# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address M.H.Alkordi ; 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620, USA. Advanced Membranes &Porous Materials Center, 4700 King Abdullah University of, Science and Technology (KAUST), Thuwal 23955-6900, Kingdom of Saudi Arabia. ; J.L.Belof ; 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620 USA ; E.Rivera ; 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620 USA ; L.Wojtas ; 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620 USA ; M.Eddaoudi ; 4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620, USA. Advanced Membranes &Porous Materials Center, 4700 King Abdullah University of, Science and Technology (KAUST), Thuwal 23955-6900, Kingdom of Saudi Arabia. ; _publ_section_title ; Insight into the Construction of Metal-Organic Polyhedra: Metal-Organic Cubes as a Case Study ; _publ_contact_author_name 'Dr. Mohamed Eddaoudi' _publ_contact_author_address ;4202 E. Fowler Avenue, CHE 205, Tampa, FL 33620 USA ; _publ_contact_author_email eddaoudi@cas.usf.edu _publ_contact_author_phone 813-974-9622 # Attachment '- Compound 1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 824164' #TrackingRef '- Compound 1.cif' _publ_section_comment ; one methylene carbon atom is disordered between two sites (C111-C112) with site occupancy (0.774 and 0.226). Several disordered water solvent molecules are present (O21-O25). ; #Added by publCIF _audit_update_record ; 2010-11-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H180 Cl12 Co8 N72 O4' _chemical_formula_weight 3736.29 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_int_tables_number 205 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 25.1026(13) _cell_length_b 25.1026(13) _cell_length_c 25.1026(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15818.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description polyhedra _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7699 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8982 _exptl_absorpt_correction_T_max 0.8982 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _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 86413 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.36 _reflns_number_total 5390 _reflns_number_gt 4141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0818P)^2^+29.1480P] 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 5390 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.196913(18) 0.466866(18) 0.051335(18) 0.01904(15) Uani 1 1 d . . . Co2 Co 0.115468(18) 0.615467(18) -0.115468(18) 0.0198(2) Uani 1 3 d S . . C1 C 0.14038(13) 0.52727(13) -0.03687(14) 0.0203(7) Uani 1 1 d . . . H1 H 0.1182 0.4999 -0.0506 0.024 Uiso 1 1 calc R . . C2 C 0.18879(15) 0.65832(15) -0.04529(15) 0.0262(8) Uani 1 1 d . . . C3 C 0.22926(14) 0.57173(15) 0.06100(15) 0.0255(8) Uani 1 1 d . . . C6 C 0.17955(14) 0.60399(14) -0.02683(14) 0.0231(7) Uani 1 1 d . . . C7 C 0.19665(14) 0.57030(14) 0.01304(15) 0.0235(7) Uani 1 1 d . . . C8 C 0.26578(16) 0.52208(16) 0.13353(16) 0.0314(9) Uani 1 1 d . . . C9 C 0.23094(19) 0.74485(18) -0.03593(19) 0.0441(11) Uani 1 1 d . . . H9A H 0.2605 0.7495 -0.0616 0.053 Uiso 1 1 calc R . . H9B H 0.2391 0.7661 -0.0037 0.053 Uiso 1 1 calc R . . C10 C 0.16343(16) 0.72701(15) -0.10493(16) 0.0313(9) Uani 1 1 d . . . H10A H 0.1285 0.7385 -0.1191 0.038 Uiso 1 1 calc R . . H10B H 0.1898 0.7291 -0.1342 0.038 Uiso 1 1 calc R . . C111 C 0.2566(3) 0.5737(2) 0.1647(2) 0.0370(19) Uani 0.774(14) 1 d P A 1 H11A H 0.2185 0.5768 0.1742 0.044 Uiso 0.774(14) 1 calc PR A 1 H11B H 0.2775 0.5728 0.1982 0.044 Uiso 0.774(14) 1 calc PR A 1 H8A H 0.3044 0.5171 0.1270 0.037 Uiso 1 1 d . B 1 H8B H 0.2526 0.4914 0.1544 0.037 Uiso 1 1 d . C 1 H12A H 0.3117 0.6192 0.1277 0.057 Uiso 1 1 d . D 1 H12B H 0.2633 0.6529 0.1521 0.057 Uiso 1 1 d . E 1 C112 C 0.2971(11) 0.5689(7) 0.1451(9) 0.042(8) Uani 0.226(14) 1 d P A 2 H11C H 0.3309 0.5663 0.1250 0.050 Uiso 0.226(14) 1 calc PR A 2 H11D H 0.3061 0.5685 0.1835 0.050 Uiso 0.226(14) 1 calc PR A 2 C12 C 0.2726(2) 0.61973(18) 0.1328(2) 0.0470(12) Uani 1 1 d . . . C13 C 0.1800(2) 0.76356(16) -0.0601(2) 0.0428(11) Uani 1 1 d . . . H13A H 0.1847 0.8002 -0.0740 0.051 Uiso 1 1 calc R . . H13B H 0.1518 0.7644 -0.0326 0.051 Uiso 1 1 calc R . . C21 C 0.14359(14) 0.44819(14) 0.14723(14) 0.0218(7) Uani 1 1 d . . . C22 C 0.18632(14) 0.40791(13) 0.14443(14) 0.0218(7) Uani 1 1 d . . . C23 C 0.23654(15) 0.33352(16) 0.18179(17) 0.0322(9) Uani 1 1 d . . . H23A H 0.2261 0.3005 0.1628 0.039 Uiso 1 1 calc R . . H23B H 0.2469 0.3239 0.2186 0.039 Uiso 1 1 calc R . . C24 C 0.26513(15) 0.37948(15) 0.09921(16) 0.0294(8) Uani 1 1 d . . . H24A H 0.2947 0.3995 0.0824 0.035 Uiso 1 1 calc R . . H24B H 0.2564 0.3488 0.0761 0.035 Uiso 1 1 calc R . . C25 C 0.28272(16) 0.35948(16) 0.15371(17) 0.0342(9) Uani 1 1 d . . . H25A H 0.3120 0.3334 0.1495 0.041 Uiso 1 1 calc R . . H25B H 0.2961 0.3897 0.1753 0.041 Uiso 1 1 calc R . . C27 C 0.10936(13) 0.39424(13) 0.01654(13) 0.0192(7) Uani 1 1 d . . . H27 H 0.0837 0.4036 0.0427 0.023 Uiso 1 1 calc R . . C28 C 0.18256(14) 0.39326(14) -0.03073(13) 0.0208(7) Uani 1 1 d . . . C29 C 0.23721(14) 0.41403(14) -0.03711(15) 0.0241(8) Uani 1 1 d . . . C31 C 0.32159(16) 0.42154(19) -0.08355(18) 0.0392(10) Uani 1 1 d . . . H31A H 0.3195 0.4537 -0.1063 0.047 Uiso 1 1 calc R . . H31B H 0.3454 0.3955 -0.1011 0.047 Uiso 1 1 calc R . . C32 C 0.34355(18) 0.4361(2) -0.03024(19) 0.0437(11) Uani 1 1 d . . . H32A H 0.3780 0.4548 -0.0347 0.052 Uiso 1 1 calc R . . H32B H 0.3500 0.4034 -0.0092 0.052 Uiso 1 1 calc R . . C33 C 0.30467(15) 0.47171(16) -0.00109(17) 0.0313(9) Uani 1 1 d . . . H33A H 0.3175 0.4778 0.0357 0.038 Uiso 1 1 calc R . . H33B H 0.3026 0.5066 -0.0193 0.038 Uiso 1 1 calc R . . N1 N 0.15968(12) 0.67203(12) -0.08595(12) 0.0236(6) Uani 1 1 d . . . N2 N 0.25135(12) 0.44724(12) 0.00048(12) 0.0237(6) Uani 1 1 d . . . N3 N 0.15764(11) 0.41554(11) 0.01270(11) 0.0198(6) Uani 1 1 d . . . N4 N 0.14206(11) 0.47871(11) 0.10198(11) 0.0191(6) Uani 1 1 d . . . N5 N 0.17247(11) 0.52209(11) 0.00500(11) 0.0199(6) Uani 1 1 d . . . N6 N 0.21835(11) 0.41418(11) 0.10403(12) 0.0224(6) Uani 1 1 d . . . N7 N 0.23724(12) 0.52513(12) 0.08255(12) 0.0230(6) Uani 1 1 d . A . N8 N 0.14374(11) 0.57647(11) -0.05677(11) 0.0203(6) Uani 1 1 d . . . N9 N 0.19188(12) 0.37076(12) 0.18284(12) 0.0265(7) Uani 1 1 d . . . H200 H 0.1640 0.3619 0.2036 0.032 Uiso 1 1 d R . . N10 N 0.24556(15) 0.61840(14) 0.08123(14) 0.0366(8) Uani 1 1 d . A . H101 H 0.2258 0.6505 0.0714 0.044 Uiso 1 1 d R . . N11 N 0.22576(15) 0.68848(14) -0.02164(15) 0.0401(9) Uani 1 1 d . . . H111 H 0.2580 0.6692 -0.0105 0.048 Uiso 1 1 d R . . N12 N 0.26845(13) 0.39845(13) -0.07734(13) 0.0305(7) Uani 1 1 d . . . H201 H 0.2553 0.3906 -0.1092 0.037 Uiso 1 1 d R . . Cl1 Cl 0.23348(4) 0.39873(5) 0.80399(4) 0.0407(3) Uani 1 1 d . . . Cl2 Cl 0.95664(8) 0.17243(7) 0.11213(6) 0.0646(5) Uani 0.83333 1 d P . . Cl3 Cl 0.5000 0.0000 0.0000 0.0435(6) Uani 1 6 d S . . O21 O 0.9607(7) 0.1246(8) 0.0992(7) 0.030(4) Uiso 0.15 1 d P . . O22 O 0.9725(14) 0.0952(15) 0.0836(14) 0.085(9) Uiso 0.15 1 d P . . O23 O 1.0817(10) 0.0817(10) 0.0817(10) 0.141(14) Uiso 0.30 3 d SP . . O24 O 1.0496(8) 0.0496(8) 0.0496(8) 0.110(10) Uiso 0.30 3 d SP . . O25 O 0.9874(15) 0.0654(16) 0.0637(16) 0.058(9) Uiso 0.10 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0174(2) 0.0187(3) 0.0210(3) -0.00163(18) -0.00041(18) 0.00078(18) Co2 0.0198(2) 0.0198(2) 0.0198(2) 0.00137(18) 0.00137(18) -0.00137(18) C1 0.0191(17) 0.0186(17) 0.0231(17) 0.0001(14) 0.0025(14) 0.0024(13) C2 0.0257(19) 0.0248(19) 0.0282(19) 0.0023(15) 0.0029(16) -0.0042(15) C3 0.0234(18) 0.0253(19) 0.0277(19) -0.0007(15) -0.0039(15) -0.0042(15) C6 0.0206(17) 0.0230(18) 0.0257(19) 0.0004(14) -0.0020(14) -0.0039(14) C7 0.0221(18) 0.0230(18) 0.0254(18) 0.0014(14) 0.0026(15) -0.0002(14) C8 0.033(2) 0.031(2) 0.030(2) 0.0014(16) -0.0131(17) -0.0031(17) C9 0.055(3) 0.034(2) 0.043(3) 0.005(2) -0.012(2) -0.021(2) C10 0.032(2) 0.0246(19) 0.037(2) 0.0055(16) -0.0044(17) -0.0054(16) C111 0.049(4) 0.037(3) 0.025(3) -0.003(2) -0.012(3) -0.010(3) C112 0.068(19) 0.023(9) 0.034(11) 0.008(8) -0.025(11) -0.017(10) C12 0.054(3) 0.036(2) 0.051(3) -0.006(2) -0.023(2) -0.006(2) C13 0.052(3) 0.022(2) 0.054(3) -0.0023(19) -0.001(2) -0.0074(19) C21 0.0202(17) 0.0227(17) 0.0227(18) 0.0016(14) -0.0037(14) -0.0010(14) C22 0.0213(17) 0.0178(16) 0.0262(18) -0.0008(14) -0.0061(15) 0.0007(14) C23 0.033(2) 0.030(2) 0.034(2) 0.0055(17) -0.0024(17) 0.0107(17) C24 0.0240(19) 0.0257(19) 0.039(2) 0.0003(17) 0.0007(16) 0.0067(15) C25 0.027(2) 0.031(2) 0.045(2) 0.0043(18) 0.0003(18) 0.0079(17) C27 0.0187(16) 0.0204(17) 0.0186(16) -0.0004(13) -0.0002(13) 0.0006(14) C28 0.0255(18) 0.0196(17) 0.0171(16) 0.0003(13) 0.0013(14) 0.0039(14) C29 0.0232(18) 0.0225(18) 0.0264(19) 0.0008(15) 0.0011(15) 0.0024(14) C31 0.028(2) 0.047(3) 0.043(3) -0.007(2) 0.0140(19) -0.0020(19) C32 0.030(2) 0.050(3) 0.052(3) -0.007(2) 0.004(2) 0.002(2) C33 0.0228(19) 0.031(2) 0.040(2) -0.0062(17) 0.0043(17) -0.0040(16) N1 0.0250(16) 0.0200(15) 0.0259(16) 0.0022(12) 0.0005(13) -0.0033(12) N2 0.0191(15) 0.0254(16) 0.0265(16) -0.0019(13) 0.0018(13) 0.0015(12) N3 0.0199(14) 0.0191(14) 0.0206(14) -0.0013(12) -0.0012(12) 0.0020(11) N4 0.0188(14) 0.0194(14) 0.0190(14) -0.0025(11) -0.0007(11) -0.0020(11) N5 0.0184(14) 0.0201(14) 0.0213(15) -0.0026(12) 0.0002(12) -0.0012(11) N6 0.0183(14) 0.0201(15) 0.0288(16) -0.0011(12) -0.0026(12) 0.0034(12) N7 0.0223(15) 0.0244(16) 0.0223(15) -0.0028(12) -0.0032(12) 0.0012(12) N8 0.0176(14) 0.0210(15) 0.0221(15) 0.0005(12) 0.0005(11) 0.0000(12) N9 0.0237(15) 0.0267(16) 0.0290(16) 0.0065(13) 0.0016(13) 0.0052(13) N10 0.044(2) 0.0269(18) 0.039(2) -0.0011(15) -0.0160(16) -0.0043(15) N11 0.044(2) 0.0306(18) 0.045(2) 0.0097(16) -0.0185(17) -0.0170(16) N12 0.0268(17) 0.0338(18) 0.0307(18) -0.0101(14) 0.0069(14) -0.0018(14) Cl1 0.0339(5) 0.0480(6) 0.0401(6) 0.0127(5) 0.0016(4) 0.0011(5) Cl2 0.0892(13) 0.0623(10) 0.0421(8) 0.0083(7) 0.0011(8) -0.0073(9) Cl3 0.0435(6) 0.0435(6) 0.0435(6) 0.0040(7) -0.0040(7) 0.0040(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.890(3) . ? Co1 N4 1.898(3) . ? Co1 N5 1.911(3) . ? Co1 N2 1.934(3) . ? Co1 N7 1.944(3) . ? Co1 N6 1.946(3) . ? Co2 N8 1.906(3) 11_455 ? Co2 N8 1.906(3) . ? Co2 N8 1.906(3) 8 ? Co2 N1 1.948(3) 11_455 ? Co2 N1 1.949(3) 8 ? Co2 N1 1.949(3) . ? C1 N5 1.331(4) . ? C1 N8 1.335(4) . ? C1 H1 0.9500 . ? C2 N1 1.301(5) . ? C2 N11 1.337(5) . ? C2 C6 1.459(5) . ? C3 N7 1.304(5) . ? C3 N10 1.341(5) . ? C3 C7 1.456(5) . ? C6 N8 1.360(4) . ? C6 C7 1.379(5) . ? C7 N5 1.369(4) . ? C8 C112 1.442(18) . ? C8 N7 1.468(5) . ? C8 C111 1.531(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9879 . ? C9 N11 1.466(5) . ? C9 C13 1.491(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N1 1.463(5) . ? C10 C13 1.510(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C111 C12 1.463(8) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C112 C12 1.45(2) . ? C112 H11C 0.9900 . ? C112 H11D 0.9900 . ? C12 N10 1.463(5) . ? C12 H12A 0.9906 . ? C12 H12B 0.9912 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C21 N4 1.371(4) . ? C21 C28 1.386(5) 23_665 ? C21 C22 1.476(5) . ? C22 N6 1.304(5) . ? C22 N9 1.348(4) . ? C23 N9 1.460(5) . ? C23 C25 1.505(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N6 1.467(4) . ? C24 C25 1.523(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 N3 1.328(4) . ? C27 N4 1.329(4) 20_565 ? C27 H27 0.9500 . ? C28 N3 1.376(4) . ? C28 C21 1.386(5) 20_565 ? C28 C29 1.476(5) . ? C29 N2 1.308(5) . ? C29 N12 1.337(5) . ? C31 N12 1.463(5) . ? C31 C32 1.493(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.513(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N2 1.473(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? N4 C27 1.329(4) 23_665 ? N9 H200 0.9003 . ? N10 H101 0.9773 . ? N11 H111 0.9827 . ? N12 H201 0.8872 . ? Cl2 O21 1.25(2) . ? Cl2 O22 2.10(4) . ? O21 O22 0.89(4) . ? O22 O25 0.97(4) . ? O23 O24 1.40(5) . ? O24 O25 1.65(4) . ? O24 O25 1.65(4) 5_645 ? O24 O25 1.65(4) 9_654 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N4 94.14(12) . . ? N3 Co1 N5 90.84(12) . . ? N4 Co1 N5 93.51(12) . . ? N3 Co1 N2 81.73(12) . . ? N4 Co1 N2 174.25(12) . . ? N5 Co1 N2 90.57(12) . . ? N3 Co1 N7 172.50(13) . . ? N4 Co1 N7 89.42(12) . . ? N5 Co1 N7 82.34(12) . . ? N2 Co1 N7 95.15(13) . . ? N3 Co1 N6 91.71(12) . . ? N4 Co1 N6 81.47(12) . . ? N5 Co1 N6 174.52(12) . . ? N2 Co1 N6 94.60(13) . . ? N7 Co1 N6 95.35(12) . . ? N8 Co2 N8 94.71(12) 11_455 . ? N8 Co2 N8 94.71(12) 11_455 8 ? N8 Co2 N8 94.71(12) . 8 ? N8 Co2 N1 82.43(12) 11_455 11_455 ? N8 Co2 N1 88.49(12) . 11_455 ? N8 Co2 N1 175.88(12) 8 11_455 ? N8 Co2 N1 88.49(12) 11_455 8 ? N8 Co2 N1 175.88(12) . 8 ? N8 Co2 N1 82.43(12) 8 8 ? N1 Co2 N1 94.51(12) 11_455 8 ? N8 Co2 N1 175.88(12) 11_455 . ? N8 Co2 N1 82.43(12) . . ? N8 Co2 N1 88.49(12) 8 . ? N1 Co2 N1 94.51(12) 11_455 . ? N1 Co2 N1 94.51(12) 8 . ? N5 C1 N8 110.4(3) . . ? N5 C1 H1 124.8 . . ? N8 C1 H1 124.8 . . ? N1 C2 N11 126.0(3) . . ? N1 C2 C6 114.0(3) . . ? N11 C2 C6 119.9(3) . . ? N7 C3 N10 125.4(3) . . ? N7 C3 C7 114.0(3) . . ? N10 C3 C7 120.4(3) . . ? N8 C6 C7 107.2(3) . . ? N8 C6 C2 113.8(3) . . ? C7 C6 C2 139.0(3) . . ? N5 C7 C6 107.3(3) . . ? N5 C7 C3 113.1(3) . . ? C6 C7 C3 139.5(3) . . ? C112 C8 N7 113.5(8) . . ? N7 C8 C111 109.2(3) . . ? C112 C8 H8A 66.6 . . ? N7 C8 H8A 109.9 . . ? C111 C8 H8A 109.8 . . ? C112 C8 H8B 135.2 . . ? N7 C8 H8B 109.8 . . ? C111 C8 H8B 109.8 . . ? H8A C8 H8B 108.4 . . ? N11 C9 C13 109.1(3) . . ? N11 C9 H9A 109.9 . . ? C13 C9 H9A 109.9 . . ? N11 C9 H9B 109.9 . . ? C13 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N1 C10 C13 110.4(3) . . ? N1 C10 H10A 109.6 . . ? C13 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C13 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C111 C8 110.3(5) . . ? C12 C111 H11A 109.6 . . ? C8 C111 H11A 109.6 . . ? C12 C111 H11B 109.6 . . ? C8 C111 H11B 109.6 . . ? H11A C111 H11B 108.1 . . ? C8 C112 C12 116.3(16) . . ? C12 C112 H8A 144.1 . . ? C8 C112 H12A 145.4 . . ? H8A C112 H12A 135.6 . . ? C8 C112 H11C 108.2 . . ? C12 C112 H11C 108.2 . . ? H8A C112 H11C 70.1 . . ? H12A C112 H11C 70.8 . . ? C8 C112 H11D 108.2 . . ? C12 C112 H11D 108.2 . . ? H8A C112 H11D 106.2 . . ? H12A C112 H11D 104.8 . . ? H11C C112 H11D 107.4 . . ? C112 C12 C111 45.9(10) . . ? C112 C12 N10 111.4(8) . . ? C111 C12 N10 109.8(4) . . ? C112 C12 H12A 66.1 . . ? C111 C12 H12A 109.4 . . ? N10 C12 H12A 110.2 . . ? C112 C12 H12B 137.4 . . ? C111 C12 H12B 109.4 . . ? N10 C12 H12B 110.0 . . ? H12A C12 H12B 108.0 . . ? C9 C13 C10 110.4(4) . . ? C9 C13 H13A 109.6 . . ? C10 C13 H13A 109.6 . . ? C9 C13 H13B 109.6 . . ? C10 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N4 C21 C28 107.3(3) . 23_665 ? N4 C21 C22 111.3(3) . . ? C28 C21 C22 141.0(3) 23_665 . ? N6 C22 N9 125.2(3) . . ? N6 C22 C21 113.7(3) . . ? N9 C22 C21 121.0(3) . . ? N9 C23 C25 108.8(3) . . ? N9 C23 H23A 109.9 . . ? C25 C23 H23A 109.9 . . ? N9 C23 H23B 109.9 . . ? C25 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N6 C24 C25 110.7(3) . . ? N6 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C23 C25 C24 109.9(3) . . ? C23 C25 H25A 109.7 . . ? C24 C25 H25A 109.7 . . ? C23 C25 H25B 109.7 . . ? C24 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? N3 C27 N4 110.6(3) . 20_565 ? N3 C27 H27 124.7 . . ? N4 C27 H27 124.7 20_565 . ? N3 C28 C21 106.4(3) . 20_565 ? N3 C28 C29 111.4(3) . . ? C21 C28 C29 142.1(3) 20_565 . ? N2 C29 N12 124.9(3) . . ? N2 C29 C28 113.5(3) . . ? N12 C29 C28 121.6(3) . . ? N12 C31 C32 109.8(3) . . ? N12 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? N12 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 C32 C33 109.9(4) . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? N2 C33 C32 110.7(3) . . ? N2 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C2 N1 C10 117.9(3) . . ? C2 N1 Co2 115.2(2) . . ? C10 N1 Co2 126.9(2) . . ? C29 N2 C33 119.5(3) . . ? C29 N2 Co1 116.5(2) . . ? C33 N2 Co1 123.6(2) . . ? C27 N3 C28 108.0(3) . . ? C27 N3 Co1 135.5(2) . . ? C28 N3 Co1 116.5(2) . . ? C27 N4 C21 107.6(3) 23_665 . ? C27 N4 Co1 134.7(2) 23_665 . ? C21 N4 Co1 116.6(2) . . ? C1 N5 C7 107.4(3) . . ? C1 N5 Co1 138.3(2) . . ? C7 N5 Co1 114.2(2) . . ? C22 N6 C24 119.1(3) . . ? C22 N6 Co1 116.1(2) . . ? C24 N6 Co1 124.7(2) . . ? C3 N7 C8 118.9(3) . . ? C3 N7 Co1 115.3(2) . . ? C8 N7 Co1 124.5(2) . . ? C1 N8 C6 107.8(3) . . ? C1 N8 Co2 137.8(2) . . ? C6 N8 Co2 114.4(2) . . ? C22 N9 C23 120.6(3) . . ? C22 N9 H200 120.3 . . ? C23 N9 H200 116.6 . . ? C3 N10 C12 119.8(3) . . ? C3 N10 H101 118.0 . . ? C12 N10 H101 116.1 . . ? C2 N11 C9 120.0(3) . . ? C2 N11 H111 114.8 . . ? C9 N11 H111 118.1 . . ? C29 N12 C31 120.0(3) . . ? C29 N12 H201 121.8 . . ? C31 N12 H201 109.4 . . ? O22 O21 Cl2 161(3) . . ? O21 O22 O25 174(5) . . ? O25 O22 Cl2 163(4) . . ? O23 O24 O25 106.5(19) . . ? O23 O24 O25 106.5(19) . 5_645 ? O25 O24 O25 112.3(16) . 5_645 ? O23 O24 O25 106.5(19) . 9_654 ? O25 O24 O25 112.3(16) . 9_654 ? O25 O24 O25 112.3(16) 5_645 9_654 ? O22 O25 O24 131(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.816 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.095 _exptl_crystal_recrystallization_method Solvothermal data_1a _database_code_depnum_ccdc_archive 'CCDC 824165' #TrackingRef '- Compound 1a.cif' _publ_section_comment ; Several Br counterions and water solvent molecules are disordered throughout the structure. ; #Added by publCIF _audit_update_record ; 2009-11-14 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H156 Br12 Co8 N72 O18' _chemical_formula_weight 4469.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.758(5) _cell_length_b 19.380(3) _cell_length_c 24.772(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.257(16) _cell_angle_gamma 90.00 _cell_volume 8525(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 9.916 _exptl_absorpt_correction_T_min 0.4371 _exptl_absorpt_correction_T_max 0.4371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36096 _diffrn_reflns_av_R_equivalents 0.1342 _diffrn_reflns_av_sigmaI/netI 0.1722 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 54.24 _reflns_number_total 9974 _reflns_number_gt 4533 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1390P)^2^+0.1000P] 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 9974 _refine_ls_number_parameters 1115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1959 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2615 _refine_ls_wR_factor_gt 0.1984 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.003 _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 Br1 Br 0.28128(11) 0.67911(12) 0.27318(8) 0.0640(6) Uani 1 1 d . . . Br2 Br 0.5000 0.0000 0.0000 0.0410(6) Uani 1 2 d S . . Br3 Br 0.3892(2) 0.1936(2) 0.59655(13) 0.1449(17) Uani 0.90 1 d P . . Br4 Br 0.48921(13) 0.84169(12) 0.64645(9) 0.0889(8) Uani 1 1 d . . . Br6 Br -0.1026(4) 0.8814(4) 0.5915(2) 0.102(2) Uani 0.60 1 d P . . Br7 Br 0.1326(2) 0.9616(2) 0.78371(18) 0.1413(17) Uani 0.80 1 d P . . Br8 Br 0.0748(6) 1.0357(5) 0.7144(4) 0.181(4) Uani 0.40 1 d P . . Br9 Br 0.2201(15) 0.9803(11) 0.8595(9) 0.235(12) Uani 0.20 1 d P . . Br10 Br -0.0878(9) 1.0039(8) 0.6596(6) 0.122(5) Uani 0.20 1 d P . . Br11 Br -0.0865(10) 0.9138(8) 0.6107(6) 0.110(5) Uani 0.30 1 d P . . Br12 Br -0.0115(18) 1.0221(16) 0.6888(14) 0.131(11) Uani 0.10 1 d P . . Co1 Co 0.26472(13) 0.40477(12) 0.44842(9) 0.0352(7) Uani 1 1 d . . . Co2 Co 0.21068(13) 0.68652(12) 0.53442(9) 0.0363(7) Uani 1 1 d . . . Co3 Co -0.05494(13) 0.70897(12) 0.38450(9) 0.0346(7) Uani 1 1 d . . . Co4 Co -0.00225(13) 0.42584(13) 0.30028(9) 0.0368(7) Uani 1 1 d . . . C1 C -0.0411(8) 0.5581(9) 0.3582(5) 0.031(4) Uani 1 1 d . . . H1 H -0.0742 0.5402 0.3847 0.038 Uiso 1 1 calc R . . C2 C 0.0240(8) 0.6287(9) 0.3128(6) 0.038(4) Uani 1 1 d . . . C3 C 0.0380(9) 0.5629(9) 0.2957(5) 0.038(4) Uani 1 1 d . . . C4 C 0.0463(9) 0.6974(10) 0.2996(6) 0.047(5) Uani 1 1 d . . . C5 C 0.0390(9) 0.8152(9) 0.3249(6) 0.050(5) Uani 1 1 d . . . H5A H 0.0450 0.8375 0.3606 0.060 Uiso 1 1 calc R . . H5B H -0.0018 0.8395 0.3052 0.060 Uiso 1 1 calc R . . C6 C 0.1147(8) 0.8224(8) 0.2922(6) 0.043(4) Uani 1 1 d . . . H6A H 0.1241 0.8714 0.2834 0.052 Uiso 1 1 calc R . . H6B H 0.1575 0.8052 0.3142 0.052 Uiso 1 1 calc R . . C7 C 0.1078(10) 0.7816(9) 0.2424(7) 0.058(5) Uani 1 1 d . . . H7A H 0.1563 0.7822 0.2229 0.070 Uiso 1 1 calc R . . H7B H 0.0690 0.8026 0.2187 0.070 Uiso 1 1 calc R . . C8 C 0.1231(8) 0.4399(8) 0.3829(5) 0.034(4) Uani 1 1 d . . . H8 H 0.1152 0.4865 0.3935 0.041 Uiso 1 1 calc R . . C9 C 0.1731(8) 0.3372(8) 0.3758(5) 0.036(4) Uani 1 1 d . . . C10 C 0.1053(8) 0.3388(8) 0.3445(5) 0.036(4) Uani 1 1 d . . . C11 C 0.2327(8) 0.2897(9) 0.3886(6) 0.041(4) Uani 1 1 d . . . C12 C 0.3411(9) 0.2629(8) 0.4446(6) 0.051(5) Uani 1 1 d . . . H12A H 0.3876 0.2706 0.4235 0.062 Uiso 1 1 calc R . . H12B H 0.3525 0.2719 0.4832 0.062 Uiso 1 1 calc R . . C13 C 0.3144(10) 0.1902(9) 0.4375(7) 0.061(5) Uani 1 1 d . . . H13A H 0.2711 0.1817 0.4616 0.073 Uiso 1 1 calc R . . H13B H 0.3553 0.1580 0.4479 0.073 Uiso 1 1 calc R . . C14 C 0.2912(11) 0.1763(9) 0.3802(7) 0.070(6) Uani 1 1 d . . . H14A H 0.3359 0.1780 0.3566 0.084 Uiso 1 1 calc R . . H14B H 0.2689 0.1296 0.3775 0.084 Uiso 1 1 calc R . . C15 C 0.0585(8) 0.2955(9) 0.3103(6) 0.040(4) Uani 1 1 d . . . C16 C 0.0224(10) 0.1831(8) 0.2765(7) 0.057(5) Uani 1 1 d . . . H16A H -0.0211 0.1639 0.2964 0.069 Uiso 1 1 calc R . . H16B H 0.0538 0.1439 0.2642 0.069 Uiso 1 1 calc R . . C17 C -0.0047(9) 0.2212(9) 0.2300(6) 0.055(5) Uani 1 1 d . . . H17A H -0.0432 0.1932 0.2110 0.066 Uiso 1 1 calc R . . H17B H 0.0377 0.2284 0.2048 0.066 Uiso 1 1 calc R . . C18 C -0.0388(9) 0.2912(9) 0.2440(6) 0.056(5) Uani 1 1 d . . . H18A H -0.0478 0.3177 0.2104 0.068 Uiso 1 1 calc R . . H18B H -0.0879 0.2842 0.2619 0.068 Uiso 1 1 calc R . . C19 C -0.0860(8) 0.3745(7) 0.3980(6) 0.033(4) Uani 1 1 d . . . H19 H -0.0456 0.3704 0.4231 0.040 Uiso 1 1 calc R . . C20 C -0.1521(9) 0.4014(8) 0.3260(6) 0.036(4) Uani 1 1 d . . . C21 C -0.1517(11) 0.4279(8) 0.2703(6) 0.042(4) Uani 1 1 d . . . C22 C -0.0817(10) 0.4724(9) 0.1967(6) 0.060(5) Uani 1 1 d . . . H22A H -0.0427 0.5089 0.1963 0.072 Uiso 1 1 calc R . . H22B H -0.0666 0.4361 0.1708 0.072 Uiso 1 1 calc R . . C23 C -0.1540(10) 0.5019(11) 0.1798(7) 0.077(6) Uani 1 1 d . . . H23A H -0.1515 0.5125 0.1408 0.092 Uiso 1 1 calc R . . H23B H -0.1614 0.5460 0.1992 0.092 Uiso 1 1 calc R . . C24 C -0.2202(11) 0.4579(11) 0.1893(7) 0.082(7) Uani 1 1 d . . . H24A H -0.2668 0.4839 0.1810 0.098 Uiso 1 1 calc R . . H24B H -0.2184 0.4171 0.1653 0.098 Uiso 1 1 calc R . . C25 C -0.1368(9) 0.7356(9) 0.2794(5) 0.051(5) Uani 1 1 d . . . H25A H -0.0940 0.7128 0.2611 0.061 Uiso 1 1 calc R . . H25B H -0.1285 0.7861 0.2780 0.061 Uiso 1 1 calc R . . C26 C -0.2026(11) 0.6894(9) 0.3522(6) 0.060(5) Uani 1 1 d . . . C227 C -0.2087(14) 0.7180(16) 0.2507(8) 0.150(14) Uani 1 1 d . . . H22C H -0.2162 0.7552 0.2239 0.180 Uiso 1 1 calc R . . H22D H -0.1973 0.6759 0.2296 0.180 Uiso 1 1 calc R . . C28 C -0.2706(12) 0.708(2) 0.2699(8) 0.196(19) Uani 1 1 d . . . H28A H -0.2977 0.6743 0.2468 0.235 Uiso 1 1 calc R . . H28B H -0.2992 0.7517 0.2689 0.235 Uiso 1 1 calc R . . C29 C 0.0786(8) 0.6699(8) 0.4558(5) 0.038(4) Uani 1 1 d . . . H29 H 0.0884 0.6246 0.4430 0.045 Uiso 1 1 calc R . . C30 C 0.0242(10) 0.7705(9) 0.4678(6) 0.050(5) Uani 1 1 d . . . C31 C 0.0851(9) 0.7647(8) 0.5045(6) 0.042(4) Uani 1 1 d . . . C32 C 