 1 d . . . H38 H 0.6358 0.7164 0.3360 0.062 Uiso 1 1 calc R . . C39 C 0.4446(4) 0.68455(14) 0.31979(19) 0.0470(8) Uani 1 1 d . . . H39 H 0.4855 0.6544 0.3485 0.056 Uiso 1 1 calc R . . C40 C 0.2956(4) 0.69110(12) 0.28611(19) 0.0458(8) Uani 1 1 d . . . H40 H 0.2363 0.6656 0.2918 0.055 Uiso 1 1 calc R . . C41 C 0.2349(4) 0.73577(13) 0.24377(18) 0.0438(8) Uani 1 1 d . . . H41 H 0.1342 0.7411 0.2209 0.053 Uiso 1 1 calc R . . C42 C 0.3243(4) 0.77178(14) 0.23607(18) 0.0472(8) Uani 1 1 d . . . H42 H 0.2828 0.8020 0.2075 0.057 Uiso 1 1 calc R . . C43 C 0.4739(3) 0.76577(12) 0.26857(17) 0.0398(7) Uani 1 1 d . . . C44 C 0.5642(3) 0.80728(12) 0.25670(17) 0.0356(7) Uani 1 1 d . . . C45 C 0.5440(4) 0.86078(13) 0.25602(17) 0.0424(7) Uani 1 1 d . . . H45 H 0.4722 0.8783 0.2634 0.051 Uiso 1 1 calc R . . C46 C 0.6502(3) 0.88385(12) 0.24235(18) 0.0388(7) Uani 1 1 d . . . C47 C 0.6773(4) 0.93962(13) 0.23599(19) 0.0444(8) Uani 1 1 d . . . C48 C 0.5601(4) 0.97335(13) 0.19782(18) 0.0451(8) Uani 1 1 d . . . H48 H 0.4655 0.9598 0.1776 0.054 Uiso 1 1 calc R . . C49 C 0.5799(4) 1.02698(14) 0.1888(2) 0.0512(9) Uani 1 1 d . . . H49 H 0.5005 1.0493 0.1629 0.061 Uiso 1 1 calc R . . C50 C 0.7207(4) 1.04571(14) 0.2195(2) 0.0493(8) Uani 1 1 d . . . H50 H 0.7359 1.0813 0.2133 0.059 Uiso 1 1 calc R . . C51 C 0.8393(4) 1.01410(14) 0.25891(19) 0.0503(9) Uani 1 1 d . . . H51 H 0.9334 1.0282 0.2798 0.060 Uiso 1 1 calc R . . C52 C 0.8181(4) 0.96144(13) 0.26728(18) 0.0435(8) Uani 1 1 d . . . H52 H 0.8986 0.9398 0.2942 0.052 Uiso 1 1 calc R . . C53 C 0.9368(4) 0.65117(13) 0.32048(18) 0.0416(8) Uani 1 1 d . . . C54 C 1.0242(4) 0.60473(13) 0.36927(18) 0.0466(8) Uani 1 1 d . . . H54A H 1.0681 0.5853 0.3438 0.070 Uiso 1 1 d R . . H54B H 0.9607 0.5816 0.3789 0.070 Uiso 1 1 d R . . H54C H 1.0995 0.6181 0.4157 0.070 Uiso 1 1 d R . . Co1 Co 0.80502(4) 0.728249(15) 0.24452(2) 0.02992(11) Uani 1 1 d . . . N1 N 0.9906(2) 0.78069(9) 0.31174(13) 0.0309(5) Uani 1 1 d . . . N2 N 0.9927(3) 0.82451(10) 0.27307(13) 0.0400(6) Uani 1 1 d . . . N3 N 0.7970(3) 0.75832(10) 0.14267(13) 0.0354(6) Uani 1 1 d . . . N4 N 0.8027(3) 0.81208(10) 0.13832(14) 0.0376(6) Uani 1 1 d . . . N5 N 0.6796(3) 0.79586(10) 0.24535(13) 0.0329(5) Uani 1 1 d . . . N6 N 0.7313(3) 0.84357(9) 0.23590(13) 0.0324(5) Uani 1 1 d . . . N7 N 0.6108(3) 0.68083(10) 0.18229(15) 0.0395(6) Uani 1 1 d . . . Ni1 Ni 0.0000 0.5000 0.0000 0.04865(17) Uani 1 2 d S . . O1 O 0.8529(3) 0.67360(9) 0.33976(13) 0.0496(6) Uani 1 1 d . . . O2 O 0.9559(2) 0.66547(9) 0.27136(12) 0.0444(5) Uani 1 1 d . . . S1 S -0.05693(10) 0.57687(4) -0.04627(5) 0.0508(2) Uani 1 1 d . . . S2 S 0.21180(10) 0.52662(3) 0.07666(5) 0.0501(2) 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 B1 0.0241(16) 0.0372(19) 0.0395(18) -0.0006(15) 0.0163(14) -0.0049(13) C1 0.045(2) 0.0402(19) 0.047(2) 0.0069(15) -0.0053(16) -0.0231(15) C2 0.0382(18) 0.047(2) 0.0415(18) 0.0022(15) 0.0040(14) -0.0198(15) C3 0.0341(16) 0.0355(17) 0.0384(16) -0.0020(13) 0.0155(14) -0.0134(13) C4 0.0338(17) 0.0430(18) 0.0356(16) 0.0039(14) 0.0006(13) 0.0019(14) C5 0.0453(18) 0.0316(16) 0.0361(16) 0.0007(13) 0.0106(14) -0.0101(13) C6 0.0370(17) 0.0365(18) 0.0376(16) 0.0015(13) 0.0035(14) -0.0073(13) C7 0.0345(17) 0.0399(18) 0.0389(17) 0.0043(14) -0.0022(14) -0.0042(13) C8 0.0455(19) 0.0403(18) 0.0404(18) 0.0024(14) 0.0141(15) -0.0033(14) C9 0.046(2) 0.0386(19) 0.050(2) 0.0104(15) 0.0053(16) 0.0082(15) C10 0.0405(19) 0.0411(19) 0.0474(19) 0.0145(15) -0.0003(16) -0.0120(15) C11 0.0402(18) 0.051(2) 0.0386(17) 0.0002(15) 0.0158(15) -0.0192(15) C12 0.0377(17) 0.0408(18) 0.0407(17) -0.0059(14) 0.0100(14) -0.0139(14) C13 0.0340(16) 0.0373(17) 0.0320(15) -0.0006(13) 0.0065(13) -0.0097(13) C14 0.0315(16) 0.0367(16) 0.0322(15) -0.0020(13) 0.0085(13) -0.0043(12) C15 0.0345(17) 0.0370(17) 0.0497(19) -0.0074(15) 0.0074(15) -0.0062(14) C16 0.0303(16) 0.0299(16) 0.0497(18) -0.0043(13) 0.0160(14) -0.0051(12) C17 0.0275(15) 0.0339(17) 0.0461(17) 0.0033(14) 0.0145(14) -0.0004(12) C18 0.0465(19) 0.0420(19) 0.0429(18) -0.0023(14) 0.0131(15) -0.0104(15) C19 0.050(2) 0.0425(19) 0.0464(19) -0.0127(15) 0.0165(16) -0.0159(15) C20 0.048(2) 0.0381(18) 0.052(2) 0.0142(15) 0.0194(17) -0.0078(15) C21 0.0486(19) 0.0375(18) 0.0427(18) 0.0187(15) 0.0154(16) 0.0024(15) C22 0.0432(18) 0.0393(18) 0.0495(19) 0.0045(15) 0.0196(15) -0.0060(14) C23 0.0476(19) 0.0404(18) 0.0420(18) -0.0151(15) 0.0169(15) -0.0065(15) C24 0.0421(18) 0.0441(19) 0.0446(18) -0.0160(15) 0.0126(15) -0.0046(15) C25 0.0455(19) 0.0442(19) 0.0450(19) -0.0175(16) 0.0156(16) -0.0158(15) C26 0.048(2) 0.0404(19) 0.0470(19) -0.0170(15) 0.0143(16) -0.0072(15) C27 0.0435(18) 0.0413(19) 0.0401(17) -0.0131(14) 0.0144(15) -0.0075(14) C28 0.0426(18) 0.0406(18) 0.0402(17) -0.0093(14) 0.0164(15) -0.0069(14) C29 0.0329(16) 0.0443(19) 0.0404(17) -0.0020(14) 0.0159(14) 0.0066(13) C30 0.0387(17) 0.051(2) 0.0277(15) 0.0038(14) 0.0108(13) 0.0025(14) C31 0.0227(14) 0.0426(17) 0.0394(16) 0.0089(14) 0.0159(13) 0.0048(12) C32 0.0390(19) 0.062(2) 0.0427(18) 0.0198(16) 0.0164(16) 0.0098(16) C33 0.0464(19) 0.051(2) 0.0419(18) 0.0171(15) 0.0188(16) 0.0160(16) C34 0.0432(18) 0.0399(18) 0.0454(18) 0.0185(14) 0.0234(15) 0.0172(14) C35 0.059(2) 0.0363(19) 0.056(2) 0.0131(16) 0.0254(18) 0.0124(16) C36 0.051(2) 0.0387(18) 0.0365(17) 0.0143(14) 0.0157(15) 0.0172(15) C37 0.050(2) 0.043(2) 0.065(2) 0.0157(18) 0.0179(18) 0.0141(17) C38 0.0418(19) 0.048(2) 0.057(2) -0.0030(17) 0.0163(17) -0.0043(16) C39 