0.1212(10) 0.8050(10) 0.5478(6) 0.047(5) Uani 1 1 d . . . C33 C 0.1226(12) 0.8995(10) 0.6087(8) 0.082(7) Uani 1 1 d . . . H33A H 0.1352 0.9462 0.5952 0.099 Uiso 1 1 calc R . . H33B H 0.0867 0.9051 0.6389 0.099 Uiso 1 1 calc R . . C34 C 0.1849(14) 0.8704(14) 0.6276(12) 0.195(19) Uani 1 1 d . . . H34A H 0.1738 0.8601 0.6659 0.233 Uiso 1 1 calc R . . H34B H 0.2225 0.9081 0.6283 0.233 Uiso 1 1 calc R . . C36 C 0.2249(10) 0.8126(9) 0.6092(6) 0.060(5) Uani 1 1 d . . . H36A H 0.2330 0.7802 0.6396 0.072 Uiso 1 1 calc R . . H36B H 0.2748 0.8274 0.5960 0.072 Uiso 1 1 calc R . . C37 C -0.0300(10) 0.8214(9) 0.4503(6) 0.048(5) Uani 1 1 d . . . C38 C -0.1374(10) 0.8458(9) 0.3976(6) 0.056(5) Uani 1 1 d . . . H38A H -0.1848 0.8194 0.3933 0.067 Uiso 1 1 calc R . . H38B H -0.1241 0.8653 0.3620 0.067 Uiso 1 1 calc R . . C39 C -0.1506(10) 0.9046(9) 0.4369(7) 0.059(5) Uani 1 1 d . . . H39A H -0.1735 0.8867 0.4704 0.071 Uiso 1 1 calc R . . H39B H -0.1854 0.9388 0.4208 0.071 Uiso 1 1 calc R . . C40 C -0.0753(11) 0.9387(9) 0.4498(8) 0.077(6) Uani 1 1 d . . . H40A H -0.0555 0.9618 0.4171 0.092 Uiso 1 1 calc R . . H40B H -0.0821 0.9740 0.4782 0.092 Uiso 1 1 calc R . . C41 C 0.2177(8) 0.5379(10) 0.5047(6) 0.039(4) Uani 1 1 d . . . H41 H 0.1900 0.5191 0.5339 0.047 Uiso 1 1 calc R . . C42 C 0.2819(8) 0.5471(10) 0.4321(6) 0.042(4) Uani 1 1 d . . . C43 C 0.2755(8) 0.6129(9) 0.4531(6) 0.037(4) Uani 1 1 d . . . C44 C 0.2965(9) 0.6828(10) 0.4435(7) 0.044(5) Uani 1 1 d . . . C45 C 0.3676(10) 0.7684(9) 0.3904(6) 0.060(5) Uani 1 1 d . . . H45A H 0.3720 0.7744 0.3508 0.071 Uiso 1 1 calc R . . H45B H 0.4169 0.7796 0.4070 0.071 Uiso 1 1 calc R . . C46 C 0.3072(10) 0.8167(9) 0.4123(6) 0.063(5) Uani 1 1 d . . . H46A H 0.2612 0.8126 0.3898 0.076 Uiso 1 1 calc R . . H46B H 0.3252 0.8649 0.4099 0.076 Uiso 1 1 calc R . . C47 C 0.2877(9) 0.8001(8) 0.4712(6) 0.047(4) Uani 1 1 d . . . H47A H 0.3303 0.8133 0.4950 0.057 Uiso 1 1 calc R . . H47B H 0.2429 0.8270 0.4822 0.057 Uiso 1 1 calc R . . C48 C 0.3218(9) 0.5136(9) 0.3863(7) 0.046(5) Uani 1 1 d . . . C49 C 0.3650(8) 0.4051(8) 0.3482(6) 0.047(4) Uani 1 1 d . . . H49A H 0.3272 0.3898 0.3213 0.056 Uiso 1 1 calc R . . H49B H 0.3890 0.3636 0.3640 0.056 Uiso 1 1 calc R . . C50 C 0.4263(10) 0.4509(9) 0.3200(6) 0.063(5) Uani 1 1 d . . . H50A H 0.4672 0.4620 0.3459 0.075 Uiso 1 1 calc R . . H50B H 0.4483 0.4257 0.2891 0.075 Uiso 1 1 calc R . . C51 C 0.3894(9) 0.5162(8) 0.3006(6) 0.046(4) Uani 1 1 d . . . H51A H 0.4284 0.5475 0.2858 0.056 Uiso 1 1 calc R . . H51B H 0.3536 0.5051 0.2711 0.056 Uiso 1 1 calc R . . C52 C 0.1351(8) 0.3549(7) 0.5194(6) 0.035(4) Uani 1 1 d . . . H52 H 0.0941 0.3586 0.4947 0.042 Uiso 1 1 calc R . . C53 C 0.2004(9) 0.3355(9) 0.5904(6) 0.046(5) Uani 1 1 d . . . C54 C 0.2488(10) 0.3613(8) 0.5536(6) 0.047(4) Uani 1 1 d . . . C55 C 0.3296(9) 0.3802(9) 0.5481(6) 0.049(5) Uani 1 1 d . . . C56 C 0.4277(9) 0.4203(8) 0.4912(6) 0.046(5) Uani 1 1 d . . . H56A H 0.4465 0.3921 0.4609 0.055 Uiso 1 1 calc R . . H56B H 0.4308 0.4695 0.4805 0.055 Uiso 1 1 calc R . . C59 C 0.1997(10) 0.6252(8) 0.6362(6) 0.049(5) Uani 1 1 d . . . C60 C 0.2796(9) 0.6445(8) 0.6292(7) 0.043(4) Uani 1 1 d . . . C61 C 0.3758(9) 0.6924(9) 0.5719(6) 0.052(5) Uani 1 1 d . . . H61A H 0.3821 0.7425 0.5786 0.063 Uiso 1 1 calc R . . H61B H 0.3876 0.6835 0.5335 0.063 Uiso 1 1 calc R . . C62 C 0.4305(8) 0.6523(8) 0.6077(6) 0.047(4) Uani 1 1 d . . . H62A H 0.4319 0.6035 0.5960 0.056 Uiso 1 1 calc R . . H62B H 0.4818 0.6717 0.6039 0.056 Uiso 1 1 calc R . . C63 C 0.4072(9) 0.6561(9) 0.6644(5) 0.051(5) Uani 1 1 d . . . H63A H 0.4407 0.6267 0.6867 0.062 Uiso 1 1 calc R . . H63B H 0.4119 0.7042 0.6774 0.062 Uiso 1 1 calc R . . C64 C 0.0899(9) 0.5287(10) 0.2577(6) 0.045(5) Uani 1 1 d . . . C65 C 0.1246(9) 0.4208(9) 0.2173(6) 0.052(5) Uani 1 1 d . . . H65A H 0.1050 0.4206 0.1798 0.063 Uiso 1 1 calc R . . H65B H 0.1250 0.3726 0.2305 0.063 Uiso 1 1 calc R . . C66 C 0.2060(10) 0.4491(9) 0.2174(7) 0.064(5) Uani 1 1 d . . . H66A H 0.2287 0.4436 0.2538 0.077 Uiso 1 1 calc R . . H66B H 0.2370 0.4230 0.1913 0.077 Uiso 1 1 calc R . . C67 C 0.2044(10) 0.5231(9) 0.2024(7) 0.063(5) Uani 1 1 d . . . H67A H 0.2551 0.5432 0.2078 0.075 Uiso 1 1 calc R . . H67B H 0.1914 0.5274 0.1636 0.075 Uiso 1 1 calc R . . N1 N -0.0072(7) 0.5181(6) 0.3236(5) 0.035(3) Uani 1 1 d . . . N2 N -0.0271(6) 0.6232(6) 0.3544(4) 0.028(3) Uani 1 1 d . . . N3 N 0.0179(6) 0.7438(7) 0.3324(5) 0.037(3) Uani 1 1 d . . . N4 N 0.0867(7) 0.7096(7) 0.2547(5) 0.050(4) Uani 1 1 d . . . N5 N 0.0746(7) 0.4617(7) 0.2510(4) 0.044(3) Uani 1 1 d . . . N6 N 0.1503(8) 0.5616(7) 0.2340(5) 0.052(4) Uani 1 1 d . . . N7 N 0.2476(6) 0.4993(6) 0.4649(4) 0.030(3) Uani 1 1 d . . . N8 N 0.2306(6) 0.6034(7) 0.4989(5) 0.034(3) Uani 1 1 d . . . N9 N 0.2721(7) 0.7254(7) 0.4771(5) 0.039(3) Uani 1 1 d . . . N10 N 0.3468(8) 0.6960(7) 0.4030(5) 0.053(4) Uani 1 1 d . . . N11 N 0.3492(7) 0.5515(7) 0.3439(5) 0.051(4) Uani 1 1 d . . . N12 N 0.3274(7) 0.4457(7) 0.3915(4) 0.039(3) Uani 1 1 d . . . N13 N 0.1197(6) 0.7014(6) 0.4939(4) 0.036(3) Uani 1 1 d . . . N14 N 0.0221(7) 0.7096(7) 0.4381(5) 0.042(4) Uani 1 1 d . . . N15 N -0.0775(6) 0.7987(6) 0.4151(5) 0.036(3) Uani 1 1 d . . . N16 N -0.0216(9) 0.8860(8) 0.4684(6) 0.075(5) Uani 1 1 d . . . N17 N 0.0856(8) 0.8610(8) 0.5656(5) 0.062(4) Uani 1 1 d . . . N18 N 0.1839(7) 0.7767(6) 0.5653(5) 0.042(3) Uani 1 1 d . . . N19 N 0.1566(7) 0.6426(6) 0.5919(4) 0.035(3) Uani 1 1 d . . . N20 N 0.2962(7) 0.6725(6) 0.5826(5) 0.042(3) Uani 1 1 d . . . N21 N 0.3294(7) 0.6330(8) 0.6704(5) 0.060(4) Uani 1 1 d . . . N22 N 0.2059(7) 0.3731(6) 0.5076(4) 0.032(3) Uani 1 1 d . . . N23 N 0.1289(6) 0.3315(6) 0.5687(4) 0.034(3) Uani 1 1 d . . . N24 N 0.3465(6) 0.4019(6) 0.5021(5) 0.037(3) Uani 1 1 d . . . N25 N 0.3765(9) 0.3710(12) 0.5900(6) 0.134(9) Uani 1 1 d . . . N26 N 0.1811(7) 0.4003(6) 0.3993(4) 0.037(3) Uani 1 1 d . . . N27 N 0.0778(6) 0.4040(7) 0.3495(4) 0.034(3) Uani 1 1 d . . . N28 N 0.0111(7) 0.3311(6) 0.2798(4) 0.037(3) Uani 1 1 d . . . N29 N 0.0662(7) 0.2261(7) 0.3124(5) 0.049(4) Uani 1 1 d . . . N30 N 0.2359(7) 0.2280(7) 0.3624(5) 0.052(4) Uani 1 1 d . . . N31 N 0.2793(7) 0.3114(6) 0.4251(4) 0.042(3) Uani 1 1 d . . . N32 N -0.0793(6) 0.3985(6) 0.3476(4) 0.036(3) Uani 1 1 d . . . N33 N -0.0864(8) 0.4422(7) 0.2520(5) 0.044(4) Uani 1 1 d . . . N34 N -0.2211(8) 0.4355(8) 0.2456(6) 0.070(5) Uani 1 1 d . . . N35 N -0.1400(7) 0.7133(6) 0.3347(4) 0.034(3) Uani 1 1 d . . . N36 N -0.2700(9) 0.6823(12) 0.3249(6) 0.133(9) Uani 1 1 d . . . O1 O 0.4951(10) 0.7780(10) 0.5064(8) 0.124(7) Uiso 0.81 1 d P . . O3 O 0.0745(16) 0.5119(14) 0.0903(11) 0.232(12) Uiso 0.90 1 d P . . O201 O 0.433(4) 0.914(4) 0.533(3) 0.24(4) Uiso 0.40 1 d P . . O202 O 0.264(2) 1.010(2) 0.4511(16) 0.161(15) Uiso 0.50 1 d P . . O203 O 0.394(4) 0.913(3) 0.543(2) 0.083(19) Uiso 0.25 1 d P . . O204 O 0.329(3) 0.989(2) 0.494(2) 0.24(2) Uiso 0.60 1 d P . . O13 O 0.397(3) 0.854(2) 0.6652(18) 0.042(13) Uiso 0.20 1 d P . . O14 O 0.283(3) 0.629(3) 0.2490(19) 0.141(17) Uiso 0.40 1 d P . . O217 O 0.470(3) 0.909(2) 0.4431(18) 0.147(16) Uiso 0.40 1 d P . . O205 O 0.341(4) 1.025(3) 0.545(3) 0.23(3) Uiso 0.40 1 d P . . O218 O 0.550(6) 0.933(5) 0.454(4) 0.16(4) Uiso 0.20 1 d P . . O206 O 0.265(2) 0.961(2) 0.5174(16) 0.120(14) Uiso 0.40 1 d P . . O103 O 0.3524(8) 0.1999(8) 0.6195(6) 0.077(5) Uiso 1 1 d . . . O302 O 0.1379(11) 0.9241(10) 0.4400(7) 0.104(7) Uiso 1 1 d . . . O303 O 0.160(2) 0.942(2) 0.4541(16) 0.121(16) Uiso 0.50 1 d P . . O405 O 0.1288(7) 0.9739(6) 0.8200(5) 0.056(4) Uiso 1 1 d . . . C57 C 0.4753(10) 0.4090(14) 0.5385(8) 0.107(9) Uani 1 1 d . . . H57A H 0.5170 0.3794 0.5255 0.128 Uiso 1 1 calc R . . H57B H 0.4982 0.4545 0.5464 0.128 Uiso 1 1 calc R . . C58 C 0.4576(11) 0.3845(17) 0.5841(9) 0.162(15) Uani 1 1 d . . . H58A H 0.4737 0.4172 0.6125 0.194 Uiso 1 1 calc R . . H58B H 0.4855 0.3408 0.5898 0.194 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0631(14) 0.0655(16) 0.0632(13) 0.0055(11) -0.0163(10) 0.0010(11) Br2 0.0473(16) 0.0394(16) 0.0362(13) -0.0005(11) -0.0077(11) -0.0021(12) Br3 0.128(3) 0.231(5) 0.076(2) 0.036(3) -0.008(2) 0.050(3) Br4 0.0940(18) 0.0867(19) 0.0858(16) 0.0035(13) -0.0182(13) -0.0002(14) Br6 0.062(4) 0.167(8) 0.077(4) 0.047(4) -0.006(3) 0.003(4) Br7 0.150(4) 0.151(4) 0.122(3) -0.012(3) -0.031(3) -0.042(3) Br8 0.190(10) 0.212(11) 0.140(8) -0.012(7) 0.033(7) 0.021(8) Br9 0.32(3) 0.18(2) 0.20(2) 0.044(16) -0.13(2) -0.10(2) Br10 0.147(14) 0.117(12) 0.103(10) 0.030(9) 0.017(9) -0.007(10) Br11 0.117(11) 0.111(12) 0.101(10) 0.032(7) -0.035(7) -0.019(8) Br12 0.09(2) 0.13(3) 0.17(3) 0.03(2) -0.01(2) 0.014(19) Co1 0.0389(16) 0.0378(17) 0.0288(13) -0.0002(12) -0.0057(11) 0.0068(13) Co2 0.0388(16) 0.0358(17) 0.0340(14) 0.0009(12) -0.0095(11) 0.0002(13) Co3 0.0379(16) 0.0348(16) 0.0312(14) 0.0031(12) -0.0077(11) 0.0006(13) Co4 0.0432(17) 0.0385(17) 0.0285(13) -0.0003(12) -0.0088(11) 0.0006(13) C1 0.041(10) 0.038(12) 0.016(8) 0.016(8) -0.001(7) -0.012(9) C2 0.039(10) 0.036(12) 0.040(10) -0.011(9) 0.005(8) -0.002(9) C3 0.050(11) 0.046(12) 0.018(8) 0.006(9) -0.013(8) -0.002(10) C4 0.050(12) 0.058(14) 0.032(10) -0.013(10) -0.007(8) 0.000(10) C5 0.058(12) 0.049(13) 0.043(10) -0.011(9) 0.003(9) 0.011(10) C6 0.053(12) 0.019(10) 0.058(11) -0.001(8) -0.006(9) 0.008(8) C7 0.069(13) 0.047(13) 0.059(12) 0.009(10) 0.010(10) 0.004(10) C8 0.044(11) 0.037(10) 0.022(8) 0.007(7) -0.008(7) 0.009(9) C9 0.039(11) 0.044(11) 0.026(8) -0.007(8) -0.012(7) -0.001(9) C10 0.050(11) 0.019(10) 0.039(9) -0.007(8) -0.002(8) 0.010(9) C11 0.034(11) 0.054(13) 0.034(9) -0.006(9) -0.011(8) 0.004(9) C12 0.057(12) 0.048(13) 0.048(10) 0.005(9) -0.012(9) 0.005(10) C13 0.060(13) 0.053(14) 0.069(13) 0.019(10) -0.025(10) 0.013(10) C14 0.105(16) 0.042(13) 0.063(12) -0.012(10) -0.006(11) 0.000(12) C15 0.038(11) 0.044(12) 0.037(9) -0.015(9) -0.009(8) 0.003(9) C16 0.067(13) 0.040(12) 0.064(12) -0.007(10) -0.006(10) -0.004(10) C17 0.065(13) 0.050(13) 0.050(11) -0.015(10) -0.020(9) -0.023(10) C18 0.071(13) 0.061(14) 0.037(10) -0.012(9) -0.014(9) 0.001(11) C19 0.030(11) 0.034(11) 0.036(10) -0.011(8) -0.008(7) -0.004(8) C20 0.044(11) 0.036(11) 0.027(9) 0.002(8) -0.007(8) -0.005(8) C21 0.066(14) 0.028(10) 0.034(10) -0.011(8) -0.015(10) 0.004(10) C22 0.070(14) 0.074(14) 0.037(10) 0.023(9) -0.020(9) -0.008(11) C23 0.059(14) 0.118(19) 0.052(12) 0.035(12) -0.020(10) 0.011(14) C24 0.061(15) 0.13(2) 0.055(12) 0.026(12) -0.041(10) 0.002(14) C25 0.069(13) 0.056(12) 0.028(9) 0.026(8) -0.005(8) -0.003(10) C26 0.069(15) 0.070(14) 0.040(11) 0.017(10) -0.029(10) -0.007(11) C227 0.11(2) 0.30(4) 0.040(13) 0.068(17) -0.049(14) -0.12(2) C28 0.031(15) 0.49(6) 0.063(16) 0.12(2) -0.028(12) -0.04(2) C29 0.047(11) 0.038(11) 0.028(9) -0.001(8) -0.009(8) -0.006(9) C30 0.071(13) 0.042(12) 0.037(10) -0.006(9) -0.015(9) -0.006(10) C31 0.044(11) 0.022(10) 0.060(11) 0.000(8) -0.008(9) 0.013(9) C32 0.054(13) 0.058(14) 0.029(9) -0.019(9) -0.007(9) -0.025(11) C33 0.089(17) 0.073(16) 0.085(15) -0.024(12) -0.034(12) 0.021(13) C34 0.15(3) 0.19(3) 0.25(3) -0.19(3) -0.15(3) 0.12(2) C36 0.058(13) 0.070(14) 0.052(11) 0.005(10) -0.028(9) -0.005(11) C37 0.066(13) 0.034(12) 0.043(10) 0.007(9) -0.018(9) 0.022(10) C38 0.071(13) 0.052(13) 0.045(10) 0.008(9) -0.005(9) 0.010(10) C39 0.057(13) 0.057(13) 0.063(12) -0.009(10) -0.012(10) 0.022(11) C40 0.096(17) 0.052(14) 0.083(15) 0.000(11) -0.010(12) 0.019(13) C41 0.018(9) 0.064(14) 0.036(10) 0.004(10) -0.010(7) 0.001(9) C42 0.045(11) 0.060(14) 0.022(9) 0.003(9) 0.002(8) 0.023(10) C43 0.029(10) 0.041(12) 0.041(10) 0.005(9) -0.015(8) -0.006(9) C44 0.034(11) 0.051(14) 0.046(11) 0.017(10) -0.016(9) -0.020(10) C45 0.091(15) 0.043(13) 0.045(11) 0.003(9) 0.025(10) -0.012(11) C46 0.081(15) 0.048(13) 0.060(12) 0.015(10) -0.011(10) -0.018(11) C47 0.054(12) 0.039(12) 0.049(11) 0.010(9) 0.001(8) -0.006(9) C48 0.040(11) 0.041(13) 0.057(12) 0.012(10) -0.020(9) -0.005(9) C49 0.048(11) 0.047(12) 0.045(10) 0.003(9) 0.001(8) 0.012(9) C50 0.069(14) 0.076(15) 0.043(11) 0.002(10) 0.001(9) 0.005(12) C51 0.046(11) 0.047(12) 0.046(10) 0.017(9) 0.008(8) 0.005(9) C52 0.033(11) 0.032(11) 0.041(10) 0.000(8) -0.006(8) 0.012(8) C53 0.038(11) 0.056(13) 0.045(10) -0.022(9) -0.006(9) 0.007(9) C54 0.054(13) 0.048(12) 0.038(10) 0.004(9) -0.010(9) -0.001(10) C55 0.050(13) 0.060(13) 0.035(10) 0.013(9) -0.010(9) 0.000(10) C56 0.054(12) 0.047(12) 0.037(9) 0.012(8) -0.015(8) -0.012(9) C59 0.056(14) 0.047(12) 0.045(11) -0.009(9) -0.028(10) 0.017(10) C60 0.033(11) 0.042(12) 0.056(12) -0.031(9) -0.016(9) 0.014(9) C61 0.047(12) 0.075(14) 0.034(9) 0.002(9) -0.009(8) 0.005(10) C62 0.027(10) 0.050(12) 0.064(12) 0.012(9) -0.006(8) -0.008(8) C63 0.052(12) 0.071(14) 0.030(9) -0.011(9) -0.017(8) 0.000(10) C64 0.045(12) 0.063(14) 0.028(10) -0.005(9) -0.027(9) 0.011(11) C65 0.061(13) 0.064(13) 0.031(9) 0.004(9) -0.004(9) -0.010(11) C66 0.079(15) 0.045(13) 0.067(13) 0.004(10) -0.012(10) 0.004(11) C67 0.070(14) 0.060(15) 0.057(12) -0.013(10) 0.006(10) 0.006(11) N1 0.056(9) 0.029(9) 0.019(7) 0.012(7) -0.002(6) -0.001(7) N2 0.046(8) 0.016(8) 0.024(7) 0.008(6) 0.007(6) -0.006(6) N3 0.039(8) 0.039(9) 0.031(7) 0.004(7) -0.015(6) -0.002(7) N4 0.063(10) 0.036(10) 0.051(9) 0.014(7) 0.009(8) 0.001(7) N5 0.064(10) 0.043(10) 0.024(7) -0.007(7) 0.012(6) 0.016(8) N6 0.047(9) 0.066(11) 0.045(8) 0.008(8) 0.018(7) 0.001(8) N7 0.028(7) 0.038(8) 0.025(7) 0.002(7) 0.006(6) -0.004(6) N8 0.033(8) 0.033(9) 0.036(8) 0.008(7) 0.001(6) 0.003(7) N9 0.040(9) 0.043(10) 0.034(8) -0.003(7) -0.012(6) -0.008(7) N10 0.077(11) 0.033(10) 0.048(9) -0.002(7) 0.010(8) -0.007(8) N11 0.055(9) 0.050(10) 0.049(9) 0.003(8) 0.007(7) -0.013(8) N12 0.048(9) 0.042(10) 0.027(7) -0.002(7) 0.002(6) 0.009(7) N13 0.039(8) 0.043(9) 0.027(7) 0.005(6) -0.011(6) -0.001(7) N14 0.037(9) 0.044(9) 0.046(8) 0.020(7) -0.021(7) -0.010(7) N15 0.031(8) 0.036(9) 0.041(8) 0.005(6) -0.014(6) 0.004(7) N16 0.102(13) 0.055(12) 0.069(11) -0.021(9) -0.040(9) 0.036(10) N17 0.092(12) 0.056(11) 0.037(8) -0.016(8) -0.018(8) 0.016(9) N18 0.037(9) 0.042(9) 0.046(8) -0.014(7) -0.021(7) 0.006(7) N19 0.036(9) 0.039(9) 0.031(7) 0.001(6) -0.011(6) -0.004(7) N20 0.046(10) 0.042(9) 0.038(8) -0.002(7) -0.008(7) 0.001(7) N21 0.027(9) 0.116(14) 0.038(8) -0.002(8) -0.010(7) -0.008(8) N22 0.046(9) 0.034(8) 0.017(6) 0.001(6) 0.000(6) 0.001(7) N23 0.036(9) 0.050(9) 0.017(7) 0.003(6) -0.008(6) 0.000(7) N24 0.026(8) 0.042(9) 0.041(8) 0.003(7) -0.016(6) 0.011(7) N25 0.066(13) 0.26(3) 0.072(12) 0.076(14) -0.045(10) -0.082(14) N26 0.050(9) 0.037(9) 0.025(7) -0.016(6) -0.002(6) -0.011(7) N27 0.028(8) 0.049(10) 0.023(7) 0.000(6) -0.011(6) -0.011(7) N28 0.053(9) 0.026(8) 0.031(7) -0.007(6) -0.018(6) 0.003(7) N29 0.060(10) 0.037(10) 0.051(9) -0.003(7) -0.009(7) -0.006(8) N30 0.062(10) 0.043(10) 0.050(9) -0.013(8) -0.021(7) 0.026(8) N31 0.045(9) 0.049(9) 0.031(7) -0.004(6) -0.008(6) 0.013(7) N32 0.033(8) 0.047(9) 0.028(7) -0.010(6) -0.006(6) 0.004(6) N33 0.051(10) 0.049(10) 0.030(8) 0.004(7) -0.013(7) -0.006(8) N34 0.049(10) 0.090(13) 0.071(10) 0.027(9) -0.035(8) -0.013(9) N35 0.037(9) 0.035(8) 0.030(7) 0.008(6) 0.000(6) -0.004(7) N36 0.055(12) 0.28(3) 0.062(11) 0.094(14) -0.028(9) -0.050(13) C57 0.033(13) 0.21(3) 0.075(15) 0.057(17) -0.011(11) -0.014(14) C58 0.052(17) 0.34(4) 0.094(19) 0.11(2) -0.041(13) -0.07(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 O14 1.14(5) . ? Br3 O103 0.877(13) . ? Br4 O13 1.73(5) . ? Br6 Br11 0.837(12) . ? Br7 O405 0.932(11) . ? Br7 Br9 2.457(19) . ? Br7 Br8 2.458(12) . ? Br8 Br12 1.68(3) . ? Br9 O405 1.89(2) . ? Br10 Br12 1.57(3) . ? Br10 Br11 2.13(2) . ? Co1 N7 1.901(12) . ? Co1 N22 1.906(11) . ? Co1 N31 1.917(12) . ? Co1 N26 1.919(12) . ? Co1 N24 1.965(11) . ? Co1 N12 1.967(12) . ? Co2 N8 1.870(13) . ? Co2 N19 1.919(12) . ? Co2 N13 1.920(11) . ? Co2 N9 1.945(13) . ? Co2 N20 1.946(12) . ? Co2 N18 1.967(12) . ? Co3 N2 1.889(12) . ? Co3 N14 1.902(11) . ? Co3 N23 1.923(12) 3_566 ? Co3 N15 1.939(12) . ? Co3 N35 1.947(11) . ? Co3 N3 1.951(12) . ? Co4 N1 1.881(12) . ? Co4 N32 1.882(12) . ? Co4 N27 1.916(11) . ? Co4 N28 1.920(11) . ? Co4 N33 1.935(12) . ? Co4 N5 1.962(13) . ? C1 N2 1.289(16) . ? C1 N1 1.303(17) . ? C2 C3 1.37(2) . ? C2 N2 1.380(17) . ? C2 C4 1.43(2) . ? C3 N1 1.373(17) . ? C3 C64 1.48(2) . ? C4 N3 1.314(18) . ? C4 N4 1.347(19) . ? C5 N3 1.447(18) . ? C5 C6 1.58(2) . ? C6 C7 1.471(19) . ? C7 N4 1.478(18) . ? C8 N27 1.345(16) . ? C8 N26 1.345(17) . ? C9 N26 1.361(17) . ? C9 C10 1.431(19) . ? C9 C11 1.44(2) . ? C10 N27 1.362(17) . ? C10 C15 1.450(19) . ? C11 N31 1.294(17) . ? C11 N30 1.361(18) . ? C12 C13 1.50(2) . ? C12 N31 1.523(17) . ? C13 C14 1.50(2) . ? C14 N30 1.470(19) . ? C15 N28 1.322(17) . ? C15 N29 1.352(18) . ? C16 N29 1.444(18) . ? C16 C17 1.45(2) . ? C17 C18 1.53(2) . ? C18 N28 1.470(17) . ? C19 N19 1.322(16) 3_566 ? C19 N32 1.338(16) . ? C20 C59 1.37(2) 3_566 ? C20 N32 1.398(17) . ? C20 C21 1.47(2) . ? C21 N33 1.278(18) . ? C21 N34 1.382(19) . ? C22 C23 1.47(2) . ? C22 N33 1.491(17) . ? C23 C24 1.47(2) . ? C24 N34 1.46(2) . ? C25 N35 1.440(16) . ? C25 C227 1.50(2) . ? C26 N35 1.282(19) . ? C26 N36 1.38(2) . ? C26 C53 1.50(2) 3_566 ? C227 C28 1.21(2) . ? C28 N36 1.45(2) . ? C29 N13 1.337(16) . ? C29 N14 1.338(17) . ? C30 N14 1.391(18) . ? C30 C31 1.42(2) . ? C30 C37 1.44(2) . ? C31 N13 1.397(17) . ? C31 C32 1.47(2) . ? C32 N18 1.315(19) . ? C32 N17 1.331(19) . ? C33 C34 1.32(2) . ? C33 N17 1.46(2) . ? C34 C36 1.40(2) . ? C36 N18 1.479(18) . ? C37 N15 1.290(18) . ? C37 N16 1.339(19) . ? C38 N15 1.465(18) . ? C38 C39 1.52(2) . ? C39 C40 1.52(2) . ? C40 N16 1.47(2) . ? C41 N8 1.299(17) . ? C41 N7 1.349(17) . ? C42 N7 1.375(18) . ? C42 C43 1.38(2) . ? C42 C48 1.49(2) . ? C43 N8 1.402(18) . ? C43 C44 1.43(2) . ? C44 N9 1.252(19) . ? C44 N10 1.368(19) . ? C45 N10 1.486(18) . ? C45 C46 1.53(2) . ? C46 C47 1.54(2) . ? C47 N9 1.482(18) . ? C48 N12 1.326(18) . ? C48 N11 1.375(19) . ? C49 N12 1.492(17) . ? C49 C50 1.57(2) . ? C50 C51 1.50(2) . ? C51 N11 1.461(18) . ? C52 N23 1.310(16) . ? C52 N22 1.338(16) . ? C53 C54 1.35(2) . ? C53 N23 1.379(17) . ? C53 C26 1.50(2) 3_566 ? C54 N22 1.387(17) . ? C54 C55 1.49(2) . ? C55 N24 1.253(17) . ? C55 N25 1.340(19) . ? C56 C57 1.46(2) . ? C56 N24 1.511(18) . ? C59 C20 1.37(2) 3_566 ? C59 N19 1.377(17) . ? C59 C60 1.48(2) . ? C60 N20 1.310(19) . ? C60 N21 1.365(18) . ? C61 N20 1.491(18) . ? C61 C62 1.525(19) . ? C62 C63 1.468(18) . ? C63 N21 1.460(18) . ? C64 N5 1.336(19) . ? C64 N6 1.381(19) . ? C65 N5 1.456(18) . ? C65 C66 1.55(2) . ? C66 C67 1.48(2) . ? C67 N6 1.449(19) . ? N19 C19 1.322(16) 3_566 ? N23 Co3 1.923(12) 3_566 ? N25 C58 1.47(2) . ? O201 O203 0.75(9) . ? O202 O204 1.61(5) . ? O204 O206 1.38(5) . ? O204 O205 1.45(7) . ? O217 O218 1.53(10) . ? O302 O303 0.62(4) . ? C57 C58 1.27(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O405 Br7 Br9 43.6(11) . . ? O405 Br7 Br8 119.4(10) . . ? Br9 Br7 Br8 135.1(6) . . ? Br12 Br8 Br7 123.4(12) . . ? O405 Br9 Br7 19.8(4) . . ? Br12 Br10 Br11 115.7(16) . . ? Br6 Br11 Br10 159(2) . . ? Br10 Br12 Br8 173(3) . . ? N7 Co1 N22 93.2(5) . . ? N7 Co1 N31 174.7(5) . . ? N22 Co1 N31 90.2(5) . . ? N7 Co1 N26 93.2(5) . . ? N22 Co1 N26 92.8(5) . . ? N31 Co1 N26 82.6(5) . . ? N7 Co1 N24 90.0(5) . . ? N22 Co1 N24 82.9(5) . . ? N31 Co1 N24 94.4(5) . . ? N26 Co1 N24 174.7(5) . . ? N7 Co1 N12 81.7(5) . . ? N22 Co1 N12 174.3(5) . . ? N31 Co1 N12 95.0(5) . . ? N26 Co1 N12 90.2(5) . . ? N24 Co1 N12 94.4(5) . . ? N8 Co2 N19 93.6(5) . . ? N8 Co2 N13 92.5(5) . . ? N19 Co2 N13 91.8(5) . . ? N8 Co2 N9 83.2(6) . . ? N19 Co2 N9 175.2(5) . . ? N13 Co2 N9 91.9(5) . . ? N8 Co2 N20 91.1(5) . . ? N19 Co2 N20 82.8(5) . . ? N13 Co2 N20 173.7(5) . . ? N9 Co2 N20 93.6(5) . . ? N8 Co2 N18 174.2(5) . . ? N19 Co2 N18 89.0(5) . . ? N13 Co2 N18 82.3(5) . . ? N9 Co2 N18 94.4(6) . . ? N20 Co2 N18 94.3(5) . . ? N2 Co3 N14 95.3(5) . . ? N2 Co3 N23 93.4(5) . 3_566 ? N14 Co3 N23 94.2(5) . 3_566 ? N2 Co3 N15 176.7(5) . . ? N14 Co3 N15 82.6(5) . . ? N23 Co3 N15 89.3(5) 3_566 . ? N2 Co3 N35 89.5(5) . . ? N14 Co3 N35 174.3(6) . . ? N23 Co3 N35 82.5(5) 3_566 . ? N15 Co3 N35 92.7(5) . . ? N2 Co3 N3 82.4(5) . . ? N14 Co3 N3 89.0(5) . . ? N23 Co3 N3 175.0(5) 3_566 . ? N15 Co3 N3 95.0(5) . . ? N35 Co3 N3 94.7(5) . . ? N1 Co4 N32 92.3(5) . . ? N1 Co4 N27 92.8(5) . . ? N32 Co4 N27 94.6(5) . . ? N1 Co4 N28 175.0(5) . . ? N32 Co4 N28 89.2(5) . . ? N27 Co4 N28 82.2(5) . . ? N1 Co4 N33 89.9(5) . . ? N32 Co4 N33 82.5(5) . . ? N27 Co4 N33 176.2(6) . . ? N28 Co4 N33 95.1(5) . . ? N1 Co4 N5 83.6(6) . . ? N32 Co4 N5 175.5(6) . . ? N27 Co4 N5 87.6(5) . . ? N28 Co4 N5 95.1(6) . . ? N33 Co4 N5 95.4(5) . . ? N2 C1 N1 116.4(13) . . ? C3 C2 N2 106.2(14) . . ? C3 C2 C4 138.4(16) . . ? N2 C2 C4 115.4(14) . . ? C2 C3 N1 109.1(14) . . ? C2 C3 C64 137.0(17) . . ? N1 C3 C64 113.9(15) . . ? N3 C4 N4 126.7(17) . . ? N3 C4 C2 112.8(15) . . ? N4 C4 C2 120.2(15) . . ? N3 C5 C6 111.8(13) . . ? C7 C6 C5 108.3(13) . . ? C6 C7 N4 110.8(13) . . ? N27 C8 N26 110.2(13) . . ? N26 C9 C10 107.4(13) . . ? N26 C9 C11 114.0(13) . . ? C10 C9 C11 138.6(14) . . ? N27 C10 C9 105.7(12) . . ? N27 C10 C15 112.7(13) . . ? C9 C10 C15 141.6(15) . . ? N31 C11 N30 126.3(14) . . ? N31 C11 C9 114.4(14) . . ? N30 C11 C9 119.4(13) . . ? C13 C12 N31 108.4(12) . . ? C12 C13 C14 111.5(14) . . ? N30 C14 C13 110.1(14) . . ? N28 C15 N29 127.2(13) . . ? N28 C15 C10 113.1(14) . . ? N29 C15 C10 119.6(14) . . ? N29 C16 C17 111.7(14) . . ? C16 C17 C18 113.7(14) . . ? N28 C18 C17 111.4(13) . . ? N19 C19 N32 110.7(12) 3_566 . ? C59 C20 N32 107.3(12) 3_566 . ? C59 C20 C21 141.2(16) 3_566 . ? N32 C20 C21 111.4(14) . . ? N33 C21 N34 128.9(15) . . ? N33 C21 C20 114.6(15) . . ? N34 C21 C20 116.4(16) . . ? C23 C22 N33 111.3(14) . . ? C22 C23 C24 115.3(17) . . ? N34 C24 C23 109.7(14) . . ? N35 C25 C227 110.2(13) . . ? N35 C26 N36 128.5(15) . . ? N35 C26 C53 114.6(15) . 3_566 ? N36 C26 C53 116.9(17) . 3_566 ? C28 C227 C25 128(2) . . ? C227 C28 N36 114.9(19) . . ? N13 C29 N14 112.0(14) . . ? N14 C30 C31 107.0(14) . . ? N14 C30 C37 114.0(14) . . ? C31 C30 C37 138.8(16) . . ? N13 C31 C30 106.5(13) . . ? N13 C31 C32 114.4(14) . . ? C30 C31 C32 139.1(16) . . ? N18 C32 N17 129.3(13) . . ? N18 C32 C31 112.6(16) . . ? N17 C32 C31 118.0(16) . . ? C34 C33 N17 114.5(17) . . ? C33 C34 C36 130.4(18) . . ? C34 C36 N18 111.5(14) . . ? N15 C37 N16 128.2(14) . . ? N15 C37 C30 113.7(15) . . ? N16 C37 C30 117.8(15) . . ? N15 C38 C39 113.1(13) . . ? C38 C39 C40 108.8(14) . . ? N16 C40 C39 109.4(15) . . ? N8 C41 N7 113.0(14) . . ? N7 C42 C43 111.4(13) . . ? N7 C42 C48 111.7(15) . . ? C43 C42 C48 136.7(17) . . ? C42 C43 N8 103.3(13) . . ? C42 C43 C44 142.5(17) . . ? N8 C43 C44 114.2(16) . . ? N9 C44 N10 126.5(16) . . ? N9 C44 C43 115.0(16) . . ? N10 C44 C43 118.1(18) . . ? N10 C45 C46 109.2(13) . . ? C45 C46 C47 111.8(13) . . ? N9 C47 C46 110.0(13) . . ? N12 C48 N11 125.4(16) . . ? N12 C48 C42 113.2(15) . . ? N11 C48 C42 121.4(16) . . ? N12 C49 C50 109.5(13) . . ? C51 C50 C49 108.5(14) . . ? N11 C51 C50 111.9(13) . . ? N23 C52 N22 112.2(12) . . ? C54 C53 N23 110.2(14) . . ? C54 C53 C26 138.0(16) . 3_566 ? N23 C53 C26 111.8(15) . 3_566 ? C53 C54 N22 105.5(14) . . ? C53 C54 C55 140.3(15) . . ? N22 C54 C55 114.2(14) . . ? N24 C55 N25 126.8(16) . . ? N24 C55 C54 113.6(13) . . ? N25 C55 C54 119.5(15) . . ? C57 C56 N24 111.9(13) . . ? C20 C59 N19 107.1(14) 3_566 . ? C20 C59 C60 140.6(14) 3_566 . ? N19 C59 C60 112.1(15) . . ? N20 C60 N21 125.3(15) . . ? N20 C60 C59 115.3(13) . . ? N21 C60 C59 119.4(16) . . ? N20 C61 C62 111.5(13) . . ? C63 C62 C61 110.4(13) . . ? N21 C63 C62 110.7(11) . . ? N5 C64 N6 123.7(16) . . ? N5 C64 C3 112.8(16) . . ? N6 C64 C3 123.4(16) . . ? N5 C65 C66 112.2(13) . . ? C67 C66 C65 109.0(14) . . ? N6 C67 C66 112.0(15) . . ? C1 N1 C3 103.1(13) . . ? C1 N1 Co4 142.2(11) . . ? C3 N1 Co4 114.7(11) . . ? C1 N2 C2 104.9(13) . . ? C1 N2 Co3 141.4(11) . . ? C2 N2 Co3 113.6(10) . . ? C4 N3 C5 118.4(14) . . ? C4 N3 Co3 115.5(12) . . ? C5 N3 Co3 126.1(11) . . ? C4 N4 C7 118.2(14) . . ? C64 N5 C65 118.4(14) . . ? C64 N5 Co4 114.1(11) . . ? C65 N5 Co4 126.3(11) . . ? C64 N6 C67 120.6(15) . . ? C41 N7 C42 103.5(13) . . ? C41 N7 Co1 139.0(11) . . ? C42 N7 Co1 116.8(10) . . ? C41 N8 C43 108.6(13) . . ? C41 N8 Co2 139.1(12) . . ? C43 N8 Co2 112.2(11) . . ? C44 N9 C47 120.8(14) . . ? C44 N9 Co2 115.4(12) . . ? C47 N9 Co2 123.8(11) . . ? C44 N10 C45 119.6(14) . . ? C48 N11 C51 119.2(14) . . ? C48 N12 C49 119.2(13) . . ? C48 N12 Co1 115.3(11) . . ? C49 N12 Co1 124.0(10) . . ? C29 N13 C31 107.2(12) . . ? C29 N13 Co2 139.0(12) . . ? C31 N13 Co2 113.8(9) . . ? C29 N14 C30 107.2(12) . . ? C29 N14 Co3 139.7(11) . . ? C30 N14 Co3 113.1(10) . . ? C37 N15 C38 117.3(13) . . ? C37 N15 Co3 115.8(10) . . ? C38 N15 Co3 126.5(10) . . ? C37 N16 C40 118.2(14) . . ? C32 N17 C33 116.6(14) . . ? C32 N18 C36 117.4(13) . . ? C32 N18 Co2 116.6(10) . . ? C36 N18 Co2 125.8(11) . . ? C19 N19 C59 108.2(13) 3_566 . ? C19 N19 Co2 136.9(10) 3_566 . ? C59 N19 Co2 114.9(11) . . ? C60 N20 C61 118.7(12) . . ? C60 N20 Co2 114.9(10) . . ? C61 N20 Co2 126.3(10) . . ? C60 N21 C63 119.0(14) . . ? C52 N22 C54 106.9(12) . . ? C52 N22 Co1 140.4(10) . . ? C54 N22 Co1 112.6(11) . . ? C52 N23 C53 105.3(12) . . ? C52 N23 Co3 139.9(10) . 3_566 ? C53 N23 Co3 114.7(10) . 3_566 ? C55 N24 C56 118.3(12) . . ? C55 N24 Co1 116.5(11) . . ? C56 N24 Co1 125.2(9) . . ? C55 N25 C58 120.3(16) . . ? C8 N26 C9 107.8(12) . . ? C8 N26 Co1 139.0(10) . . ? C9 N26 Co1 112.9(10) . . ? C8 N27 C10 108.9(12) . . ? C8 N27 Co4 135.9(11) . . ? C10 N27 Co4 114.3(9) . . ? C15 N28 C18 116.8(13) . . ? C15 N28 Co4 115.3(9) . . ? C18 N28 Co4 125.9(10) . . ? C15 N29 C16 119.8(13) . . ? C11 N30 C14 119.0(12) . . ? C11 N31 C12 118.6(13) . . ? C11 N31 Co1 115.6(11) . . ? C12 N31 Co1 125.8(9) . . ? C19 N32 C20 106.5(11) . . ? C19 N32 Co4 138.4(10) . . ? C20 N32 Co4 115.1(9) . . ? C21 N33 C22 117.7(13) . . ? C21 N33 Co4 116.4(11) . . ? C22 N33 Co4 125.8(11) . . ? C21 N34 C24 116.2(14) . . ? C26 N35 C25 117.9(13) . . ? C26 N35 Co3 116.3(10) . . ? C25 N35 Co3 125.6(10) . . ? C26 N36 C28 115.4(16) . . ? O206 O204 O205 87(4) . . ? O206 O204 O202 78(3) . . ? O205 O204 O202 124(5) . . ? Br7 O405 Br9 116.6(14) . . ? C58 C57 C56 128.9(18) . . ? C57 C58 N25 113.7(17) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 54.24 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.740 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.127 # Attachment '- Compound 1c.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 824166' _symmetry_space_group_name_hall '-C 2y' #Added by publCIF _audit_update_record ; 2010-03-23 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C138 H156 Cl16 Co10 N72 O11.50 S3' _chemical_formula_weight 4260.03 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' Cl Cl 0.1484 0.1585 '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' 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 'C 2/m' _symmetry_int_tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 28.550(2) _cell_length_b 22.5268(19) _cell_length_c 19.4189(16) _cell_angle_alpha 90.00 _cell_angle_beta 131.977(3) _cell_angle_gamma 90.00 _cell_volume 9284.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedra _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4340 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.8889 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30149 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 24.41 _reflns_number_total 7712 _reflns_number_gt 3582 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1403P)^2^+13.7520P] 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 7712 _refine_ls_number_parameters 582 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1740 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2748 _refine_ls_wR_factor_gt 0.2286 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Co01 Co 0.69700(5) 0.36775(6) 0.65704(8) 0.0581(4) Uani 1 1 d . C . Co02 Co 0.46766(5) 0.36878(6) 0.25672(8) 0.0608(4) Uani 1 1 d . . . Co3 Co 0.5000 0.22332(9) 0.0000 0.0866(7) Uani 1 2 d S . . Cl1 Cl 0.5000 0.5000 0.5000 0.0833(16) Uani 1 4 d S . . Cl2 Cl 0.8210(2) 0.5000 0.0498(4) 0.1153(16) Uani 1 2 d S . . Cl3 Cl 0.0000 0.6439(2) 0.5000 0.1335(19) Uani 1 2 d S . . Cl4 Cl 0.7726(3) 0.9822(4) 0.6131(4) 0.116(5) Uani 0.50 1 d P . . Cl5 Cl 0.7500 0.2500 0.0000 0.127(4) Uani 0.50 2 d SP . . Cl6 Cl 0.52826(11) 0.16990(12) 0.12246(17) 0.0748(8) Uani 1 1 d . . . Cl7 Cl 0.58523(15) 0.27956(15) 0.0563(2) 0.1237(14) Uani 1 1 d . . . C3 C 0.7303(3) 0.4694(4) 0.6180(5) 0.051(2) Uani 1 1 d . . . C4 C 0.7550(4) 0.4198(5) 0.6037(6) 0.061(3) Uani 1 1 d . . . C6 C 0.7699(4) 0.3154(5) 0.6097(7) 0.076(3) Uani 1 1 d . . . H6A H 0.7350 0.2906 0.5609 0.092 Uiso 1 1 calc . A 1 H6B H 0.7955 0.2926 0.6668 0.092 Uiso 1 1 calc . B 1 C13 C 0.5476(4) 0.2979(4) 0.4131(6) 0.054(2) Uani 1 1 d . . . C14 C 0.6018(4) 0.2979(4) 0.5071(6) 0.055(2) Uani 1 1 d . C . C16 C 0.5026(5) 0.2573(5) 0.3367(7) 0.069(3) Uani 1 1 d . . . C18 C 0.4147(5) 0.2457(5) 0.1762(7) 0.089(4) Uani 1 1 d . . . H18A H 0.3747 0.2664 0.1370 0.107 Uiso 1 1 calc R . . H18B H 0.4272 0.2401 0.1408 0.107 Uiso 1 1 calc R . . C19 C 0.4068(7) 0.1873(7) 0.2011(11) 0.147(6) Uani 1 1 d . . . H19A H 0.3799 0.1925 0.2148 0.177 Uiso 1 1 calc R . . H19B H 0.3843 0.1619 0.1471 0.177 Uiso 1 1 calc R . . C20 C 0.4604(9) 0.1576(6) 0.2748(12) 0.147(6) Uani 1 1 d . . . H20A H 0.4795 0.1385 0.2540 0.176 Uiso 1 1 calc R . . H20B H 0.4487 0.1268 0.2957 0.176 Uiso 1 1 calc R . . C22 C 0.6442(4) 0.2555(5) 0.5832(6) 0.067(3) Uani 1 1 d . C . C24 C 0.6769(7) 0.1540(6) 0.6461(11) 0.177(9) Uani 1 1 d . . . H24A H 0.6565 0.1375 0.6664 0.212 Uiso 1 1 calc R . . H24B H 0.6865 0.1217 0.6242 0.212 Uiso 1 1 calc R . . C25 C 0.7300(8) 0.1809(7) 0.7168(10) 0.170(8) Uani 1 1 d . . . H25A H 0.7601 0.1714 0.7104 0.204 Uiso 1 1 calc R . . H25B H 0.7442 0.1599 0.7715 0.204 Uiso 1 1 calc R . . C26 C 0.7399(4) 0.2436(5) 0.7417(7) 0.081(3) Uani 1 1 d . . . H26A H 0.7822 0.2549 0.7694 0.097 Uiso 1 1 calc R . . H26B H 0.7361 0.2501 0.7872 0.097 Uiso 1 1 calc R . . C33 C 0.6923(4) 0.3771(4) 0.7949(5) 0.059(3) Uani 1 1 d . . . C34 C 0.3456(4) 0.3804(4) 0.1858(5) 0.056(2) Uani 1 1 d . . . C36 C 0.7592(4) 0.3761(5) 0.8423(6) 0.075(3) Uani 1 1 d . . . C38 C 0.8353(4) 0.3772(5) 0.8303(6) 0.070(3) Uani 1 1 d . . . H38A H 0.8384 0.4018 0.7926 0.084 Uiso 1 1 calc R . . H38B H 0.8495 0.3375 0.8326 0.084 Uiso 1 1 calc R . . C39 C 0.8778(4) 0.4033(6) 0.9304(7) 0.100(4) Uani 1 1 d . . . H39A H 0.9216 0.4012 0.9594 0.120 Uiso 1 1 calc R . . H39B H 0.8672 0.4448 0.9270 0.120 Uiso 1 1 calc R . . C40 C 0.8697(4) 0.3716(7) 0.9854(7) 0.115(5) Uani 1 1 d . . . H40A H 0.8936 0.3906 1.0454 0.137 Uiso 1 1 calc R . . H40B H 0.8847 0.3312 0.9950 0.137 Uiso 1 1 calc R . . C42 C 0.3405(4) 0.3882(4) 0.1058(6) 0.060(3) Uani 1 1 d . . . C44 C 0.2793(6) 0.4061(8) -0.0588(7) 0.142(6) Uani 1 1 d . . . H44A H 0.2468 0.3787 -0.1055 0.171 Uiso 1 1 calc R . . H44B H 0.2664 0.4458 -0.0848 0.171 Uiso 1 1 calc R . . C45 C 0.3342(6) 0.3923(10) -0.0366(8) 0.195(10) Uani 1 1 d . . . H45A H 0.3384 0.4210 -0.0695 0.235 Uiso 1 1 calc R . . H45B H 0.3267 0.3544 -0.0661 0.235 Uiso 1 1 calc R . . C46 C 0.3960(4) 0.3877(5) 0.0537(6) 0.081(3) Uani 1 1 d . . . H46A H 0.4193 0.4238 0.0672 0.097 Uiso 1 1 calc R . . H46B H 0.4182 0.3549 0.0541 0.097 Uiso 1 1 calc R . . C53 C 0.5248(4) 0.4700(4) 0.2597(5) 0.054(2) Uani 1 1 d . . . C54 C 0.5528(5) 0.4183(5) 0.2496(6) 0.063(3) Uani 1 1 d . . . C56 C 0.6260(6) 0.3774(7) 0.2383(12) 0.133(6) Uani 1 1 d . . . H56A H 0.6037 0.3724 0.1732 0.160 Uiso 1 1 calc R . . H56B H 0.6701 0.3846 0.2715 0.160 Uiso 1 1 calc R . . C57 C 0.6199(5) 0.3245(5) 0.2735(9) 0.094(4) Uani 1 1 d . . . H57A H 0.6467 0.3277 0.3401 0.113 Uiso 1 1 calc R . . H57B H 0.6338 0.2904 0.2607 0.113 Uiso 1 1 calc R . . C58 C 0.5514(4) 0.3148(4) 0.2291(6) 0.070(3) Uani 1 1 d . . . H58A H 0.5255 0.3063 0.1637 0.084 Uiso 1 1 calc R . . H58B H 0.5494 0.2809 0.2578 0.084 Uiso 1 1 calc R . . C62 C 0.5237(14) 0.0000 0.127(2) 0.210(12) Uiso 1 2 d S . . C63 C 0.502(3) 0.0000 0.245(4) 0.43(4) Uiso 1 2 d S . . C71 C 0.8081(9) 0.3318(7) 0.5868(14) 0.147(7) Uani 1 1 d . C 1 H71A H 0.8506 0.3191 0.6399 0.177 Uiso 1 1 calc . D 1 H71B H 0.7940 0.3054 0.5366 0.177 Uiso 1 1 calc . E 1 C81 C 0.8150(10) 0.3814(8) 0.5647(19) 0.202(11) Uani 1 1 d . C 1 H81A H 0.7955 0.3801 0.5004 0.243 Uiso 1 1 calc . F 1 H81B H 0.8596 0.3891 0.6022 0.243 Uiso 1 1 calc . G 1 C91 C 1.0000 0.9364(13) 1.0000 0.177(10) Uiso 1 2 d S . . C500 C 0.5796(3) 0.3904(4) 0.4590(5) 0.0398(19) Uani 1 1 d . . . H500 H 0.5813 0.4316 0.4584 0.048 Uiso 1 1 calc R . . C501 C 0.4596(5) 0.5000 0.2722(7) 0.047(3) Uani 1 2 d S . . H501 H 0.4303 0.5000 0.2788 0.057 Uiso 1 2 calc SR . . C502 C 0.6770(5) 0.5000 0.6552(7) 0.050(3) Uani 1 2 d S . . H502 H 0.6522 0.5000 0.6703 0.060 Uiso 1 2 calc SR . . C503 C 0.4042(4) 0.3733(3) 0.3334(6) 0.046(2) Uani 1 1 d . . . H503 H 0.4394 0.3712 0.3965 0.055 Uiso 1 1 calc R . . N2 N 0.6976(3) 0.4500(3) 0.6426(4) 0.0449(18) Uani 1 1 d . . . N5 N 0.7456(3) 0.3677(4) 0.6205(5) 0.0519(18) Uani 1 1 d . C . N12 N 0.5350(3) 0.3564(3) 0.3850(4) 0.0491(18) Uani 1 1 d . . . N15 N 0.6210(3) 0.3561(3) 0.5335(4) 0.0487(18) Uani 1 1 d . . . N17 N 0.4624(3) 0.2827(3) 0.2582(5) 0.060(2) Uani 1 1 d . . . N21 N 0.5088(5) 0.1987(4) 0.3561(6) 0.118(4) Uani 1 1 d . . . N23 N 0.6332(4) 0.1976(4) 0.5683(7) 0.118(4) Uani 1 1 d . . . N24 N 0.6932(3) 0.2814(3) 0.6589(5) 0.0562(19) Uani 1 1 d . . . N32 N 0.6536(3) 0.3733(3) 0.7004(4) 0.0497(19) Uani 1 1 d . . . N35 N 0.4072(3) 0.3766(3) 0.2689(4) 0.0476(18) Uani 1 1 d . . . N37 N 0.7710(3) 0.3751(3) 0.7900(4) 0.0528(19) Uani 1 1 d . . . N41 N 0.8013(4) 0.3716(6) 0.9357(5) 0.133(5) Uani 1 1 d . . . N43 N 0.2856(3) 0.4034(5) 0.0246(5) 0.088(3) Uani 1 1 d . . . N44 N 0.3936(3) 0.3781(3) 0.1258(4) 0.060(2) Uani 1 1 d . . . N52 N 0.4822(3) 0.4501(3) 0.2671(4) 0.0459(18) Uani 1 1 d . . . N55 N 0.5996(4) 0.4287(4) 0.2502(7) 0.092(3) Uani 1 1 d . . . N59 N 0.5276(3) 0.3666(4) 0.2404(5) 0.0549(19) Uani 1 1 d . . . N91 N 0.7867(6) 0.4311(5) 0.5773(10) 0.147(5) Uani 1 1 d . C 1 O1 O 0.9098(17) 1.0000 0.909(2) 0.182(13) Uiso 0.50 2 d SP . . O2 O 0.6037(11) -0.0190(10) 0.3030(15) 0.072(8) Uiso 0.25 1 d P . . O100 O 0.6613(8) 1.0000 0.6950(12) 0.167(6) Uiso 1 2 d S . . O101 O 0.617(2) 1.0000 0.585(3) 0.219(16) Uiso 0.50 2 d SP . . O102 O 0.9149(18) 0.588(2) 0.548(3) 0.212(17) Uiso 0.33 1 d P . . O103 O 0.7943(19) 0.0000 0.793(3) 0.273(18) Uiso 0.60 2 d SP . . O104 O 0.9374(7) 0.5354(7) 0.5222(11) 0.254(7) Uiso 1 1 d . . . S11 S 0.9733(5) 1.0000 1.0056(7) 0.116(3) Uani 0.50 2 d SP . . S61 S 0.5398(4) 0.0278(4) 0.2270(6) 0.163(4) Uani 0.50 1 d P . . 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 Co01 0.0432(7) 0.0747(10) 0.0479(7) 0.0044(6) 0.0270(6) 0.0078(6) Co02 0.0476(7) 0.0826(10) 0.0478(7) -0.0101(6) 0.0301(6) -0.0030(7) Co3 0.0653(13) 0.0725(15) 0.0913(15) 0.000 0.0397(11) 0.000 Cl1 0.077(4) 0.083(4) 0.079(3) 0.000 0.048(3) 0.000 Cl2 0.082(3) 0.141(4) 0.139(4) 0.000 0.081(3) 0.000 Cl3 0.132(4) 0.113(4) 0.133(4) 0.000 0.079(4) 0.000 Cl4 0.078(3) 0.148(14) 0.090(3) 0.016(4) 0.043(3) -0.013(4) Cl5 0.058(5) 0.139(9) 0.125(8) 0.039(6) 0.037(5) 0.015(5) Cl6 0.0577(15) 0.0769(19) 0.0809(16) 0.0049(14) 0.0426(13) 0.0017(13) Cl7 0.100(2) 0.096(2) 0.110(2) 0.0092(19) 0.0438(19) -0.0422(19) C3 0.033(4) 0.079(7) 0.040(4) -0.005(4) 0.025(4) 0.002(4) C4 0.045(6) 0.085(9) 0.069(6) -0.009(6) 0.044(5) -0.004(5) C6 0.052(6) 0.095(9) 0.092(7) -0.004(6) 0.052(6) 0.009(6) C13 0.046(5) 0.057(6) 0.050(5) -0.015(5) 0.028(4) -0.005(5) C14 0.033(5) 0.062(7) 0.061(6) 0.003(5) 0.028(4) 0.009(5) C16 0.069(7) 0.066(8) 0.067(7) -0.029(6) 0.044(6) -0.012(6) C18 0.091(8) 0.085(9) 0.074(7) -0.035(7) 0.048(7) -0.021(7) C19 0.114(12) 0.106(13) 0.126(12) -0.038(10) 0.040(10) -0.045(10) C20 0.194(18) 0.062(9) 0.160(15) -0.042(10) 0.108(14) -0.031(11) C22 0.038(5) 0.062(7) 0.067(6) 0.008(5) 0.020(5) 0.002(5) C24 0.116(12) 0.071(10) 0.143(13) 0.033(10) 0.004(10) 0.015(9) C25 0.186(17) 0.088(12) 0.095(10) 0.039(9) 0.035(11) 0.039(11) C26 0.052(6) 0.079(8) 0.075(7) 0.036(6) 0.027(5) 0.033(6) C33 0.036(5) 0.101(8) 0.041(5) 0.011(5) 0.026(4) 0.017(5) C34 0.045(5) 0.084(7) 0.044(5) -0.017(5) 0.032(4) -0.011(5) C36 0.031(5) 0.131(10) 0.040(5) 0.013(5) 0.014(4) 0.024(5) C38 0.028(5) 0.115(9) 0.053(5) -0.001(5) 0.021(4) 0.004(5) C39 0.025(5) 0.154(12) 0.072(7) -0.044(8) 0.013(5) -0.005(6) C40 0.041(6) 0.258(18) 0.039(5) -0.002(8) 0.024(5) 0.021(8) C42 0.049(6) 0.087(7) 0.049(5) -0.022(5) 0.035(5) -0.012(5) C44 0.084(9) 0.30(2) 0.044(6) -0.007(9) 0.044(6) 0.020(11) C45 0.054(8) 0.47(3) 0.056(7) 0.026(12) 0.033(6) 0.082(13) C46 0.059(6) 0.141(10) 0.041(5) -0.008(6) 0.032(5) -0.002(6) C53 0.051(5) 0.060(6) 0.036(4) -0.003(4) 0.023(4) 0.004(4) C54 0.059(6) 0.091(9) 0.057(6) 0.012(6) 0.046(5) 0.023(6) C56 0.096(10) 0.134(14) 0.221(17) 0.030(12) 0.127(12) 0.020(9) C57 0.081(8) 0.093(10) 0.123(10) 0.014(8) 0.074(8) 0.033(7) C58 0.068(7) 0.076(7) 0.070(6) -0.013(5) 0.048(5) 0.017(5) C71 0.222(18) 0.082(11) 0.253(19) 0.020(12) 0.205(17) 0.047(12) C81 0.27(2) 0.110(14) 0.44(3) -0.079(18) 0.32(3) -0.035(15) C500 0.029(4) 0.049(5) 0.040(4) -0.004(4) 0.022(4) 0.002(4) C501 0.036(7) 0.073(10) 0.027(6) 0.000 0.019(5) 0.000 C502 0.027(6) 0.082(11) 0.039(6) 0.000 0.022(5) 0.000 C503 0.029(5) 0.058(6) 0.044(4) -0.010(4) 0.022(4) -0.009(4) N2 0.025(3) 0.066(5) 0.038(4) -0.003(3) 0.019(3) -0.001(3) N5 0.042(4) 0.060(5) 0.059(4) -0.006(4) 0.036(4) -0.001(4) N12 0.043(4) 0.057(5) 0.042(4) -0.008(4) 0.027(3) 0.002(4) N15 0.037(4) 0.056(5) 0.044(4) 0.000(4) 0.024(3) 0.008(3) N17 0.050(4) 0.063(5) 0.048(4) -0.026(4) 0.025(4) -0.015(4) N21 0.138(9) 0.042(6) 0.095(7) -0.013(5) 0.046(6) -0.016(6) N23 0.099(7) 0.047(6) 0.109(7) 0.005(5) 0.028(6) 0.005(5) N24 0.043(4) 0.059(5) 0.057(4) 0.010(4) 0.029(4) 0.006(4) N32 0.036(4) 0.077(5) 0.039(4) 0.013(3) 0.026(3) 0.011(4) N35 0.026(3) 0.063(5) 0.038(4) -0.011(3) 0.015(3) -0.005(3) N37 0.032(4) 0.084(6) 0.042(4) 0.006(4) 0.025(3) 0.012(4) N41 0.035(5) 0.306(16) 0.038(4) 0.026(6) 0.016(4) 0.058(7) N43 0.048(5) 0.158(9) 0.043(4) 0.001(5) 0.024(4) 0.002(5) N44 0.054(5) 0.090(6) 0.042(4) -0.010(4) 0.035(4) -0.007(4) N52 0.037(4) 0.061(5) 0.046(4) -0.006(3) 0.030(3) -0.001(3) N55 0.086(7) 0.106(8) 0.135(8) 0.019(6) 0.095(7) 0.025(6) N59 0.045(4) 0.071(6) 0.050(4) -0.011(4) 0.032(4) 0.005(4) N91 0.212(13) 0.078(7) 0.302(17) -0.035(9) 0.235(15) -0.022(8) S11 0.116(8) 0.139(9) 0.114(8) 0.000 0.086(7) 0.000 S61 0.143(7) 0.114(7) 0.130(7) -0.005(5) 0.049(6) -0.036(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 Co01 N2 1.876(7) . ? Co01 N15 1.889(6) . ? Co01 N32 1.913(7) . ? Co01 N5 1.935(7) . ? Co01 N24 1.951(7) . ? Co01 N37 1.965(6) . ? Co02 N52 1.860(7) . ? Co02 N12 1.890(6) . ? Co02 N35 1.900(7) . ? Co02 N59 1.937(7) . ? Co02 N44 1.946(7) . ? Co02 N17 1.947(8) . ? Co3 Cl7 2.272(3) . ? Co3 Cl7 2.272(3) 2_655 ? Co3 Cl6 2.278(3) 2_655 ? Co3 Cl6 2.278(3) . ? Cl4 Cl4 0.80(2) 6_575 ? C3 N2 1.373(10) . ? C3 C3 1.381(17) 6_565 ? C3 C4 1.443(12) . ? C4 N5 1.292(11) . ? C4 N91 1.331(12) . ? C6 N5 1.453(12) . ? C6 C71 1.476(18) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C13 N12 1.379(11) . ? C13 C14 1.396(11) . ? C13 C16 1.461(11) . ? C14 N15 1.381(11) . ? C14 C22 1.474(12) . ? C16 N17 1.275(11) . ? C16 N21 1.353(13) . ? C18 C19 1.471(17) . ? C18 N17 1.478(11) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.382(19) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N21 1.530(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 N24 1.307(10) . ? C22 N23 1.327(12) . ? C24 C25 1.328(18) . ? C24 N23 1.511(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.458(17) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N24 1.489(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C33 C34 1.364(11) 2_656 ? C33 N32 1.372(10) . ? C33 C36 1.464(12) . ? C34 C33 1.364(11) 2_656 ? C34 N35 1.382(9) . ? C34 C42 1.472(11) . ? C36 N37 1.265(11) . ? C36 N41 1.353(11) . ? C38 N37 1.436(10) . ? C38 C39 1.562(13) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.427(15) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 N41 1.491(12) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 N44 1.307(11) . ? C42 N43 1.324(11) . ? C44 C45 1.356(15) . ? C44 N43 1.505(12) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.434(13) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 N44 1.463(11) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C53 C53 1.351(16) 6_565 ? C53 N52 1.393(11) . ? C53 C54 1.498(12) . ? C54 N59 1.319(12) . ? C54 N55 1.346(12) . ? C56 C57 1.443(15) . ? C56 N55 1.480(15) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.535(13) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 N59 1.440(10) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C62 S61 1.79(3) . ? C62 S61 1.79(3) 6 ? C63 S61 1.49(6) . ? C63 S61 1.49(6) 6 ? C71 C81 1.26(2) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C81 N91 1.493(16) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C91 S11 1.66(2) 5_777 ? C91 S11 1.66(2) . ? C500 N15 1.342(9) . ? C500 N12 1.352(9) . ? C500 H500 0.9300 . ? C501 N52 1.330(8) 6_565 ? C501 N52 1.330(8) . ? C501 H501 0.9300 . ? C502 N2 1.365(9) 6_565 ? C502 N2 1.365(9) . ? C502 H502 0.9300 . ? C503 N32 1.304(9) 2_656 ? C503 N35 1.316(9) . ? C503 H503 0.9300 . ? N32 C503 1.304(9) 2_656 ? O1 S11 1.50(3) . ? O2 O2 0.86(4) 6 ? O2 S61 1.39(2) 6 ? O2 S61 1.74(2) . ? O100 O101 1.59(4) . ? O101 O104 1.75(4) 7_666 ? O101 O104 1.75(4) 4_656 ? O102 O104 1.58(4) . ? O104 O104 1.59(3) 6_565 ? O104 O101 1.75(4) 7_666 ? S11 C91 1.66(2) 5_777 ? S11 S11 1.68(2) 5_777 ? S61 S61 1.253(16) 6 ? S61 O2 1.39(2) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co01 N15 93.7(3) . . ? N2 Co01 N32 94.3(3) . . ? N15 Co01 N32 92.1(3) . . ? N2 Co01 N5 82.2(3) . . ? N15 Co01 N5 91.7(3) . . ? N32 Co01 N5 175.0(3) . . ? N2 Co01 N24 173.9(3) . . ? N15 Co01 N24 81.6(3) . . ? N32 Co01 N24 89.8(3) . . ? N5 Co01 N24 93.9(3) . . ? N2 Co01 N37 90.3(3) . . ? N15 Co01 N37 173.1(3) . . ? N32 Co01 N37 81.9(3) . . ? N5 Co01 N37 94.4(3) . . ? N24 Co01 N37 94.8(3) . . ? N52 Co02 N12 92.6(3) . . ? N52 Co02 N35 92.9(3) . . ? N12 Co02 N35 93.3(3) . . ? N52 Co02 N59 83.5(3) . . ? N12 Co02 N59 88.9(3) . . ? N35 Co02 N59 175.8(3) . . ? N52 Co02 N44 90.2(3) . . ? N12 Co02 N44 175.0(3) . . ? N35 Co02 N44 82.4(3) . . ? N59 Co02 N44 95.5(3) . . ? N52 Co02 N17 173.6(3) . . ? N12 Co02 N17 81.6(3) . . ? N35 Co02 N17 90.3(3) . . ? N59 Co02 N17 93.5(3) . . ? N44 Co02 N17 95.7(3) . . ? Cl7 Co3 Cl7 112.2(2) . 2_655 ? Cl7 Co3 Cl6 108.35(12) . 2_655 ? Cl7 Co3 Cl6 105.93(10) 2_655 2_655 ? Cl7 Co3 Cl6 105.93(10) . . ? Cl7 Co3 Cl6 108.34(12) 2_655 . ? Cl6 Co3 Cl6 116.21(16) 2_655 . ? N2 C3 C3 108.5(5) . 6_565 ? N2 C3 C4 110.8(8) . . ? C3 C3 C4 140.7(6) 6_565 . ? N5 C4 N91 125.4(10) . . ? N5 C4 C3 116.3(9) . . ? N91 C4 C3 118.2(10) . . ? N5 C6 C71 111.1(10) . . ? N5 C6 H6A 109.4 . . ? C71 C6 H6A 109.4 . . ? N5 C6 H6B 109.4 . . ? C71 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N12 C13 C14 106.5(7) . . ? N12 C13 C16 112.1(8) . . ? C14 C13 C16 141.3(10) . . ? N15 C14 C13 107.7(8) . . ? N15 C14 C22 112.8(7) . . ? C13 C14 C22 139.5(9) . . ? N17 C16 N21 128.0(9) . . ? N17 C16 C13 114.3(9) . . ? N21 C16 C13 117.8(10) . . ? C19 C18 N17 112.5(10) . . ? C19 C18 H18A 109.1 . . ? N17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? N17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 117.8(13) . . ? C20 C19 H19A 107.9 . . ? C18 C19 H19A 107.9 . . ? C20 C19 H19B 107.9 . . ? C18 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? C19 C20 N21 112.7(12) . . ? C19 C20 H20A 109.1 . . ? N21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? N21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? N24 C22 N23 127.1(9) . . ? N24 C22 C14 112.5(9) . . ? N23 C22 C14 120.2(9) . . ? C25 C24 N23 110.2(12) . . ? C25 C24 H24A 109.6 . . ? N23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? N23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 128.3(13) . . ? C24 C25 H25A 105.2 . . ? C26 C25 H25A 105.2 . . ? C24 C25 H25B 105.2 . . ? C26 C25 H25B 105.2 . . ? H25A C25 H25B 105.9 . . ? C25 C26 N24 111.1(9) . . ? C25 C26 H26A 109.4 . . ? N24 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? N24 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C34 C33 N32 107.0(7) 2_656 . ? C34 C33 C36 140.3(8) 2_656 . ? N32 C33 C36 112.6(8) . . ? C33 C34 N35 107.5(7) 2_656 . ? C33 C34 C42 139.6(8) 2_656 . ? N35 C34 C42 112.9(8) . . ? N37 C36 N41 126.9(9) . . ? N37 C36 C33 115.6(7) . . ? N41 C36 C33 117.3(9) . . ? N37 C38 C39 109.7(8) . . ? N37 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? N37 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C40 C39 C38 111.3(10) . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? C38 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C40 N41 108.3(9) . . ? C39 C40 H40A 110.0 . . ? N41 C40 H40A 110.0 . . ? C39 C40 H40B 110.0 . . ? N41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? N44 C42 N43 127.7(9) . . ? N44 C42 C34 112.9(8) . . ? N43 C42 C34 119.3(8) . . ? C45 C44 N43 111.6(10) . . ? C45 C44 H44A 109.3 . . ? N43 C44 H44A 109.3 . . ? C45 C44 H44B 109.3 . . ? N43 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C46 128.3(11) . . ? C44 C45 H45A 105.2 . . ? C46 C45 H45A 105.2 . . ? C44 C45 H45B 105.2 . . ? C46 C45 H45B 105.2 . . ? H45A C45 H45B 105.9 . . ? C45 C46 N44 112.0(9) . . ? C45 C46 H46A 109.2 . . ? N44 C46 H46A 109.2 . . ? C45 C46 H46B 109.2 . . ? N44 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C53 C53 N52 108.8(4) 6_565 . ? C53 C53 C54 141.0(6) 6_565 . ? N52 C53 C54 110.1(8) . . ? N59 C54 N55 127.2(9) . . ? N59 C54 C53 114.4(9) . . ? N55 C54 C53 118.4(10) . . ? C57 C56 N55 109.6(11) . . ? C57 C56 H56A 109.7 . . ? N55 C56 H56A 109.7 . . ? C57 C56 H56B 109.7 . . ? N55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? C56 C57 C58 111.3(9) . . ? C56 C57 H57A 109.4 . . ? C58 C57 H57A 109.4 . . ? C56 C57 H57B 109.4 . . ? C58 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? N59 C58 C57 110.7(8) . . ? N59 C58 H58A 109.5 . . ? C57 C58 H58A 109.5 . . ? N59 C58 H58B 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 108.1 . . ? S61 C62 S61 41.0(9) . 6 ? S61 C63 S61 50(2) . 