0.044(2) 0.0440(19) 0.051(2) 0.0007(15) 0.0204(16) -0.0096(15) C40 0.050(2) 0.0329(17) 0.056(2) -0.0191(15) 0.0256(17) -0.0139(15) C41 0.0452(19) 0.0408(19) 0.0428(18) -0.0149(14) 0.0182(15) -0.0138(15) C42 0.046(2) 0.0462(19) 0.0428(18) -0.0085(15) 0.0152(16) -0.0059(15) C43 0.0342(17) 0.0383(17) 0.0398(17) -0.0107(14) 0.0111(14) -0.0089(13) C44 0.0270(15) 0.0397(17) 0.0395(16) -0.0073(13) 0.0148(13) -0.0060(12) C45 0.0363(17) 0.050(2) 0.0381(17) -0.0019(14) 0.0153(14) 0.0034(14) C46 0.0338(16) 0.0352(17) 0.0429(17) -0.0018(13) 0.0141(14) 0.0026(13) C47 0.052(2) 0.0341(17) 0.0485(19) 0.0046(14) 0.0241(16) 0.0022(14) C48 0.0468(19) 0.0433(19) 0.0469(19) 0.0060(15) 0.0231(16) 0.0038(15) C49 0.049(2) 0.046(2) 0.053(2) 0.0088(16) 0.0182(17) 0.0102(16) C50 0.051(2) 0.0412(19) 0.056(2) 0.0022(16) 0.0249(18) 0.0007(16) C51 0.045(2) 0.050(2) 0.053(2) 0.0042(16) 0.0206(17) -0.0060(16) C52 0.0461(19) 0.0395(18) 0.0450(18) -0.0046(14) 0.0211(16) -0.0041(15) C53 0.0381(18) 0.0376(18) 0.0337(17) 0.0008(14) 0.0035(14) -0.0055(14) C54 0.049(2) 0.0412(19) 0.0445(18) -0.0017(15) 0.0174(16) -0.0015(15) Co1 0.02489(19) 0.0308(2) 0.0334(2) -0.00293(16) 0.01282(16) -0.00747(15) N1 0.0279(12) 0.0284(13) 0.0329(12) 0.0011(10) 0.0110(10) -0.0029(9) N2 0.0420(15) 0.0351(14) 0.0325(13) -0.0007(11) 0.0085(11) -0.0099(11) N3 0.0333(13) 0.0400(15) 0.0350(13) 0.0043(11) 0.0176(11) 0.0015(11) N4 0.0389(14) 0.0384(15) 0.0362(13) 0.0048(11) 0.0179(12) -0.0004(11) N5 0.0294(13) 0.0369(13) 0.0340(13) -0.0025(10) 0.0160(11) -0.0062(10) N6 0.0295(13) 0.0290(13) 0.0410(14) -0.0032(10) 0.0183(11) -0.0062(10) N7 0.0300(13) 0.0288(13) 0.0490(15) -0.0019(11) 0.0091(12) -0.0065(10) Ni1 0.0423(3) 0.0444(4) 0.0417(3) -0.0016(3) 0.0045(3) -0.0157(3) O1 0.0480(14) 0.0484(14) 0.0464(13) 0.0093(11) 0.0168(12) -0.0009(11) O2 0.0448(13) 0.0436(13) 0.0352(12) -0.0010(10) 0.0104(10) 0.0037(10) S1 0.0440(5) 0.0456(5) 0.0428(5) 0.0008(4) 0.0032(4) -0.0159(4) S2 0.0434(5) 0.0443(5) 0.0432(5) 0.0003(4) 0.0037(4) -0.0157(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 B1 N4 1.537(4) . ? B1 N6 1.539(4) . ? B1 N2 1.542(4) . ? B1 H1A 0.9800 . ? C1 C2 1.360(5) . ? C1 S1 1.659(3) . ? C1 H1 0.9300 . ? C2 C3 1.482(4) . ? C2 S2 1.691(3) . ? C3 C4 1.332(4) . ? C3 C6 1.364(4) . ? C4 C5 1.377(4) . ? C4 H4 0.9300 . ? C5 N7 1.304(4) . ? C5 H5 0.9300 . ? C6 C7 1.384(4) . ? C6 H6 0.9300 . ? C7 N7 1.318(4) . ? C7 H7 0.9300 . ? C8 C13 1.380(5) . ? C8 C9 1.387(5) . ? C8 H8 0.9300 . ? C9 C10 1.341(5) . ? C9 H9 0.9300 . ? C10 C11 1.385(5) . ? C10 H10 0.9300 . ? C11 C12 1.375(4) . ? C11 H11 0.9300 . ? C12 C13 1.397(4) . ? C12 H12 0.9300 . ? C13 C14 1.463(4) . ? C14 N1 1.341(4) . ? C14 C15 1.386(4) . ? C15 C16 1.355(4) . ? C15 H15 0.9300 . ? C16 N2 1.358(4) . ? C16 C17 1.460(4) . ? C17 C22 1.390(4) . ? C17 C18 1.395(4) . ? C18 C19 1.359(5) . ? C18 H18 0.9300 . ? C19 C20 1.371(5) . ? C19 H19 0.9300 . ? C20 C21 1.338(5) . ? C20 H20 0.9300 . ? C21 C22 1.376(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.371(5) . ? C23 C24 1.405(4) . ? C23 H23 0.9300 . ? C24 C25 1.356(4) . ? C24 H24 0.9300 . ? C25 C26 1.361(5) . ? C25 H25 0.9300 . ? C26 C27 1.371(4) . ? C26 H26 0.9300 . ? C27 C28 1.379(4) . ? C27 H27 0.9300 . ? C28 C29 1.442(4) . ? C29 N3 1.344(4) . ? C29 C30 1.391(4) . ? C30 C31 1.354(4) . ? C30 H30 0.9300 . ? C31 N4 1.349(4) . ? C31 C32 1.473(5) . ? C32 C33 1.380(5) . ? C32 C37 1.398(5) . ? C33 C34 1.378(4) . ? C33 H33 0.9300 . ? C34 C35 1.353(5) . ? C34 H34 0.9300 . ? C35 C36 1.369(5) . ? C35 H35 0.9300 . ? C36 C37 1.370(5) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.370(5) . ? C38 C43 1.383(5) . ? C38 H38 0.9300 . ? C39 C40 1.371(5) . ? C39 H39 0.9300 . ? C40 C41 1.376(5) . ? C40 H40 0.9300 . ? C41 C42 1.352(5) . ? C41 H41 0.9300 . ? C42 C43 1.377(5) . ? C42 H42 0.9300 . ? C43 C44 1.492(4) . ? C44 N5 1.342(4) . ? C44 C45 1.363(4) . ? C45 C46 1.375(5) . ? C45 H45 0.9300 . ? C46 N6 1.359(4) . ? C46 C47 1.450(4) . ? C47 C48 1.384(5) . ? C47 C52 1.399(5) . ? C48 C49 1.391(5) . ? C48 H48 0.9300 . ? C49 C50 1.371(5) . ? C49 H49 0.9300 . ? C50 C51 1.364(5) . ? C50 H50 0.9300 . ? C51 C52 1.368(5) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 O2 1.154(4) . ? C53 O1 1.237(4) . ? C53 C54 1.527(4) . ? C53 Co1 2.458(3) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? Co1 O2 2.106(2) . ? Co1 N5 2.143(3) . ? Co1 N3 2.157(2) . ? Co1 N7 2.164(2) . ? Co1 N1 2.201(2) . ? Co1 O1 2.227(2) . ? N1 N2 1.358(3) . ? N3 N4 1.360(3) . ? N5 N6 1.363(3) . ? Ni1 S1 2.1121(9) . ? Ni1 S1 2.1121(9) 3_565 ? Ni1 S2 2.1172(8) 3_565 ? Ni1 S2 2.1172(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 B1 N6 110.6(2) . . ? N4 B1 N2 110.6(2) . . ? N6 B1 N2 107.6(2) . . ? N4 B1 H1A 109.4 . . ? N6 B1 H1A 109.5 . . ? N2 B1 H1A 109.2 . . ? C2 C1 S1 123.8(3) . . ? C2 C1 H1 118.1 . . ? S1 C1 H1 118.1 . . ? C1 C2 C3 123.8(3) . . ? C1 C2 S2 115.4(2) . . ? C3 C2 S2 120.8(2) . . ? C4 C3 C6 116.4(3) . . ? C4 C3 C2 122.9(3) . . ? C6 C3 C2 120.7(3) . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? N7 C5 C4 123.9(3) . . ? N7 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C3 C6 C7 119.2(3) . . ? C3 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? N7 C7 C6 124.2(3) . . ? N7 C7 H7 117.9 . . ? C6 C7 H7 117.9 . . ? C13 C8 C9 120.1(3) . . ? C13 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 118.4(3) . . ? C8 C13 C14 120.6(3) . . ? C12 C13 C14 120.7(3) . . ? N1 C14 C15 109.0(3) . . ? N1 C14 C13 125.8(3) . . ? C15 C14 C13 125.1(3) . . ? C16 C15 C14 107.2(3) . . ? C16 C15 H15 126.4 . . ? C14 C15 H15 126.4 . . ? C15 C16 N2 107.2(3) . . ? C15 C16 C17 129.7(3) . . ? N2 C16 C17 123.0(3) . . ? C22 C17 C18 117.0(3) . . ? C22 C17 C16 123.6(3) . . ? C18 C17 C16 119.4(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 120.6(3) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? C28 C23 C24 120.6(3) . . ? C28 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.1(3) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 122.0(3) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 117.7(3) . . ? C25 C26 H26 121.1 . . ? C27 C26 H26 121.1 . . ? C26 C27 C28 123.2(3) . . ? C26 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C23 C28 C27 117.3(3) . . ? C23 C28 C29 123.2(3) . . ? C27 C28 C29 119.5(3) . . ? N3 C29 C30 108.2(3) . . ? N3 C29 C28 124.2(3) . . ? C30 C29 C28 127.6(3) . . ? C31 C30 C29 107.9(3) . . ? C31 C30 H30 126.0 . . ? C29 C30 H30 126.0 . . ? N4 C31 C30 106.6(3) . . ? N4 C31 C32 125.2(3) . . ? C30 C31 C32 128.1(3) . . ? C33 C32 C37 117.7(3) . . ? C33 C32 C31 119.8(3) . . ? C37 C32 C31 122.5(3) . . ? C34 C33 C32 121.0(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C33 121.1(3) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 118.6(3) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C35 C36 C37 121.8(3) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C32 119.8(4) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? C39 C38 C43 119.2(3) . . ? C39 C38 H38 120.4 . . ? C43 C38 H38 120.4 . . ? C38 C39 C40 121.7(3) . . ? C38 C39 H39 119.2 . . ? C40 C39 H39 119.2 . . ? C39 C40 C41 119.3(3) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 118.8(3) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C41 C42 C43 122.9(3) . . ? C41 C42 H42 118.5 . . ? C43 C42 H42 118.5 . . ? C42 C43 C38 118.1(3) . . ? C42 C43 C44 119.4(3) . . ? C38 C43 C44 122.5(3) . . ? N5 C44 C45 110.7(3) . . ? N5 C44 C43 123.0(3) . . ? C45 C44 C43 126.2(3) . . ? C44 C45 C46 106.7(3) . . ? C44 C45 H45 126.6 . . ? C46 C45 H45 126.6 . . ? N6 C46 C45 106.6(3) . . ? N6 C46 C47 124.3(3) . . ? C45 C46 C47 129.1(3) . . ? C48 C47 C52 117.8(3) . . ? C48 C47 C46 119.4(3) . . ? C52 C47 C46 122.9(3) . . ? C47 C48 C49 121.8(3) . . ? C47 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C50 C49 C48 117.7(3) . . ? C50 C49 H49 121.2 . . ? C48 C49 H49 121.2 . . ? C51 C50 C49 122.5(3) . . ? C51 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? C50 C51 C52 119.1(3) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? C51 C52 C47 121.1(3) . . ? C51 C52 H52 119.4 . . ? C47 C52 H52 119.4 . . ? O2 C53 O1 123.3(3) . . ? O2 C53 C54 120.6(3) . . ? O1 C53 C54 115.9(3) . . ? O2 C53 Co1 58.80(18) . . ? O1 C53 Co1 64.57(17) . . ? C54 C53 Co1 177.6(2) . . ? C53 C54 H54A 109.2 . . ? C53 C54 H54B 109.9 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.3 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O2 Co1 N5 166.25(9) . . ? O2 Co1 N3 101.96(9) . . ? N5 Co1 N3 88.33(9) . . ? O2 Co1 N7 96.25(9) . . ? N5 Co1 N7 92.55(9) . . ? N3 Co1 N7 91.33(10) . . ? O2 Co1 N1 87.99(9) . . ? N5 Co1 N1 82.69(9) . . ? N3 Co1 N1 90.92(9) . . ? N7 Co1 N1 174.68(10) . . ? O2 Co1 O1 58.06(9) . . ? N5 Co1 O1 112.24(9) . . ? N3 Co1 O1 159.37(10) . . ? N7 Co1 O1 86.32(9) . . ? N1 Co1 O1 93.24(9) . . ? O2 Co1 C53 27.97(10) . . ? N5 Co1 C53 141.66(11) . . ? N3 Co1 C53 129.71(11) . . ? N7 Co1 C53 91.23(10) . . ? N1 Co1 C53 91.04(9) . . ? O1 Co1 C53 30.10(10) . . ? C14 N1 N2 106.7(2) . . ? C14 N1 Co1 139.1(2) . . ? N2 N1 Co1 111.97(16) . . ? C16 N2 N1 109.9(2) . . ? C16 N2 B1 128.6(3) . . ? N1 N2 B1 119.9(2) . . ? C29 N3 N4 106.6(2) . . ? C29 N3 Co1 136.6(2) . . ? N4 N3 Co1 115.32(18) . . ? C31 N4 N3 110.6(2) . . ? C31 N4 B1 129.8(3) . . ? N3 N4 B1 119.6(2) . . ? C44 N5 N6 105.6(2) . . ? C44 N5 Co1 139.2(2) . . ? N6 N5 Co1 115.09(17) . . ? C46 N6 N5 110.4(2) . . ? C46 N6 B1 128.8(3) . . ? N5 N6 B1 120.2(2) . . ? C5 N7 C7 115.1(3) . . ? C5 N7 Co1 120.9(2) . . ? C7 N7 Co1 123.9(2) . . ? S1 Ni1 S1 180.000(19) . 3_565 ? S1 Ni1 S2 89.19(3) . 3_565 ? S1 Ni1 S2 90.81(3) 3_565 3_565 ? S1 Ni1 S2 90.81(3) . . ? S1 Ni1 S2 89.19(3) 3_565 . ? S2 Ni1 S2 180.00(5) 3_565 . ? C53 O1 Co1 85.34(19) . . ? C53 O2 Co1 93.2(2) . . ? C1 S1 Ni1 103.69(13) . . ? C2 S2 Ni1 106.28(11) . . ? 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 S1 C1 C2 C3 178.7(3) . . . . ? S1 C1 C2 S2 -1.9(5) . . . . ? C1 C2 C3 C4 -2.8(6) . . . . ? S2 C2 C3 C4 177.9(3) . . . . ? C1 C2 C3 C6 177.9(4) . . . . ? S2 C2 C3 C6 -1.5(5) . . . . ? C6 C3 C4 C5 1.0(5) . . . . ? C2 C3 C4 C5 -178.4(3) . . . . ? C3 C4 C5 N7 0.3(6) . . . . ? C4 C3 C6 C7 -0.3(5) . . . . ? C2 C3 C6 C7 179.1(3) . . . . ? C3 C6 C7 N7 -1.9(6) . . . . ? C13 C8 C9 C10 -1.8(5) . . . . ? C8 C9 C10 C11 0.9(5) . . . . ? C9 C10 C11 C12 0.6(5) . . . . ? C10 C11 C12 C13 -1.1(5) . . . . ? C9 C8 C13 C12 1.2(5) . . . . ? C9 C8 C13 C14 174.8(3) . . . . ? C11 C12 C13 C8 0.2(5) . . . . ? C11 C12 C13 C14 -173.4(3) . . . . ? C8 C13 C14 N1 133.7(3) . . . . ? C12 C13 C14 N1 -52.8(4) . . . . ? C8 C13 C14 C15 -49.2(5) . . . . ? C12 C13 C14 C15 124.3(4) . . . . ? N1 C14 C15 C16 1.0(4) . . . . ? C13 C14 C15 C16 -176.4(3) . . . . ? C14 C15 C16 N2 -1.2(4) . . . . ? C14 C15 C16 C17 -178.2(3) . . . . ? C15 C16 C17 C22 134.9(4) . . . . ? N2 C16 C17 C22 -41.8(5) . . . . ? C15 C16 C17 C18 -43.6(5) . . . . ? N2 C16 C17 C18 139.7(3) . . . . ? C22 C17 C18 C19 -0.9(5) . . . . ? C16 C17 