6 ? C81 C71 C6 129.9(13) . . ? C81 C71 H71A 104.8 . . ? C6 C71 H71A 104.8 . . ? C81 C71 H71B 104.8 . . ? C6 C71 H71B 104.8 . . ? H71A C71 H71B 105.8 . . ? C71 C81 N91 112.7(14) . . ? C71 C81 H81A 109.1 . . ? N91 C81 H81A 109.1 . . ? C71 C81 H81B 109.1 . . ? N91 C81 H81B 109.1 . . ? H81A C81 H81B 107.8 . . ? S11 C91 S11 60.6(13) 5_777 . ? N15 C500 N12 110.1(7) . . ? N15 C500 H500 125.0 . . ? N12 C500 H500 125.0 . . ? N52 C501 N52 115.2(11) 6_565 . ? N52 C501 H501 122.4 6_565 . ? N52 C501 H501 122.4 . . ? N2 C502 N2 111.1(11) 6_565 . ? N2 C502 H502 124.4 6_565 . ? N2 C502 H502 124.4 . . ? N32 C503 N35 112.7(7) 2_656 . ? N32 C503 H503 123.6 2_656 . ? N35 C503 H503 123.6 . . ? C502 N2 C3 105.9(8) . . ? C502 N2 Co01 137.7(6) . . ? C3 N2 Co01 116.2(5) . . ? C4 N5 C6 120.1(8) . . ? C4 N5 Co01 114.3(6) . . ? C6 N5 Co01 125.5(7) . . ? C500 N12 C13 108.1(6) . . ? C500 N12 Co02 136.2(6) . . ? C13 N12 Co02 115.4(5) . . ? C500 N15 C14 107.6(7) . . ? C500 N15 Co01 136.4(6) . . ? C14 N15 Co01 115.9(5) . . ? C16 N17 C18 118.7(9) . . ? C16 N17 Co02 116.5(6) . . ? C18 N17 Co02 124.8(7) . . ? C16 N21 C20 116.4(10) . . ? C22 N23 C24 120.3(10) . . ? C22 N24 C26 118.1(8) . . ? C22 N24 Co01 117.1(6) . . ? C26 N24 Co01 124.6(6) . . ? C503 N32 C33 106.9(7) 2_656 . ? C503 N32 Co01 138.7(6) 2_656 . ? C33 N32 Co01 114.4(5) . . ? C503 N35 C34 105.8(7) . . ? C503 N35 Co02 139.2(5) . . ? C34 N35 Co02 114.4(6) . . ? C36 N37 C38 119.4(7) . . ? C36 N37 Co01 115.3(6) . . ? C38 N37 Co01 125.3(6) . . ? C36 N41 C40 118.2(9) . . ? C42 N43 C44 119.1(9) . . ? C42 N44 C46 118.4(7) . . ? C42 N44 Co02 116.0(6) . . ? C46 N44 Co02 124.1(6) . . ? C501 N52 C53 103.6(8) . . ? C501 N52 Co02 139.2(7) . . ? C53 N52 Co02 116.9(5) . . ? C54 N55 C56 118.0(10) . . ? C54 N59 C58 117.7(8) . . ? C54 N59 Co02 114.8(6) . . ? C58 N59 Co02 127.2(7) . . ? C4 N91 C81 120.1(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 C4 N5 -3.5(11) . . . . ? C3 C3 C4 N5 173.7(4) 6_565 . . . ? N2 C3 C4 N91 178.4(9) . . . . ? C3 C3 C4 N91 -4.4(14) 6_565 . . . ? N12 C13 C14 N15 -0.5(10) . . . . ? C16 C13 C14 N15 176.7(11) . . . . ? N12 C13 C14 C22 -178.1(11) . . . . ? C16 C13 C14 C22 -1(2) . . . . ? N12 C13 C16 N17 3.3(12) . . . . ? C14 C13 C16 N17 -173.8(11) . . . . ? N12 C13 C16 N21 -177.9(9) . . . . ? C14 C13 C16 N21 5.0(19) . . . . ? N17 C18 C19 C20 -42(2) . . . . ? C18 C19 C20 N21 41(2) . . . . ? N15 C14 C22 N24 -3.5(12) . . . . ? C13 C14 C22 N24 174.0(11) . . . . ? N15 C14 C22 N23 -178.1(10) . . . . ? C13 C14 C22 N23 -0.5(19) . . . . ? N23 C24 C25 C26 26(3) . . . . ? C24 C25 C26 N24 -26(3) . . . . ? C34 C33 C36 N37 -176.8(12) 2_656 . . . ? N32 C33 C36 N37 3.5(13) . . . . ? C34 C33 C36 N41 8(2) 2_656 . . . ? N32 C33 C36 N41 -171.4(10) . . . . ? N37 C38 C39 C40 53.7(12) . . . . ? C38 C39 C40 N41 -54.8(14) . . . . ? C33 C34 C42 N44 -169.2(11) 2_656 . . . ? N35 C34 C42 N44 13.0(11) . . . . ? C33 C34 C42 N43 10.1(18) 2_656 . . . ? N35 C34 C42 N43 -167.7(9) . . . . ? N43 C44 C45 C46 -13(3) . . . . ? C44 C45 C46 N44 21(3) . . . . ? C53 C53 C54 N59 -169.3(4) 6_565 . . . ? N52 C53 C54 N59 6.4(10) . . . . ? C53 C53 C54 N55 10.5(12) 6_565 . . . ? N52 C53 C54 N55 -173.8(8) . . . . ? N55 C56 C57 C58 54.1(15) . . . . ? C56 C57 C58 N59 -54.3(14) . . . . ? N5 C6 C71 C81 -10(3) . . . . ? C6 C71 C81 N91 9(4) . . . . ? N2 C502 N2 C3 -2.2(11) 6_565 . . . ? N2 C502 N2 Co01 173.0(2) 6_565 . . . ? C3 C3 N2 C502 1.3(6) 6_565 . . . ? C4 C3 N2 C502 179.4(7) . . . . ? C3 C3 N2 Co01 -175.1(2) 6_565 . . . ? C4 C3 N2 Co01 3.1(8) . . . . ? N15 Co01 N2 C502 92.4(9) . . . . ? N32 Co01 N2 C502 0.0(9) . . . . ? N5 Co01 N2 C502 -176.4(9) . . . . ? N24 Co01 N2 C502 132(3) . . . . ? N37 Co01 N2 C502 -81.9(9) . . . . ? N15 Co01 N2 C3 -92.8(5) . . . . ? N32 Co01 N2 C3 174.8(5) . . . . ? N5 Co01 N2 C3 -1.6(5) . . . . ? N24 Co01 N2 C3 -53(3) . . . . ? N37 Co01 N2 C3 92.8(5) . . . . ? N91 C4 N5 C6 -0.9(15) . . . . ? C3 C4 N5 C6 -178.8(7) . . . . ? N91 C4 N5 Co01 -179.7(10) . . . . ? C3 C4 N5 Co01 2.3(10) . . . . ? C71 C6 N5 C4 4.8(14) . . . . ? C71 C6 N5 Co01 -176.5(9) . . . . ? N2 Co01 N5 C4 -0.4(6) . . . . ? N15 Co01 N5 C4 93.1(7) . . . . ? N32 Co01 N5 C4 -47(4) . . . . ? N24 Co01 N5 C4 174.8(6) . . . . ? N37 Co01 N5 C4 -90.1(7) . . . . ? N2 Co01 N5 C6 -179.3(7) . . . . ? N15 Co01 N5 C6 -85.7(7) . . . . ? N32 Co01 N5 C6 134(3) . . . . ? N24 Co01 N5 C6 -4.0(7) . . . . ? N37 Co01 N5 C6 91.1(7) . . . . ? N15 C500 N12 C13 0.9(9) . . . . ? N15 C500 N12 Co02 -172.3(6) . . . . ? C14 C13 N12 C500 -0.2(9) . . . . ? C16 C13 N12 C500 -178.3(7) . . . . ? C14 C13 N12 Co02 174.6(6) . . . . ? C16 C13 N12 Co02 -3.5(10) . . . . ? N52 Co02 N12 C500 -2.1(8) . . . . ? N35 Co02 N12 C500 -95.1(8) . . . . ? N59 Co02 N12 C500 81.3(8) . . . . ? N44 Co02 N12 C500 -127(4) . . . . ? N17 Co02 N12 C500 175.1(8) . . . . ? N52 Co02 N12 C13 -174.9(6) . . . . ? N35 Co02 N12 C13 92.0(6) . . . . ? N59 Co02 N12 C13 -91.5(6) . . . . ? N44 Co02 N12 C13 60(4) . . . . ? N17 Co02 N12 C13 2.2(6) . . . . ? N12 C500 N15 C14 -1.2(9) . . . . ? N12 C500 N15 Co01 175.4(6) . . . . ? C13 C14 N15 C500 1.1(9) . . . . ? C22 C14 N15 C500 179.4(7) . . . . ? C13 C14 N15 Co01 -176.3(6) . . . . ? C22 C14 N15 Co01 2.0(10) . . . . ? N2 Co01 N15 C500 -0.5(8) . . . . ? N32 Co01 N15 C500 93.9(8) . . . . ? N5 Co01 N15 C500 -82.8(8) . . . . ? N24 Co01 N15 C500 -176.6(8) . . . . ? N37 Co01 N15 C500 124(2) . . . . ? N2 Co01 N15 C14 175.9(6) . . . . ? N32 Co01 N15 C14 -89.7(6) . . . . ? N5 Co01 N15 C14 93.5(6) . . . . ? N24 Co01 N15 C14 -0.2(6) . . . . ? N37 Co01 N15 C14 -59(3) . . . . ? N21 C16 N17 C18 1.4(17) . . . . ? C13 C16 N17 C18 -179.9(8) . . . . ? N21 C16 N17 Co02 179.7(9) . . . . ? C13 C16 N17 Co02 -1.6(11) . . . . ? C19 C18 N17 C16 19.5(15) . . . . ? C19 C18 N17 Co02 -158.7(10) . . . . ? N52 Co02 N17 C16 26(3) . . . . ? N12 Co02 N17 C16 -0.3(7) . . . . ? N35 Co02 N17 C16 -93.6(7) . . . . ? N59 Co02 N17 C16 88.0(7) . . . . ? N44 Co02 N17 C16 -176.0(7) . . . . ? N52 Co02 N17 C18 -155(3) . . . . ? N12 Co02 N17 C18 178.0(8) . . . . ? N35 Co02 N17 C18 84.7(8) . . . . ? N59 Co02 N17 C18 -93.7(8) . . . . ? N44 Co02 N17 C18 2.2(8) . . . . ? N17 C16 N21 C20 -2.1(19) . . . . ? C13 C16 N21 C20 179.2(11) . . . . ? C19 C20 N21 C16 -19(2) . . . . ? N24 C22 N23 C24 6(2) . . . . ? C14 C22 N23 C24 179.4(13) . . . . ? C25 C24 N23 C22 -14(2) . . . . ? N23 C22 N24 C26 -6.2(17) . . . . ? C14 C22 N24 C26 179.7(8) . . . . ? N23 C22 N24 Co01 177.6(10) . . . . ? C14 C22 N24 Co01 3.5(11) . . . . ? C25 C26 N24 C22 13.7(15) . . . . ? C25 C26 N24 Co01 -170.4(10) . . . . ? N2 Co01 N24 C22 -42(3) . . . . ? N15 Co01 N24 C22 -2.0(7) . . . . ? N32 Co01 N24 C22 90.2(7) . . . . ? N5 Co01 N24 C22 -93.1(7) . . . . ? N37 Co01 N24 C22 172.1(7) . . . . ? N2 Co01 N24 C26 142(3) . . . . ? N15 Co01 N24 C26 -177.9(8) . . . . ? N32 Co01 N24 C26 -85.8(7) . . . . ? N5 Co01 N24 C26 90.9(7) . . . . ? N37 Co01 N24 C26 -3.9(8) . . . . ? C34 C33 N32 C503 -1.1(10) 2_656 . . 2_656 ? C36 C33 N32 C503 178.7(8) . . . 2_656 ? C34 C33 N32 Co01 -179.8(6) 2_656 . . . ? C36 C33 N32 Co01 0.0(10) . . . . ? N2 Co01 N32 C503 90.2(9) . . . 2_656 ? N15 Co01 N32 C503 -3.7(9) . . . 2_656 ? N5 Co01 N32 C503 136(3) . . . 2_656 ? N24 Co01 N32 C503 -85.3(9) . . . 2_656 ? N37 Co01 N32 C503 179.9(9) . . . 2_656 ? N2 Co01 N32 C33 -91.7(6) . . . . ? N15 Co01 N32 C33 174.4(6) . . . . ? N5 Co01 N32 C33 -46(4) . . . . ? N24 Co01 N32 C33 92.8(6) . . . . ? N37 Co01 N32 C33 -2.1(6) . . . . ? N32 C503 N35 C34 1.4(9) 2_656 . . . ? N32 C503 N35 Co02 -169.3(6) 2_656 . . . ? C33 C34 N35 C503 -2.1(10) 2_656 . . . ? C42 C34 N35 C503 176.4(7) . . . . ? C33 C34 N35 Co02 171.3(6) 2_656 . . . ? C42 C34 N35 Co02 -10.2(10) . . . . ? N52 Co02 N35 C503 -95.9(9) . . . . ? N12 Co02 N35 C503 -3.0(9) . . . . ? N59 Co02 N35 C503 -124(4) . . . . ? N44 Co02 N35 C503 174.3(9) . . . . ? N17 Co02 N35 C503 78.6(9) . . . . ? N52 Co02 N35 C34 93.9(6) . . . . ? N12 Co02 N35 C34 -173.3(6) . . . . ? N59 Co02 N35 C34 65(4) . . . . ? N44 Co02 N35 C34 4.1(6) . . . . ? N17 Co02 N35 C34 -91.7(6) . . . . ? N41 C36 N37 C38 -8.9(17) . . . . ? C33 C36 N37 C38 176.7(9) . . . . ? N41 C36 N37 Co01 169.1(11) . . . . ? C33 C36 N37 Co01 -5.3(12) . . . . ? C39 C38 N37 C36 -20.6(13) . . . . ? C39 C38 N37 Co01 161.7(7) . . . . ? N2 Co01 N37 C36 98.5(8) . . . . ? N15 Co01 N37 C36 -26(3) . . . . ? N32 Co01 N37 C36 4.2(7) . . . . ? N5 Co01 N37 C36 -179.2(8) . . . . ? N24 Co01 N37 C36 -84.9(8) . . . . ? N2 Co01 N37 C38 -83.7(8) . . . . ? N15 Co01 N37 C38 151(2) . . . . ? N32 Co01 N37 C38 -178.0(8) . . . . ? N5 Co01 N37 C38 -1.4(8) . . . . ? N24 Co01 N37 C38 92.9(8) . . . . ? N37 C36 N41 C40 7(2) . . . . ? C33 C36 N41 C40 -178.9(11) . . . . ? C39 C40 N41 C36 27.0(18) . . . . ? N44 C42 N43 C44 4.4(17) . . . . ? C34 C42 N43 C44 -174.8(11) . . . . ? C45 C44 N43 C42 -1(2) . . . . ? N43 C42 N44 C46 4.3(15) . . . . ? C34 C42 N44 C46 -176.5(8) . . . . ? N43 C42 N44 Co02 170.8(9) . . . . ? C34 C42 N44 Co02 -9.9(10) . . . . ? C45 C46 N44 C42 -15.2(16) . . . . ? C45 C46 N44 Co02 179.4(11) . . . . ? N52 Co02 N44 C42 -89.2(7) . . . . ? N12 Co02 N44 C42 36(4) . . . . ? N35 Co02 N44 C42 3.6(7) . . . . ? N59 Co02 N44 C42 -172.7(7) . . . . ? N17 Co02 N44 C42 93.2(7) . . . . ? N52 Co02 N44 C46 76.5(8) . . . . ? N12 Co02 N44 C46 -158(3) . . . . ? N35 Co02 N44 C46 169.3(8) . . . . ? N59 Co02 N44 C46 -7.0(8) . . . . ? N17 Co02 N44 C46 -101.1(8) . . . . ? N52 C501 N52 C53 1.2(11) 6_565 . . . ? N52 C501 N52 Co02 -171.6(3) 6_565 . . . ? C53 C53 N52 C501 -0.7(6) 6_565 . . . ? C54 C53 N52 C501 -177.8(7) . . . . ? C53 C53 N52 Co02 174.0(3) 6_565 . . . ? C54 C53 N52 Co02 -3.1(8) . . . . ? N12 Co02 N52 C501 -99.6(9) . . . . ? N35 Co02 N52 C501 -6.1(9) . . . . ? N59 Co02 N52 C501 171.9(9) . . . . ? N44 Co02 N52 C501 76.4(9) . . . . ? N17 Co02 N52 C501 -126(3) . . . . ? N12 Co02 N52 C53 88.3(5) . . . . ? N35 Co02 N52 C53 -178.2(5) . . . . ? N59 Co02 N52 C53 -0.3(5) . . . . ? N44 Co02 N52 C53 -95.8(6) . . . . ? N17 Co02 N52 C53 62(3) . . . . ? N59 C54 N55 C56 0.9(16) . . . . ? C53 C54 N55 C56 -178.8(10) . . . . ? C57 C56 N55 C54 -28.7(17) . . . . ? N55 C54 N59 C58 -0.5(14) . . . . ? C53 C54 N59 C58 179.2(7) . . . . ? N55 C54 N59 Co02 173.4(8) . . . . ? C53 C54 N59 Co02 -6.8(9) . . . . ? C57 C58 N59 C54 26.4(12) . . . . ? C57 C58 N59 Co02 -146.7(7) . . . . ? N52 Co02 N59 C54 4.1(6) . . . . ? N12 Co02 N59 C54 -88.7(6) . . . . ? N35 Co02 N59 C54 33(4) . . . . ? N44 Co02 N59 C54 93.7(6) . . . . ? N17 Co02 N59 C54 -170.2(6) . . . . ? N52 Co02 N59 C58 177.4(7) . . . . ? N12 Co02 N59 C58 84.6(7) . . . . ? N35 Co02 N59 C58 -154(4) . . . . ? N44 Co02 N59 C58 -93.0(7) . . . . ? N17 Co02 N59 C58 3.1(7) . . . . ? N5 C4 N91 C81 0(2) . . . . ? C3 C4 N91 C81 177.9(14) . . . . ? C71 C81 N91 C4 -4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.934 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.101 # Attachment '- Compound 1d.cif' data_1d _database_code_depnum_ccdc_archive 'CCDC 824167' #TrackingRef '- Compound 1d.cif' _publ_section_comment ; Disordered methylene carbon atom (C103-C104) and several disordered water solvent molecules are pres ; _symmetry_space_group_name_hall '-P 2yn' #Added by publCIF _audit_update_record ; 2010-04-04 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H156 Co8 N84 O58.50' _chemical_formula_weight 4326.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.155(5) _cell_length_b 19.422(5) _cell_length_c 22.792(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.221(2) _cell_angle_gamma 90.00 _cell_volume 8922(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedra _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4440 _exptl_absorpt_coefficient_mu 6.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5572 _exptl_absorpt_correction_T_max 0.5572 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59827 _diffrn_reflns_av_R_equivalents 0.1172 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 65.07 _reflns_number_total 14148 _reflns_number_gt 9068 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0982P)^2^+27.9401P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14148 _refine_ls_number_parameters 1277 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1293 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2213 _refine_ls_wR_factor_gt 0.1921 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.07075(5) 0.79175(5) 0.86557(4) 0.0179(3) Uani 1 1 d . . . Co2 Co 1.01140(5) 1.07637(5) 0.77950(4) 0.0183(3) Uani 1 1 d . . . Co3 Co 0.77569(5) 1.08651(5) 0.93569(5) 0.0188(3) Uani 1 1 d . . . Co4 Co 0.83331(5) 0.80431(5) 1.02184(4) 0.0171(3) Uani 1 1 d . . . C1 C 0.9007(3) 1.0584(3) 0.8674(3) 0.0183(15) Uani 1 1 d . . . H1 H 0.9084 1.0130 0.8784 0.022 Uiso 1 1 calc R . . C2 C 0.8592(3) 1.1620(3) 0.8646(3) 0.0171(14) Uani 1 1 d . . . C3 C 0.9102(3) 1.1579(3) 0.8236(3) 0.0198(15) Uani 1 1 d . . . C4 C 0.9423(3) 1.2002(3) 0.7793(3) 0.0200(15) Uani 1 1 d . . . C5 C 0.9499(4) 1.3034(4) 0.7195(3) 0.0335(19) Uani 1 1 d . . . H5A H 0.9430 1.3520 0.7271 0.040 Uiso 1 1 calc R . . H5B H 0.9310 1.2925 0.6814 0.040 Uiso 1 1 calc R . . C6 C 1.0218(4) 1.2877(4) 0.7197(4) 0.041(2) Uani 1 1 d . . . H6A H 1.0415 1.3040 0.7560 0.049 Uiso 1 1 calc R . . H6B H 1.0430 1.3118 0.6875 0.049 Uiso 1 1 calc R . . C7 C 1.0341(4) 1.2113(3) 0.7136(3) 0.0241(16) Uani 1 1 d . . . H7A H 1.0227 1.1969 0.6741 0.029 Uiso 1 1 calc R . . H7B H 1.0809 1.2020 0.7198 0.029 Uiso 1 1 calc R . . C8 C 0.8105(3) 1.2113(3) 0.8866(3) 0.0213(15) Uani 1 1 d . . . C9 C 0.7100(4) 1.2267(3) 0.9397(3) 0.0271(17) Uani 1 1 d . . . H9A H 0.7212 1.2382 0.9799 0.032 Uiso 1 1 calc R . . H9B H 0.6682 1.2019 0.9398 0.032 Uiso 1 1 calc R . . C10 C 0.7024(4) 1.2918(3) 0.9046(3) 0.0312(18) Uani 1 1 d . . . H10A H 0.6707 1.3219 0.9236 0.037 Uiso 1 1 calc R . . H10B H 0.6856 1.2808 0.8657 0.037 Uiso 1 1 calc R . . C11 C 0.7685(4) 1.3283(3) 0.8992(4) 0.0331(19) Uani 1 1 d . . . H11A H 0.7647 1.3660 0.8715 0.040 Uiso 1 1 calc R . . H11B H 0.7815 1.3470 0.9370 0.040 Uiso 1 1 calc R . . C12 C 1.0526(3) 0.9442(3) 0.8411(3) 0.0198(16) Uani 1 1 d . . . H12 H 1.0799 0.9621 0.8703 0.024 Uiso 1 1 calc R . . C13 C 0.9834(3) 0.9364(3) 0.7679(3) 0.0189(15) Uani 1 1 d . . . C14 C 0.9994(3) 0.8711(3) 0.7861(3) 0.0196(16) Uani 1 1 d . . . C15 C 0.9410(4) 0.9710(3) 0.7247(3) 0.0233(16) Uani 1 1 d . . . C16 C 0.9125(4) 1.0763(4) 0.6779(3) 0.0310(18) Uani 1 1 d . . . H16A H 0.9384 1.1142 0.6624 0.037 Uiso 1 1 calc R . . H16B H 0.8745 1.0954 0.6981 0.037 Uiso 1 1 calc R . . C17 C 0.8886(4) 1.0309(3) 0.6272(3) 0.0348(19) Uani 1 1 d . . . H17A H 0.8588 1.0570 0.6021 0.042 Uiso 1 1 calc R . . H17B H 0.9262 1.0165 0.6038 0.042 Uiso 1 1 calc R . . C18 C 0.8531(4) 0.9685(4) 0.6509(4) 0.042(2) Uani 1 1 d . . . H18A H 0.8108 0.9822 0.6675 0.050 Uiso 1 1 calc R . . H18B H 0.8445 0.9362 0.6193 0.050 Uiso 1 1 calc R . . C19 C 0.9884(4) 0.7995(3) 0.7682(3) 0.0259(17) Uani 1 1 d . . . C20 C 0.9446(5) 0.7132(4) 0.7002(4) 0.052(3) Uani 1 1 d . . . H20A H 0.9793 0.6979 0.6738 0.062 Uiso 1 1 calc R . . H20B H 0.9024 0.7095 0.6798 0.062 Uiso 1 1 calc R . . C21 C 0.9439(5) 0.6693(4) 0.7538(4) 0.050(2) Uani 1 1 d . . . H21A H 0.9422 0.6213 0.7423 0.060 Uiso 1 1 calc R . . H21B H 0.9043 0.6793 0.7763 0.060 Uiso 1 1 calc R . . C22 C 1.0043(4) 0.6808(3) 0.7923(3) 0.0301(18) Uani 1 1 d . . . H22A H 0.9983 0.6569 0.8292 0.036 Uiso 1 1 calc R . . H22B H 1.0430 0.6615 0.7732 0.036 Uiso 1 1 calc R . . C23 C 0.9471(3) 0.8241(3) 0.9363(3) 0.0195(15) Uani 1 1 d . . . H23 H 0.9344 0.8653 0.9189 0.023 Uiso 1 1 calc R . . C24 C 1.0009(3) 0.7299(3) 0.9556(3) 0.0193(15) Uani 1 1 d . . . C25 C 0.9498(3) 0.7357(3) 0.9950(3) 0.0193(15) Uani 1 1 d . . . C26 C 1.0528(4) 0.6812(3) 0.9408(3) 0.0234(16) Uani 1 1 d . . . C27 C 1.1497(4) 0.6581(4) 0.8842(3) 0.0311(18) Uani 1 1 d . . . H27A H 1.1876 0.6868 0.8749 0.037 Uiso 1 1 calc R . . H27B H 1.1385 0.6315 0.8495 0.037 Uiso 1 1 calc R . . C28 C 1.1678(5) 0.6098(5) 0.9337(5) 0.068(3) Uani 1 1 d . . . H28A H 1.2009 0.5773 0.9202 0.082 Uiso 1 1 calc R . . H28B H 1.1869 0.6360 0.9658 0.082 Uiso 1 1 calc R . . C29 C 1.1092(4) 0.5717(4) 0.9550(4) 0.048(3) Uani 1 1 d . . . H29A H 1.0931 0.5410 0.9246 0.058 Uiso 1 1 calc R . . H29B H 1.1213 0.5442 0.9889 0.058 Uiso 1 1 calc R . . C30 C 0.9197(4) 0.6969(3) 1.0432(3) 0.0235(17) Uani 1 1 d . . . C31 C 0.9229(4) 0.6089(4) 1.1194(3) 0.0302(18) Uani 1 1 d . . . H31A H 0.9336 0.6300 1.1568 0.036 Uiso 1 1 calc R . . H31B H 0.9395 0.5620 1.1197 0.036 Uiso 1 1 calc R . . C32 C 0.8492(4) 0.6088(3) 1.1101(3) 0.0311(19) Uani 1 1 d . . . H32A H 0.8277 0.5873 1.1434 0.037 Uiso 1 1 calc R . . H32B H 0.8384 0.5821 1.0753 0.037 Uiso 1 1 calc R . . C33 C 0.8235(4) 0.6816(3) 1.1028(3) 0.0312(19) Uani 1 1 d . . . H33A H 0.7765 0.6805 1.0934 0.037 Uiso 1 1 calc R . . H33B H 0.8292 0.7067 1.1392 0.037 Uiso 1 1 calc R . . C34 C 0.8218(3) 0.9553(3) 0.9930(3) 0.0200(15) Uani 1 1 d . . . H34 H 0.8451 0.9738 1.0246 0.024 Uiso 1 1 calc R . . C35 C 0.7647(3) 0.9468(3) 0.9116(3) 0.0193(15) Uani 1 1 d . . . C36 C 0.7749(3) 0.8814(3) 0.9336(3) 0.0168(15) Uani 1 1 d . . . C37 C 0.7352(4) 0.9817(3) 0.8608(3) 0.0226(16) Uani 1 1 d . . . C38 C 0.7017(4) 1.0891(3) 0.8199(3) 0.0291(18) Uani 1 1 d . . . H38A H 0.7202 1.1352 0.8204 0.035 Uiso 1 1 calc R . . H38B H 0.6541 1.0929 0.8256 0.035 Uiso 1 1 calc R . . C39 C 0.7153(4) 1.0557(4) 0.7606(3) 0.0330(19) Uani 1 1 d . . . H39A H 0.6932 1.0814 0.7297 0.040 Uiso 1 1 calc R . . H39B H 0.7626 1.0559 0.7528 0.040 Uiso 1 1 calc R . . C40 C 0.6899(4) 0.9823(4) 0.7614(3) 0.0299(18) Uani 1 1 d . . . H40A H 0.6418 0.9823 0.7622 0.036 Uiso 1 1 calc R . . H40B H 0.7041 0.9585 0.7262 0.036 Uiso 1 1 calc R . . C41 C 0.7575(3) 0.8101(3) 0.9204(3) 0.0211(16) Uani 1 1 d . . . C42 C 0.6963(4) 0.7221(3) 0.8678(3) 0.0312(18) Uani 1 1 d . . . H42A H 0.6826 0.7152 0.8273 0.037 Uiso 1 1 calc R . . H42B H 0.6598 0.7090 0.8930 0.037 Uiso 1 1 calc R . . C43 C 0.7559(4) 0.6787(3) 0.8812(3) 0.0288(18) Uani 1 1 d . . . H43A H 0.7910 0.6893 0.8536 0.035 Uiso 1 1 calc R . . H43B H 0.7446 0.6304 0.8767 0.035 Uiso 1 1 calc R . . C44 C 0.7804(4) 0.6916(3) 0.9433(3) 0.0271(17) Uani 1 1 d . . . H44A H 0.7492 0.6720 0.9709 0.033 Uiso 1 1 calc R . . H44B H 0.8228 0.6688 0.9489 0.033 Uiso 1 1 calc R . . C45 C 0.7752(3) 1.1207(3) 1.0535(3) 0.0217(16) Uani 1 1 d . . . C46 C 0.7094(4) 1.0951(3) 1.0413(3) 0.0268(17) Uani 1 1 d . . . C47 C 0.7579(3) 0.8503(3) 1.1157(3) 0.0205(16) Uani 1 1 d . . . C48 C 0.5975(5) 1.0602(7) 1.0728(4) 0.072(4) Uani 1 1 d . . . C50 C 0.6329(4) 1.0530(4) 0.9687(4) 0.040(2) Uani 1 1 d . . . C51 C 0.6372(4) 0.8573(4) 1.1313(4) 0.037(2) Uani 1 1 d . . . H51A H 0.6196 0.8958 1.1089 0.045 Uiso 1 1 calc R . . H51B H 0.6099 0.8513 1.1658 0.045 Uiso 1 1 calc R . . C52 C 0.6356(4) 0.7927(5) 1.0944(4) 0.049(2) Uani 1 1 d . . . H52A H 0.6446 0.7531 1.1192 0.058 Uiso 1 1 calc R . . H52B H 0.5916 0.7870 1.0776 0.058 Uiso 1 1 calc R . . C53 C 0.6855(4) 0.7955(4) 1.0463(3) 0.0305(18) Uani 1 1 d . . . H53A H 0.6871 0.7511 1.0268 0.037 Uiso 1 1 calc R . . H53B H 0.6716 0.8295 1.0176 0.037 Uiso 1 1 calc R . . C54 C 1.0695(3) 1.1342(3) 0.8914(3) 0.0194(16) Uani 1 1 d . . . H54 H 1.0305 1.1408 0.9123 0.023 Uiso 1 1 calc R . . C55 C 1.1240(3) 0.8572(3) 0.9762(3) 0.0177(15) Uani 1 1 d . . . H55 H 1.0863 0.8548 0.9996 0.021 Uiso 1 1 calc R . . C56 C 1.1377(3) 1.1061(3) 0.8218(3) 0.0192(16) Uani 1 1 d . . . C57 C 1.1743(3) 1.1329(3) 0.8681(3) 0.0211(16) Uani 1 1 d . . . C58 C 1.1903(3) 0.8474(3) 0.9021(3) 0.0215(16) Uani 1 1 d . . . C59 C 1.2024(4) 0.8212(4) 0.8429(3) 0.0298(18) Uani 1 1 d . . . C60 C 1.1567(4) 0.7695(4) 0.7569(3) 0.0284(17) Uani 1 1 d . . . H60A H 1.1187 0.7846 0.7340 0.034 Uiso 1 1 calc R . . H60B H 1.1570 0.7196 0.7570 0.034 Uiso 1 1 calc R . . C61 C 1.2188(5) 0.7954(6) 0.7290(4) 0.060(3) Uani 1 1 d . . . H61A H 1.2264 0.7685 0.6938 0.072 Uiso 1 1 calc R . . H61B H 1.2111 0.8426 0.7167 0.072 Uiso 1 1 calc R . . C62 C 1.2775(5) 0.7940(6) 0.7629(4) 0.073(4) Uani 1 1 d . . . H62A H 1.3116 0.8211 0.7438 0.087 Uiso 1 1 calc R . . H62B H 1.2934 0.7470 0.7664 0.087 Uiso 1 1 calc R . . C63 C 1.1467(4) 1.0832(4) 0.7612(3) 0.0274(18) Uani 1 1 d . . . C64 C 1.0944(4) 1.0414(4) 0.6737(3) 0.0308(18) Uani 1 1 d . . . H64A H 1.0641 1.0029 0.6696 0.037 Uiso 1 1 calc R . . H64B H 1.0802 1.0773 0.6470 0.037 Uiso 1 1 calc R . . C65 C 1.1619(5) 1.0191(8) 0.6580(5) 0.097(5) Uani 1 1 d . . . H65A H 1.1675 0.9725 0.6726 0.116 Uiso 1 1 calc R . . H65B H 1.1638 1.0166 0.6156 0.116 Uiso 1 1 calc R . . C66 C 1.2153(5) 1.0562(8) 0.6763(4) 0.091(5) Uani 1 1 d . . . H66A H 1.2219 1.0946 0.6498 0.109 Uiso 1 1 calc R . . H66B H 1.2545 1.0273 0.6747 0.109 Uiso 1 1 calc R . . C103 C 0.5796(8) 1.0829(14) 1.0111(9) 0.042(8) Uani 0.48(4) 1 d P . . C104 C 0.5970(11) 1.0241(19) 1.0225(8) 0.073(13) Uani 0.52(4) 1 d P . . H300 H 1.000(5) 0.646(5) 1.069(5) 0.087 Uiso 1 1 d . . . H301 H 0.742(5) 0.906(5) 0.805(4) 0.087 Uiso 1 1 d . . . H302 H 0.847(5) 1.293(6) 0.864(5) 0.087 Uiso 1 1 d . . . H303 H 1.020(5) 0.603(6) 0.976(5) 0.087 Uiso 1 1 d . . . H304 H 0.685(6) 1.082(6) 1.114(5) 0.087 Uiso 1 1 d . . . H305 H 0.712(5) 0.908(5) 1.169(5) 0.087 Uiso 1 1 d . . . N1 N 0.9155(3) 0.7950(2) 0.9815(2) 0.0169(12) Uani 1 1 d . . . N2 N 0.9986(3) 0.7868(2) 0.9195(2) 0.0184(13) Uani 1 1 d . . . N3 N 1.0927(3) 0.7024(3) 0.9003(2) 0.0220(13) Uani 1 1 d . . . N4 N 1.0572(3) 0.6206(3) 0.9709(3) 0.0335(17) Uani 1 1 d . . . N5 N 0.9541(3) 0.6478(3) 1.0716(2) 0.0249(14) Uani 1 1 d . . . N6 N 0.8597(3) 0.7168(2) 1.0556(2) 0.0192(13) Uani 1 1 d . . . N7 N 0.7520(3) 0.8132(3) 1.0680(2) 0.0201(13) Uani 1 1 d . . . N8 N 0.6655(4) 1.0846(5) 1.0842(3) 0.058(3) Uani 1 1 d . . . N9 N 0.6987(3) 1.0809(3) 0.9864(3) 0.0227(13) Uani 1 1 d . . . N10 N 0.7064(3) 0.8718(3) 1.1489(3) 0.0311(16) Uani 1 1 d . . . N11 N 0.8174(3) 1.1161(2) 1.0063(2) 0.0169(12) Uani 1 1 d . . . N12 N 0.8118(3) 0.8879(3) 0.9842(2) 0.0198(13) Uani 1 1 d . . . N13 N 0.7937(3) 0.9922(2) 0.9504(2) 0.0175(12) Uani 1 1 d . . . N14 N 0.7307(3) 1.0488(3) 0.8675(2) 0.0199(13) Uani 1 1 d . . . N15 N 0.7160(3) 0.9469(3) 0.8135(2) 0.0246(14) Uani 1 1 d . . . N16 N 0.7139(3) 0.7954(3) 0.8776(3) 0.0263(14) Uani 1 1 d . . . N17 N 0.7880(3) 0.7652(3) 0.9551(2) 0.0212(13) Uani 1 1 d . . . N18 N 1.0157(3) 0.7543(3) 0.8037(2) 0.0198(13) Uani 1 1 d . . . N19 N 0.9565(3) 0.7856(3) 0.7176(3) 0.0386(17) Uani 1 1 d . . . N20 N 0.8942(3) 0.9354(3) 0.6963(3) 0.0357(16) Uani 1 1 d . . . N21 N 0.9535(3) 1.0368(3) 0.7199(2) 0.0226(13) Uani 1 1 d . . . N22 N 0.9356(3) 1.0927(2) 0.8272(2) 0.0179(12) Uani 1 1 d . . . N23 N 0.8531(3) 1.0984(2) 0.8895(2) 0.0185(13) Uani 1 1 d . . . N24 N 0.7620(3) 1.1826(3) 0.9149(2) 0.0207(13) Uani 1 1 d . . . N25 N 0.8183(3) 1.2790(3) 0.8789(3) 0.0251(15) Uani 1 1 d . . . N26 N 0.9951(3) 1.1716(3) 0.7557(2) 0.0209(13) Uani 1 1 d . . . N27 N 0.9174(3) 1.2620(3) 0.7654(2) 0.0282(15) Uani 1 1 d . . . N28 N 1.0720(3) 1.1076(2) 0.8376(2) 0.0172(12) Uani 1 1 d . . . N29 N 1.1297(3) 1.1501(2) 0.9116(2) 0.0174(12) Uani 1 1 d . . . N30 N 1.0916(3) 1.0675(3) 0.7345(2) 0.0203(13) Uani 1 1 d . . . N31 N 1.2077(3) 1.0831(4) 0.7371(3) 0.051(2) Uani 1 1 d . . . N32 N 1.1270(3) 0.8348(3) 0.9215(2) 0.0201(13) Uani 1 1 d . . . N33 N 1.1503(3) 0.7950(3) 0.8178(2) 0.0213(13) Uani 1 1 d . . . N34 N 1.2644(4) 0.8223(4) 0.8218(3) 0.059(2) Uani 1 1 d . . . N35 N 1.0185(3) 0.9817(3) 0.8032(2) 0.0194(13) Uani 1 1 d . . . N36 N 1.0424(3) 0.8770(3) 0.8320(2) 0.0192(13) Uani 1 1 d . . . N101 N 0.7640(4) 0.7961(3) 0.7478(3) 0.0405(18) Uani 1 1 d . . . N102 N 0.3610(5) 0.7248(4) 0.9152(4) 0.059(2) Uani 1 1 d . . . N103 N 0.3514(4) 0.9914(4) 0.7690(3) 0.049(2) Uani 1 1 d . . . N104 N 0.4118(5) 0.9556(4) 0.4138(4) 0.068(3) Uani 1 1 d . . . N105 N 0.0000 0.0000 1.0000 0.027(2) Uani 1 2 d S . . N106 N 0.4770(7) 0.3757(9) 0.8888(9) 0.149(7) Uiso 0.75 1 d PD . . N107 N 0.0784(7) 0.6326(8) 0.4371(6) 0.116(5) Uiso 0.75 1 d PD . . O103 O 0.8131(3) 0.8329(3) 0.7593(3) 0.065(2) Uani 1 1 d . . . O104 O 0.7688(3) 0.7329(3) 0.7395(2) 0.0553(18) Uani 1 1 d . . . O105 O 0.7075(3) 0.8237(3) 0.7467(2) 0.0386(14) Uani 1 1 d . . . O106 O 0.3777(5) 0.7770(4) 0.8916(4) 0.101(3) Uani 1 1 d . . . O107 O 0.3054(4) 0.7030(4) 0.9224(4) 0.087(3) Uani 1 1 d . . . O108 O 0.4059(6) 0.6908(7) 0.9372(7) 0.176(6) Uani 1 1 d . . . O109 O 0.3852(3) 0.9390(3) 0.7623(3) 0.0631(19) Uani 1 1 d . . . O110 O 0.3029(3) 0.9893(3) 0.8048(2) 0.0471(15) Uani 1 1 d . . . O111 O 0.3635(3) 1.0467(3) 0.7433(3) 0.0607(18) Uani 1 1 d . . . O112 O 0.4149(4) 0.9257(3) 0.4590(3) 0.0616(19) Uani 1 1 d . . . O113 O 0.4611(6) 0.9512(4) 0.3781(4) 0.105(3) Uani 1 1 d . . . O114 O 0.3586(4) 0.9918(4) 0.3996(4) 0.085(2) Uani 1 1 d . . . O115 O 0.0163(10) -0.0175(10) 0.9503(7) 0.087(6) Uani 0.50 1 d P . . O116 O 0.0130(12) 0.0407(12) 0.9624(8) 0.113(7) Uani 0.50 1 d P . . O117 O 0.0025(10) 0.0583(7) 1.0114(12) 0.106(7) Uani 0.50 1 d P . . O200 O 0.5305(5) 0.3473(5) 0.8962(4) 0.074(3) Uiso 0.75 1 d PD . . O201 O 0.4595(18) 0.4178(17) 0.9251(14) 0.42(2) Uiso 0.75 1 d PD . . O202 O 0.4281(11) 0.3664(12) 0.8586(9) 0.229(10) Uiso 0.75 1 d PD . . O205 O 0.0592(10) 0.5917(10) 0.4746(8) 0.212(9) Uiso 0.75 1 d PD . . O206 O 0.0632(9) 0.6945(8) 0.4422(8) 0.167(7) Uiso 0.75 1 d PD . . O207 O 0.1059(3) 0.6086(3) 0.3979(3) 0.0287(15) Uiso 0.75 1 d PD . . O501 O 0.0145(12) 0.7125(11) 0.4382(10) 0.039(5) Uiso 0.25 1 d P . . O503 O 0.4994(9) 0.8856(9) 0.0825(8) 0.108(6) Uiso 0.50 1 d P . . O504 O 0.4422(6) 0.3399(6) 0.0475(5) 0.140(4) Uiso 1 1 d . . . O505 O 0.0837(3) 0.6148(3) 0.1366(2) 0.0460(15) Uiso 1 1 d . . . O506 O 0.5411(13) 0.2197(13) 0.9510(12) 0.152(10) Uiso 0.50 1 d P . . O507 O 0.6625(6) 0.4185(5) 1.0009(5) 0.085(3) Uiso 0.75 1 d P . . O508 O 0.6100(16) 0.4250(15) 0.9908(13) 0.073(8) Uiso 0.25 1 d P . . O509 O 0.5299(8) 0.4367(8) 0.9996(7) 0.083(5) Uiso 0.50 1 d P . . O512 O 0.5000 0.5000 1.0000 0.51(5) Uiso 0.60 2 d SP . . O514 O 0.5160(3) 0.9719(3) 0.7264(3) 0.0515(16) Uiso 1 1 d . . . O515 O 0.5516(13) 0.9837(14) 0.8504(11) 0.050(7) Uiso 0.25 1 d P . . O516 O 0.5365(4) 1.0162(5) 0.8494(4) 0.088(3) Uiso 1 1 d . . . O517 O 0.3937(17) 0.9155(17) 0.3632(15) 0.061(9) Uiso 0.20 1 d P . . O518 O 0.467(2) 1.002(3) 0.444(2) 0.117(16) Uiso 0.20 1 d P . . O519 O 0.3030(19) 1.0100(18) 0.3982(15) 0.091(10) Uiso 0.25 1 d P . . O520 O 0.250(2) 0.992(2) 0.454(2) 0.083(13) Uiso 0.20 1 d P . . O521 O 0.2461(5) 0.9813(5) 0.4882(5) 0.115(4) Uiso 1 1 d . . . O522 O 0.3691(15) 0.3798(14) 0.8983(13) 0.178(10) Uiso 0.50 1 d P . . O528 O 0.3384(9) 0.3792(8) 0.9575(8) 0.061(4) Uiso 0.50 1 d P . . O524 O 0.3040(14) 0.3996(14) 0.9361(12) 0.152(10) Uiso 0.50 1 d P . . O526 O 0.3637(12) 0.3735(12) 0.9850(11) 0.126(9) Uiso 0.50 1 d P . . O527 O 0.550(3) 0.253(3) 0.950(2) 0.024(11) Uiso 0.10 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0216(6) 0.0159(5) 0.0162(6) -0.0004(4) 0.0038(5) 0.0023(5) Co2 0.0242(6) 0.0166(5) 0.0141(5) 0.0005(4) 0.0025(5) 0.0006(5) Co3 0.0214(6) 0.0166(5) 0.0184(6) -0.0002(4) 0.0022(5) 0.0005(5) Co4 0.0203(6) 0.0157(5) 0.0155(6) 0.0001(4) 0.0024(5) 0.0001(5) C1 0.023(4) 0.016(3) 0.016(4) 0.001(3) 0.001(3) 0.002(3) C2 0.020(4) 0.016(3) 0.015(3) 0.001(3) -0.007(3) -0.002(3) C3 0.024(4) 0.021(3) 0.014(3) -0.001(3) -0.005(3) -0.001(3) C4 0.024(4) 0.022(3) 0.014(3) -0.001(3) -0.004(3) -0.004(3) C5 0.036(5) 0.030(4) 0.035(5) 0.016(3) 0.002(4) -0.001(4) C6 0.047(5) 0.035(4) 0.040(5) 0.011(4) 0.011(4) -0.005(4) C7 0.031(4) 0.022(3) 0.019(4) 0.007(3) 0.004(3) -0.005(3) C8 0.021(4) 0.025(3) 0.018(4) 0.000(3) -0.003(3) 0.002(3) C9 0.029(4) 0.023(3) 0.029(4) 0.001(3) 0.009(4) 0.006(3) C10 0.030(4) 0.025(4) 0.039(5) 0.002(3) 0.006(4) 0.002(3) C11 0.039(5) 0.020(3) 0.041(5) 0.003(3) 0.007(4) 0.009(3) C12 0.025(4) 0.022(3) 0.013(3) 0.001(3) 0.005(3) 0.003(3) C13 0.016(4) 0.025(3) 0.017(4) 0.002(3) 0.004(3) 0.003(3) C14 0.028(4) 0.016(3) 0.015(4) -0.001(3) -0.002(3) -0.001(3) C15 0.023(4) 0.023(3) 0.023(4) 0.002(3) -0.001(3) 0.003(3) C16 0.038(5) 0.030(4) 0.026(4) -0.001(3) -0.006(4) -0.003(4) C17 0.046(5) 0.025(4) 0.033(4) 0.003(3) -0.014(4) -0.002(4) C18 0.053(6) 0.029(4) 0.043(5) 0.000(4) -0.020(5) 0.000(4) C19 0.029(4) 0.019(3) 0.030(4) -0.002(3) -0.004(4) -0.002(3) C20 0.074(7) 0.029(4) 0.052(6) -0.011(4) -0.028(6) -0.003(5) C21 0.063(6) 0.023(4) 0.063(6) 0.001(4) -0.031(6) -0.013(4) C22 0.029(4) 0.024(3) 0.038(5) -0.006(3) -0.004(4) -0.003(3) C23 0.022(4) 0.018(3) 0.019(4) -0.001(3) 0.004(3) 0.007(3) C24 0.025(4) 0.012(3) 0.021(4) 0.001(3) 0.003(3) -0.002(3) C25 0.022(4) 0.019(3) 0.016(3) 0.005(3) 0.001(3) -0.001(3) C26 0.026(4) 0.022(3) 0.022(4) 0.001(3) -0.001(3) 0.000(3) C27 0.030(4) 0.030(4) 0.033(4) 0.000(3) 0.013(4) 0.007(3) C28 0.071(7) 0.062(6) 0.073(7) 0.018(5) 0.034(6) 0.033(6) C29 0.059(6) 0.030(4) 0.055(6) 0.014(4) 0.028(5) 0.015(4) C30 0.038(5) 0.018(3) 0.015(3) 0.001(3) 0.005(4) 0.004(3) C31 0.042(5) 0.028(4) 0.022(4) 0.010(3) 0.004(4) 0.001(4) C32 0.036(5) 0.025(4) 0.032(4) 0.013(3) 0.011(4) 0.000(3) C33 0.037(5) 0.028(4) 0.028(4) 0.005(3) 0.014(4) 0.002(4) C34 0.023(4) 0.021(3) 0.016(3) -0.001(3) -0.006(3) -0.002(3) C35 0.019(4) 0.015(3) 0.023(4) 0.001(3) 0.002(3) 0.000(3) C36 0.015(3) 0.020(3) 0.016(4) 0.000(3) 0.001(3) 0.002(3) C37 0.025(4) 0.025(3) 0.018(4) 0.001(3) -0.004(3) -0.007(3) C38 0.043(5) 0.021(3) 0.023(4) 0.000(3) -0.006(4) 0.003(3) C39 0.041(5) 0.032(4) 0.026(4) 0.002(3) 0.001(4) 0.003(4) C40 0.034(5) 0.032(4) 0.023(4) -0.003(3) -0.007(4) 0.004(4) C41 0.018(4) 0.022(3) 0.023(4) -0.002(3) 0.006(3) -0.003(3) C42 0.036(5) 0.022(3) 0.035(4) -0.002(3) -0.007(4) -0.006(3) C43 0.043(5) 0.015(3) 0.028(4) -0.004(3) -0.002(4) 0.000(3) C44 0.033(4) 0.018(3) 0.031(4) -0.003(3) 0.000(4) 0.002(3) C45 0.025(4) 0.022(3) 0.019(4) 0.000(3) 0.002(3) 0.001(3) C46 0.028(4) 0.028(4) 0.024(4) 0.002(3) 0.005(4) 0.002(3) C47 0.020(4) 0.021(3) 0.021(4) 0.003(3) 0.002(3) -0.005(3) C48 0.030(5) 0.145(11) 0.042(6) -0.029(7) 0.006(5) -0.041(6) C50 0.019(4) 0.062(5) 0.040(5) -0.018(4) 0.000(4) -0.014(4) C51 0.028(4) 0.045(5) 0.039(5) 0.002(4) 0.008(4) 0.005(4) C52 0.035(5) 0.058(5) 0.053(6) -0.003(5) 0.005(5) -0.009(4) C53 0.023(4) 0.031(4) 0.038(5) 0.002(3) 0.006(4) -0.005(3) C54 0.021(4) 0.018(3) 0.020(4) -0.002(3) 0.007(3) -0.005(3) C55 0.021(4) 0.020(3) 0.013(3) 0.003(3) 0.006(3) -0.002(3) C56 0.023(4) 0.016(3) 0.019(4) 0.003(3) 0.005(3) 0.001(3) C57 0.025(4) 0.021(3) 0.017(4) 0.000(3) 0.002(3) -0.002(3) C58 0.024(4) 0.023(3) 0.018(4) 0.005(3) 0.005(3) 0.004(3) C59 0.034(5) 0.037(4) 0.018(4) -0.004(3) 0.004(4) 0.000(4) C60 0.029(4) 0.032(4) 0.024(4) -0.007(3) 0.003(4) 0.002(3) C61 0.044(6) 0.104(8) 0.034(5) -0.028(5) 0.018(5) -0.027(6) C62 0.047(6) 0.124(9) 0.048(6) -0.046(6) 0.030(5) -0.032(6) C63 0.029(4) 0.031(4) 0.022(4) 0.004(3) 0.009(4) -0.003(3) C64 0.043(5) 0.034(4) 0.016(4) -0.008(3) 0.004(4) -0.004(4) C65 0.053(7) 0.179(14) 0.059(7) -0.075(8) 0.020(6) -0.009(8) C66 0.046(7) 0.188(14) 0.038(6) -0.048(7) 0.012(5) -0.007(8) C103 0.009(9) 0.061(17) 0.056(14) -0.007(11) 0.003(9) -0.007(9) C104 0.044(14) 0.14(3) 0.036(12) 0.002(13) 0.000(10) -0.053(17) N1 0.021(3) 0.018(3) 0.012(3) -0.003(2) -0.003(3) -0.002(2) N2 0.022(3) 0.016(2) 0.016(3) 0.001(2) 0.006(3) -0.001(2) N3 0.027(3) 0.022(3) 0.017(3) 0.000(2) 0.006(3) 0.003(3) N4 0.040(4) 0.024(3) 0.037(4) 0.011(3) 0.013(4) 0.010(3) N5 0.030(4) 0.024(3) 0.021(3) 0.011(2) 0.003(3) 0.007(3) N6 0.026(3) 0.016(3) 0.015(3) 0.003(2) 0.004(3) -0.001(2) N7 0.019(3) 0.023(3) 0.018(3) -0.001(2) 0.001(3) -0.004(2) N8 0.035(5) 0.105(7) 0.034(4) -0.023(5) 0.015(4) -0.031(5) N9 0.018(3) 0.022(3) 0.029(3) -0.003(2) -0.001(3) -0.003(2) N10 0.029(4) 0.034(3) 0.031(4) -0.008(3) 0.005(3) -0.001(3) N11 0.021(3) 0.018(3) 0.012(3) 0.000(2) -0.002(3) -0.003(2) N12 0.021(3) 0.020(3) 0.019(3) -0.001(2) 0.003(3) 0.000(2) N13 0.020(3) 0.016(3) 0.016(3) 0.003(2) -0.002(3) 0.001(2) N14 0.023(3) 0.018(3) 0.019(3) 0.001(2) -0.001(3) 0.005(2) N15 0.033(4) 0.023(3) 0.017(3) 0.000(2) -0.006(3) 0.009(3) N16 0.031(4) 0.023(3) 0.025(3) -0.003(3) -0.004(3) -0.009(3) N17 0.027(3) 0.013(3) 0.024(3) -0.001(2) 0.001(3) 0.001(2) N18 0.022(3) 0.019(3) 0.019(3) -0.003(2) 0.003(3) 0.000(2) N19 0.045(4) 0.024(3) 0.047(4) -0.008(3) -0.026(4) 0.000(3) N20 0.038(4) 0.026(3) 0.043(4) 0.000(3) -0.023(4) -0.006(3) N21 0.025(3) 0.021(3) 0.022(3) 0.002(2) -0.002(3) 0.006(3) N22 0.021(3) 0.018(3) 0.015(3) 0.002(2) -0.005(3) -0.001(2) N23 0.028(3) 0.015(2) 0.013(3) -0.003(2) 0.002(3) -0.003(2) N24 0.023(3) 0.023(3) 0.017(3) 0.001(2) 0.000(3) 0.006(3) N25 0.028(4) 0.022(3) 0.026(3) 0.000(2) 0.002(3) -0.003(3) N26 0.027(3) 0.022(3) 0.013(3) 0.002(2) 0.001(3) -0.003(3) N27 0.038(4) 0.022(3) 0.025(3) 0.011(3) 0.003(3) 0.002(3) N28 0.024(3) 0.012(2) 0.015(3) 0.002(2) 0.003(3) -0.002(2) N29 0.020(3) 0.016(3) 0.016(3) -0.002(2) 0.002(3) -0.001(2) N30 0.026(3) 0.025(3) 0.011(3) -0.002(2) 0.003(3) -0.001(3) N31 0.035(4) 0.090(6) 0.026(4) -0.018(4) 0.011(3) -0.007(4) N32 0.022(3) 0.019(3) 0.020(3) 0.005(2) 0.003(3) 0.005(2) N33 0.026(3) 0.022(3) 0.016(3) -0.003(2) 0.006(3) -0.002(3) N34 0.039(4) 0.101(6) 0.036(4) -0.032(4) 0.019(4) -0.025(4) N35 0.022(3) 0.018(3) 0.019(3) -0.001(2) 0.003(3) -0.002(3) N36 0.023(3) 0.018(3) 0.016(3) 0.000(2) 0.005(3) -0.002(2) N101 0.054(5) 0.035(4) 0.033(4) -0.011(3) 0.010(4) -0.001(4) N102 0.080(7) 0.046(5) 0.053(5) 0.018(4) 0.021(5) 0.019(5) N103 0.066(6) 0.046(4) 0.035(4) -0.004(3) 0.005(4) 0.009(4) N104 0.083(7) 0.057(5) 0.063(6) 0.010(5) 0.006(6) -0.014(5) N105 0.040(6) 0.019(5) 0.023(5) 0.002(4) 0.008(4) 0.005(4) O103 0.046(4) 0.068(4) 0.081(5) -0.010(4) 0.015(4) -0.025(4) O104 0.091(5) 0.033(3) 0.042(3) -0.007(3) 0.010(4) 0.014(3) O105 0.045(4) 0.033(3) 0.038(3) -0.013(2) -0.004(3) 0.000(3) O106 0.120(8) 0.073(5) 0.110(7) 0.023(5) 0.032(6) 0.009(5) O107 0.066(5) 0.098(6) 0.096(6) -0.025(5) 0.015(5) -0.017(5) O108 0.109(9) 0.189(13) 0.229(15) 0.097(11) -0.026(9) 0.009(9) O109 0.066(5) 0.047(4) 0.076(5) -0.020(3) 0.020(4) 0.009(3) O110 0.058(4) 0.045(3) 0.039(3) 0.001(3) 0.017(3) 0.006(3) O111 0.068(5) 0.056(4) 0.058(4) 0.023(3) 0.009(4) 0.001(4) O112 0.078(5) 0.047(4) 0.060(4) 0.021(3) 0.002(4) -0.003(3) O113 0.174(10) 0.065(5) 0.076(6) -0.007(4) 0.034(6) 0.030(6) O114 0.065(5) 0.084(5) 0.105(7) 0.019(5) 0.001(5) 0.024(5) O115 0.142(16) 0.067(11) 0.051(10) -0.014(9) 0.033(10) 0.026(11) O116 0.19(2) 0.109(17) 0.042(10) 0.038(11) 0.030(12) -0.032(15) O117 0.147(18) 0.036(9) 0.135(19) -0.016(11) 0.053(15) -0.002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N32 1.896(6) . ? Co1 N36 1.910(5) . ? Co1 N2 1.909(5) . ? Co1 N18 1.933(6) . ? Co1 N33 1.942(5) . ? Co1 N3 1.956(5) . ? Co2 N28 1.896(6) . ? Co2 N22 1.905(5) . ? Co2 N35 1.921(5) . ? Co2 N30 1.926(5) . ? Co2 N21 1.945(6) . ? Co2 N26 1.954(5) . ? Co3 N13 1.897(5) . ? Co3 N23 1.899(5) . ? Co3 N11 1.902(5) . ? Co3 N9 1.942(5) . ? Co3 N14 1.941(6) . ? Co3 N24 1.945(5) . ? Co4 N12 1.886(5) . ? Co4 N1 1.906(5) . ? Co4 N29 1.906(5) 3_777 ? Co4 N17 1.927(6) . ? Co4 N6 1.939(5) . ? Co4 N7 1.958(5) . ? C1 N22 1.336(8) . ? C1 N23 1.335(8) . ? C2 N23 1.365(8) . ? C2 C3 1.394(9) . ? C2 C8 1.460(9) . ? C3 N22 1.368(8) . ? C3 C4 1.456(9) . ? C4 N26 1.319(8) . ? C4 N27 1.338(8) . ? C5 N27 1.475(8) . ? C5 C6 1.480(11) . ? C6 C7 1.511(9) . ? C7 N26 1.463(8) . ? C8 N24 1.299(8) . ? C8 N25 1.336(8) . ? C9 N24 1.469(8) . ? C9 C10 1.503(9) . ? C10 C11 1.513(10) . ? C11 N25 1.464(9) . ? C12 N35 1.323(8) . ? C12 N36 1.337(8) . ? C13 C14 1.373(9) . ? C13 N35 1.384(8) . ? C13 C15 1.465(10) . ? C14 N36 1.361(9) . ? C14 C19 1.466(9) . ? C15 N21 1.307(8) . ? C15 N20 1.335(9) . ? C16 N21 1.477(9) . ? C16 C17 1.530(10) . ? C17 C18 1.509(10) . ? C18 N20 1.472(10) . ? C19 N18 1.314(9) . ? C19 N19 1.346(10) . ? C20 N19 1.481(9) . ? C20 C21 1.491(12) . ? C21 C22 1.513(11) . ? C22 N18 1.468(8) . ? C23 N2 1.325(8) . ? C23 N1 1.337(8) . ? C24 C25 1.372(9) . ? C24 N2 1.379(8) . ? C24 C26 1.451(9) . ? C25 N1 1.379(8) . ? C25 C30 1.466(8) . ? C26 N3 1.295(8) . ? C26 N4 1.365(8) . ? C27 N3 1.483(8) . ? C27 C28 1.511(12) . ? C28 C29 1.478(12) . ? C29 N4 1.461(9) . ? C30 N6 1.302(9) . ? C30 N5 1.344(9) . ? C31 N5 1.467(8) . ? C31 C32 1.501(10) . ? C32 C33 1.515(9) . ? C33 N6 1.470(8) . ? C34 N13 1.331(8) . ? C34 N12 1.341(8) . ? C35 N13 1.378(8) . ? C35 C36 1.379(8) . ? C35 C37 1.467(10) . ? C36 N12 1.375(8) . ? C36 C41 1.460(9) . ? C37 N14 1.315(8) . ? C37 N15 1.329(9) . ? C38 N14 1.459(9) . ? C38 C39 1.525(9) . ? C39 C40 1.513(10) . ? C40 N15 1.468(9) . ? C41 N17 1.328(9) . ? C41 N16 1.341(9) . ? C42 N16 1.485(8) . ? C42 C43 1.499(10) . ? C43 C44 1.518(10) . ? C44 N17 1.462(8) . ? C45 C58 1.373(10) 3_777 ? C45 N11 1.376(8) . ? C45 C46 1.444(10) . ? C46 N9 1.297(9) . ? C46 N8 1.337(9) . ? C47 N7 1.310(8) . ? C47 N10 1.354(8) . ? C47 C57 1.450(9) 3_777 ? C48 C104 1.34(2) . ? C48 N8 1.474(11) . ? C48 C103 1.52(3) . ? C50 N9 1.486(9) . ? C50 C104 1.53(2) . ? C50 C103 1.558(19) . ? C51 N10 1.477(10) . ? C51 C52 1.511(11) . ? C52 C53 1.492(10) . ? C53 N7 1.468(9) . ? C54 N28 1.332(8) . ? C54 N29 1.332(8) . ? C55 N32 1.322(8) . ? C55 N11 1.350(8) 3_777 ? C56 N28 1.375(8) . ? C56 C57 1.386(10) . ? C56 C63 1.465(9) . ? C57 N29 1.381(8) . ? C57 C47 1.450(9) 3_777 ? C58 C45 1.373(10) 3_777 ? C58 N32 1.373(8) . ? C58 C59 1.463(9) . ? C59 N33 1.298(9) . ? C59 N34 1.343(9) . ? C60 N33 1.481(8) . ? C60 C61 1.492(10) . ? C61 C62 1.413(13) . ? C62 N34 1.474(10) . ? C63 N30 1.300(9) . ? C63 N31 1.349(9) . ? C64 C65 1.472(12) . ? C64 N30 1.475(8) . ? C65 C66 1.360(14) . ? C66 N31 1.488(11) . ? C103 C104 1.22(3) . ? N11 C55 1.350(8) 3_777 ? N29 Co4 1.906(5) 3_777 ? N101 O104 1.246(8) . ? N101 O103 1.248(9) . ? N101 O105 1.258(8) . ? N102 O106 1.198(10) . ? N102 O107 1.209(10) . ? N102 O108 1.228(12) . ? N103 O109 1.236(9) . ? N103 O111 1.248(9) . ? N103 O110 1.276(8) . ? N104 O112 1.183(10) . ? N104 O113 1.290(12) . ? N104 O114 1.321(11) . ? N105 O117 1.162(14) . ? N105 O117 1.162(14) 3_557 ? N105 O116 1.196(14) 3_557 ? N105 O116 1.196(14) . ? N105 O115 1.228(13) . ? N105 O115 1.228(13) 3_557 ? N106 O202 1.212(10) . ? N106 O201 1.217(10) . ? N106 O200 1.223(9) . ? N107 O207 1.151(9) . ? N107 O205 1.231(9) . ? N107 O206 1.247(9) . ? 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 N32 Co1 N36 93.6(2) . . ? N32 Co1 N2 92.6(2) . . ? N36 Co1 N2 94.3(2) . . ? N32 Co1 N18 174.9(2) . . ? N36 Co1 N18 82.2(2) . . ? N2 Co1 N18 90.8(2) . . ? N32 Co1 N33 82.5(2) . . ? N36 Co1 N33 89.6(2) . . ? N2 Co1 N33 173.9(3) . . ? N18 Co1 N33 94.4(2) . . ? N32 Co1 N3 89.2(2) . . ? N36 Co1 N3 175.7(2) . . ? N2 Co1 N3 82.4(2) . . ? N18 Co1 N3 95.1(2) . . ? N33 Co1 N3 94.0(2) . . ? N28 Co2 N22 93.7(2) . . ? N28 Co2 N35 93.6(2) . . ? N22 Co2 N35 93.3(2) . . ? N28 Co2 N30 82.0(2) . . ? N22 Co2 N30 174.6(2) . . ? N35 Co2 N30 90.1(2) . . ? N28 Co2 N21 175.0(2) . . ? N22 Co2 N21 89.1(2) . . ? N35 Co2 N21 82.0(2) . . ? N30 Co2 N21 95.5(2) . . ? N28 Co2 N26 89.9(2) . . ? N22 Co2 N26 82.3(2) . . ? N35 Co2 N26 174.6(2) . . ? N30 Co2 N26 94.4(2) . . ? N21 Co2 N26 94.6(2) . . ? N13 Co3 N23 93.4(2) . . ? N13 Co3 N11 93.3(2) . . ? N23 Co3 N11 94.1(2) . . ? N13 Co3 N9 89.6(2) . . ? N23 Co3 N9 175.4(2) . . ? N11 Co3 N9 82.2(2) . . ? N13 Co3 N14 82.3(2) . . ? N23 Co3 N14 89.1(2) . . ? N11 Co3 N14 174.7(2) . . ? N9 Co3 N14 94.8(2) . . ? N13 Co3 N24 175.2(2) . . ? N23 Co3 N24 82.2(2) . . ? N11 Co3 N24 88.7(2) . . ? N9 Co3 N24 95.0(2) . . ? N14 Co3 N24 95.9(2) . . ? N12 Co4 N1 93.5(2) . . ? N12 Co4 N29 92.9(2) . 3_777 ? N1 Co4 N29 95.2(2) . 3_777 ? N12 Co4 N17 82.7(2) . . ? N1 Co4 N17 89.5(2) . . ? N29 Co4 N17 173.8(2) 3_777 . ? N12 Co4 N6 175.7(2) . . ? N1 Co4 N6 82.6(2) . . ? N29 Co4 N6 89.2(2) 3_777 . ? N17 Co4 N6 95.5(2) . . ? N12 Co4 N7 88.7(2) . . ? N1 Co4 N7 176.4(2) . . ? N29 Co4 N7 81.8(2) 3_777 . ? N17 Co4 N7 93.7(2) . . ? N6 Co4 N7 95.3(2) . . ? N22 C1 N23 110.5(5) . . ? N23 C2 C3 107.2(5) . . ? N23 C2 C8 112.8(5) . . ? C3 C2 C8 140.0(6) . . ? N22 C3 C2 106.9(5) . . ? N22 C3 C4 113.4(6) . . ? C2 C3 C4 139.8(6) . . ? N26 C4 N27 125.8(6) . . ? N26 C4 C3 114.0(6) . . ? N27 C4 C3 120.2(6) . . ? N27 C5 C6 108.9(6) . . ? C5 C6 C7 111.3(7) . . ? N26 C7 C6 111.7(6) . . ? N24 C8 N25 125.2(6) . . ? N24 C8 C2 113.4(6) . . ? N25 C8 C2 121.4(6) . . ? N24 C9 C10 110.9(5) . . ? C9 C10 C11 110.5(6) . . ? N25 C11 C10 108.9(6) . . ? N35 C12 N36 110.9(6) . . ? C14 C13 N35 107.0(6) . . ? C14 C13 C15 139.7(7) . . ? N35 C13 C15 113.2(6) . . ? N36 C14 C13 107.7(6) . . ? N36 C14 C19 112.8(6) . . ? C13 C14 C19 139.3(7) . . ? N21 C15 N20 127.1(7) . . ? N21 C15 C13 113.1(6) . . ? N20 C15 C13 119.8(6) . . ? N21 C16 C17 111.5(6) . . ? C18 C17 C16 109.9(6) . . ? N20 C18 C17 109.7(7) . . ? N18 C19 N19 126.3(6) . . ? N18 C19 C14 113.6(6) . . ? N19 C19 C14 120.0(6) . . ? N19 C20 C21 109.0(7) . . ? C20 C21 C22 112.4(7) . . ? N18 C22 C21 111.8(6) . . ? N2 C23 N1 111.7(6) . . ? C25 C24 N2 107.6(5) . . ? C25 C24 C26 138.5(6) . . ? N2 C24 C26 113.9(5) . . ? C24 C25 N1 107.5(5) . . ? C24 C25 C30 139.6(6) . . ? N1 C25 C30 112.8(6) . . ? N3 C26 N4 126.4(6) . . ? N3 C26 C24 114.2(6) . . ? N4 C26 C24 119.4(6) . . ? N3 C27 C28 111.1(6) . . ? C29 C28 C27 111.4(8) . . ? N4 C29 C28 109.3(7) . . ? N6 C30 N5 125.7(6) . . ? N6 C30 C25 113.4(6) . . ? N5 C30 C25 120.8(6) . . ? N5 C31 C32 108.8(6) . . ? C31 C32 C33 110.6(6) . . ? N6 C33 C32 110.1(5) . . ? N13 C34 N12 110.7(6) . . ? N13 C35 C36 107.1(6) . . ? N13 C35 C37 112.4(5) . . ? C36 C35 C37 140.5(6) . . ? N12 C36 C35 107.5(6) . . ? N12 C36 C41 112.8(6) . . ? C35 C36 C41 139.7(7) . . ? N14 C37 N15 125.3(6) . . ? N14 C37 C35 113.2(6) . . ? N15 C37 C35 121.5(6) . . ? N14 C38 C39 110.9(6) . . ? C40 C39 C38 109.2(6) . . ? N15 C40 C39 109.3(6) . . ? N17 C41 N16 126.5(6) . . ? N17 C41 C36 112.9(6) . . ? N16 C41 C36 120.5(6) . . ? N16 C42 C43 108.5(6) . . ? C42 C43 C44 110.8(6) . . ? N17 C44 C43 111.5(6) . . ? C58 C45 N11 107.0(6) 3_777 . ? C58 C45 C46 139.5(6) 3_777 . ? N11 C45 C46 113.4(6) . . ? N9 C46 N8 124.4(7) . . ? N9 C46 C45 114.1(6) . . ? N8 C46 C45 121.4(7) . . ? N7 C47 N10 124.5(6) . . ? N7 C47 C57 114.7(6) . 3_777 ? N10 C47 C57 120.8(6) . 3_777 ? C104 C48 N8 108.8(11) . . ? C104 C48 C103 50.2(13) . . ? N8 C48 C103 106.7(10) . . ? N9 C50 C104 109.9(9) . . ? N9 C50 C103 108.2(9) . . ? C104 C50 C103 46.6(12) . . ? N10 C51 C52 109.1(6) . . ? C53 C52 C51 111.4(7) . . ? N7 C53 C52 112.2(7) . . ? N28 C54 N29 111.9(6) . . ? N32 C55 N11 111.2(5) . 3_777 ? N28 C56 C57 107.7(5) . . ? N28 C56 C63 112.0(6) . . ? C57 C56 C63 140.0(6) . . ? N29 C57 C56 106.9(6) . . ? N29 C57 C47 112.2(6) . 3_777 ? C56 C57 C47 140.8(6) . 3_777 ? C45 C58 N32 108.2(6) 3_777 . ? C45 C58 C59 138.6(7) 3_777 . ? N32 C58 C59 113.1(6) . . ? N33 C59 N34 127.0(6) . . ? N33 C59 C58 113.9(6) . . ? N34 C59 C58 119.0(7) . . ? N33 C60 C61 111.4(6) . . ? C62 C61 C60 117.6(8) . . ? C61 C62 N34 109.8(8) . . ? N30 C63 N31 126.0(7) . . ? N30 C63 C56 113.9(6) . . ? N31 C63 C56 120.0(7) . . ? C65 C64 N30 111.7(7) . . ? C66 C65 C64 120.0(10) . . ? C65 C66 N31 112.8(9) . . ? C104 C103 C48 57.5(16) . . ? C104 C103 C50 65.7(13) . . ? C48 C103 C50 107.7(15) . . ? C103 C104 C48 72(2) . . ? C103 C104 C50 67.8(15) . . ? C48 C104 C50 119(2) . . ? C23 N1 C25 106.5(5) . . ? C23 N1 Co4 138.5(5) . . ? C25 N1 Co4 114.1(4) . . ? C23 N2 C24 106.7(5) . . ? C23 N2 Co1 139.4(4) . . ? C24 N2 Co1 113.7(4) . . ? C26 N3 C27 118.4(5) . . ? C26 N3 Co1 115.4(4) . . ? C27 N3 Co1 126.1(4) . . ? C26 N4 C29 118.8(6) . . ? C30 N5 C31 120.1(6) . . ? C30 N6 C33 119.0(6) . . ? C30 N6 Co4 115.3(4) . . ? C33 N6 Co4 124.2(4) . . ? C47 N7 C53 119.3(6) . . ? C47 N7 Co4 114.9(4) . . ? C53 N7 Co4 124.3(4) . . ? C46 N8 C48 122.4(7) . . ? C46 N9 C50 118.9(6) . . ? C46 N9 Co3 115.6(5) . . ? C50 N9 Co3 125.0(5) . . ? C47 N10 C51 121.0(6) . . ? C55 N11 C45 106.6(5) 3_777 . ? C55 N11 Co3 138.6(4) 3_777 . ? C45 N11 Co3 114.1(5) . . ? C34 N12 C36 107.2(5) . . ? C34 N12 Co4 137.6(5) . . ? C36 N12 Co4 115.2(4) . . ? C34 N13 C35 107.5(5) . . ? C34 N13 Co3 136.9(5) . . ? C35 N13 Co3 115.1(4) . . ? C37 N14 C38 118.3(6) . . ? C37 N14 Co3 115.8(5) . . ? C38 N14 Co3 125.3(4) . . ? C37 N15 C40 121.3(6) . . ? C41 N16 C42 118.0(6) . . ? C41 N17 C44 118.9(6) . . ? C41 N17 Co4 115.4(4) . . ? C44 N17 Co4 125.5(5) . . ? C19 N18 C22 118.4(6) . . ? C19 N18 Co1 115.8(4) . . ? C22 N18 Co1 125.8(5) . . ? C19 N19 C20 119.8(6) . . ? C15 N20 C18 120.6(6) . . ? C15 N21 C16 117.0(6) . . ? C15 N21 Co2 116.3(5) . . ? C16 N21 Co2 125.5(4) . . ? C1 N22 C3 107.7(5) . . ? C1 N22 Co2 137.2(4) . . ? C3 N22 Co2 114.9(4) . . ? C1 N23 C2 107.7(5) . . ? C1 N23 Co3 137.0(4) . . ? C2 N23 Co3 114.6(4) . . ? C8 N24 C9 118.7(5) . . ? C8 N24 Co3 115.3(4) . . ? C9 N24 Co3 124.5(4) . . ? C8 N25 C11 121.4(6) . . ? C4 N26 C7 118.8(5) . . ? C4 N26 Co2 114.9(4) . . ? C7 N26 Co2 126.3(4) . . ? C4 N27 C5 119.3(6) . . ? C54 N28 C56 106.7(6) . . ? C54 N28 Co2 137.8(5) . . ? C56 N28 Co2 115.5(4) . . ? C54 N29 C57 106.8(5) . . ? C54 N29 Co4 137.4(4) . 3_777 ? C57 N29 Co4 115.4(5) . 3_777 ? C63 N30 C64 118.9(6) . . ? C63 N30 Co2 116.5(4) . . ? C64 N30 Co2 124.5(5) . . ? C63 N31 C66 118.4(7) . . ? C55 N32 C58 106.9(6) . . ? C55 N32 Co1 138.5(5) . . ? C58 N32 Co1 114.6(4) . . ? C59 N33 C60 118.1(6) . . ? C59 N33 Co1 115.7(4) . . ? C60 N33 Co1 126.2(5) . . ? C59 N34 C62 119.4(7) . . ? C12 N35 C13 107.0(5) . . ? C12 N35 Co2 138.5(5) . . ? C13 N35 Co2 114.1(4) . . ? C12 N36 C14 107.3(5) . . ? C12 N36 Co1 137.6(5) . . ? C14 N36 Co1 115.1(4) . . ? O104 N101 O103 122.3(8) . . ? O104 N101 O105 119.2(7) . . ? O103 N101 O105 118.5(7) . . ? O106 N102 O107 128.3(11) . . ? O106 N102 O108 115.6(12) . . ? O107 N102 O108 116.1(10) . . ? O109 N103 O111 122.7(8) . . ? O109 N103 O110 118.5(7) . . ? O111 N103 O110 118.7(7) . . ? O112 N104 O113 118.6(10) . . ? O112 N104 O114 120.9(10) . . ? O113 N104 O114 120.5(9) . . ? O117 N105 O117 180.0(3) . 3_557 ? O117 N105 O116 119.6(12) . 3_557 ? O117 N105 O116 60.4(12) 3_557 3_557 ? O117 N105 O116 60.4(12) . . ? O117 N105 O116 119.6(12) 3_557 . ? O116 N105 O116 180.000(6) 3_557 . ? O117 N105 O115 117.6(12) . . ? O117 N105 O115 62.4(12) 3_557 . ? O116 N105 O115 122.6(12) 3_557 . ? O116 N105 O115 57.4(12) . . ? O117 N105 O115 62.4(12) . 3_557 ? O117 N105 O115 117.6(12) 3_557 3_557 ? O116 N105 O115 57.4(12) 3_557 3_557 ? O116 N105 O115 122.6(12) . 3_557 ? O115 N105 O115 180.0(5) . 3_557 ? O202 N106 O201 104(2) . . ? O202 N106 O200 137(2) . . ? O201 N106 O200 118(2) . . ? O207 N107 O205 115.6(17) . . ? O207 N107 O206 125.5(17) . . ? O205 N107 O206 118.7(16) . . ? O116 O115 N105 59.9(9) . . ? O116 O115 O117 115.9(15) . 3_557 ? N105 O115 O117 56.2(10) . 3_557 ? O115 O116 N105 62.7(12) . . ? O115 O116 O117 120.8(17) . . ? N105 O116 O117 58.4(10) . . ? N105 O117 O116 61.2(12) . . ? N105 O117 O115 61.4(10) . 3_557 ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 65.07 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.925 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.105 # Attachment '- Compound 1e.cif' data_1e _database_code_depnum_ccdc_archive 'CCDC 824168' #TrackingRef '- Compound 1e.cif' _publ_section_comment ; The structure contains disordered borontetraflouride counterions and water solvent molecules. ; _audit_update_record ; 2009-11-14 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C138 H178 B12 Co8 F48 N74 O16.75' _chemical_formula_weight 4654.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 '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 1 2/c 1' 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 31.693(6) _cell_length_b 20.047(4) _cell_length_c 32.309(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.50(3) _cell_angle_gamma 90.00 _cell_volume 19351(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9448 _exptl_absorpt_coefficient_mu 6.