C18 C19 177.7(3) . . . . ? C17 C18 C19 C20 1.5(6) . . . . ? C18 C19 C20 C21 0.3(6) . . . . ? C19 C20 C21 C22 -2.6(6) . . . . ? C20 C21 C22 C17 3.2(5) . . . . ? C18 C17 C22 C21 -1.4(5) . . . . ? C16 C17 C22 C21 -179.9(3) . . . . ? C28 C23 C24 C25 1.4(5) . . . . ? C23 C24 C25 C26 2.4(5) . . . . ? C24 C25 C26 C27 -3.9(5) . . . . ? C25 C26 C27 C28 1.7(5) . . . . ? C24 C23 C28 C27 -3.4(5) . . . . ? C24 C23 C28 C29 176.0(3) . . . . ? C26 C27 C28 C23 1.9(5) . . . . ? C26 C27 C28 C29 -177.5(3) . . . . ? C23 C28 C29 N3 -34.8(5) . . . . ? C27 C28 C29 N3 144.6(3) . . . . ? C23 C28 C29 C30 148.1(4) . . . . ? C27 C28 C29 C30 -32.5(5) . . . . ? N3 C29 C30 C31 -1.1(4) . . . . ? C28 C29 C30 C31 176.4(3) . . . . ? C29 C30 C31 N4 1.5(3) . . . . ? C29 C30 C31 C32 -178.8(3) . . . . ? N4 C31 C32 C33 136.8(3) . . . . ? C30 C31 C32 C33 -42.7(5) . . . . ? N4 C31 C32 C37 -43.0(5) . . . . ? C30 C31 C32 C37 137.4(4) . . . . ? C37 C32 C33 C34 1.0(5) . . . . ? C31 C32 C33 C34 -178.9(3) . . . . ? C32 C33 C34 C35 1.0(5) . . . . ? C33 C34 C35 C36 -2.4(5) . . . . ? C34 C35 C36 C37 2.0(5) . . . . ? C35 C36 C37 C32 0.0(5) . . . . ? C33 C32 C37 C36 -1.4(5) . . . . ? C31 C32 C37 C36 178.5(3) . . . . ? C43 C38 C39 C40 -0.9(5) . . . . ? C38 C39 C40 C41 -0.2(5) . . . . ? C39 C40 C41 C42 0.6(5) . . . . ? C40 C41 C42 C43 0.2(5) . . . . ? C41 C42 C43 C38 -1.3(5) . . . . ? C41 C42 C43 C44 179.5(3) . . . . ? C39 C38 C43 C42 1.7(5) . . . . ? C39 C38 C43 C44 -179.3(3) . . . . ? C42 C43 C44 N5 -140.1(3) . . . . ? C38 C43 C44 N5 40.8(5) . . . . ? C42 C43 C44 C45 40.2(5) . . . . ? C38 C43 C44 C45 -138.8(4) . . . . ? N5 C44 C45 C46 1.1(4) . . . . ? C43 C44 C45 C46 -179.2(3) . . . . ? C44 C45 C46 N6 -0.5(4) . . . . ? C44 C45 C46 C47 180.0(3) . . . . ? N6 C46 C47 C48 139.4(3) . . . . ? C45 C46 C47 C48 -41.2(5) . . . . ? N6 C46 C47 C52 -40.9(5) . . . . ? C45 C46 C47 C52 138.5(4) . . . . ? C52 C47 C48 C49 1.5(5) . . . . ? C46 C47 C48 C49 -178.8(3) . . . . ? C47 C48 C49 C50 -0.3(5) . . . . ? C48 C49 C50 C51 -1.1(6) . . . . ? C49 C50 C51 C52 1.1(6) . . . . ? C50 C51 C52 C47 0.2(5) . . . . ? C48 C47 C52 C51 -1.5(5) . . . . ? C46 C47 C52 C51 178.8(3) . . . . ? O1 C53 Co1 O2 178.4(3) . . . . ? C54 C53 Co1 O2 76(7) . . . . ? O2 C53 Co1 N5 -163.26(17) . . . . ? O1 C53 Co1 N5 15.2(3) . . . . ? C54 C53 Co1 N5 -87(7) . . . . ? O2 C53 Co1 N3 8.3(2) . . . . ? O1 C53 Co1 N3 -173.26(16) . . . . ? C54 C53 Co1 N3 85(7) . . . . ? O2 C53 Co1 N7 101.1(2) . . . . ? O1 C53 Co1 N7 -80.50(19) . . . . ? C54 C53 Co1 N7 177(100) . . . . ? O2 C53 Co1 N1 -83.8(2) . . . . ? O1 C53 Co1 N1 94.69(18) . . . . ? C54 C53 Co1 N1 -7(7) . . . . ? O2 C53 Co1 O1 -178.4(3) . . . . ? C54 C53 Co1 O1 -102(7) . . . . ? C15 C14 N1 N2 -0.5(3) . . . . ? C13 C14 N1 N2 177.0(3) . . . . ? C15 C14 N1 Co1 160.2(2) . . . . ? C13 C14 N1 Co1 -22.4(5) . . . . ? O2 Co1 N1 C14 -32.4(3) . . . . ? N5 Co1 N1 C14 137.5(3) . . . . ? N3 Co1 N1 C14 -134.3(3) . . . . ? N7 Co1 N1 C14 110.6(10) . . . . ? O1 Co1 N1 C14 25.4(3) . . . . ? C53 Co1 N1 C14 -4.6(3) . . . . ? O2 Co1 N1 N2 127.6(2) . . . . ? N5 Co1 N1 N2 -62.53(19) . . . . ? N3 Co1 N1 N2 25.7(2) . . . . ? N7 Co1 N1 N2 -89.4(10) . . . . ? O1 Co1 N1 N2 -174.5(2) . . . . ? C53 Co1 N1 N2 155.4(2) . . . . ? C15 C16 N2 N1 0.9(4) . . . . ? C17 C16 N2 N1 178.2(3) . . . . ? C15 C16 N2 B1 166.0(3) . . . . ? C17 C16 N2 B1 -16.7(5) . . . . ? C14 N1 N2 C16 -0.2(3) . . . . ? Co1 N1 N2 C16 -166.7(2) . . . . ? C14 N1 N2 B1 -166.8(3) . . . . ? Co1 N1 N2 B1 26.7(3) . . . . ? N4 B1 N2 C16 118.2(3) . . . . ? N6 B1 N2 C16 -120.9(3) . . . . ? N4 B1 N2 N1 -78.0(3) . . . . ? N6 B1 N2 N1 42.9(3) . . . . ? C30 C29 N3 N4 0.2(3) . . . . ? C28 C29 N3 N4 -177.4(3) . . . . ? C30 C29 N3 Co1 165.0(2) . . . . ? C28 C29 N3 Co1 -12.6(5) . . . . ? O2 Co1 N3 C29 61.0(3) . . . . ? N5 Co1 N3 C29 -128.1(3) . . . . ? N7 Co1 N3 C29 -35.6(3) . . . . ? N1 Co1 N3 C29 149.2(3) . . . . ? O1 Co1 N3 C29 47.5(4) . . . . ? C53 Co1 N3 C29 57.1(3) . . . . ? O2 Co1 N3 N4 -135.18(19) . . . . ? N5 Co1 N3 N4 35.6(2) . . . . ? N7 Co1 N3 N4 128.1(2) . . . . ? N1 Co1 N3 N4 -47.0(2) . . . . ? O1 Co1 N3 N4 -148.8(2) . . . . ? C53 Co1 N3 N4 -139.15(19) . . . . ? C30 C31 N4 N3 -1.4(3) . . . . ? C32 C31 N4 N3 178.9(3) . . . . ? C30 C31 N4 B1 176.7(3) . . . . ? C32 C31 N4 B1 -2.9(5) . . . . ? C29 N3 N4 C31 0.7(3) . . . . ? Co1 N3 N4 C31 -167.71(19) . . . . ? C29 N3 N4 B1 -177.6(2) . . . . ? Co1 N3 N4 B1 13.9(3) . . . . ? N6 B1 N4 C31 113.3(3) . . . . ? N2 B1 N4 C31 -127.6(3) . . . . ? N6 B1 N4 N3 -68.7(3) . . . . ? N2 B1 N4 N3 50.4(3) . . . . ? C45 C44 N5 N6 -1.2(3) . . . . ? C43 C44 N5 N6 179.1(3) . . . . ? C45 C44 N5 Co1 174.3(2) . . . . ? C43 C44 N5 Co1 -5.4(5) . . . . ? O2 Co1 N5 C44 -86.0(5) . . . . ? N3 Co1 N5 C44 135.2(3) . . . . ? N7 Co1 N5 C44 43.9(3) . . . . ? N1 Co1 N5 C44 -133.7(3) . . . . ? O1 Co1 N5 C44 -43.2(3) . . . . ? C53 Co1 N5 C44 -51.3(4) . . . . ? O2 Co1 N5 N6 89.2(4) . . . . ? N3 Co1 N5 N6 -49.69(19) . . . . ? N7 Co1 N5 N6 -140.95(19) . . . . ? N1 Co1 N5 N6 41.45(18) . . . . ? O1 Co1 N5 N6 131.98(18) . . . . ? C53 Co1 N5 N6 123.8(2) . . . . ? C45 C46 N6 N5 -0.2(3) . . . . ? C47 C46 N6 N5 179.4(3) . . . . ? C45 C46 N6 B1 169.9(3) . . . . ? C47 C46 N6 B1 -10.5(5) . . . . ? C44 N5 N6 C46 0.8(3) . . . . ? Co1 N5 N6 C46 -175.89(19) . . . . ? C44 N5 N6 B1 -170.3(2) . . . . ? Co1 N5 N6 B1 13.0(3) . . . . ? N4 B1 N6 C46 -117.9(3) . . . . ? N2 B1 N6 C46 121.2(3) . . . . ? N4 B1 N6 N5 51.3(3) . . . . ? N2 B1 N6 N5 -69.5(3) . . . . ? C4 