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.5703 _exptl_absorpt_correction_T_max 0.5703 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _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 21764 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_sigmaI/netI 0.1616 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 54.24 _reflns_number_total 10552 _reflns_number_gt 5226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1371P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10552 _refine_ls_number_parameters 1453 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1715 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2358 _refine_ls_wR_factor_gt 0.1871 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.69859(5) 0.03284(9) 0.55034(6) 0.0315(5) Uani 1 1 d . . . Co2 Co 0.88908(5) 0.11974(9) 0.60378(5) 0.0314(5) Uani 1 1 d . . . Co3 Co 0.83466(5) 0.39443(9) 0.63749(6) 0.0333(5) Uani 1 1 d . . . Co4 Co 0.64338(5) 0.30681(9) 0.58387(5) 0.0318(5) Uani 1 1 d . . . B1 B 0.0478(5) 0.3714(9) 0.5834(6) 0.054(4) Uani 1 1 d . . . B2 B 0.8071(6) 0.1471(12) 0.7791(7) 0.072(6) Uani 1 1 d . . . B3 B 0.7500 0.2500 0.5000 0.025(4) Uiso 1 2 d SD . . B4 B 1.0000 0.2894(16) 0.7500 0.068(8) Uani 1 2 d S . . B5 B 1.0000 1.0000 0.5000 0.102(11) Uiso 1 2 d SD . . B6 B 0.6462(5) 0.2004(7) 0.9345(5) 0.163(15) Uani 1 1 d D . . B7 B 0.5860(6) 0.0762(8) 0.7149(6) 0.179 Uiso 1 1 d D . . B9 B 0.4689(7) 0.4101(13) 0.8106(8) 0.17(2) Uiso 0.50 1 d PD . . C1 C 0.7915(3) 0.0853(5) 0.5621(4) 0.032(3) Uani 1 1 d . . . H1 H 0.7886 0.0926 0.5322 0.039 Uiso 1 1 calc R . . C2 C 0.7757(3) 0.0612(6) 0.6207(4) 0.038(3) Uani 1 1 d . . . C3 C 0.8199(3) 0.0787(6) 0.6332(3) 0.032(3) Uani 1 1 d . . . C4 C 0.7418(4) 0.0382(6) 0.6394(4) 0.041(3) Uani 1 1 d . . . C5 C 0.7179(4) 0.0218(7) 0.7042(4) 0.060(4) Uani 1 1 d . . . C6 C 0.6699(8) 0.0313(17) 0.6684(9) 0.058(9) Uani 0.50 1 d P . . C7 C 0.6885(8) -0.0283(19) 0.6732(10) 0.076(11) Uani 0.50 1 d P . . C8 C 0.6681(4) -0.0069(6) 0.6266(4) 0.047(4) Uani 1 1 d . . . C9 C 0.6880(3) 0.1776(5) 0.5715(3) 0.028(3) Uani 1 1 d . . . H9 H 0.7186 0.1907 0.5824 0.034 Uiso 1 1 calc R . . C10 C 0.6272(3) 0.1168(6) 0.5444(3) 0.033(3) Uani 1 1 d . . . C11 C 0.6145(3) 0.1790(6) 0.5535(3) 0.026(3) Uani 1 1 d . . . C12 C 0.5745(3) 0.2149(6) 0.5522(3) 0.028(3) Uani 1 1 d . . . C13 C 0.4948(3) 0.2197(6) 0.5388(4) 0.048(3) Uani 1 1 d . . . H13A H 0.4904 0.2196 0.5677 0.058 Uiso 1 1 calc R . . H13B H 0.4685 0.1984 0.5170 0.058 Uiso 1 1 calc R . . C14 C 0.5002(3) 0.2913(6) 0.5248(4) 0.056(4) Uani 1 1 d . . . H14A H 0.5026 0.2913 0.4951 0.067 Uiso 1 1 calc R . . H14B H 0.4737 0.3180 0.5240 0.067 Uiso 1 1 calc R . . C15 C 0.5422(3) 0.3219(6) 0.5574(4) 0.040(3) Uani 1 1 d . . . H15A H 0.5477 0.3663 0.5467 0.048 Uiso 1 1 calc R . . H15B H 0.5379 0.3279 0.5862 0.048 Uiso 1 1 calc R . . C16 C 0.6076(3) 0.0542(6) 0.5239(3) 0.031(3) Uani 1 1 d . . . C17 C 0.6189(3) -0.0583(6) 0.5048(4) 0.040(3) Uani 1 1 d . . . H17A H 0.6101 -0.0879 0.5251 0.048 Uiso 1 1 calc R . . H17B H 0.6430 -0.0805 0.4969 0.048 Uiso 1 1 calc R . . C18 C 0.5794(3) -0.0463(6) 0.4642(4) 0.046(3) Uani 1 1 d . . . H18A H 0.5672 -0.0895 0.4505 0.056 Uiso 1 1 calc R . . H18B H 0.5888 -0.0202 0.4428 0.056 Uiso 1 1 calc R . . C19 C 0.5437(3) -0.0085(6) 0.4760(4) 0.047(3) Uani 1 1 d . . . H19A H 0.5195 0.0053 0.4489 0.056 Uiso 1 1 calc R . . H19B H 0.5304 -0.0376 0.4932 0.056 Uiso 1 1 calc R . . C20 C 0.8455(3) 0.2491(6) 0.6154(3) 0.029(3) Uani 1 1 d . . . H20 H 0.8161 0.2332 0.6113 0.035 Uiso 1 1 calc R . . C21 C 0.9162(3) 0.2512(6) 0.6223(3) 0.031(3) Uani 1 1 d . . . C22 C 0.9031(3) 0.3147(6) 0.6276(3) 0.031(3) Uani 1 1 d . . . C23 C 0.9220(3) 0.3822(6) 0.6389(4) 0.037(3) Uani 1 1 d . . . C24 C 0.9138(3) 0.4918(6) 0.6631(4) 0.042(3) Uani 1 1 d . . . H24A H 0.9006 0.5101 0.6844 0.051 Uiso 1 1 calc R . . H24B H 0.9053 0.5213 0.6370 0.051 Uiso 1 1 calc R . . C25 C 0.9635(4) 0.4899(6) 0.6833(4) 0.055(4) Uani 1 1 d . . . H25A H 0.9749 0.5357 0.6913 0.066 Uiso 1 1 calc R . . H25B H 0.9718 0.4628 0.7104 0.066 Uiso 1 1 calc R . . C26 C 0.9842(4) 0.4613(6) 0.6529(4) 0.057(4) Uani 1 1 d . . . H26A H 1.0165 0.4535 0.6685 0.069 Uiso 1 1 calc R . . H26B H 0.9813 0.4929 0.6285 0.069 Uiso 1 1 calc R . . C27 C 0.9575(3) 0.2135(7) 0.6260(3) 0.032(3) Uani 1 1 d . . . C28 C 1.0380(4) 0.2064(7) 0.6439(4) 0.056(4) Uani 1 1 d . . . H28A H 1.0604 0.2352 0.6374 0.067 Uiso 1 1 calc R . . H28B H 1.0510 0.1901 0.6744 0.067 Uiso 1 1 calc R . . C29 C 1.0273(3) 0.1501(7) 0.6138(4) 0.055(4) Uani 1 1 d . . . H29A H 1.0539 0.1209 0.6203 0.066 Uiso 1 1 calc R . . H29B H 1.0202 0.1668 0.5834 0.066 Uiso 1 1 calc R . . C30 C 0.9883(3) 0.1095(6) 0.6168(4) 0.037(3) Uani 1 1 d . . . H30A H 0.9789 0.0778 0.5919 0.045 Uiso 1 1 calc R . . H30B H 0.9981 0.0833 0.6443 0.045 Uiso 1 1 calc R . . C31 C 0.8674(3) 0.1799(6) 0.5130(4) 0.031(3) Uani 1 1 d . . . H31 H 0.8636 0.2251 0.5198 0.037 Uiso 1 1 calc R . . C32 C 0.8711(3) 0.0899(6) 0.4768(4) 0.034(3) Uani 1 1 d . . . C33 C 0.8812(3) 0.0737(6) 0.5202(4) 0.030(3) Uani 1 1 d . . . C34 C 0.8962(3) 0.0171(6) 0.5495(4) 0.034(3) Uani 1 1 d . . . C35 C 0.9209(4) -0.0988(6) 0.5627(4) 0.059(4) Uani 1 1 d . . . H35A H 0.9103 -0.1413 0.5470 0.071 Uiso 1 1 calc R . . H35B H 0.9540 -0.0988 0.5732 0.071 Uiso 1 1 calc R . . C36 C 0.9044(4) -0.0929(7) 0.6007(4) 0.062(4) Uani 1 1 d . . . H36A H 0.8716 -0.0996 0.5906 0.074 Uiso 1 1 calc R . . H36B H 0.9184 -0.1281 0.6225 0.074 Uiso 1 1 calc R . . C37 C 0.9155(3) -0.0262(6) 0.6217(4) 0.040(3) Uani 1 1 d . . . H37A H 0.9012 -0.0216 0.6445 0.048 Uiso 1 1 calc R . . H37B H 0.9483 -0.0231 0.6364 0.048 Uiso 1 1 calc R . . C38 C 0.8685(3) 0.0585(7) 0.4356(4) 0.035(3) Uani 1 1 d . . . C39 C 0.8679(4) 0.0752(6) 0.3620(4) 0.046(3) Uani 1 1 d . . . H39A H 0.8859 0.1043 0.3496 0.055 Uiso 1 1 calc R . . H39B H 0.8367 0.0753 0.3414 0.055 Uiso 1 1 calc R . . C40 C 0.8864(4) 0.0042(6) 0.3664(4) 0.054(4) Uani 1 1 d . . . H40A H 0.8825 -0.0141 0.3369 0.065 Uiso 1 1 calc R . . H40B H 0.9188 0.0048 0.3834 0.065 Uiso 1 1 calc R . . C41 C 0.8632(4) -0.0389(6) 0.3887(4) 0.050(4) Uani 1 1 d . . . H41A H 0.8773 -0.0836 0.3938 0.060 Uiso 1 1 calc R . . H41B H 0.8315 -0.0441 0.3702 0.060 Uiso 1 1 calc R . . C42 C 0.8211(3) 0.4059(6) 0.5400(4) 0.030(3) Uani 1 1 d . . . H42 H 0.8323 0.3637 0.5353 0.036 Uiso 1 1 calc R . . C43 C 0.8022(3) 0.4913(6) 0.5719(4) 0.034(3) Uani 1 1 d . . . C44 C 0.7904(3) 0.5046(6) 0.5281(4) 0.027(3) Uani 1 1 d . . . C45 C 0.8025(4) 0.5223(7) 0.6131(5) 0.044(3) Uani 1 1 d . . . C46 C 0.8117(4) 0.5064(6) 0.6891(4) 0.049(4) Uani 1 1 d . . . H46A H 0.8425 0.5105 0.7102 0.058 Uiso 1 1 calc R . . H46B H 0.7956 0.4732 0.7009 0.058 Uiso 1 1 calc R . . C47 C 0.7887(5) 0.5720(8) 0.6847(5) 0.084(5) Uani 1 1 d . . . H47A H 0.7559 0.5645 0.6729 0.100 Uiso 1 1 calc R . . H47B H 0.7957 0.5919 0.7143 0.100 Uiso 1 1 calc R . . C48 C 0.8009(5) 0.6201(7) 0.6562(4) 0.065(4) Uani 1 1 d . . . H48A H 0.8327 0.6334 0.6694 0.078 Uiso 1 1 calc R . . H48B H 0.7821 0.6606 0.6521 0.078 Uiso 1 1 calc R . . C49 C 0.7702(3) 0.5575(6) 0.4977(4) 0.032(3) Uani 1 1 d . . . C50 C 0.7255(4) 0.6595(6) 0.4769(4) 0.048(3) Uani 1 1 d . . . H50A H 0.7256 0.7016 0.4929 0.057 Uiso 1 1 calc R . . H50B H 0.6942 0.6477 0.4600 0.057 Uiso 1 1 calc R . . C51 C 0.7527(4) 0.6678(6) 0.4460(4) 0.055(4) Uani 1 1 d . . . H51A H 0.7376 0.7001 0.4225 0.066 Uiso 1 1 calc R . . H51B H 0.7828 0.6854 0.4625 0.066 Uiso 1 1 calc R . . C52 C 0.7570(4) 0.6016(6) 0.4260(4) 0.048(3) Uani 1 1 d . . . H52A H 0.7270 0.5860 0.4074 0.058 Uiso 1 1 calc R . . H52B H 0.7757 0.6067 0.4070 0.058 Uiso 1 1 calc R . . C53 C 0.7373(3) 0.3548(5) 0.5948(4) 0.032(3) Uani 1 1 d . . . H53 H 0.7326 0.3697 0.5657 0.038 Uiso 1 1 calc R . . C54 C 0.7264(4) 0.3115(6) 0.6519(4) 0.040(3) Uani 1 1 d . . . C55 C 0.7700(3) 0.3338(6) 0.6642(3) 0.033(3) Uani 1 1 d . . . C56 C 0.8085(4) 0.3402(6) 0.7034(4) 0.035(3) Uani 1 1 d . . . C57 C 0.8460(4) 0.3285(8) 0.7826(4) 0.071(5) Uani 1 1 d . . . H57A H 0.8468 0.3718 0.7975 0.085 Uiso 1 1 calc R . . H57B H 0.8446 0.2925 0.8030 0.085 Uiso 1 1 calc R . . C58 C 0.8859(4) 0.3208(8) 0.7705(4) 0.064(4) Uani 1 1 d . . . H58A H 0.8881 0.2740 0.7616 0.077 Uiso 1 1 calc R . . H58B H 0.9126 0.3304 0.7964 0.077 Uiso 1 1 calc R . . C59 C 0.8860(3) 0.3663(7) 0.7337(4) 0.048(4) Uani 1 1 d . . . H59A H 0.8914 0.4126 0.7449 0.058 Uiso 1 1 calc R . . H59B H 0.9110 0.3536 0.7233 0.058 Uiso 1 1 calc R . . C60 C 0.6949(4) 0.2771(6) 0.6705(4) 0.033(3) Uani 1 1 d . . . C61 C 0.6188(3) 0.2465(6) 0.6586(3) 0.043(3) Uani 1 1 d . . . H61A H 0.6135 0.2003 0.6473 0.052 Uiso 1 1 calc R . . H61B H 0.5902 0.2714 0.6470 0.052 Uiso 1 1 calc R . . C62 C 0.6341(3) 0.2456(6) 0.7085(4) 0.047(3) Uani 1 1 d . . . H62A H 0.6352 0.2919 0.7194 0.056 Uiso 1 1 calc R . . H62B H 0.6121 0.2206 0.7181 0.056 Uiso 1 1 calc R . . C63 C 0.6793(4) 0.2142(7) 0.7281(4) 0.060(4) Uani 1 1 d . . . H63A H 0.6899 0.2189 0.7604 0.072 Uiso 1 1 calc R . . H63B H 0.6779 0.1661 0.7207 0.072 Uiso 1 1 calc R . . C64 C 0.8353(4) 0.2669(8) 0.8936(4) 0.081(5) Uani 1 1 d . . . H64A H 0.8046 0.2664 0.8729 0.122 Uiso 1 1 calc R . . H64B H 0.8564 0.2634 0.8774 0.122 Uiso 1 1 calc R . . H64C H 0.8406 0.3087 0.9103 0.122 Uiso 1 1 calc R . . C65 C 0.8853(4) 0.2038(8) 0.9566(5) 0.094(6) Uani 1 1 d . . . H65A H 0.8863 0.2296 0.9827 0.141 Uiso 1 1 calc R . . H65B H 0.9081 0.2207 0.9450 0.141 Uiso 1 1 calc R . . H65C H 0.8911 0.1567 0.9646 0.141 Uiso 1 1 calc R . . C66 C 0.8106(4) 0.1677(7) 0.9225(5) 0.060(4) Uani 1 1 d . . . H66 H 0.7821 0.1747 0.9009 0.072 Uiso 1 1 calc R . . C090 C 0.8594(4) 0.0812(6) 0.6718(4) 0.040(3) Uani 1 1 d . . . C097 C 0.9385(3) 0.1023(7) 0.7015(3) 0.046(4) Uani 1 1 d . . . H09A H 0.9558 0.1421 0.6986 0.055 Uiso 1 1 calc R . . H09B H 0.9563 0.0624 0.7002 0.055 Uiso 1 1 calc R . . C120 C 0.8990(4) 0.0597(10) 0.7499(4) 0.106(7) Uani 1 1 d . . . H12A H 0.8910 0.0726 0.7759 0.127 Uiso 1 1 calc R . . H12B H 0.9114 0.0139 0.7548 0.127 Uiso 1 1 calc R . . C128 C 0.9320(4) 0.1043(9) 0.7452(4) 0.103(7) Uani 1 1 d . . . H12C H 0.9610 0.0939 0.7682 0.123 Uiso 1 1 calc R . . H12D H 0.9237 0.1503 0.7505 0.123 Uiso 1 1 calc R . . F5 F 0.0014(2) 0.3683(4) 0.5635(2) 0.070(2) Uani 1 1 d . . . F6 F 0.0612(2) 0.4381(4) 0.5782(3) 0.084(3) Uani 1 1 d . . . F7 F 0.0682(3) 0.3277(5) 0.5659(3) 0.101(3) Uani 1 1 d . . . F8 F 0.0568(2) 0.3625(4) 0.6278(3) 0.086(3) Uani 1 1 d . . . F13 F 0.7798(2) 0.1799(5) 0.7970(3) 0.095(3) Uani 1 1 d . . . F14 F 0.8041(2) 0.0778(5) 0.7798(2) 0.086(3) Uani 1 1 d . . . F15 F 0.8523(2) 0.1624(4) 0.8020(3) 0.092(3) Uani 1 1 d . . . F16 F 0.7963(2) 0.1654(4) 0.7358(3) 0.085(3) Uani 1 1 d . . . F19 F 0.7597(8) 0.2511(16) 0.5456(3) 0.036(8) Uiso 0.25 1 d PD . . F20 F 0.7609(10) 0.2205(15) 0.5413(5) 0.167(13) Uiso 0.50 1 d PD . . F21 F 0.7299(6) 0.3071(7) 0.5087(6) 0.093(7) Uiso 0.50 1 d PD . . F22 F 0.7500(14) 0.1808(6) 0.4940(12) 0.042(10) Uiso 0.20 1 d PD . . F23 F 0.7899(10) 0.276(3) 0.5275(14) 0.046(16) Uiso 0.15 1 d PD . . F24 F 0.7654(17) 0.312(3) 0.4913(18) 0.011(12) Uiso 0.10 1 d P . . F25 F 0.7992(12) 0.257(2) 0.5183(18) 0.055(15) Uiso 0.20 1 d P . . F30 F 0.9631(3) 0.2514(5) 0.7313(3) 0.119(4) Uani 1 1 d . . . F31 F 1.0078(2) 0.3307(5) 0.7189(2) 0.086(3) Uani 1 1 d . . . F100 F 0.9581(4) 1.0205(13) 0.4847(7) 0.082(7) Uani 0.50 1 d PD . . F101 F 1.0074(19) 0.994(3) 0.5446(5) 0.10(3) Uiso 0.20 1 d PD . . F102 F 0.9701(4) 0.9446(7) 0.4846(5) 0.102(6) Uani 0.55 1 d PD . . F103 F 0.6868(4) 0.2041(5) 0.9281(4) 0.143(4) Uani 1 1 d D . . F104 F 0.6251(5) 0.2513(6) 0.9078(6) 0.310(13) Uani 1 1 d D . . F105 F 0.6273(3) 0.1432(5) 0.9127(4) 0.142(4) Uani 1 1 d D . . F106 F 0.6510(6) 0.2107(9) 0.9775(5) 0.091(6) Uani 0.50 1 d PD . . F107 F 0.9745(5) 1.0462(8) 0.5093(6) 0.065(6) Uani 0.55 1 d PD . . F110 F 0.6259(9) 0.0697(18) 0.7062(11) 0.112(11) Uiso 0.30 1 d PD . . F111 F 0.5956(11) 0.0103(10) 0.7081(11) 0.136(11) Uiso 0.35 1 d PD . . F112 F 0.5765(6) 0.0142(8) 0.7272(6) 0.118(6) Uiso 0.60 1 d PD . . F118 F 0.4903(8) 0.4508(14) 0.7887(8) 0.131(9) Uiso 0.40 1 d PD . . F119 F 0.451(3) 0.364(4) 0.777(2) 0.28(4) Uiso 0.20 1 d PD . . F121 F 0.4237(6) 0.3985(10) 0.7903(6) 0.117(7) Uiso 0.50 1 d PD . . F122 F 0.4690(10) 0.4757(14) 0.8237(12) 0.165(11) Uiso 0.40 1 d PD . . F124 F 0.4697(16) 0.429(3) 0.8519(12) 0.21(2) Uiso 0.30 1 d PD . . F125 F 0.4748(9) 0.3600(16) 0.8417(9) 0.140(10) Uiso 0.40 1 d PD . . F126 F 0.5007(11) 0.390(2) 0.7929(13) 0.148(14) Uiso 0.30 1 d PD . . F128 F 0.597(2) 0.095(3) 0.6780(13) 0.22(2) Uiso 0.30 1 d PD . . F129 F 0.5544(4) 0.1080(7) 0.6804(4) 0.142(5) Uiso 0.85 1 d PD . . F135 F 0.5526(10) 0.0890(18) 0.7340(11) 0.281(14) Uiso 0.60 1 d PD . . F141 F 0.7915(6) 0.2731(16) 0.5000(10) 0.052(8) Uiso 0.30 1 d PD . . F556 F 0.6122(5) 0.1105(8) 0.7521(5) 0.213(6) Uiso 1 1 d D . . N1 N 0.8293(3) 0.0942(4) 0.5953(3) 0.028(2) Uani 1 1 d . . . N2 N 0.7579(3) 0.0649(4) 0.5752(3) 0.033(2) Uani 1 1 d . . . N3 N 0.8960(2) 0.1006(4) 0.6642(3) 0.031(2) Uani 1 1 d . . . N4 N 0.8583(3) 0.0607(7) 0.7101(4) 0.076(5) Uani 1 1 d . . . N5 N 0.7504(3) 0.0427(7) 0.6832(4) 0.055(4) Uani 1 1 d . . . N6 N 0.7054(3) 0.0160(5) 0.6112(3) 0.030(2) Uani 1 1 d . . . N7 N 0.6732(3) 0.1175(5) 0.5556(3) 0.032(2) Uani 1 1 d . . . N8 N 0.6529(3) 0.2174(4) 0.5698(3) 0.029(2) Uani 1 1 d . . . N9 N 0.5354(3) 0.1838(5) 0.5413(3) 0.041(3) Uani 1 1 d . . . N10 N 0.5812(2) 0.2777(5) 0.5625(3) 0.032(2) Uani 1 1 d . . . N11 N 0.6354(3) 0.0063(5) 0.5268(3) 0.032(2) Uani 1 1 d . . . N12 N 0.5633(5) 0.0496(5) 0.5016(5) 0.045(4) Uani 1 1 d . . . N13 N 0.7061(3) 0.3262(4) 0.6073(3) 0.032(2) Uani 1 1 d . . . N14 N 0.7760(3) 0.3604(5) 0.6274(3) 0.033(2) Uani 1 1 d . . . N15 N 0.8441(3) 0.3643(4) 0.6965(3) 0.030(2) Uani 1 1 d . . . N16 N 0.8065(3) 0.3255(6) 0.7431(4) 0.062(4) Uani 1 1 d . . . N17 N 0.7098(3) 0.2491(6) 0.7094(4) 0.050(3) Uani 1 1 d . . . N18 N 0.6529(3) 0.2784(5) 0.6437(3) 0.035(3) Uani 1 1 d . . . N19 N 0.8585(2) 0.3124(5) 0.6240(3) 0.027(2) Uani 1 1 d . . . N20 N 0.8790(3) 0.2116(4) 0.6137(2) 0.028(2) Uani 1 1 d . . . N21 N 0.8962(3) 0.4243(5) 0.6499(3) 0.034(2) Uani 1 1 d . . . N22 N 0.9617(3) 0.3968(5) 0.6349(3) 0.050(3) Uani 1 1 d . . . N23 N 0.9498(3) 0.1509(5) 0.6160(3) 0.027(2) Uani 1 1 d . . . N24 N 0.9968(3) 0.2455(5) 0.6391(3) 0.042(3) Uani 1 1 d . . . N25 N 0.8204(2) 0.4274(5) 0.5790(3) 0.029(2) Uani 1 1 d . . . N26 N 0.8041(3) 0.4512(5) 0.5085(3) 0.033(2) Uani 1 1 d . . . N27 N 0.7772(2) 0.5522(4) 0.4599(3) 0.029(2) Uani 1 1 d . . . N28 N 0.7465(3) 0.6061(5) 0.5077(3) 0.040(3) Uani 1 1 d . . . N29 N 0.7934(3) 0.5865(6) 0.6136(3) 0.049(3) Uani 1 1 d . . . N30 N 0.8138(3) 0.4829(5) 0.6472(3) 0.039(3) Uani 1 1 d . . . N31 N 0.8779(2) 0.1314(5) 0.5428(3) 0.028(2) Uani 1 1 d . . . N32 N 0.8628(2) 0.1583(5) 0.4727(3) 0.030(2) Uani 1 1 d . . . N33 N 0.8686(3) 0.1022(5) 0.4046(3) 0.035(2) Uani 1 1 d . . . N34 N 0.8662(4) -0.0078(6) 0.4311(4) 0.049(3) Uani 1 1 d . . . N35 N 0.9036(3) -0.0414(5) 0.5322(3) 0.040(3) Uani 1 1 d . . . N36 N 0.9010(3) 0.0292(5) 0.5905(3) 0.036(2) Uani 1 1 d . . . N37 N 0.8418(3) 0.2105(5) 0.9238(3) 0.046(3) Uani 1 1 d . . . O1 O 0.8145(3) 0.1188(5) 0.9467(3) 0.057(2) Uani 1 1 d . . . O2 O 0.4481(3) 0.0696(5) 0.9019(3) 0.076(3) Uani 1 1 d . . . O400 O 0.4908(12) 0.300(2) 0.8489(13) 0.048(11) Uiso 0.20 1 d P . . O401 O 0.507(4) 0.217(8) 0.835(4) 0.17(5) Uiso 0.20 1 d P . . O402 O 0.537(3) 0.167(5) 0.863(3) 0.07(3) Uiso 0.10 1 d P . . O403 O 0.5277(19) 0.214(4) 0.833(2) 0.062(17) Uiso 0.20 1 d P . . O404 O 0.5623(17) 0.198(3) 0.8041(15) 0.069(15) Uiso 0.20 1 d P . . O405 O 0.553(4) 0.272(7) 0.788(4) 0.10(4) Uiso 0.10 1 d P . . O406 O 0.511(3) 0.269(5) 0.826(2) 0.13(3) Uiso 0.20 1 d P . . O500 O 0.667(3) 0.408(5) 0.756(3) 0.09(3) Uiso 0.15 1 d P . . O501 O 0.695(2) 0.393(3) 0.7604(16) 0.070(15) Uiso 0.20 1 d P . . O505 O 0.691(2) 0.306(3) 0.8249(18) 0.14(2) Uiso 0.25 1 d P . . O506 O 0.7258(15) 0.359(2) 0.7719(18) 0.051(12) Uiso 0.20 1 d P . . O508 O 0.7513(7) 0.3476(11) 0.8031(8) 0.090(6) Uiso 0.50 1 d P . . O509 O 0.6872(8) 0.3670(14) 0.7975(8) 0.106(8) Uiso 0.50 1 d P . . O510 O 0.6924(11) 0.423(2) 0.8117(11) 0.038(10) Uiso 0.20 1 d P . . O512 O 0.6553(19) 0.315(3) 0.8295(17) 0.21(2) Uiso 0.35 1 d P . . O513 O 0.7235(17) 0.382(3) 0.7498(18) 0.078(17) Uiso 0.20 1 d P . . O514 O 0.6545(15) 0.387(2) 0.8062(14) 0.248(18) Uiso 0.50 1 d P . . O515 O 0.677(2) 0.439(4) 0.752(2) 0.09(2) Uiso 0.20 1 d P . . O517 O 0.586(3) 0.322(5) 0.787(3) 0.16(3) Uiso 0.18 1 d P . . O600 O 0.7182(9) 0.3174(14) 0.8172(9) 0.122(9) Uiso 0.50 1 d P . . O604 O 0.535(3) 0.187(5) 0.800(3) 0.06(3) Uiso 0.10 1 d P . . O602 O 0.547(4) 0.243(5) 0.809(3) 0.04(3) Uiso 0.10 1 d P . . O608 O 0.568(2) 0.147(4) 0.778(3) 0.23(3) Uiso 0.25 1 d P . . O607 O 0.491(3) 0.327(6) 0.820(4) 0.08(3) Uiso 0.10 1 d P . . O606 O 0.514(3) 0.233(5) 0.858(3) 0.05(3) Uiso 0.10 1 d P . . O605 O 0.502(5) 0.164(8) 0.845(5) 0.13(5) Uiso 0.10 1 d P . . O601 O 0.590(3) 0.265(5) 0.809(3) 0.06(3) Uiso 0.10 1 d P . . O603 O 0.529(3) 0.236(4) 0.812(2) 0.006(17) Uiso 0.10 1 d P . . H501 H 0.736(3) 0.234(4) 0.727(3) 0.008 Uiso 1 1 d . . . H502 H 0.737(3) 0.601(4) 0.531(3) 0.008 Uiso 1 1 d . . . H503 H 0.841(3) 0.034(4) 0.716(3) 0.008 Uiso 1 1 d . . . H605 H 0.769(3) 0.057(5) 0.698(3) 0.008 Uiso 1 1 d . . . H606 H 0.785(3) 0.320(5) 0.747(3) 0.008 Uiso 1 1 d . . . H602 H 0.558(5) 0.074(6) 0.497(5) 0.008 Uiso 1 1 d . . . H600 H 0.790(3) 0.609(5) 0.592(3) 0.008 Uiso 1 1 d . . . H604 H 1.011(2) 0.308(4) 0.671(2) 0.008 Uiso 1 1 d . . . H601 H 0.534(3) 0.147(4) 0.551(3) 0.008 Uiso 1 1 d . . . H607 H 0.857(3) -0.021(5) 0.445(3) 0.008 Uiso 1 1 d . . . O111 O 1.0086(8) 0.9787(14) 0.5559(10) 0.035(9) Uiso 0.35(2) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0262(9) 0.0373(13) 0.0313(13) -0.0014(9) 0.0101(8) -0.0009(9) Co2 0.0246(9) 0.0407(14) 0.0281(12) 0.0009(9) 0.0076(8) 0.0006(9) Co3 0.0276(9) 0.0420(14) 0.0294(13) -0.0019(9) 0.0083(8) -0.0019(9) Co4 0.0283(9) 0.0364(13) 0.0313(13) -0.0021(9) 0.0106(8) 0.0002(9) B1 0.049(10) 0.055(13) 0.054(14) 0.015(10) 0.014(9) 0.009(10) B2 0.076(14) 0.077(17) 0.055(16) 0.004(12) 0.009(11) -0.002(13) B4 0.042(14) 0.10(3) 0.07(2) 0.000 0.037(14) 0.000 B6 0.091(19) 0.08(2) 0.33(5) -0.01(3) 0.09(3) -0.053(19) C1 0.025(6) 0.038(8) 0.037(9) 0.007(6) 0.015(6) 0.012(6) C2 0.026(6) 0.046(9) 0.041(10) -0.003(7) 0.010(6) -0.010(6) C3 0.036(7) 0.039(8) 0.020(8) 0.005(6) 0.008(6) 0.007(6) C4 0.040(8) 0.047(9) 0.038(10) 0.013(7) 0.018(7) 0.015(7) C5 0.040(7) 0.098(13) 0.049(10) -0.007(8) 0.023(7) -0.020(8) C6 0.033(15) 0.09(3) 0.06(2) -0.008(18) 0.018(13) -0.001(16) C7 0.034(15) 0.14(4) 0.06(2) 0.04(2) 0.019(15) -0.03(2) C8 0.041(7) 0.073(11) 0.039(9) -0.007(8) 0.029(6) -0.014(7) C9 0.037(6) 0.014(7) 0.039(8) -0.009(6) 0.019(5) -0.009(6) C10 0.024(6) 0.047(9) 0.033(8) 0.002(6) 0.014(5) 0.006(6) C11 0.023(6) 0.031(8) 0.021(7) -0.007(6) 0.002(5) 0.000(6) C12 0.025(6) 0.036(9) 0.025(7) -0.007(6) 0.010(5) -0.008(6) C13 0.035(7) 0.038(9) 0.070(10) -0.013(7) 0.017(6) -0.003(7) C14 0.018(6) 0.049(10) 0.090(11) -0.025(8) 0.002(6) 0.016(6) C15 0.038(7) 0.036(9) 0.047(9) -0.010(6) 0.017(6) -0.001(6) C16 0.018(6) 0.046(9) 0.028(8) 0.003(6) 0.005(5) -0.008(6) C17 0.034(7) 0.047(9) 0.040(9) -0.010(7) 0.013(6) 0.000(6) C18 0.032(7) 0.050(10) 0.058(10) -0.020(7) 0.017(6) -0.010(6) C19 0.034(7) 0.052(10) 0.048(10) -0.005(7) 0.005(6) -0.005(7) C20 0.011(5) 0.062(10) 0.013(7) 0.000(6) 0.002(4) 0.002(6) C21 0.033(7) 0.044(9) 0.014(7) 0.008(6) 0.005(5) -0.009(7) C22 0.025(6) 0.037(9) 0.027(8) 0.003(6) 0.004(5) 0.008(6) C23 0.028(6) 0.040(9) 0.048(9) 0.000(6) 0.019(6) -0.003(7) C24 0.044(7) 0.035(9) 0.052(9) 0.005(7) 0.022(6) -0.002(7) C25 0.041(7) 0.046(10) 0.072(11) -0.013(8) 0.014(7) -0.015(7) C26 0.047(8) 0.044(10) 0.082(12) -0.008(8) 0.023(7) -0.017(7) C27 0.014(6) 0.047(9) 0.035(8) 0.008(6) 0.005(5) 0.004(6) C28 0.033(7) 0.065(11) 0.079(11) 0.000(9) 0.030(7) 0.002(7) C29 0.025(6) 0.063(11) 0.074(11) -0.012(8) 0.015(6) 0.015(7) C30 0.022(6) 0.045(9) 0.044(8) 0.007(6) 0.011(5) 0.012(6) C31 0.020(6) 0.032(8) 0.043(9) -0.006(7) 0.014(6) -0.008(6) C32 0.020(6) 0.038(9) 0.049(10) -0.011(7) 0.019(6) 0.003(6) C33 0.027(6) 0.043(9) 0.019(8) 0.002(7) 0.006(5) 0.005(6) C34 0.029(6) 0.042(9) 0.033(9) -0.001(7) 0.011(6) 0.001(6) C35 0.073(9) 0.042(10) 0.072(11) -0.001(8) 0.038(8) 0.015(8) C36 0.087(10) 0.038(10) 0.060(11) 0.005(8) 0.023(8) 0.007(8) C37 0.037(6) 0.051(10) 0.032(9) -0.001(7) 0.011(6) 0.016(7) C38 0.026(6) 0.030(9) 0.049(10) -0.018(7) 0.014(6) 0.006(6) C39 0.050(7) 0.059(10) 0.030(9) 0.003(7) 0.016(6) -0.003(7) C40 0.075(9) 0.037(9) 0.056(10) -0.010(7) 0.030(8) 0.004(8) C41 0.059(8) 0.036(9) 0.057(10) -0.008(7) 0.022(7) -0.008(7) C42 0.023(6) 0.038(9) 0.030(9) -0.002(7) 0.010(6) -0.007(6) C43 0.034(6) 0.023(8) 0.046(10) -0.012(7) 0.015(6) 0.004(6) C44 0.027(6) 0.040(9) 0.019(8) 0.003(6) 0.014(5) -0.002(6) C45 0.033(7) 0.042(10) 0.055(11) -0.008(8) 0.011(6) 0.007(7) C46 0.069(8) 0.048(10) 0.032(9) -0.003(7) 0.022(7) 0.016(7) C47 0.111(13) 0.077(13) 0.063(12) -0.008(10) 0.028(10) 0.015(11) C48 0.082(10) 0.061(11) 0.061(12) -0.003(9) 0.036(8) -0.003(9) C49 0.022(6) 0.033(9) 0.043(9) 0.006(7) 0.015(6) 0.002(6) C50 0.055(8) 0.031(9) 0.061(10) -0.002(7) 0.024(7) 0.003(7) C51 0.067(9) 0.053(10) 0.050(10) 0.009(7) 0.027(7) 0.015(8) C52 0.063(8) 0.037(9) 0.048(10) 0.005(7) 0.022(7) 0.014(7) C53 0.031(7) 0.040(9) 0.026(8) 0.000(6) 0.011(6) 0.002(6) C54 0.036(7) 0.044(9) 0.046(10) 0.007(7) 0.020(6) 0.013(7) C55 0.026(6) 0.050(9) 0.023(8) -0.002(6) 0.008(6) 0.007(6) C56 0.039(7) 0.049(9) 0.017(8) 0.004(6) 0.011(7) 0.007(6) C57 0.056(9) 0.114(14) 0.044(10) 0.013(9) 0.019(8) -0.022(9) C58 0.039(7) 0.113(14) 0.031(9) 0.010(8) -0.002(6) 0.001(8) C59 0.029(6) 0.077(11) 0.028(9) 0.019(7) -0.004(6) 0.003(7) C60 0.040(7) 0.034(8) 0.021(8) 0.003(6) 0.004(6) 0.002(6) C61 0.039(7) 0.067(10) 0.031(9) -0.003(7) 0.021(6) -0.008(7) C62 0.039(7) 0.071(10) 0.035(9) 0.007(7) 0.018(6) -0.014(7) C63 0.048(8) 0.080(12) 0.057(10) 0.030(8) 0.024(7) -0.005(8) C64 0.076(10) 0.098(14) 0.058(11) 0.036(10) 0.007(8) 0.008(9) C65 0.073(10) 0.107(15) 0.077(13) 0.023(10) -0.008(9) -0.038(10) C66 0.051(8) 0.052(11) 0.076(12) 0.003(9) 0.020(8) -0.010(9) C090 0.042(8) 0.067(10) 0.013(8) 0.010(6) 0.011(7) 0.004(7) C097 0.030(6) 0.077(11) 0.021(8) -0.008(7) -0.006(6) 0.005(6) C120 0.048(9) 0.23(2) 0.033(11) 0.019(11) 0.006(8) 0.012(11) C128 0.050(9) 0.22(2) 0.029(10) 0.029(11) -0.003(7) -0.038(11) F5 0.064(5) 0.077(6) 0.061(6) 0.000(4) 0.012(4) 0.015(4) F6 0.073(5) 0.084(7) 0.106(7) 0.029(5) 0.044(5) 0.007(5) F7 0.076(6) 0.108(8) 0.126(8) -0.021(6) 0.041(5) 0.036(6) F8 0.088(6) 0.097(7) 0.063(7) 0.007(5) 0.012(4) -0.033(5) F13 0.056(5) 0.130(9) 0.101(7) -0.028(6) 0.031(5) -0.014(5) F14 0.071(5) 0.103(8) 0.070(7) 0.005(6) 0.005(4) -0.006(6) F15 0.052(5) 0.111(8) 0.095(7) -0.014(5) 0.000(4) -0.014(5) F16 0.073(5) 0.092(7) 0.071(7) 0.009(5) 0.000(4) 0.006(5) F30 0.087(6) 0.115(9) 0.169(10) -0.071(7) 0.063(6) -0.042(6) F31 0.084(6) 0.106(8) 0.064(7) 0.008(5) 0.020(5) 0.011(5) F100 0.074(14) 0.088(19) 0.08(2) 0.034(13) 0.020(11) 0.019(13) F102 0.078(11) 0.17(2) 0.067(12) 0.003(11) 0.029(8) 0.021(12) F103 0.155(10) 0.083(8) 0.175(12) -0.061(7) 0.035(8) -0.025(8) F104 0.253(17) 0.066(10) 0.41(3) -0.024(12) -0.154(16) 0.047(10) F105 0.128(8) 0.107(9) 0.225(13) -0.064(8) 0.103(8) -0.059(7) F106 0.126(14) 0.098(15) 0.070(13) -0.051(11) 0.062(11) -0.007(11) F107 0.039(9) 0.073(15) 0.073(17) 0.019(10) 0.008(8) 0.018(9) N1 0.028(5) 0.040(7) 0.015(6) 0.000(4) 0.007(5) 0.000(4) N2 0.028(5) 0.036(7) 0.039(7) 0.004(5) 0.016(5) -0.001(5) N3 0.020(5) 0.048(7) 0.023(6) -0.002(5) 0.004(4) -0.001(4) N4 0.029(6) 0.157(14) 0.038(9) 0.021(8) 0.003(6) -0.024(7) N5 0.029(6) 0.100(11) 0.037(10) -0.005(7) 0.013(6) -0.018(6) N6 0.021(5) 0.051(7) 0.015(6) -0.002(5) 0.002(4) 0.006(5) N7 0.029(5) 0.041(7) 0.028(6) -0.004(5) 0.014(4) 0.003(5) N8 0.030(5) 0.027(6) 0.032(6) -0.004(4) 0.011(4) 0.000(5) N9 0.035(6) 0.037(8) 0.058(8) -0.004(6) 0.023(5) -0.002(6) N10 0.020(5) 0.033(7) 0.046(7) -0.005(5) 0.016(4) -0.006(5) N11 0.028(5) 0.036(7) 0.036(7) 0.000(5) 0.017(4) -0.003(5) N12 0.047(8) 0.033(10) 0.053(9) -0.007(8) 0.014(6) -0.012(8) N13 0.034(5) 0.025(6) 0.044(8) 0.006(5) 0.020(5) -0.007(5) N14 0.031(5) 0.051(7) 0.021(6) 0.007(5) 0.015(5) 0.003(5) N15 0.026(5) 0.040(7) 0.023(6) -0.006(5) 0.006(4) -0.002(5) N16 0.027(6) 0.103(11) 0.048(9) 0.001(7) 0.002(6) -0.026(7) N17 0.034(6) 0.074(9) 0.037(8) 0.021(6) 0.004(5) 0.007(6) N18 0.032(5) 0.061(8) 0.011(6) -0.005(5) 0.007(4) 0.001(5) N19 0.023(5) 0.027(6) 0.026(6) 0.001(5) 0.001(4) -0.004(5) N20 0.024(5) 0.038(7) 0.022(6) 0.004(4) 0.005(4) -0.003(5) N21 0.034(5) 0.035(7) 0.035(7) 0.000(5) 0.016(4) -0.002(5) N22 0.035(6) 0.052(8) 0.062(8) -0.010(6) 0.015(5) -0.011(6) N23 0.032(5) 0.034(7) 0.015(6) 0.010(5) 0.006(4) 0.001(5) N24 0.025(5) 0.040(7) 0.061(7) 0.004(5) 0.014(5) 0.003(5) N25 0.022(5) 0.047(7) 0.019(6) -0.002(5) 0.009(4) -0.002(5) N26 0.024(5) 0.042(7) 0.035(7) -0.007(6) 0.013(5) 0.004(5) N27 0.025(5) 0.030(7) 0.029(7) 0.003(5) 0.008(4) 0.001(4) N28 0.043(6) 0.037(7) 0.043(8) 0.012(6) 0.020(5) 0.019(5) N29 0.066(7) 0.046(9) 0.038(9) -0.003(6) 0.020(6) 0.001(7) N30 0.041(6) 0.036(7) 0.036(8) -0.008(6) 0.007(5) 0.001(5) N31 0.024(5) 0.027(6) 0.034(7) -0.001(5) 0.013(4) 0.002(5) N32 0.020(5) 0.038(7) 0.033(7) -0.006(5) 0.011(4) 0.007(5) N33 0.035(5) 0.034(7) 0.033(7) 0.001(5) 0.008(5) -0.016(5) N34 0.063(8) 0.055(10) 0.033(9) -0.012(7) 0.020(5) 0.001(7) N35 0.046(6) 0.037(7) 0.036(7) 0.004(6) 0.013(5) 0.006(5) N36 0.035(5) 0.039(7) 0.029(7) 0.004(5) 0.003(5) -0.002(5) N37 0.040(6) 0.045(8) 0.057(8) 0.000(6) 0.020(5) -0.009(6) O1 0.074(6) 0.043(7) 0.066(7) 0.007(5) 0.039(5) 0.005(5) O2 0.061(6) 0.090(8) 0.071(7) -0.013(6) 0.015(5) 0.016(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 Co1 N2 1.894(8) . ? Co1 N26 1.901(9) 7_656 ? Co1 N7 1.911(9) . ? Co1 N6 1.934(8) . ? Co1 N27 1.942(9) 7_656 ? Co1 N11 1.964(8) . ? Co2 N1 1.891(8) . ? Co2 N31 1.897(9) . ? Co2 N20 1.913(9) . ? Co2 N3 1.928(8) . ? Co2 N36 1.930(10) . ? Co2 N23 1.936(8) . ? Co3 N14 1.905(8) . ? Co3 N25 1.908(8) . ? Co3 N19 1.921(9) . ? Co3 N15 1.926(8) . ? Co3 N21 1.951(8) . ? Co3 N30 1.955(10) . ? Co4 N8 1.899(9) . ? Co4 N32 1.906(9) 7_656 ? Co4 N13 1.917(8) . ? Co4 N33 1.925(10) 7_656 ? Co4 N18 1.941(8) . ? Co4 N10 1.946(8) . ? B1 F7 1.324(17) . ? B1 F8 1.376(17) . ? B1 F5 1.396(15) . ? B1 F6 1.430(17) . ? B2 F13 1.36(2) . ? B2 F16 1.375(19) . ? B2 F14 1.39(2) . ? B2 F15 1.411(19) . ? B3 F21 1.383(9) 7_656 ? B3 F21 1.383(9) . ? B3 F23 1.384(11) 7_656 ? B3 F23 1.384(11) . ? B3 F141 1.393(10) . ? B3 F141 1.393(10) 7_656 ? B3 F20 1.394(10) 7_656 ? B3 F20 1.394(10) . ? B3 F22 1.400(10) . ? B3 F22 1.400(10) 7_656 ? B3 F19 1.402(10) 7_656 ? B3 F19 1.402(10) . ? B4 F30 1.358(17) . ? B4 F30 1.358(17) 2_756 ? B4 F31 1.385(18) 2_756 ? B4 F31 1.385(18) . ? B5 F100 1.319(9) . ? B5 F100 1.319(9) 5_776 ? B5 F107 1.328(9) . ? B5 F107 1.328(9) 5_776 ? B5 F101 1.384(11) 5_776 ? B5 F101 1.384(11) . ? B5 F102 1.437(9) . ? B5 F102 1.437(9) 5_776 ? B5 O111 1.79(3) 5_776 ? B6 F104 1.360(10) . ? B6 F106 1.361(10) . ? B6 F103 1.373(10) . ? B6 F105 1.373(10) . ? B7 F112 1.368(10) . ? B7 F129 1.382(10) . ? B7 F111 1.390(10) . ? B7 F110 1.392(10) . ? B7 F556 1.393(10) . ? B7 F128 1.394(11) . ? B7 F135 1.414(10) . ? B9 F126 1.377(11) . ? B9 F124 1.382(11) . ? B9 F122 1.382(11) . ? B9 F121 1.382(11) . ? B9 F119 1.385(11) . ? B9 F125 1.386(8) . ? B9 F118 1.397(10) . ? C1 N1 1.326(12) . ? C1 N2 1.335(11) . ? C2 C3 1.368(13) . ? C2 N2 1.389(13) . ? C2 C4 1.472(14) . ? C3 N1 1.389(12) . ? C3 C090 1.443(15) . ? C4 N6 1.287(13) . ? C4 N5 1.352(15) . ? C5 N5 1.471(15) . ? C5 C7 1.50(3) . ? C5 C6 1.59(3) . ? C6 C7 1.32(4) . ? C6 C8 1.54(3) . ? C7 C8 1.49(3) . ? C8 N6 1.501(12) . ? C9 N7 1.333(12) . ? C9 N8 1.356(12) . ? C10 C11 1.372(14) . ? C10 N7 1.379(11) . ? C10 C16 1.460(15) . ? C11 N8 1.386(11) . ? C11 C12 1.446(13) . ? C12 N10 1.302(12) . ? C12 N9 1.326(13) . ? C13 N9 1.452(13) . ? C13 C14 1.529(16) . ? C14 C15 1.523(14) . ? C15 N10 1.486(12) . ? C16 N11 1.284(12) . ? C16 N12 1.350(19) . ? C17 N11 1.486(13) . ? C17 C18 1.500(14) . ? C18 C19 1.513(14) . ? C19 N12 1.443(18) . ? C20 N20 1.319(11) . ? C20 N19 1.335(12) . ? C21 C22 1.369(14) . ? C21 N20 1.371(12) . ? C21 C27 1.479(14) . ? C22 N19 1.379(11) . ? C22 C23 1.474(15) . ? C23 N21 1.304(13) . ? C23 N22 1.338(12) . ? C24 N21 1.470(13) . ? C24 C25 1.490(14) . ? C25 C26 1.468(15) . ? C26 N22 1.497(14) . ? C27 N23 1.299(13) . ? C27 N24 1.339(12) . ? C28 C29 1.452(15) . ? C28 N24 1.488(13) . ? C29 C30 1.509(14) . ? C30 N23 1.467(12) . ? C31 N31 1.329(13) . ? C31 N32 1.334(12) . ? C32 C33 1.369(14) . ? C32 N32 1.394(13) . ? C32 C38 1.450(15) . ? C33 N31 1.390(13) . ? C33 C34 1.451(15) . ? C34 N36 1.306(13) . ? C34 N35 1.354(14) . ? C35 C36 1.491(15) . ? C35 N35 1.494(14) . ? C36 C37 1.489(15) . ? C37 N36 1.466(13) . ? C38 N33 1.332(14) . ? C38 N34 1.337(15) . ? C39 N33 1.470(13) . ? C39 C40 1.529(15) . ? C40 C41 1.468(14) . ? C41 N34 1.477(15) . ? C42 N26 1.336(13) . ? C42 N25 1.340(12) . ? C43 C44 1.366(14) . ? C43 N25 1.392(13) . ? C43 C45 1.465(16) . ? C44 N26 1.385(13) . ? C44 C49 1.442(14) . ? C45 N30 1.304(14) . ? C45 N29 1.320(15) . ? C46 N30 1.455(13) . ? C46 C47 1.490(16) . ? C47 C48 1.472(17) . ? C48 N29 1.478(15) . ? C49 N27 1.317(12) . ? C49 N28 1.334(13) . ? C50 N28 1.461(14) . ? C50 C51 1.531(14) . ? C51 C52 1.502(15) . ? C52 N27 1.457(13) . ? C53 N13 1.317(11) . ? C53 N14 1.329(12) . ? C54 C55 1.380(14) . ? C54 N13 1.400(13) . ? C54 C60 1.493(14) . ? C55 N14 1.374(12) . ? C55 C56 1.440(15) . ? C56 N15 1.315(12) . ? C56 N16 1.336(13) . ? C57 C58 1.453(14) . ? C57 N16 1.459(15) . ? C58 C59 1.499(15) . ? C59 N15 1.463(12) . ? C60 N17 1.312(13) . ? C60 N18 1.324(13) . ? C61 N18 1.469(12) . ? C61 C62 1.518(14) . ? C62 C63 1.498(14) . ? C63 N17 1.477(13) . ? C64 N37 1.463(14) . ? C65 N37 1.438(14) . ? C66 O1 1.233(14) . ? C66 N37 1.299(14) . ? C090 N4 1.317(13) . ? C090 N3 1.322(12) . ? C097 N3 1.477(12) . ? C097 C128 1.494(15) . ? C120 C128 1.422(18) . ? C120 N4 1.489(15) . ? N12 H602 0.51(12) . ? N26 Co1 1.901(9) 7_656 ? N27 Co1 1.942(9) 7_656 ? N29 H600 0.81(8) . ? N32 Co4 1.906(9) 7_656 ? N33 Co4 1.925(9) 7_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N26 94.2(4) . 7_656 ? N2 Co1 N7 92.8(4) . . ? N26 Co1 N7 93.4(4) 7_656 . ? N2 Co1 N6 82.5(4) . . ? N26 Co1 N6 176.3(3) 7_656 . ? N7 Co1 N6 88.4(4) . . ? N2 Co1 N27 88.7(3) . 7_656 ? N26 Co1 N27 82.3(4) 7_656 7_656 ? N7 Co1 N27 175.6(4) . 7_656 ? N6 Co1 N27 96.0(4) . 7_656 ? N2 Co1 N11 175.0(4) . . ? N26 Co1 N11 87.7(3) 7_656 . ? N7 Co1 N11 82.5(4) . . ? N6 Co1 N11 95.7(3) . . ? N27 Co1 N11 96.1(4) 7_656 . ? N1 Co2 N31 93.0(3) . . ? N1 Co2 N20 94.0(3) . . ? N31 Co2 N20 94.1(4) . . ? N1 Co2 N3 82.2(3) . . ? N31 Co2 N3 174.2(4) . . ? N20 Co2 N3 89.5(4) . . ? N1 Co2 N36 88.5(3) . . ? N31 Co2 N36 82.4(4) . . ? N20 Co2 N36 175.8(4) . . ? N3 Co2 N36 94.2(4) . . ? N1 Co2 N23 175.5(4) . . ? N31 Co2 N23 89.9(3) . . ? N20 Co2 N23 82.3(4) . . ? N3 Co2 N23 95.1(3) . . ? N36 Co2 N23 95.4(4) . . ? N14 Co3 N25 93.4(3) . . ? N14 Co3 N19 95.2(4) . . ? N25 Co3 N19 93.0(4) . . ? N14 Co3 N15 83.0(3) . . ? N25 Co3 N15 175.0(3) . . ? N19 Co3 N15 90.8(4) . . ? N14 Co3 N21 176.4(4) . . ? N25 Co3 N21 89.3(3) . . ? N19 Co3 N21 82.3(4) . . ? N15 Co3 N21 94.4(3) . . ? N14 Co3 N30 89.4(4) . . ? N25 Co3 N30 82.1(4) . . ? N19 Co3 N30 173.5(4) . . ? N15 Co3 N30 94.3(4) . . ? N21 Co3 N30 93.3(4) . . ? N8 Co4 N32 95.2(4) . 7_656 ? N8 Co4 N13 93.4(4) . . ? N32 Co4 N13 93.8(4) 7_656 . ? N8 Co4 N33 177.1(4) . 7_656 ? N32 Co4 N33 82.8(4) 7_656 7_656 ? N13 Co4 N33 88.7(4) . 7_656 ? N8 Co4 N18 88.7(4) . . ? N32 Co4 N18 174.8(4) 7_656 . ? N13 Co4 N18 82.5(4) . . ? N33 Co4 N18 93.5(4) 7_656 . ? N8 Co4 N10 81.6(4) . . ? N32 Co4 N10 90.1(3) 7_656 . ? N13 Co4 N10 174.0(4) . . ? N33 Co4 N10 96.3(4) 7_656 . ? N18 Co4 N10 93.9(3) . . ? N1 C1 N2 112.7(10) . . ? C3 C2 N2 108.2(9) . . ? C3 C2 C4 140.9(12) . . ? N2 C2 C4 110.9(9) . . ? C2 C3 N1 107.3(9) . . ? C2 C3 C090 140.5(11) . . ? N1 C3 C090 112.0(9) . . ? N6 C4 N5 125.8(10) . . ? N6 C4 C2 114.9(11) . . ? N5 C4 C2 119.3(11) . . ? N5 C5 C7 104.9(13) . . ? N5 C5 C6 106.2(13) . . ? C7 C5 C6 50.5(15) . . ? C7 C6 C8 62.3(19) . . ? C7 C6 C5 61.5(19) . . ? C8 C6 C5 108.9(18) . . ? C6 C7 C8 66.1(18) . . ? C6 C7 C5 68(2) . . ? C8 C7 C5 116(2) . . ? C7 C8 N6 107.5(12) . . ? C7 C8 C6 51.7(16) . . ? N6 C8 C6 109.7(12) . . ? N7 C9 N8 109.6(9) . . ? C11 C10 N7 107.2(10) . . ? C11 C10 C16 140.2(10) . . ? N7 C10 C16 112.3(10) . . ? C10 C11 N8 107.5(9) . . ? C10 C11 C12 139.8(10) . . ? N8 C11 C12 112.6(9) . . ? N10 C12 N9 125.6(10) . . ? N10 C12 C11 114.0(9) . . ? N9 C12 C11 120.4(10) . . ? N9 C13 C14 107.4(9) . . ? C15 C14 C13 109.4(10) . . ? N10 C15 C14 109.9(9) . . ? N11 C16 N12 123.6(12) . . ? N11 C16 C10 115.6(9) . . ? N12 C16 C10 120.7(11) . . ? N11 C17 C18 109.7(10) . . ? C17 C18 C19 109.7(9) . . ? N12 C19 C18 109.4(10) . . ? N20 C20 N19 110.6(9) . . ? C22 C21 N20 106.7(9) . . ? C22 C21 C27 139.7(11) . . ? N20 C21 C27 113.4(10) . . ? C21 C22 N19 107.6(10) . . ? C21 C22 C23 140.3(10) . . ? N19 C22 C23 111.9(10) . . ? N21 C23 N22 125.3(11) . . ? N21 C23 C22 114.9(9) . . ? N22 C23 C22 119.6(10) . . ? N21 C24 C25 110.2(9) . . ? C26 C25 C24 111.2(11) . . ? C25 C26 N22 109.5(9) . . ? N23 C27 N24 128.2(10) . . ? N23 C27 C21 112.8(9) . . ? N24 C27 C21 119.0(11) . . ? C29 C28 N24 109.8(10) . . ? C28 C29 C30 112.9(10) . . ? N23 C30 C29 112.8(9) . . ? N31 C31 N32 112.8(11) . . ? C33 C32 N32 107.6(9) . . ? C33 C32 C38 139.4(13) . . ? N32 C32 C38 112.9(11) . . ? C32 C33 N31 107.9(10) . . ? C32 C33 C34 140.1(12) . . ? N31 C33 C34 111.9(10) . . ? N36 C34 N35 127.0(11) . . ? N36 C34 C33 114.8(11) . . ? N35 C34 C33 118.2(11) . . ? C36 C35 N35 109.2(10) . . ? C37 C36 C35 110.7(11) . . ? N36 C37 C36 113.3(10) . . ? N33 C38 N34 125.8(11) . . ? N33 C38 C32 113.1(12) . . ? N34 C38 C32 121.1(12) . . ? N33 C39 C40 111.7(9) . . ? C41 C40 C39 110.7(9) . . ? C40 C41 N34 108.6(10) . . ? N26 C42 N25 111.7(11) . . ? C44 C43 N25 107.8(9) . . ? C44 C43 C45 140.9(12) . . ? N25 C43 C45 111.3(11) . . ? C43 C44 N26 107.7(10) . . ? C43 C44 C49 139.1(11) . . ? N26 C44 C49 113.2(10) . . ? N30 C45 N29 125.3(12) . . ? N30 C45 C43 115.3(13) . . ? N29 C45 C43 119.3(13) . . ? N30 C46 C47 111.8(10) . . ? C48 C47 C46 114.5(12) . . ? C47 C48 N29 106.8(12) . . ? N27 C49 N28 124.5(11) . . ? N27 C49 C44 113.4(10) . . ? N28 C49 C44 122.1(10) . . ? N28 C50 C51 107.3(9) . . ? C52 C51 C50 109.6(10) . . ? N27 C52 C51 110.9(10) . . ? N13 C53 N14 112.4(10) . . ? C55 C54 N13 107.4(9) . . ? C55 C54 C60 140.6(12) . . ? N13 C54 C60 112.0(9) . . ? N14 C55 C54 106.9(9) . . ? N14 C55 C56 113.9(10) . . ? C54 C55 C56 139.1(11) . . ? N15 C56 N16 124.1(10) . . ? N15 C56 C55 114.1(9) . . ? N16 C56 C55 121.8(10) . . ? C58 C57 N16 109.3(10) . . ? C57 C58 C59 112.4(11) . . ? N15 C59 C58 113.2(9) . . ? N17 C60 N18 126.6(10) . . ? N17 C60 C54 120.5(10) . . ? N18 C60 C54 112.9(10) . . ? N18 C61 C62 110.0(8) . . ? C63 C62 C61 112.1(9) . . ? N17 C63 C62 107.0(10) . . ? O1 C66 N37 126.1(13) . . ? N4 C090 N3 124.6(10) . . ? N4 C090 C3 120.9(10) . . ? N3 C090 C3 114.3(9) . . ? N3 C097 C128 113.4(9) . . ? C128 C120 N4 111.0(12) . . ? C120 C128 C097 114.9(13) . . ? C1 N1 C3 106.3(9) . . ? C1 N1 Co2 138.1(7) . . ? C3 N1 Co2 115.5(7) . . ? C1 N2 C2 105.5(8) . . ? C1 N2 Co1 138.8(8) . . ? C2 N2 Co1 115.2(6) . . ? C090 N3 C097 118.1(9) . . ? C090 N3 Co2 115.8(7) . . ? C097 N3 Co2 125.9(7) . . ? C090 N4 C120 121.8(10) . . ? C4 N5 C5 122.4(9) . . ? C4 N6 C8 119.2(9) . . ? C4 N6 Co1 115.5(8) . . ? C8 N6 Co1 123.9(7) . . ? C9 N7 C10 108.4(9) . . ? C9 N7 Co1 137.1(7) . . ? C10 N7 Co1 114.0(8) . . ? C9 N8 C11 107.2(8) . . ? C9 N8 Co4 137.6(7) . . ? C11 N8 Co4 115.2(7) . . ? C12 N9 C13 120.8(10) . . ? C12 N10 C15 119.3(8) . . ? C12 N10 Co4 116.1(7) . . ? C15 N10 Co4 124.6(7) . . ? C16 N11 C17 119.5(9) . . ? C16 N11 Co1 114.3(8) . . ? C17 N11 Co1 124.9(7) . . ? H602 N12 C16 104(10) . . ? H602 N12 C19 124(10) . . ? C16 N12 C19 122.3(12) . . ? C53 N13 C54 106.1(9) . . ? C53 N13 Co4 138.8(8) . . ? C54 N13 Co4 114.9(6) . . ? C53 N14 C55 107.3(9) . . ? C53 N14 Co3 139.1(8) . . ? C55 N14 Co3 113.6(7) . . ? C56 N15 C59 117.8(9) . . ? C56 N15 Co3 115.1(7) . . ? C59 N15 Co3 127.1(7) . . ? C56 N16 C57 122.0(9) . . ? C60 N17 C63 121.2(9) . . ? C60 N18 C61 117.9(9) . . ? C60 N18 Co4 116.4(7) . . ? C61 N18 Co4 124.6(7) . . ? C20 N19 C22 106.8(9) . . ? C20 N19 Co3 137.9(7) . . ? C22 N19 Co3 114.9(8) . . ? C20 N20 C21 108.2(9) . . ? C20 N20 Co2 137.5(8) . . ? C21 N20 Co2 114.3(7) . . ? C23 N21 C24 117.6(9) . . ? C23 N21 Co3 114.8(8) . . ? C24 N21 Co3 126.7(7) . . ? C23 N22 C26 119.6(10) . . ? C27 N23 C30 117.2(8) . . ? C27 N23 Co2 116.8(7) . . ? C30 N23 Co2 125.9(7) . . ? C27 N24 C28 118.2(10) . . ? C42 N25 C43 106.1(9) . . ? C42 N25 Co3 138.4(9) . . ? C43 N25 Co3 115.4(7) . . ? C42 N26 C44 106.6(9) . . ? C42 N26 Co1 138.4(8) . 7_656 ? C44 N26 Co1 114.2(8) . 7_656 ? C49 N27 C52 118.3(9) . . ? C49 N27 Co1 115.3(8) . 7_656 ? C52 N27 Co1 124.6(7) . 7_656 ? C49 N28 C50 122.3(10) . . ? H600 N29 C45 120(7) . . ? H600 N29 C48 119(7) . . ? C45 N29 C48 119.3(11) . . ? C45 N30 C46 120.4(11) . . ? C45 N30 Co3 115.2(9) . . ? C46 N30 Co3 124.4(8) . . ? C31 N31 C33 105.9(9) . . ? C31 N31 Co2 139.1(9) . . ? C33 N31 Co2 115.0(8) . . ? C31 N32 C32 105.7(9) . . ? C31 N32 Co4 139.5(9) . 7_656 ? C32 N32 Co4 114.1(7) . 7_656 ? C38 N33 C39 117.3(10) . . ? C38 N33 Co4 115.2(8) . 7_656 ? C39 N33 Co4 126.0(8) . 7_656 ? C38 N34 C41 120.3(11) . . ? C34 N35 C35 118.2(10) . . ? C34 N36 C37 117.4(10) . . ? C34 N36 Co2 115.8(8) . . ? C37 N36 Co2 126.8(8) . . ? C66 N37 C65 119.6(12) . . ? C66 N37 C64 123.7(11) . . ? C65 N37 C64 116.7(11) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 54.24 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.703 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.088 # Attachment '- Compound 1f.cif' data_1f _database_code_depnum_ccdc_archive 'CCDC 824169' #TrackingRef '- Compound 1f.cif' _publ_section_comment ; The structure contains disordered water solvent molecules. ; #Added by publCIF #Added by publCIF _audit_update_record ; 2009-09-02 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H168 Cl12 Co8 N72 O40' _chemical_formula_weight 4300.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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 1 2/c 1' 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 33.008(8) _cell_length_b 19.253(5) _cell_length_c 32.654(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.116(5) _cell_angle_gamma 90.00 _cell_volume 18633(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_description polyhedra _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8816 _exptl_absorpt_coefficient_mu 7.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _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 48750 _diffrn_reflns_av_R_equivalents 0.1568 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 55.09 _reflns_number_total 11569 _reflns_number_gt 7037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0961P)^2^+49.0272P] 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 11569 _refine_ls_number_parameters 1272 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1305 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.1988 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36601(4) 0.14912(6) 0.15675(4) 0.0225(3) Uani 1 1 d . . . Co2 Co 0.22839(4) 0.51481(6) 0.01444(4) 0.0231(3) Uani 1 1 d . . . Co3 Co 0.40164(4) 0.37469(6) 0.05090(4) 0.0225(3) Uani 1 1 d . . . Co4 Co 0.19189(4) 0.29134(7) 0.11887(4) 0.0251(3) Uani 1 1 d . . . C1 C 0.3186(2) 0.0904(4) 0.0612(3) 0.0233(19) Uani 1 1 d . . . H1 H 0.3249 0.1258 0.0445 0.028 Uiso 1 1 calc R . . C2 C 0.3164(3) 0.0309(4) 0.1169(3) 0.028(2) Uani 1 1 d . . . C3 C 0.2921(2) -0.0039(4) 0.0770(3) 0.0246(19) Uani 1 1 d . . . C4 C 0.2640(2) -0.0663(4) 0.0614(3) 0.027(2) Uani 1 1 d . . . C5 C 0.2216(3) -0.1614(5) 0.0727(3) 0.040(2) Uani 1 1 d . . . H5A H 0.1894 -0.1481 0.0610 0.048 Uiso 1 1 calc R . . H5B H 0.2288 -0.1945 0.0982 0.048 Uiso 1 1 calc R . . C6 C 0.2296(3) -0.1955(4) 0.0352(3) 0.038(2) Uani 1 1 d . . . H6A H 0.2072 -0.2331 0.0211 0.046 Uiso 1 1 calc R . . H6B H 0.2601 -0.2164 0.0483 0.046 Uiso 1 1 calc R . . C7 C 0.2254(3) -0.1429(4) -0.0010(3) 0.034(2) Uani 1 1 d . . . H7A H 0.2340 -0.1650 -0.0234 0.041 Uiso 1 1 calc R . . H7B H 0.1936 -0.1276 -0.0174 0.041 Uiso 1 1 calc R . . C8 C 0.3316(3) 0.0223(5) 0.1664(3) 0.030(2) Uani 1 1 d . . . C9 C 0.3648(3) 0.0768(4) 0.2392(3) 0.033(2) Uani 1 1 d . . . H9A H 0.3589 0.1231 0.2486 0.040 Uiso 1 1 calc R . . H9B H 0.3976 0.0675 0.2559 0.040 Uiso 1 1 calc R . . C10 C 0.3392(4) 0.0225(5) 0.2515(3) 0.056(3) Uani 1 1 d . . . H10A H 0.3072 0.0365 0.2396 0.068 Uiso 1 1 calc R . . H10B H 0.3518 0.0189 0.2851 0.068 Uiso 1 1 calc R . . C11 C 0.3423(4) -0.0478(5) 0.2318(3) 0.060(3) Uani 1 1 d . . . H11A H 0.3739 -0.0644 0.2458 0.071 Uiso 1 1 calc R . . H11B H 0.3235 -0.0824 0.2380 0.071 Uiso 1 1 calc R . . C12 C 0.2707(3) 0.2076(4) 0.1204(2) 0.0236(19) Uani 1 1 d . . . H12 H 0.2556 0.1787 0.0945 0.028 Uiso 1 1 calc R . . C13 C 0.2837(3) 0.2884(4) 0.1714(2) 0.0226(18) Uani 1 1 d . . . C14 C 0.3229(3) 0.2523(4) 0.1825(2) 0.027(2) Uani 1 1 d . . . C15 C 0.2685(3) 0.3471(4) 0.1881(3) 0.030(2) Uani 1 1 d . . . C16 C 0.2058(3) 0.4112(5) 0.1856(3) 0.040(2) Uani 1 1 d . . . H16A H 0.2035 0.3993 0.2140 0.048 Uiso 1 1 calc R . . H16B H 0.1752 0.4220 0.1617 0.048 Uiso 1 1 calc R . . C17 C 0.2361(3) 0.4748(5) 0.1939(3) 0.043(2) Uani 1 1 d . . . H17A H 0.2378 0.4881 0.1654 0.052 Uiso 1 1 calc R . . H17B H 0.2238 0.5145 0.2040 0.052 Uiso 1 1 calc R . . C18 C 0.2825(3) 0.4562(5) 0.2302(3) 0.043(2) Uani 1 1 d . . . H18A H 0.3039 0.4942 0.2333 0.052 Uiso 1 1 calc R . . H18B H 0.2815 0.4507 0.2599 0.052 Uiso 1 1 calc R . . C19 C 0.3693(3) 0.2502(4) 0.2188(3) 0.028(2) Uani 1 1 d . . . C20 C 0.4432(3) 0.2035(4) 0.2443(3) 0.034(2) Uani 1 1 d . . . H20A H 0.4623 0.1942 0.2286 0.041 Uiso 1 1 calc R . . H20B H 0.4469 0.1643 0.2653 0.041 Uiso 1 1 calc R . . C21 C 0.4582(3) 0.2702(5) 0.2713(3) 0.043(2) Uani 1 1 d . . . H21A H 0.4894 0.2648 0.2956 0.051 Uiso 1 1 calc R . . H21B H 0.4582 0.3084 0.2509 0.051 Uiso 1 1 calc R . . C22 C 0.4271(3) 0.2877(6) 0.2920(3) 0.056(3) Uani 1 1 d . . . H22A H 0.4298 0.2524 0.3151 0.067 Uiso 1 1 calc R . . H22B H 0.4351 0.3335 0.3072 0.067 Uiso 1 1 calc R . . C23 C 0.3062(3) 0.4262(4) 0.0204(3) 0.0236(19) Uani 1 1 d . . . H23 H 0.2913 0.4005 -0.0070 0.028 Uiso 1 1 calc R . . C24 C 0.3172(2) 0.4976(4) 0.0760(2) 0.0236(19) Uani 1 1 d . . . C25 C 0.3584(3) 0.4672(4) 0.0836(2) 0.027(2) Uani 1 1 d . . . C26 C 0.2996(3) 0.5454(4) 0.0980(3) 0.0255(19) Uani 1 1 d . . . C27 C 0.2356(3) 0.6115(4) 0.0907(3) 0.032(2) Uani 1 1 d . . . H27A H 0.2176 0.5846 0.1028 0.038 Uiso 1 1 calc R . . H27B H 0.2145 0.6416 0.0658 0.038 Uiso 1 1 calc R . . C28 C 0.2692(3) 0.6569(5) 0.1285(3) 0.043(2) Uani 1 1 d . . . H28A H 0.2827 0.6909 0.1153 0.051 Uiso 1 1 calc R . . H28B H 0.2535 0.6830 0.1433 0.051 Uiso 1 1 calc R . . C29 C 0.3060(3) 0.6129(5) 0.1634(3) 0.044(2) Uani 1 1 d . . . H29A H 0.3301 0.6432 0.1852 0.053 Uiso 1 1 calc R . . H29B H 0.2935 0.5853 0.1808 0.053 Uiso 1 1 calc R . . C30 C 0.4063(3) 0.4708(5) 0.1164(3) 0.031(2) Uani 1 1 d . . . C31 C 0.4695(3) 0.5185(5) 0.1822(3) 0.051(3) Uani 1 1 d . . . H31A H 0.4874 0.5495 0.1723 0.061 Uiso 1 1 calc R . . H31B H 0.4724 0.5353 0.2121 0.061 Uiso 1 1 calc R . . C32 C 0.4868(3) 0.4470(5) 0.1870(3) 0.042(2) Uani 1 1 d . . . H32A H 0.4713 0.4172 0.2004 0.050 Uiso 1 1 calc R . . H32B H 0.5195 0.4464 0.2077 0.050 Uiso 1 1 calc R . . C33 C 0.4789(2) 0.4191(5) 0.1414(3) 0.035(2) Uani 1 1 d . . . H33A H 0.4977 0.4452 0.1299 0.041 Uiso 1 1 calc R . . H33B H 0.4882 0.3698 0.1445 0.041 Uiso 1 1 calc R . . C34 C 0.3862(3) 0.4425(4) -0.0300(3) 0.027(2) Uani 1 1 d . . . C35 C 0.4299(3) 0.5170(4) 0.0326(3) 0.033(2) Uani 1 1 d . . . H35A H 0.4572 0.5102 0.0617 0.040 Uiso 1 1 calc R . . H35B H 0.4086 0.5465 0.0388 0.040 Uiso 1 1 calc R . . C36 C 0.4425(3) 0.5530(5) -0.0015(3) 0.045(2) Uani 1 1 d . . . H36A H 0.4554 0.5993 0.0103 0.054 Uiso 1 1 calc R . . H36B H 0.4655 0.5253 -0.0059 0.054 Uiso 1 1 calc R . . C37 C 0.4013(3) 0.5609(5) -0.0462(3) 0.044(2) Uani 1 1 d . . . H37A H 0.3801 0.5941 -0.0430 0.052 Uiso 1 1 calc R . . H37B H 0.4100 0.5790 -0.0696 0.052 Uiso 1 1 calc R . . C38 C 0.3675(2) 0.3734(4) -0.0430(3) 0.0251(19) Uani 1 1 d . . . C39 C 0.3483(2) 0.3332(4) -0.0819(2) 0.0249(19) Uani 1 1 d . . . C40 C 0.3487(2) 0.2734(4) -0.0249(2) 0.0236(19) Uani 1 1 d . . . H40 H 0.3443 0.2369 -0.0078 0.028 Uiso 1 1 calc R . . C41 C 0.3391(3) 0.3367(5) -0.1302(3) 0.030(2) Uani 1 1 d . . . C42 C 0.3445(4) 0.3917(5) -0.1939(3) 0.054(3) Uani 1 1 d . . . H42A H 0.3682 0.3670 -0.1989 0.065 Uiso 1 1 calc R . . H42B H 0.3433 0.4403 -0.2043 0.065 Uiso 1 1 calc R . . C43 C 0.3001(4) 0.3574(5) -0.2204(3) 0.058(3) Uani 1 1 d . . . H43A H 0.2934 0.3561 -0.2531 0.070 Uiso 1 1 calc R . . H43B H 0.2761 0.3847 -0.2174 0.070 Uiso 1 1 calc R . . C44 C 0.3004(3) 0.2843(5) -0.2034(3) 0.038(2) Uani 1 1 d . . . H44A H 0.2696 0.2644 -0.2189 0.045 Uiso 1 1 calc R . . H44B H 0.3209 0.2551 -0.2108 0.045 Uiso 1 1 calc R . . C45 C 0.2232(2) 0.3880(4) 0.0663(2) 0.0188(17) Uani 1 1 d . . . H45 H 0.2515 0.3674 0.0727 0.023 Uiso 1 1 calc R . . C46 C 0.1572(2) 0.4075(4) 0.0640(3) 0.027(2) Uani 1 1 d . . . C47 C 0.1652(3) 0.4579(4) 0.0399(3) 0.029(2) Uani 1 1 d . . . C48 C 0.1436(3) 0.5187(5) 0.0124(3) 0.039(2) Uani 1 1 d . . . C49 C 0.1495(3) 0.6159(4) -0.0312(3) 0.035(2) Uani 1 1 d . . . H49A H 0.1640 0.6215 -0.0518 0.042 Uiso 1 1 calc R . . H49B H 0.1557 0.6582 -0.0121 0.042 Uiso 1 1 calc R . . C50 C 0.0994(4) 0.6073(7) -0.0589(5) 0.094(5) Uani 1 1 d . . . H50A H 0.0864 0.6507 -0.0759 0.113 Uiso 1 1 calc R . . H50B H 0.0934 0.5695 -0.0814 0.113 Uiso 1 1 calc R . . C51 C 0.0776(4) 0.5909(7) -0.0292(6) 0.120(7) Uani 1 1 d . . . H51A H 0.0783 0.6324 -0.0111 0.144 Uiso 1 1 calc R . . H51B H 0.0457 0.5782 -0.0483 0.144 Uiso 1 1 calc R . . C52 C 0.0544(6) 0.4085(12) 0.0860(8) 0.211(14) Uani 1 1 d . . . H52A H 0.0560 0.4398 0.1107 0.253 Uiso 1 1 calc R . . H52B H 0.0243 0.4147 0.0599 0.253 Uiso 1 1 calc R . . C53 C 0.0577(5) 0.3462(8) 0.0999(7) 0.124(7) Uani 1 1 d . . . H53A H 0.0373 0.3181 0.0735 0.149 Uiso 1 1 calc R . . H53B H 0.0447 0.3452 0.1221 0.149 Uiso 1 1 calc R . . C54 C 0.1013(3) 0.3077(6) 0.1215(3) 0.053(3) Uani 1 1 d . . . H54A H 0.1146 0.3138 0.1550 0.063 Uiso 1 1 calc R . . H54B H 0.0956 0.2575 0.1148 0.063 Uiso 1 1 calc R . . C55 C 0.3673(2) 0.2719(4) 0.0988(2) 0.0194(18) Uani 1 1 d . . . H55 H 0.3406 0.2953 0.0955 0.023 Uiso 1 1 calc R . . C56 C 0.4294(3) 0.2479(4) 0.0945(3) 0.028(2) Uani 1 1 d . . . C57 C 0.4204(3) 0.1948(4) 0.1174(2) 0.0243(19) Uani 1 1 d . . . C58 C 0.4393(3) 0.1287(4) 0.1385(3) 0.030(2) Uani 1 1 d . . . C59 C 0.4911(4) 0.0313(6) 0.1506(4) 0.061(3) Uani 1 1 d . . . H59A H 0.5235 0.0291 0.1579 0.074 Uiso 1 1 calc R . . H59B H 0.4753 -0.0062 0.1285 0.074 Uiso 1 1 calc R . . C60 C 0.4368(3) 0.0344(4) 0.1838(3) 0.037(2) Uani 1 1 d . . . H60A H 0.4172 -0.0022 0.1633 0.045 Uiso 1 1 calc R . . H60B