C5 N7 C7 -2.3(5) . . . . ? C4 C5 N7 Co1 -178.3(3) . . . . ? C6 C7 N7 C5 3.1(5) . . . . ? C6 C7 N7 Co1 178.9(3) . . . . ? O2 Co1 N7 C5 -152.3(3) . . . . ? N5 Co1 N7 C5 38.2(3) . . . . ? N3 Co1 N7 C5 -50.2(3) . . . . ? N1 Co1 N7 C5 64.9(11) . . . . ? O1 Co1 N7 C5 150.4(3) . . . . ? C53 Co1 N7 C5 -179.9(3) . . . . ? O2 Co1 N7 C7 32.1(3) . . . . ? N5 Co1 N7 C7 -137.3(3) . . . . ? N3 Co1 N7 C7 134.3(3) . . . . ? N1 Co1 N7 C7 -110.7(10) . . . . ? O1 Co1 N7 C7 -25.2(3) . . . . ? C53 Co1 N7 C7 4.5(3) . . . . ? O2 C53 O1 Co1 1.6(3) . . . . ? C54 C53 O1 Co1 177.4(2) . . . . ? O2 Co1 O1 C53 -0.86(17) . . . . ? N5 Co1 O1 C53 -169.89(17) . . . . ? N3 Co1 O1 C53 14.8(4) . . . . ? N7 Co1 O1 C53 98.85(19) . . . . ? N1 Co1 O1 C53 -86.46(19) . . . . ? O1 C53 O2 Co1 -1.7(3) . . . . ? C54 C53 O2 Co1 -177.3(3) . . . . ? N5 Co1 O2 C53 48.7(5) . . . . ? N3 Co1 O2 C53 -173.48(19) . . . . ? N7 Co1 O2 C53 -80.8(2) . . . . ? N1 Co1 O2 C53 96.0(2) . . . . ? O1 Co1 O2 C53 0.92(19) . . . . ? C2 C1 S1 Ni1 1.5(4) . . . . ? S1 Ni1 S1 C1 -38(9) 3_565 . . . ? S2 Ni1 S1 C1 179.58(16) 3_565 . . . ? S2 Ni1 S1 C1 -0.42(16) . . . . ? C1 C2 S2 Ni1 1.2(3) . . . . ? C3 C2 S2 Ni1 -179.4(2) . . . . ? S1 Ni1 S2 C2 -0.34(14) . . . . ? S1 Ni1 S2 C2 179.66(14) 3_565 . . . ? S2 Ni1 S2 C2 -103(100) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.226 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.055 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 782322' #TrackingRef '- 1-4-all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 Cu F6 N2 O4 S6' _chemical_formula_sum 'C32 H18 Cu F6 N2 O4 S6' _chemical_formula_weight 864.45 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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.866(3) _cell_length_b 17.281(2) _cell_length_c 11.1077(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.479(2) _cell_angle_gamma 90.00 _cell_volume 3752.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2700 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26.1 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8585 _exptl_absorpt_correction_T_max 0.8745 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 '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 9848 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3688 _reflns_number_gt 2291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1182P)^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 3688 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1769 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 Cu1 Cu 0.2500 0.2500 0.5000 0.0680(3) Uani 1 2 d S . . C1 C 0.1525(5) 0.0541(5) -0.0189(8) 0.143(3) Uani 1 1 d . . . H1 H 0.1174 0.0226 -0.0701 0.171 Uiso 1 1 calc R . . C2 C 0.2039(5) 0.0868(5) -0.0551(8) 0.131(3) Uani 1 1 d . . . H2 H 0.2059 0.0765 -0.1359 0.158 Uiso 1 1 calc R . . C3 C 0.2513(4) 0.1338(4) 0.0279(6) 0.101(2) Uani 1 1 d . . . H3 H 0.2871 0.1598 0.0139 0.121 Uiso 1 1 calc R . . C4 C 0.2329(4) 0.1342(4) 0.1468(6) 0.105(2) Uani 1 1 d . . . C5 C 0.2674(3) 0.1722(3) 0.2700(5) 0.0811(15) Uani 1 1 d . . . C6 C 0.3240(4) 0.2185(4) 0.2833(6) 0.101(2) Uani 1 1 d . . . H6 H 0.3402 0.2182 0.2152 0.121 Uiso 1 1 calc R . . C7 C 0.3585(3) 0.2647(4) 0.3866(7) 0.0936(19) Uani 1 1 d . . . C8 C 0.4224(5) 0.3076(7) 0.3936(12) 0.155(4) Uani 1 1 d . . . C9 C 0.3502(2) 0.2050(3) 0.7475(4) 0.0622(11) Uani 1 1 d . . . H9 H 0.3641 0.2561 0.7476 0.075 Uiso 1 1 calc R . . C10 C 0.3833(2) 0.1604(2) 0.8524(4) 0.0572(11) Uani 1 1 d . . . H10 H 0.4176 0.1816 0.9227 0.069 Uiso 1 1 calc R . . C11 C 0.2824(2) 0.1052(3) 0.6460(4) 0.0702(13) Uani 1 1 d . . . H11 H 0.2470 0.0858 0.5755 0.084 Uiso 1 1 calc R . . C12 C 0.3142(2) 0.0560(3) 0.7447(4) 0.0707(13) Uani 1 1 d . . . H12 H 0.3015 0.0042 0.7388 0.085 Uiso 1 1 calc R . . C13 C 0.3651(2) 0.0826(2) 0.8531(4) 0.0551(10) Uani 1 1 d . . . C14 C 0.3987(2) 0.0328(3) 0.9625(4) 0.0541(10) Uani 1 1 d . . . C15 C 0.3994(2) -0.0447(3) 0.9622(4) 0.0580(10) Uani 1 1 d . . . H15 H 0.3756 -0.0718 0.8876 0.070 Uiso 1 1 calc R . . C16 C 0.4772(2) -0.0110(2) 1.1906(3) 0.0516(10) Uani 1 1 d . . . F1 F 0.4754(3) 0.2850(4) 0.4785(7) 0.214(3) Uani 1 1 d . . . F2 F 0.4157(3) 0.3806(4) 0.3901(6) 0.188(2) Uani 1 1 d . . . F3 F 0.4390(3) 0.2967(5) 0.2882(7) 0.213(3) Uani 1 1 d . . . N1 N 0.29926(17) 0.1793(2) 0.6450(3) 0.0605(9) Uani 1 1 d . . . O1 O 0.24454(18) 0.1613(2) 0.3574(3) 0.0842(10) Uani 1 1 d . . . O2 O 0.3436(2) 0.2790(3) 0.4849(4) 0.0987(12) Uani 1 1 d . . . S1 S 0.16417(14) 0.08085(15) 0.1324(2) 0.1433(8) Uani 1 1 d . . . S2 S 0.44505(6) 0.07644(6) 1.11059(10) 0.0666(4) Uani 1 1 d . . . S3 S 0.44462(6) -0.09394(6) 1.10068(9) 0.0608(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 Cu1 0.0541(5) 0.0957(6) 0.0469(5) 0.0196(4) 0.0086(3) 0.0139(4) C1 0.138(7) 0.148(7) 0.125(7) -0.023(5) 0.024(6) 0.019(6) C2 0.150(8) 0.143(7) 0.104(6) 0.007(5) 0.048(6) 0.039(6) C3 0.126(6) 0.111(5) 0.073(4) 0.009(3) 0.044(4) 0.049(4) C4 0.120(5) 0.112(5) 0.094(4) 0.020(4) 0.050(4) 0.048(4) C5 0.085(4) 0.090(4) 0.075(4) 0.033(3) 0.037(3) 0.038(3) C6 0.116(5) 0.116(5) 0.086(4) 0.033(4) 0.055(4) 0.048(4) C7 0.082(4) 0.108(5) 0.103(5) 0.047(4) 0.048(4) 0.036(3) C8 0.109(7) 0.176(9) 0.213(11) 0.073(8) 0.096(7) 0.025(6) C9 0.054(2) 0.067(3) 0.057(3) 0.008(2) 0.009(2) 0.008(2) C10 0.049(2) 0.069(3) 0.043(2) -0.0018(18) 0.0030(18) 0.0035(19) C11 0.055(3) 0.094(3) 0.043(2) 0.005(2) -0.0061(19) -0.007(2) C12 0.069(3) 0.073(3) 0.053(3) 0.006(2) 0.000(2) -0.010(2) C13 0.048(2) 0.069(3) 0.041(2) 0.0011(18) 0.0065(17) -0.0040(19) C14 0.044(2) 0.072(3) 0.038(2) -0.0018(18) 0.0050(17) -0.0049(19) C15 0.054(2) 0.067(3) 0.041(2) -0.0039(18) 0.0020(18) -0.011(2) C16 0.053(2) 0.064(2) 0.0352(19) -0.0010(16) 0.0115(17) -0.0050(18) F1 0.092(3) 0.248(7) 0.275(8) 0.099(6) 0.028(4) 0.000(4) F2 0.175(5) 0.152(4) 0.259(7) 0.047(5) 0.102(5) -0.010(4) F3 0.171(5) 0.270(7) 0.256(7) 0.004(6) 0.148(5) -0.035(5) N1 0.051(2) 0.079(3) 0.0430(18) 0.0095(17) 0.0065(16) 0.0084(18) O1 0.081(2) 0.103(3) 0.070(2) 0.0299(18) 0.0286(18) 0.0218(18) O2 0.082(3) 0.132(3) 0.078(2) 0.034(2) 0.022(2) 0.017(2) S1 0.140(2) 0.157(2) 0.1307(18) 0.0089(14) 0.0445(15) 0.0283(15) S2 0.0794(8) 0.0631(7) 0.0391(6) -0.0016(4) -0.0021(5) 0.0018(5) S3 0.0709(7) 0.0611(7) 0.0420(6) 0.0007(4) 0.0093(5) -0.0055(5) _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 N1 1.996(3) 7_556 ? Cu1 N1 1.996(3) . ? Cu1 O2 2.078(4) . ? Cu1 O2 2.078(4) 7_556 ? Cu1 O1 2.178(4) 7_556 ? Cu1 O1 2.178(4) . ? C1 C2 1.391(12) . ? C1 S1 1.676(9) . ? C1 H1 0.9300 . ? C2 C3 1.360(11) . ? C2 H2 0.9300 . ? C3 C4 1.499(8) . ? C3 H3 0.9300 . ? C4 C5 1.461(8) . ? C4 S1 1.666(8) . ? C5 O1 1.237(6) . ? C5 C6 1.389(9) . ? C6 C7 1.376(9) . ? C6 H6 0.9300 . ? C7 O2 1.260(7) . ? C7 C8 1.503(11) . ? C8 F1 1.239(10) . ? C8 F2 1.269(11) . ? C8 F3 1.346(11) . ? C9 N1 1.332(5) . ? C9 C10 1.365(5) . ? C9 H9 0.9300 . ? C10 C13 1.399(6) . ? C10 H10 0.9300 . ? C11 N1 1.330(6) . ? C11 C12 1.362(6) . ? C11 H11 0.9300 . ? C12 C13 1.376(6) . ? C12 H12 0.9300 . ? C13 C14 1.453(6) . ? C14 C15 1.339(6) . ? C14 S2 1.760(4) . ? C15 S3 1.722(4) . ? C15 H15 0.9300 . ? C16 C16 1.329(7) 2_657 ? C16 S3 1.743(4) . ? C16 S2 1.763(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.00(15) 7_556 . ? N1 Cu1 O2 91.19(15) 7_556 . ? N1 Cu1 O2 88.81(15) . . ? N1 Cu1 O2 88.81(15) 7_556 7_556 ? N1 Cu1 O2 91.19(15) . 7_556 ? O2 Cu1 O2 180.0 . 7_556 ? N1 Cu1 O1 92.14(14) 7_556 7_556 ? N1 Cu1 O1 87.86(14) . 7_556 ? O2 Cu1 O1 94.45(16) . 7_556 ? O2 Cu1 O1 85.55(16) 7_556 7_556 ? N1 Cu1 O1 87.86(14) 7_556 . ? N1 Cu1 O1 92.14(14) . . ? O2 Cu1 O1 85.55(16) . . ? O2 Cu1 O1 94.45(16) 7_556 . ? O1 Cu1 O1 180.0 7_556 . ? C2 C1 S1 108.8(7) . . ? C2 C1 H1 125.6 . . ? S1 C1 H1 125.6 . . ? C3 C2 C1 119.9(8) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 104.5(7) . . ? C2 C3 H3 127.7 . . ? C4 C3 H3 127.7 . . ? C5 C4 C3 129.4(7) . . ? C5 C4 S1 117.7(5) . . ? C3 C4 S1 112.9(6) . . ? O1 C5 C6 123.4(6) . . ? O1 C5 C4 117.9(6) . . ? C6 C5 C4 118.7(6) . . ? C7 C6 C5 126.8(6) . . ? C7 C6 H6 116.6 . . ? C5 C6 H6 116.6 . . ? O2 C7 C6 128.3(6) . . ? O2 C7 C8 110.0(8) . . ? C6 C7 C8 121.7(8) . . ? F1 C8 F2 113.3(12) . . ? F1 C8 F3 100.6(8) . . ? F2 C8 F3 99.8(8) . . ? F1 C8 C7 115.0(8) . . ? F2 C8 C7 113.9(8) . . ? F3 C8 C7 112.3(10) . . ? N1 C9 C10 123.8(4) . . ? N1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C9 C10 C13 119.3(4) . . ? C9 C10 H10 120.3 . . ? C13 C10 H10 120.3 . . ? N1 C11 C12 123.5(4) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 120.4(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C10 116.3(4) . . ? C12 C13 C14 122.2(4) . . ? C10 C13 C14 121.5(3) . . ? C15 C14 C13 126.3(3) . . ? C15 C14 S2 115.3(3) . . ? C13 C14 S2 118.3(3) . . ? C14 C15 S3 119.7(3) . . ? C14 C15 H15 120.2 . . ? S3 C15 H15 120.2 . . ? C16 C16 S3 124.68(13) 2_657 . ? C16 C16 S2 120.97(12) 2_657 . ? S3 C16 S2 114.4(2) . . ? C11 N1 C9 116.6(3) . . ? C11 N1 Cu1 122.2(3) . . ? C9 N1 Cu1 121.2(3) . . ? C5 O1 Cu1 121.8(4) . . ? C7 O2 Cu1 123.1(4) . . ? C4 S1 C1 93.9(5) . . ? C14 S2 C16 95.27(19) . . ? C15 S3 C16 95.04(19) . . ? 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 S1 C1 C2 C3 -1.8(10) . . . . ? C1 C2 C3 C4 1.7(9) . . . . ? C2 C3 C4 C5 177.3(6) . . . . ? C2 C3 C4 S1 -0.9(7) . . . . ? C3 C4 C5 O1 -176.5(5) . . . . ? S1 C4 C5 O1 1.6(6) . . . . ? C3 C4 C5 C6 3.4(9) . . . . ? S1 C4 C5 C6 -178.5(4) . . . . ? O1 C5 C6 C7 -7.1(9) . . . . ? C4 C5 C6 C7 173.0(5) . . . . ? C5 C6 C7 O2 -5.6(10) . . . . ? C5 C6 C7 C8 175.4(6) . . . . ? O2 C7 C8 F1 68.2(12) . . . . ? C6 C7 C8 F1 -112.6(11) . . . . ? O2 C7 C8 F2 -65.0(11) . . . . ? C6 C7 C8 F2 114.2(10) . . . . ? O2 C7 C8 F3 -177.5(7) . . . . ? C6 C7 C8 F3 1.7(12) . . . . ? N1 C9 C10 C13 2.1(7) . . . . ? N1 C11 C12 C13 2.4(8) . . . . ? C11 C12 C13 C10 -2.6(7) . . . . ? C11 C12 C13 C14 177.7(4) . . . . ? C9 C10 C13 C12 0.4(6) . . . . ? C9 C10 C13 C14 -179.8(4) . . . . ? C12 C13 C14 C15 18.8(7) . . . . ? C10 C13 C14 C15 -160.9(4) . . . . ? C12 C13 C14 S2 -162.8(4) . . . . ? C10 C13 C14 S2 17.4(6) . . . . ? C13 C14 C15 S3 177.7(4) . . . . ? S2 C14 C15 S3 -0.7(5) . . . . ? C12 C11 N1 C9 0.1(7) . . . . ? C12 C11 N1 Cu1 -178.7(4) . . . . ? C10 C9 N1 C11 -2.4(7) . . . . ? C10 C9 N1 Cu1 176.4(3) . . . . ? N1 Cu1 N1 C11 59(57) 7_556 . . . ? O2 Cu1 N1 C11 -126.4(4) . . . . ? O2 Cu1 N1 C11 53.6(4) 7_556 . . . ? O1 Cu1 N1 C11 139.1(4) 7_556 . . . ? O1 Cu1 N1 C11 -40.9(4) . . . . ? N1 Cu1 N1 C9 -120(57) 7_556 . . . ? O2 Cu1 N1 C9 54.9(4) . . . . ? O2 Cu1 N1 C9 -125.1(4) 7_556 . . . ? O1 Cu1 N1 C9 -39.6(3) 7_556 . . . ? O1 Cu1 N1 C9 140.4(3) . . . . ? C6 C5 O1 Cu1 32.5(6) . . . . ? C4 C5 O1 Cu1 -147.7(4) . . . . ? N1 Cu1 O1 C5 55.9(4) 7_556 . . . ? N1 Cu1 O1 C5 -124.1(4) . . . . ? O2 Cu1 O1 C5 -35.5(4) . . . . ? O2 Cu1 O1 C5 144.5(4) 7_556 . . . ? O1 Cu1 O1 C5 174(100) 7_556 . . . ? C6 C7 O2 Cu1 -11.5(8) . . . . ? C8 C7 O2 Cu1 167.6(5) . . . . ? N1 Cu1 O2 C7 -63.2(4) 7_556 . . . ? N1 Cu1 O2 C7 116.8(4) . . . . ? O2 Cu1 O2 C7 157(92) 7_556 . . . ? O1 Cu1 O2 C7 -155.5(4) 7_556 . . . ? O1 Cu1 O2 C7 24.5(4) . . . . ? C5 C4 S1 C1 -178.5(5) . . . . ? C3 C4 S1 C1 -0.1(5) . . . . ? C2 C1 S1 C4 1.0(7) . . . . ? C15 C14 S2 C16 3.9(4) . . . . ? C13 C14 S2 C16 -174.6(3) . . . . ? C16 C16 S2 C14 173.8(5) 2_657 . . . ? S3 C16 S2 C14 -5.8(3) . . . . ? C14 C15 S3 C16 -2.9(4) . . . . ? C16 C16 S3 C15 -174.1(5) 2_657 . . . ? S2 C16 S3 C15 5.5(3) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.006 201 8 ' ' 2 0.500 0.500 -0.006 201 8 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.811 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.095 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 782323' #TrackingRef '- 1-4-all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 F6 Mn N2 O4 S6' _chemical_formula_sum 'C32 H18 F6 Mn N2 O4 S6' _chemical_formula_weight 855.84 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' Mn Mn 0.3368 0.7283 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.761(7) _cell_length_b 17.151(6) _cell_length_c 10.831(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.841(7) _cell_angle_gamma 90.00 _cell_volume 3869(2) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1783 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 23.6 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8983 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 '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 9468 _diffrn_reflns_av_R_equivalents 0.1107 _diffrn_reflns_av_sigmaI/netI 0.1787 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3409 _reflns_number_gt 1167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0650P)^2^+1.0000P] 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 3409 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1717 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _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 Mn1 Mn 0.2500 0.2500 0.0000 0.0829(7) Uani 1 2 d S . . C1 C 0.1544(7) 0.0454(8) -0.5187(12) 0.153(5) Uani 1 1 d . . . H1 H 0.1227 0.0128 -0.5685 0.183 Uiso 1 1 d R . . C2 C 0.2049(8) 0.0818(8) -0.5542(14) 0.144(5) Uani 1 1 d . . . H2 H 0.2090 0.0734 -0.6363 0.172 Uiso 1 1 d R . . C3 C 0.2485(6) 0.1267(6) -0.4784(9) 0.104(4) Uani 1 1 d . . . H3 H 0.2824 0.1525 -0.4967 0.124 Uiso 1 1 d R . . C4 C 0.2324(6) 0.1305(6) -0.3658(11) 0.108(4) Uani 1 1 d . . . C5 C 0.2644(6) 0.1708(7) -0.2443(11) 0.101(4) Uani 1 1 d . . . C6 C 0.3185(8) 0.2164(8) -0.2398(13) 0.115(4) Uani 1 1 d . . . H6 H 0.3328 0.2153 -0.3128 0.138 Uiso 1 1 d R . . C7 C 0.3529(7) 0.2621(9) -0.1402(16) 0.122(5) Uani 1 1 d . . . C8 C 0.4139(10) 0.3001(13) -0.144(2) 0.181(7) Uani 1 1 d . . . C9 C 0.2926(4) 0.0945(6) 0.1594(7) 0.083(3) Uani 1 1 d . . . H9 H 0.2624 0.0737 0.0879 0.100 Uiso 1 1 d R . . C10 C 0.3231(4) 0.0451(5) 0.2559(7) 0.077(3) Uani 1 1 d . . . H10 H 0.3131 -0.0078 0.2494 0.093 Uiso 1 1 d R . . C11 C 0.3482(4) 0.1972(5) 0.2647(7) 0.074(2) Uani 1 1 d . . . H11 H 0.3578 0.2501 0.2676 0.089 Uiso 1 1 d R . . C12 C 0.3811(4) 0.1516(5) 0.3667(7) 0.072(2) Uani 1 1 d . . . H12 H 0.4113 0.1741 0.4365 0.086 Uiso 1 1 d R . . C13 C 0.3692(4) 0.0726(5) 0.3650(6) 0.064(2) Uani 1 1 d . . . C14 C 0.4024(3) 0.0225(5) 0.4702(6) 0.062(2) Uani 1 1 d . . . C15 C 0.4043(4) -0.0557(5) 0.4711(6) 0.071(2) Uani 1 1 d . . . H15 H 0.3816 -0.0834 0.3983 0.085 Uiso 1 1 d R . . C16 C 0.4781(3) -0.0213(4) 0.6913(5) 0.058(2) Uani 1 1 d . . . F1 F 0.4145(5) 0.3754(6) -0.1321(10) 0.202(4) Uani 1 1 d . . . F2 F 0.4228(4) 0.2927(6) -0.2647(10) 0.218(4) Uani 1 1 d . . . F3 F 0.4646(4) 0.2757(6) -0.0644(10) 0.221(5) Uani 1 1 d . . . N1 N 0.3038(3) 0.1702(5) 0.1615(6) 0.071(2) Uani 1 1 d . . . O1 O 0.3378(3) 0.2779(4) -0.0379(6) 0.111(2) Uani 1 1 d . . . O2 O 0.2425(3) 0.1648(3) -0.1494(5) 0.0855(18) Uani 1 1 d . . . S1 S 0.1678(2) 0.0760(2) -0.3617(3) 0.1587(15) Uani 1 1 d . . . S2 S 0.44804(11) -0.10519(11) 0.60430(17) 0.0701(7) Uani 1 1 d . . . S3 S 0.44697(11) 0.06662(12) 0.61520(16) 0.0736(7) 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 Mn1 0.0702(13) 0.1181(16) 0.0556(10) 0.0202(10) 0.0106(9) 0.0217(12) C1 0.183(15) 0.138(12) 0.118(11) -0.021(8) 0.013(10) 0.022(11) C2 0.193(17) 0.132(13) 0.105(10) 0.008(9) 0.041(11) 0.044(12) C3 0.160(12) 0.101(8) 0.052(6) 0.001(6) 0.035(7) 0.057(8) C4 0.139(11) 0.104(8) 0.079(8) 0.011(6) 0.030(8) 0.042(8) C5 0.105(10) 0.115(9) 0.098(9) 0.056(8) 0.055(8) 0.061(8) C6 0.111(12) 0.133(11) 0.123(11) 0.063(9) 0.067(9) 0.054(9) C7 0.097(11) 0.133(12) 0.151(14) 0.077(11) 0.060(10) 0.038(9) C8 0.136(17) 0.19(2) 0.23(2) 0.081(18) 0.082(16) 0.005(17) C9 0.071(6) 0.110(8) 0.050(5) 0.012(5) -0.012(4) -0.001(6) C10 0.067(6) 0.092(6) 0.059(5) -0.004(5) -0.002(5) -0.024(5) C11 0.066(6) 0.076(6) 0.069(5) 0.003(5) 0.002(5) 0.008(5) C12 0.078(6) 0.076(6) 0.050(5) 0.000(5) -0.001(4) 0.009(5) C13 0.062(6) 0.075(6) 0.047(4) -0.004(4) 0.005(4) -0.003(5) C14 0.060(5) 0.075(6) 0.044(4) -0.001(4) 0.008(4) -0.009(5) C15 0.085(6) 0.066(6) 0.053(5) 0.002(4) 0.005(4) 0.000(5) C16 0.069(6) 0.060(4) 0.044(4) 0.005(3) 0.012(4) -0.003(4) F1 0.174(8) 0.185(8) 0.266(10) 0.053(8) 0.091(7) -0.017(8) F2 0.182(8) 0.247(11) 0.263(10) 0.043(9) 0.123(8) -0.011(7) F3 0.113(6) 0.247(10) 0.301(12) 0.115(8) 0.057(7) -0.006(7) N1 0.061(5) 0.086(5) 0.059(4) 0.008(4) 0.004(4) 0.009(4) O1 0.080(5) 0.155(7) 0.099(5) 0.040(5) 0.029(4) 0.019(4) O2 0.084(4) 0.100(4) 0.074(4) 0.031(3) 0.026(3) 0.022(4) S1 0.178(4) 0.173(3) 0.120(3) 0.004(2) 0.035(3) 0.023(3) S2 0.0847(16) 0.0629(14) 0.0548(12) 0.0004(10) 0.0079(11) -0.0054(12) S3 0.0851(16) 0.0681(14) 0.0514(11) -0.0039(10) -0.0057(11) -0.0001(13) _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 Mn1 O1 2.122(7) . ? Mn1 O1 2.122(7) 7 ? Mn1 O2 2.150(6) 7 ? Mn1 O2 2.150(6) . ? Mn1 N1 2.262(6) 7 ? Mn1 N1 2.262(6) . ? C1 C2 1.410(16) . ? C1 S1 1.721(12) . ? C1 H1 0.9300 . ? C2 C3 1.309(15) . ? C2 H2 0.9300 . ? C3 C4 1.364(12) . ? C3 H3 0.9300 . ? C4 C5 1.471(14) . ? C4 S1 1.701(12) . ? C5 O2 1.256(10) . ? C5 C6 1.402(14) . ? C6 C7 1.368(15) . ? C6 H6 0.9300 . ? C7 O1 1.273(15) . ? C7 C8 1.49(2) . ? C8 F3 1.256(18) . ? C8 F1 1.30(2) . ? C8 F2 1.39(2) . ? C9 N1 1.319(9) . ? C9 C10 1.361(10) . ? C9 H9 0.9300 . ? C10 C13 1.392(9) . ? C10 H10 0.9300 . ? C11 N1 1.331(8) . ? C11 C12 1.373(9) . ? C11 H11 0.9300 . ? C12 C13 1.379(9) . ? C12 H12 0.9300 . ? C13 C14 1.443(10) . ? C14 C15 1.341(9) . ? C14 S3 1.760(7) . ? C15 S2 1.707(7) . ? C15 H15 0.9300 . ? C16 C16 1.351(11) 2_656 ? C16 S2 1.741(7) . ? C16 S3 1.757(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 180.00(11) . 7 ? O1 Mn1 O2 96.6(3) . 7 ? O1 Mn1 O2 83.4(3) 7 7 ? O1 Mn1 O2 83.4(3) . . ? O1 Mn1 O2 96.6(3) 7 . ? O2 Mn1 O2 180.0(3) 7 . ? O1 Mn1 N1 90.4(2) . 7 ? O1 Mn1 N1 89.6(2) 7 7 ? O2 Mn1 N1 94.6(2) 7 7 ? O2 Mn1 N1 85.4(2) . 7 ? O1 Mn1 N1 89.6(2) . . ? O1 Mn1 N1 90.4(2) 7 . ? O2 Mn1 N1 85.4(2) 7 . ? O2 Mn1 N1 94.6(2) . . ? N1 Mn1 N1 180.0(3) 7 . ? C2 C1 S1 102.3(11) . . ? C2 C1 H1 127.9 . . ? S1 C1 H1 129.8 . . ? C3 C2 C1 124.7(15) . . ? C3 C2 H2 116.0 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 105.2(13) . . ? C2 C3 H3 128.4 . . ? C4 C3 H3 126.3 . . ? C3 C4 C5 130.2(13) . . ? C3 C4 S1 115.1(10) . . ? C5 C4 S1 114.5(9) . . ? O2 C5 C6 122.0(12) . . ? O2 C5 C4 120.1(13) . . ? C6 C5 C4 117.8(12) . . ? C7 C6 C5 127.5(13) . . ? C7 C6 H6 116.1 . . ? C5 C6 H6 116.4 . . ? O1 C7 C6 126.0(14) . . ? O1 C7 C8 112.7(19) . . ? C6 C7 C8 121.3(18) . . ? F3 C8 F1 107(2) . . ? F3 C8 F2 106.3(19) . . ? F1 C8 F2 100.5(15) . . ? F3 C8 C7 116.7(15) . . ? F1 C8 C7 114.6(19) . . ? F2 C8 C7 110.7(19) . . ? N1 C9 C10 123.6(7) . . ? N1 C9 H9 118.4 . . ? C10 C9 H9 118.0 . . ? C9 C10 C13 120.8(8) . . ? C9 C10 H10 119.9 . . ? C13 C10 H10 119.3 . . ? N1 C11 C12 124.1(8) . . ? N1 C11 H11 117.9 . . ? C12 C11 H11 118.0 . . ? C11 C12 C13 119.8(7) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 120.3 . . ? C12 C13 C10 115.5(7) . . ? C12 C13 C14 121.7(7) . . ? C10 C13 C14 122.8(8) . . ? C15 C14 C13 127.5(7) . . ? C15 C14 S3 114.6(6) . . ? C13 C14 S3 118.0(6) . . ? C14 C15 S2 120.8(6) . . ? C14 C15 H15 119.8 . . ? S2 C15 H15 119.4 . . ? C16 C16 S2 124.2(2) 2_656 . ? C16 C16 S3 120.8(2) 2_656 . ? S2 C16 S3 115.0(3) . . ? C9 N1 C11 116.2(7) . . ? C9 N1 Mn1 122.0(5) . . ? C11 N1 Mn1 121.8(6) . . ? C7 O1 Mn1 126.5(10) . . ? C5 O2 Mn1 126.6(8) . . ? C4 S1 C1 92.6(7) . . ? C15 S2 C16 94.4(3) . . ? C16 S3 C14 95.0(4) . . ? 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 S1 C1 C2 C3 0.0(17) . . . . ? C1 C2 C3 C4 -1.6(18) . . . . ? C2 C3 C4 C5 178.5(10) . . . . ? C2 C3 C4 S1 2.6(12) . . . . ? C3 C4 C5 O2 -177.7(9) . . . . ? S1 C4 C5 O2 -1.7(11) . . . . ? C3 C4 C5 C6 3.4(15) . . . . ? S1 C4 C5 C6 179.4(7) . . . . ? O2 C5 C6 C7 -3.1(17) . . . . ? C4 C5 C6 C7 175.8(11) . . . . ? C5 C6 C7 O1 -8(2) . . . . ? C5 C6 C7 C8 172.8(12) . . . . ? O1 C7 C8 F3 69(3) . . . . ? C6 C7 C8 F3 -112(2) . . . . ? O1 C7 C8 F1 -57(2) . . . . ? C6 C7 C8 F1 123(2) . . . . ? O1 C7 C8 F2 -169.7(13) . . . . ? C6 C7 C8 F2 10(2) . . . . ? N1 C9 C10 C13 -0.2(13) . . . . ? N1 C11 C12 C13 0.9(13) . . . . ? C11 C12 C13 C10 -0.2(12) . . . . ? C11 C12 C13 C14 -179.7(7) . . . . ? C9 C10 C13 C12 -0.1(12) . . . . ? C9 C10 C13 C14 179.4(8) . . . . ? C12 C13 C14 C15 -166.9(9) . . . . ? C10 C13 C14 C15 13.7(13) . . . . ? C12 C13 C14 S3 12.1(11) . . . . ? C10 C13 C14 S3 -167.3(6) . . . . ? C13 C14 C15 S2 178.3(6) . . . . ? S3 C14 C15 S2 -0.7(10) . . . . ? C10 C9 N1 C11 0.8(13) . . . . ? C10 C9 N1 Mn1 -178.6(6) . . . . ? C12 C11 N1 C9 -1.1(12) . . . . ? C12 C11 N1 Mn1 178.3(6) . . . . ? O1 Mn1 N1 C9 -117.7(7) . . . . ? O1 Mn1 N1 C9 62.3(7) 7 . . . ? O2 Mn1 N1 C9 145.6(7) 7 . . . ? O2 Mn1 N1 C9 -34.4(7) . . . . ? N1 Mn1 N1 C9 55(24) 7 . . . ? O1 Mn1 N1 C11 62.9(6) . . . . ? O1 Mn1 N1 C11 -117.1(6) 7 . . . ? O2 Mn1 N1 C11 -33.8(6) 7 . . . ? O2 Mn1 N1 C11 146.2(6) . . . . ? N1 Mn1 N1 C11 -124(24) 7 . . . ? C6 C7 O1 Mn1 -7.9(16) . . . . ? C8 C7 O1 Mn1 171.5(10) . . . . ? O1 Mn1 O1 C7 106(64) 7 . . . ? O2 Mn1 O1 C7 -159.5(8) 7 . . . ? O2 Mn1 O1 C7 20.5(8) . . . . ? N1 Mn1 O1 C7 -64.8(9) 7 . . . ? N1 Mn1 O1 C7 115.2(9) . . . . ? C6 C5 O2 Mn1 28.0(12) . . . . ? C4 C5 O2 Mn1 -150.9(7) . . . . ? O1 Mn1 O2 C5 -31.0(7) . . . . ? O1 Mn1 O2 C5 149.0(7) 7 . . . ? O2 Mn1 O2 C5 171(100) 7 . . . ? N1 Mn1 O2 C5 60.0(7) 7 . . . ? N1 Mn1 O2 C5 -120.0(7) . . . . ? C3 C4 S1 C1 -2.4(9) . . . . ? C5 C4 S1 C1 -179.0(8) . . . . ? C2 C1 S1 C4 1.3(10) . . . . ? C14 C15 S2 C16 -2.6(8) . . . . ? C16 C16 S2 C15 -175.0(9) 2_656 . . . ? S3 C16 S2 C15 5.0(5) . . . . ? C16 C16 S3 C14 174.7(8) 2_656 . . . ? S2 C16 S3 C14 -5.3(5) . . . . ? C15 C14 S3 C16 3.6(7) . . . . ? C13 C14 S3 C16 -175.5(6) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.006 256 53 ' ' 2 0.500 0.500 -0.003 256 53 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.353 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.083 #===END