H 0.4347 0.0317 0.2130 0.045 Uiso 1 1 calc R . . C61 C 0.4852(3) 0.0216(6) 0.1923(3) 0.057(3) Uani 1 1 d . . . H61A H 0.5053 0.0540 0.2161 0.068 Uiso 1 1 calc R . . H61B H 0.4940 -0.0264 0.2037 0.068 Uiso 1 1 calc R . . C62 C 0.4647(3) 0.2691(5) 0.0810(3) 0.031(2) Uani 1 1 d . . . C63 C 0.4872(3) 0.3490(5) 0.0396(3) 0.035(2) Uani 1 1 d . . . H63A H 0.5077 0.3847 0.0602 0.042 Uiso 1 1 calc R . . H63B H 0.4702 0.3703 0.0092 0.042 Uiso 1 1 calc R . . C64 C 0.5145(3) 0.2892(5) 0.0359(4) 0.059(3) Uani 1 1 d . . . H64A H 0.4944 0.2568 0.0121 0.071 Uiso 1 1 calc R . . H64B H 0.5372 0.3068 0.0263 0.071 Uiso 1 1 calc R . . C65 C 0.5375(3) 0.2515(6) 0.0792(4) 0.064(3) Uani 1 1 d . . . H65A H 0.5612 0.2810 0.1021 0.076 Uiso 1 1 calc R . . H65B H 0.5519 0.2089 0.0747 0.076 Uiso 1 1 calc R . . C086 C 0.1239(3) 0.3885(6) 0.0799(3) 0.047(3) Uani 1 1 d . . . Cl1 Cl 0.88803(9) 0.9724(2) 0.23002(11) 0.0871(11) Uani 1 1 d . . . Cl2 Cl 0.71112(9) 0.46519(16) 0.15320(8) 0.0653(8) Uani 1 1 d . . . Cl3 Cl 0.10506(18) 0.7887(3) 0.9818(2) 0.0756(16) Uani 0.60 1 d P . . Cl4 Cl 0.4704(2) 0.0947(3) 0.03341(17) 0.0588(15) Uani 0.50 1 d P . . Cl5 Cl 0.5808(3) 0.1321(5) 0.1574(2) 0.165(3) Uani 0.70 1 d P . . Cl6 Cl 0.1471(3) 0.2356(6) 0.4099(3) 0.226(5) Uani 0.80 1 d P . . Cl9 Cl 0.9248(4) 0.1303(8) 0.2521(4) 0.143(4) Uani 0.40 1 d P . . Cl11 Cl 0.2500 0.2500 0.0000 0.0404(8) Uani 1 2 d S . . Cl12 Cl 0.0840(4) 0.1662(5) 0.3337(4) 0.146(3) Uani 0.50 1 d P . . N1 N 0.33229(19) 0.0912(3) 0.10617(19) 0.0227(15) Uani 1 1 d . . . N2 N 0.2948(2) 0.0327(3) 0.0427(2) 0.0239(15) Uani 1 1 d . . . N3 N 0.31467(19) 0.2021(3) 0.1498(2) 0.0234(15) Uani 1 1 d . . . N4 N 0.2509(2) 0.2597(3) 0.13270(19) 0.0235(15) Uani 1 1 d . . . N5 N 0.2543(2) -0.0826(3) 0.0193(2) 0.0256(16) Uani 1 1 d . . . N6 N 0.2501(2) -0.0993(3) 0.0892(2) 0.0310(17) Uani 1 1 d . . . N7 N 0.3262(2) -0.0388(4) 0.1829(2) 0.0389(18) Uani 1 1 d . . . N8 N 0.3515(2) 0.0771(3) 0.1901(2) 0.0279(16) Uani 1 1 d . . . N9 N 0.3959(2) 0.2083(3) 0.2106(2) 0.0270(16) Uani 1 1 d . . . N10 N 0.3812(2) 0.2892(4) 0.2561(2) 0.0385(19) Uani 1 1 d D . . N11 N 0.2982(3) 0.3918(4) 0.2184(2) 0.0369(19) Uani 1 1 d . . . N12 N 0.2242(2) 0.3519(3) 0.1711(2) 0.0297(17) Uani 1 1 d . . . N13 N 0.3501(2) 0.4210(3) 0.04866(19) 0.0223(15) Uani 1 1 d . . . N14 N 0.28608(19) 0.4720(3) 0.03577(19) 0.0226(15) Uani 1 1 d . . . N15 N 0.2578(2) 0.5637(3) 0.0724(2) 0.0276(16) Uani 1 1 d . . . N16 N 0.3245(2) 0.5667(4) 0.1409(2) 0.0395(19) Uani 1 1 d D . . N17 N 0.4212(2) 0.5200(4) 0.1480(2) 0.044(2) Uani 1 1 d . . . N18 N 0.4309(2) 0.4249(3) 0.1081(2) 0.0278(16) Uani 1 1 d . . . N19 N 0.45571(19) 0.3260(3) 0.0575(2) 0.0235(15) Uani 1 1 d . . . N20 N 0.5030(3) 0.2333(4) 0.0949(3) 0.047(2) Uani 1 1 d D . . N21 N 0.4725(2) 0.0991(4) 0.1304(3) 0.047(2) Uani 1 1 d . . . N22 N 0.4212(2) 0.1024(3) 0.16306(19) 0.0236(15) Uani 1 1 d . . . N23 N 0.3953(2) 0.2956(3) 0.08261(19) 0.0212(15) Uani 1 1 d . . . N24 N 0.3812(2) 0.2120(3) 0.12012(19) 0.0220(15) Uani 1 1 d . . . N25 N 0.36829(19) 0.3339(3) -0.00783(19) 0.0211(15) Uani 1 1 d . . . N26 N 0.3361(2) 0.2717(3) -0.0698(2) 0.0258(16) Uani 1 1 d . . . N27 N 0.3152(2) 0.2843(3) -0.1541(2) 0.0269(16) Uani 1 1 d . . . N28 N 0.3550(2) 0.3904(4) -0.1455(2) 0.0405(19) Uani 1 1 d . . . N29 N 0.3799(2) 0.4929(4) -0.0601(2) 0.0397(19) Uani 1 1 d D . . N30 N 0.4092(2) 0.4503(3) 0.0149(2) 0.0249(15) Uani 1 1 d . . . N31 N 0.2071(2) 0.4456(3) 0.0418(2) 0.0234(15) Uani 1 1 d . . . N32 N 0.1939(2) 0.3638(3) 0.0805(2) 0.0245(15) Uani 1 1 d . . . N33 N 0.1336(2) 0.3320(4) 0.1048(2) 0.0296(17) Uani 1 1 d . . . N34 N 0.0894(4) 0.4303(7) 0.0714(5) 0.134(6) Uani 1 1 d . . . N35 N 0.1004(3) 0.5339(5) 0.0012(4) 0.073(3) Uani 1 1 d D . . N36 N 0.1688(2) 0.5544(3) -0.0015(2) 0.0308(17) Uani 1 1 d . . . O1 O -0.0027(6) 0.2020(9) 0.3213(6) 0.103(5) Uiso 0.55 1 d P . . O6 O 0.5838(4) 0.4549(6) 0.1642(4) 0.116(3) Uiso 1 1 d . . . O8 O 0.6809(5) 0.2230(8) 0.2030(5) 0.093(4) Uiso 0.70 1 d P . . O9 O 0.6720(5) 0.2135(8) 0.1760(6) 0.107(4) Uiso 0.78 1 d P . . O10 O 0.6624(7) 0.1345(12) 0.1468(8) 0.121(7) Uiso 0.50 1 d P . . O11 O 0.6370(7) 0.2561(12) 0.0742(8) 0.117(7) Uiso 0.50 1 d P . . O13 O 0.5764(4) 0.0833(7) 0.0731(4) 0.091(4) Uiso 0.70 1 d P . . O14 O 0.5902(11) 0.0388(17) 0.1125(10) 0.086(9) Uiso 0.30 1 d P . . O16 O 0.8181(6) 0.3002(9) 0.1853(6) 0.118(6) Uiso 0.70 1 d P . . O17 O 0.8840(8) 0.2579(13) 0.2639(8) 0.038(5) Uiso 0.30 1 d P . . O18 O 0.9093(14) 0.291(2) 0.2796(13) 0.070(11) Uiso 0.20 1 d P . . O29 O 0.6333(4) 0.1911(8) 0.0668(5) 0.095(4) Uiso 0.70 1 d P . . O101 O 0.5457(4) 0.5680(7) 0.1047(4) 0.109(4) Uiso 1 1 d . . . O102 O 0.6431(6) 0.3550(10) 0.1452(6) 0.139(6) Uiso 0.70 1 d P . . O103 O 0.8377(9) 0.2742(13) 0.2125(9) 0.059(6) Uiso 0.30 1 d P . . O104 O -0.0553(13) 0.366(2) 0.2184(19) 0.121(15) Uiso 0.30 1 d P . . O107 O 0.4925(5) 0.0629(8) 0.0468(5) 0.089(5) Uiso 0.70 1 d P . . O108 O -0.0594(10) 0.3532(18) 0.1938(13) 0.164(11) Uiso 0.60 1 d P . . O109 O 0.6498(15) 0.254(3) 0.1504(16) 0.094(13) Uiso 0.20 1 d P . . O110 O 0.0086(6) 0.1701(10) 0.4062(6) 0.232(8) Uiso 1 1 d . . . O111 O 0.5561(9) 0.5225(17) 0.1143(12) 0.018(7) Uiso 0.20 1 d P . . O112 O 0.7520(4) 0.3222(5) 0.2025(3) 0.100(3) Uiso 1 1 d . . . O200 O 0.8817(7) 0.9321(13) 0.2022(8) 0.014(6) Uiso 0.20 1 d P . . O203 O 0.921(2) 0.060(3) 0.273(2) 0.130(19) Uiso 0.20 1 d P . . O205 O 0.6352(6) 0.3750(10) 0.1683(7) 0.095(6) Uiso 0.50 1 d P . . O300 O -0.034(4) 0.313(6) 0.197(4) 0.24(4) Uiso 0.20 1 d P . . O301 O 0.010(2) 0.307(3) 0.345(2) 0.24(3) Uiso 0.30 1 d P . . O302 O 0.910(2) 0.232(3) 0.264(2) 0.21(2) Uiso 0.30 1 d P . . O303 O 0.112(2) 0.181(3) 0.391(2) 0.15(2) Uiso 0.20 1 d P . . O304 O 0.6260(10) 0.2261(19) 0.0478(11) 0.043(8) Uiso 0.20 1 d P . . O305 O 0.6507(15) 0.137(3) 0.1119(18) 0.098(14) Uiso 0.20 1 d P . . O400 O 0.8550(4) 0.3383(6) 0.1383(4) 0.131(4) Uiso 1 1 d . . . O401 O -0.0358(3) 0.3553(4) 0.2977(4) 0.092(3) Uani 1 1 d . . . O555 O 0.4889(16) 0.031(3) 0.0153(16) 0.025(12) Uiso 0.10 1 d P . . O556 O 0.6008(14) 0.420(2) 0.1683(13) 0.006(10) Uiso 0.10 1 d P . . O558 O 0.013(2) 0.225(4) 0.428(2) 0.055(18) Uiso 0.10 1 d P . . O559 O 0.6936(13) 0.267(2) 0.2084(13) 0.005(9) Uiso 0.10 1 d P . . O560 O 0.954(5) 0.187(8) 0.243(5) 0.19(6) Uiso 0.10 1 d P . . O561 O 0.9344(17) 0.103(3) 0.2899(18) 0.026(13) Uiso 0.10 1 d P . . O562 O -0.051(2) 0.376(4) 0.254(3) 0.062(19) Uiso 0.10 1 d P . . O563 O 0.051(3) 0.209(5) 0.323(3) 0.08(2) Uiso 0.10 1 d P . . O564 O 0.5528(6) 0.5518(10) 0.0897(6) 0.019(4) Uiso 0.30 1 d P . . O600 O -0.040(2) 0.181(4) 0.325(2) 0.17(2) Uiso 0.20 1 d P . . O601 O 0.777(2) 0.311(4) 0.194(2) 0.054(18) Uiso 0.10 1 d P . . O602 O 0.679(3) 0.417(4) 0.141(3) 0.08(2) Uiso 0.10 1 d P . . O604 O 0.829(2) 0.308(3) 0.168(2) 0.040(16) Uiso 0.10 1 d P . . O605 O 0.566(2) 0.063(3) 0.099(2) 0.13(2) Uiso 0.20 1 d P . . O606 O 0.876(3) 0.276(5) 0.243(4) 0.19(4) Uiso 0.20 1 d P . . O607 O -0.062(5) 0.369(7) 0.161(5) 0.31(7) Uiso 0.20 1 d P . . O701 O 0.102(3) 0.810(5) 0.960(3) 0.07(3) Uiso 0.10 1 d P . . O702 O 0.5624(18) 0.505(3) 0.133(2) 0.028(17) Uiso 0.10 1 d P . . O703 O 0.725(3) 0.280(5) 0.197(3) 0.08(2) Uiso 0.10 1 d P . . O704 O 0.036(2) 0.228(4) 0.379(2) 0.16(2) Uiso 0.20 1 d P . . O705 O -0.044(3) 0.158(5) 0.362(3) 0.02(2) Uiso 0.05 1 d P . . H101 H 0.327(3) 0.392(4) 0.221(2) 0.025 Uiso 1 1 d . . . H102 H 0.3589(17) 0.292(4) 0.263(2) 0.025 Uiso 1 1 d D . . H103 H 0.508(2) 0.198(2) 0.113(2) 0.025 Uiso 1 1 d D . . H202 H 0.085(2) 0.496(2) -0.002(2) 0.025 Uiso 1 1 d D . . H200 H 0.3485(15) 0.543(3) 0.158(2) 0.025 Uiso 1 1 d D . . H201 H 0.3564(15) 0.493(4) -0.0863(12) 0.025 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0241(7) 0.0222(8) 0.0190(7) 0.0004(6) 0.0075(5) -0.0025(6) Co2 0.0241(7) 0.0204(8) 0.0223(7) -0.0003(6) 0.0077(5) 0.0010(5) Co3 0.0218(7) 0.0210(8) 0.0213(7) 0.0020(6) 0.0064(5) -0.0002(5) Co4 0.0247(7) 0.0298(8) 0.0214(7) 0.0004(6) 0.0106(5) -0.0006(6) C1 0.025(5) 0.019(5) 0.027(5) 0.001(4) 0.013(3) -0.001(4) C2 0.033(5) 0.028(5) 0.026(5) -0.003(4) 0.017(4) -0.001(4) C3 0.024(5) 0.021(5) 0.027(5) -0.003(4) 0.010(4) -0.001(4) C4 0.023(5) 0.023(5) 0.033(5) -0.002(4) 0.009(4) -0.001(4) C5 0.036(6) 0.030(6) 0.055(6) 0.004(5) 0.021(4) -0.010(4) C6 0.057(6) 0.019(5) 0.035(5) -0.005(4) 0.017(4) -0.006(4) C7 0.045(5) 0.023(5) 0.030(5) -0.003(4) 0.013(4) -0.004(4) C8 0.031(5) 0.037(6) 0.027(5) 0.003(4) 0.019(4) -0.001(4) C9 0.052(6) 0.029(5) 0.023(5) -0.003(4) 0.020(4) -0.011(4) C10 0.078(8) 0.055(7) 0.037(6) -0.001(5) 0.026(5) -0.024(6) C11 0.102(9) 0.045(7) 0.032(6) 0.003(5) 0.030(5) -0.021(6) C12 0.031(5) 0.020(5) 0.018(4) 0.005(4) 0.009(4) 0.000(4) C13 0.030(5) 0.021(5) 0.021(4) 0.000(4) 0.015(4) 0.003(4) C14 0.027(5) 0.029(5) 0.022(4) 0.001(4) 0.009(4) -0.003(4) C15 0.032(6) 0.038(6) 0.018(4) -0.003(4) 0.011(4) -0.001(4) C16 0.042(6) 0.049(6) 0.028(5) -0.012(4) 0.014(4) 0.001(5) C17 0.047(6) 0.037(6) 0.047(6) -0.015(5) 0.021(5) -0.004(5) C18 0.056(6) 0.040(6) 0.036(5) -0.013(5) 0.023(5) 0.004(5) C19 0.028(5) 0.026(5) 0.029(5) -0.005(4) 0.010(4) -0.003(4) C20 0.029(5) 0.034(6) 0.034(5) -0.005(4) 0.009(4) 0.001(4) C21 0.023(5) 0.057(7) 0.037(5) -0.020(5) 0.002(4) -0.005(4) C22 0.032(6) 0.068(8) 0.042(6) -0.024(5) -0.007(4) 0.005(5) C23 0.028(5) 0.019(5) 0.022(4) -0.002(4) 0.009(4) 0.002(4) C24 0.025(5) 0.021(5) 0.022(4) -0.001(4) 0.008(3) 0.005(4) C25 0.029(5) 0.026(5) 0.021(4) -0.001(4) 0.007(3) -0.005(4) C26 0.030(5) 0.019(5) 0.026(5) -0.001(4) 0.012(4) 0.003(4) C27 0.035(5) 0.033(5) 0.029(5) -0.006(4) 0.015(4) 0.011(4) C28 0.046(6) 0.031(6) 0.048(6) -0.010(5) 0.019(4) 0.002(4) C29 0.049(6) 0.043(6) 0.034(5) -0.010(5) 0.012(4) 0.003(5) C30 0.024(5) 0.033(6) 0.028(5) 0.005(4) 0.004(4) 0.001(4) C31 0.032(6) 0.059(7) 0.042(6) -0.023(5) -0.003(4) -0.003(5) C32 0.029(5) 0.051(7) 0.030(5) -0.008(5) 0.000(4) 0.003(4) C33 0.016(5) 0.034(6) 0.042(5) 0.001(4) 0.002(4) -0.001(4) C34 0.028(5) 0.031(5) 0.025(5) -0.002(4) 0.014(4) 0.000(4) C35 0.034(5) 0.028(5) 0.034(5) 0.005(4) 0.012(4) -0.007(4) C36 0.059(7) 0.031(6) 0.044(6) 0.006(5) 0.022(5) -0.009(5) C37 0.048(6) 0.027(6) 0.045(6) 0.014(4) 0.010(4) -0.003(4) C38 0.020(4) 0.029(5) 0.025(5) -0.002(4) 0.009(3) -0.001(4) C39 0.023(5) 0.022(5) 0.026(5) 0.003(4) 0.007(3) 0.002(4) C40 0.024(5) 0.030(5) 0.020(5) 0.001(4) 0.013(3) -0.003(4) C41 0.025(5) 0.042(6) 0.025(5) 0.004(4) 0.012(4) 0.006(4) C42 0.087(8) 0.042(7) 0.040(6) 0.002(5) 0.034(5) -0.010(6) C43 0.076(8) 0.061(8) 0.027(5) 0.006(5) 0.013(5) -0.009(6) C44 0.046(6) 0.047(6) 0.022(5) 0.004(4) 0.017(4) -0.009(4) C45 0.021(4) 0.013(5) 0.020(4) -0.003(4) 0.007(3) 0.004(3) C46 0.022(5) 0.035(5) 0.031(5) 0.005(4) 0.018(4) 0.005(4) C47 0.027(5) 0.030(5) 0.024(4) -0.006(4) 0.006(3) 0.007(4) C48 0.042(6) 0.031(6) 0.046(6) 0.000(5) 0.021(5) 0.001(5) C49 0.035(5) 0.029(5) 0.038(5) 0.005(4) 0.012(4) 0.003(4) C50 0.036(7) 0.068(9) 0.136(12) 0.043(8) 0.000(7) -0.001(6) C51 0.047(8) 0.081(10) 0.238(19) 0.101(12) 0.068(10) 0.037(7) C52 0.144(16) 0.26(3) 0.34(3) 0.24(2) 0.210(19) 0.157(17) C53 0.099(12) 0.085(11) 0.24(2) 0.080(13) 0.122(13) 0.039(9) C54 0.036(6) 0.070(8) 0.061(7) 0.022(6) 0.030(5) 0.016(5) C55 0.023(5) 0.014(5) 0.020(4) -0.001(4) 0.009(3) 0.000(3) C56 0.025(5) 0.029(5) 0.027(5) 0.000(4) 0.010(4) -0.011(4) C57 0.028(5) 0.018(5) 0.021(4) 0.002(4) 0.005(3) 0.003(4) C58 0.029(5) 0.031(5) 0.027(5) 0.006(4) 0.011(4) 0.007(4) C59 0.053(7) 0.077(9) 0.060(7) 0.012(6) 0.030(5) 0.012(6) C60 0.023(5) 0.035(6) 0.048(5) 0.012(5) 0.011(4) 0.000(4) C61 0.049(7) 0.054(7) 0.064(7) 0.019(6) 0.021(5) 0.014(5) C62 0.026(5) 0.033(6) 0.033(5) 0.003(4) 0.014(4) 0.010(4) C63 0.024(5) 0.038(6) 0.047(5) 0.009(4) 0.020(4) 0.005(4) C64 0.059(7) 0.056(7) 0.078(8) 0.022(6) 0.046(6) 0.010(6) C65 0.047(7) 0.082(9) 0.082(8) 0.038(7) 0.048(6) 0.019(6) C086 0.037(6) 0.065(8) 0.045(6) 0.016(5) 0.023(4) 0.018(5) Cl1 0.0510(18) 0.117(3) 0.078(2) 0.040(2) 0.0148(14) 0.0024(17) Cl2 0.0624(18) 0.088(2) 0.0438(14) 0.0014(14) 0.0222(12) 0.0163(16) Cl3 0.079(4) 0.064(4) 0.078(4) -0.018(3) 0.029(3) 0.006(3) Cl4 0.076(4) 0.065(4) 0.040(3) -0.022(3) 0.031(3) -0.035(3) Cl5 0.168(7) 0.187(8) 0.134(6) 0.054(5) 0.060(5) 0.014(6) Cl6 0.134(6) 0.303(12) 0.192(7) -0.095(8) 0.027(5) 0.042(7) Cl9 0.115(9) 0.166(12) 0.139(10) -0.002(9) 0.048(7) -0.002(8) Cl11 0.0439(19) 0.0363(19) 0.0419(18) -0.0007(15) 0.0198(14) -0.0021(14) Cl12 0.158(9) 0.118(8) 0.165(9) -0.013(7) 0.074(7) -0.031(7) N1 0.025(4) 0.022(4) 0.019(4) 0.007(3) 0.009(3) -0.003(3) N2 0.024(4) 0.025(4) 0.023(4) 0.000(3) 0.011(3) -0.003(3) N3 0.018(4) 0.031(4) 0.020(3) -0.001(3) 0.007(3) 0.002(3) N4 0.029(4) 0.021(4) 0.016(3) 0.003(3) 0.006(3) 0.000(3) N5 0.035(4) 0.015(4) 0.021(4) -0.001(3) 0.007(3) 0.001(3) N6 0.032(4) 0.026(4) 0.035(4) -0.002(3) 0.015(3) -0.010(3) N7 0.054(5) 0.034(5) 0.028(4) 0.004(3) 0.018(3) -0.010(4) N8 0.035(4) 0.028(4) 0.018(4) 0.000(3) 0.010(3) 0.000(3) N9 0.027(4) 0.021(4) 0.025(4) 0.000(3) 0.004(3) -0.002(3) N10 0.029(5) 0.057(5) 0.023(4) -0.019(4) 0.006(3) 0.001(4) N11 0.034(4) 0.045(5) 0.028(4) -0.013(4) 0.009(3) 0.004(4) N12 0.043(5) 0.023(4) 0.025(4) -0.006(3) 0.016(3) 0.001(3) N13 0.022(4) 0.023(4) 0.019(3) 0.001(3) 0.007(3) 0.002(3) N14 0.024(4) 0.024(4) 0.020(3) -0.001(3) 0.009(3) -0.001(3) N15 0.036(5) 0.029(4) 0.016(3) -0.002(3) 0.009(3) -0.003(3) N16 0.033(5) 0.042(5) 0.034(4) -0.015(4) 0.005(3) 0.010(4) N17 0.033(4) 0.051(5) 0.031(4) -0.019(4) -0.001(3) -0.005(4) N18 0.021(4) 0.024(4) 0.025(4) -0.002(3) -0.003(3) 0.001(3) N19 0.020(4) 0.025(4) 0.024(3) 0.009(3) 0.009(3) 0.005(3) N20 0.051(5) 0.036(5) 0.067(6) 0.030(4) 0.037(4) 0.016(4) N21 0.047(5) 0.035(5) 0.072(6) 0.021(4) 0.038(4) 0.017(4) N22 0.031(4) 0.025(4) 0.018(3) 0.002(3) 0.014(3) 0.002(3) N23 0.027(4) 0.014(4) 0.019(3) 0.004(3) 0.007(3) 0.005(3) N24 0.025(4) 0.027(4) 0.015(3) 0.001(3) 0.010(3) -0.005(3) N25 0.024(4) 0.021(4) 0.017(3) 0.007(3) 0.008(3) 0.005(3) N26 0.025(4) 0.025(4) 0.029(4) 0.001(3) 0.013(3) -0.004(3) N27 0.026(4) 0.031(4) 0.023(4) 0.006(3) 0.010(3) -0.002(3) N28 0.060(5) 0.038(5) 0.033(4) 0.005(4) 0.029(4) -0.011(4) N29 0.050(5) 0.034(5) 0.025(4) 0.010(4) 0.007(3) -0.003(4) N30 0.025(4) 0.020(4) 0.025(4) 0.005(3) 0.008(3) -0.001(3) N31 0.029(4) 0.017(4) 0.022(3) -0.007(3) 0.010(3) -0.001(3) N32 0.023(4) 0.021(4) 0.028(4) -0.001(3) 0.009(3) 0.000(3) N33 0.023(4) 0.044(5) 0.030(4) 0.005(4) 0.019(3) 0.005(3) N34 0.088(8) 0.175(13) 0.196(13) 0.140(11) 0.113(9) 0.090(9) N35 0.028(5) 0.044(6) 0.156(9) 0.054(6) 0.046(5) 0.014(4) N36 0.032(4) 0.024(4) 0.029(4) 0.004(3) 0.007(3) 0.000(3) O401 0.092(6) 0.053(5) 0.135(8) -0.019(5) 0.053(6) -0.018(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 Co1 N1 1.895(6) . ? Co1 N3 1.904(6) . ? Co1 N24 1.917(6) . ? Co1 N8 1.949(7) . ? Co1 N9 1.958(6) . ? Co1 N22 1.959(6) . ? Co2 N31 1.903(6) . ? Co2 N14 1.904(6) . ? Co2 N2 1.910(6) 7 ? Co2 N15 1.946(6) . ? Co2 N5 1.948(6) 7 ? Co2 N36 1.955(7) . ? Co3 N13 1.892(6) . ? Co3 N23 1.904(6) . ? Co3 N25 1.910(6) . ? Co3 N18 1.941(6) . ? Co3 N19 1.942(6) . ? Co3 N30 1.955(6) . ? Co4 N32 1.895(6) . ? Co4 N26 1.895(6) 7 ? Co4 N4 1.896(6) . ? Co4 N27 1.934(6) 7 ? Co4 N33 1.937(6) . ? Co4 N12 1.951(6) . ? C1 N1 1.333(9) . ? C1 N2 1.342(9) . ? C2 C3 1.369(10) . ? C2 N1 1.382(10) . ? C2 C8 1.473(11) . ? C3 N2 1.357(9) . ? C3 C4 1.466(11) . ? C4 N5 1.305(10) . ? C4 N6 1.342(10) . ? C5 N6 1.469(10) . ? C5 C6 1.513(12) . ? C6 C7 1.516(11) . ? C7 N5 1.463(10) . ? C8 N8 1.303(10) . ? C8 N7 1.338(10) . ? C9 N8 1.464(10) . ? C9 C10 1.507(12) . ? C10 C11 1.522(14) . ? C11 N7 1.453(11) . ? C12 N3 1.346(9) . ? C12 N4 1.351(10) . ? C13 N4 1.368(9) . ? C13 C14 1.370(11) . ? C13 C15 1.438(11) . ? C14 N3 1.375(10) . ? C14 C19 1.467(11) . ? C15 N12 1.319(10) . ? C15 N11 1.350(10) . ? C16 N12 1.466(10) . ? C16 C17 1.528(12) . ? C17 C18 1.510(12) . ? C18 N11 1.459(11) . ? C19 N9 1.306(10) . ? C19 N10 1.335(10) . ? C20 N9 1.463(10) . ? C20 C21 1.513(11) . ? C21 C22 1.497(13) . ? C22 N10 1.450(10) . ? C23 N14 1.326(9) . ? C23 N13 1.338(9) . ? C24 N14 1.355(9) . ? C24 C25 1.396(11) . ? C24 C26 1.439(11) . ? C25 N13 1.375(9) . ? C25 C30 1.471(11) . ? C26 N15 1.309(9) . ? C26 N16 1.339(10) . ? C27 N15 1.460(10) . ? C27 C28 1.521(11) . ? C28 C29 1.508(12) . ? C29 N16 1.450(11) . ? C30 N18 1.308(10) . ? C30 N17 1.326(10) . ? C31 C32 1.472(12) . ? C31 N17 1.491(10) . ? C32 C33 1.493(11) . ? C33 N18 1.479(9) . ? C34 N30 1.329(9) . ? C34 N29 1.330(10) . ? C34 C38 1.449(11) . ? C35 N30 1.451(10) . ? C35 C36 1.517(12) . ? C36 C37 1.501(12) . ? C37 N29 1.463(11) . ? C38 N25 1.369(9) . ? C38 C39 1.380(10) . ? C39 N26 1.364(10) . ? C39 C41 1.472(11) . ? C40 N25 1.330(10) . ? C40 N26 1.335(9) . ? C41 N27 1.305(10) . ? C41 N28 1.350(10) . ? C42 N28 1.463(11) . ? C42 C43 1.488(13) . ? C43 C44 1.511(12) . ? C44 N27 1.463(10) . ? C45 N32 1.326(9) . ? C45 N31 1.333(9) . ? C46 C47 1.348(11) . ? C46 N32 1.375(10) . ? C46 C086 1.455(12) . ? C47 N31 1.375(10) . ? C47 C48 1.457(12) . ? C48 N36 1.306(11) . ? C48 N35 1.337(11) . ? C49 N36 1.483(10) . ? C49 C50 1.506(13) . ? C50 C51 1.471(19) . ? C51 N35 1.449(13) . ? C52 C53 1.272(19) . ? C52 N34 1.490(16) . ? C53 C54 1.492(15) . ? C54 N33 1.470(11) . ? C55 N24 1.322(9) . ? C55 N23 1.332(9) . ? C56 N23 1.369(10) . ? C56 C57 1.375(11) . ? C56 C62 1.476(11) . ? C57 N24 1.374(10) . ? C57 C58 1.452(11) . ? C58 N22 1.294(10) . ? C58 N21 1.361(10) . ? C59 N21 1.470(12) . ? C59 C61 1.470(13) . ? C60 N22 1.461(10) . ? C60 C61 1.515(12) . ? C62 N19 1.296(10) . ? C62 N20 1.332(10) . ? C63 N19 1.467(10) . ? C63 C64 1.499(12) . ? C64 C65 1.469(13) . ? C65 N20 1.483(11) . ? C086 N33 1.311(11) . ? C086 N34 1.319(13) . ? Cl2 O602 1.35(8) . ? Cl3 O701 0.77(9) . ? Cl4 O107 0.905(13) . ? Cl4 O555 1.59(5) . ? Cl9 O561 1.25(5) . ? Cl9 O560 1.56(16) . ? Cl12 O563 1.29(9) . ? N2 Co2 1.910(6) 7 ? N5 Co2 1.948(6) 7 ? N26 Co4 1.895(6) 7 ? N27 Co4 1.934(6) 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 N1 Co1 N3 93.5(3) . . ? N1 Co1 N24 92.4(3) . . ? N3 Co1 N24 92.9(3) . . ? N1 Co1 N8 82.8(3) . . ? N3 Co1 N8 91.3(3) . . ? N24 Co1 N8 173.8(3) . . ? N1 Co1 N9 174.4(3) . . ? N3 Co1 N9 82.3(3) . . ? N24 Co1 N9 91.5(3) . . ? N8 Co1 N9 93.6(3) . . ? N1 Co1 N22 89.1(3) . . ? N3 Co1 N22 174.8(3) . . ? N24 Co1 N22 82.5(3) . . ? N8 Co1 N22 93.5(3) . . ? N9 Co1 N22 95.4(3) . . ? N31 Co2 N14 92.4(3) . . ? N31 Co2 N2 92.9(3) . 7 ? N14 Co2 N2 93.2(3) . 7 ? N31 Co2 N15 90.7(3) . . ? N14 Co2 N15 82.1(3) . . ? N2 Co2 N15 174.3(3) 7 . ? N31 Co2 N5 174.4(3) . 7 ? N14 Co2 N5 90.1(3) . 7 ? N2 Co2 N5 81.9(3) 7 7 ? N15 Co2 N5 94.6(3) . 7 ? N31 Co2 N36 82.0(3) . . ? N14 Co2 N36 173.6(3) . . ? N2 Co2 N36 90.2(3) 7 . ? N15 Co2 N36 94.8(3) . . ? N5 Co2 N36 95.7(3) 7 . ? N13 Co3 N23 94.9(3) . . ? N13 Co3 N25 92.5(3) . . ? N23 Co3 N25 93.7(3) . . ? N13 Co3 N18 82.0(3) . . ? N23 Co3 N18 90.1(3) . . ? N25 Co3 N18 173.6(3) . . ? N13 Co3 N19 176.2(3) . . ? N23 Co3 N19 82.5(3) . . ? N25 Co3 N19 90.5(3) . . ? N18 Co3 N19 95.2(3) . . ? N13 Co3 N30 88.6(3) . . ? N23 Co3 N30 175.0(3) . . ? N25 Co3 N30 82.6(3) . . ? N18 Co3 N30 93.9(3) . . ? N19 Co3 N30 94.1(3) . . ? N32 Co4 N26 93.3(3) . 7 ? N32 Co4 N4 93.6(3) . . ? N26 Co4 N4 93.6(3) 7 . ? N32 Co4 N27 175.2(3) . 7 ? N26 Co4 N27 83.0(3) 7 7 ? N4 Co4 N27 89.9(3) . 7 ? N32 Co4 N33 82.3(3) . . ? N26 Co4 N33 89.7(3) 7 . ? N4 Co4 N33 174.9(3) . . ? N27 Co4 N33 94.4(3) 7 . ? N32 Co4 N12 88.5(3) . . ? N26 Co4 N12 176.1(3) 7 . ? N4 Co4 N12 82.8(3) . . ? N27 Co4 N12 95.3(3) 7 . ? N33 Co4 N12 94.0(3) . . ? N1 C1 N2 110.6(7) . . ? C3 C2 N1 107.3(6) . . ? C3 C2 C8 139.7(8) . . ? N1 C2 C8 112.9(7) . . ? N2 C3 C2 108.0(7) . . ? N2 C3 C4 113.6(6) . . ? C2 C3 C4 138.4(8) . . ? N5 C4 N6 126.9(7) . . ? N5 C4 C3 112.7(7) . . ? N6 C4 C3 120.3(7) . . ? N6 C5 C6 109.7(7) . . ? C5 C6 C7 110.7(7) . . ? N5 C7 C6 111.1(6) . . ? N8 C8 N7 126.4(7) . . ? N8 C8 C2 113.6(7) . . ? N7 C8 C2 120.0(8) . . ? N8 C9 C10 111.2(7) . . ? C9 C10 C11 110.7(8) . . ? N7 C11 C10 107.4(8) . . ? N3 C12 N4 110.9(7) . . ? N4 C13 C14 108.1(7) . . ? N4 C13 C15 113.7(7) . . ? C14 C13 C15 138.2(7) . . ? C13 C14 N3 108.1(6) . . ? C13 C14 C19 139.1(8) . . ? N3 C14 C19 112.8(7) . . ? N12 C15 N11 125.2(8) . . ? N12 C15 C13 113.7(7) . . ? N11 C15 C13 121.1(8) . . ? N12 C16 C17 110.4(7) . . ? C18 C17 C16 107.9(8) . . ? N11 C18 C17 110.4(7) . . ? N9 C19 N10 125.5(7) . . ? N9 C19 C14 114.1(7) . . ? N10 C19 C14 120.4(7) . . ? N9 C20 C21 110.6(7) . . ? C22 C21 C20 109.8(8) . . ? N10 C22 C21 108.7(7) . . ? N14 C23 N13 111.1(6) . . ? N14 C24 C25 106.5(6) . . ? N14 C24 C26 114.6(7) . . ? C25 C24 C26 138.9(7) . . ? N13 C25 C24 107.6(6) . . ? N13 C25 C30 113.0(7) . . ? C24 C25 C30 139.4(8) . . ? N15 C26 N16 125.1(7) . . ? N15 C26 C24 113.3(7) . . ? N16 C26 C24 121.5(7) . . ? N15 C27 C28 112.0(7) . . ? C29 C28 C27 110.4(7) . . ? N16 C29 C28 109.8(7) . . ? N18 C30 N17 126.3(7) . . ? N18 C30 C25 112.6(7) . . ? N17 C30 C25 120.9(8) . . ? C32 C31 N17 109.5(7) . . ? C31 C32 C33 110.0(7) . . ? N18 C33 C32 111.4(7) . . ? N30 C34 N29 124.1(7) . . ? N30 C34 C38 112.9(7) . . ? N29 C34 C38 123.0(7) . . ? N30 C35 C36 110.1(7) . . ? C37 C36 C35 109.8(8) . . ? N29 C37 C36 108.5(7) . . ? N25 C38 C39 106.9(7) . . ? N25 C38 C34 114.6(6) . . ? C39 C38 C34 138.5(7) . . ? N26 C39 C38 107.3(7) . . ? N26 C39 C41 113.7(7) . . ? C38 C39 C41 139.0(8) . . ? N25 C40 N26 110.0(7) . . ? N27 C41 N28 126.9(7) . . ? N27 C41 C39 113.0(7) . . ? N28 C41 C39 120.0(8) . . ? N28 C42 C43 108.9(8) . . ? C42 C43 C44 110.8(8) . . ? N27 C44 C43 110.4(7) . . ? N32 C45 N31 110.1(7) . . ? C47 C46 N32 107.7(7) . . ? C47 C46 C086 139.8(8) . . ? N32 C46 C086 112.4(7) . . ? C46 C47 N31 107.6(7) . . ? C46 C47 C48 140.3(8) . . ? N31 C47 C48 112.1(8) . . ? N36 C48 N35 123.7(8) . . ? N36 C48 C47 115.0(8) . . ? N35 C48 C47 121.2(8) . . ? N36 C49 C50 110.3(7) . . ? C51 C50 C49 110.6(11) . . ? N35 C51 C50 111.0(10) . . ? C53 C52 N34 115.1(13) . . ? C52 C53 C54 123.4(13) . . ? N33 C54 C53 111.9(9) . . ? N24 C55 N23 111.5(7) . . ? N23 C56 C57 107.8(7) . . ? N23 C56 C62 112.9(7) . . ? C57 C56 C62 139.2(8) . . ? N24 C57 C56 106.9(7) . . ? N24 C57 C58 113.6(7) . . ? C56 C57 C58 139.4(8) . . ? N22 C58 N21 126.1(7) . . ? N22 C58 C57 114.6(7) . . ? N21 C58 C57 119.3(7) . . ? N21 C59 C61 109.2(9) . . ? N22 C60 C61 111.1(7) . . ? C59 C61 C60 111.6(8) . . ? N19 C62 N20 125.2(7) . . ? N19 C62 C56 113.9(7) . . ? N20 C62 C56 120.8(8) . . ? N19 C63 C64 110.9(7) . . ? C65 C64 C63 112.1(9) . . ? C64 C65 N20 107.4(8) . . ? N33 C086 N34 126.1(9) . . ? N33 C086 C46 114.4(8) . . ? N34 C086 C46 119.3(9) . . ? O107 Cl4 O555 45.6(18) . . ? O561 Cl9 O560 125(6) . . ? C1 N1 C2 106.7(6) . . ? C1 N1 Co1 138.7(5) . . ? C2 N1 Co1 114.5(5) . . ? C1 N2 C3 107.3(6) . . ? C1 N2 Co2 137.7(5) . 7 ? C3 N2 Co2 114.4(5) . 7 ? C12 N3 C14 106.3(6) . . ? C12 N3 Co1 138.6(5) . . ? C14 N3 Co1 115.0(5) . . ? C12 N4 C13 106.6(6) . . ? C12 N4 Co4 138.4(5) . . ? C13 N4 Co4 113.7(5) . . ? C4 N5 C7 118.4(7) . . ? C4 N5 Co2 116.0(5) . 7 ? C7 N5 Co2 124.8(5) . 7 ? C4 N6 C5 119.5(7) . . ? C8 N7 C11 120.0(7) . . ? C8 N8 C9 118.6(7) . . ? C8 N8 Co1 115.3(5) . . ? C9 N8 Co1 125.8(5) . . ? C19 N9 C20 118.4(7) . . ? C19 N9 Co1 115.2(5) . . ? C20 N9 Co1 126.0(5) . . ? C19 N10 C22 120.6(7) . . ? C15 N11 C18 120.5(7) . . ? C15 N12 C16 117.3(7) . . ? C15 N12 Co4 113.9(5) . . ? C16 N12 Co4 127.0(5) . . ? C23 N13 C25 106.3(6) . . ? C23 N13 Co3 138.2(5) . . ? C25 N13 Co3 115.3(5) . . ? C23 N14 C24 108.4(6) . . ? C23 N14 Co2 137.3(5) . . ? C24 N14 Co2 114.0(5) . . ? C26 N15 C27 119.1(6) . . ? C26 N15 Co2 115.2(5) . . ? C27 N15 Co2 125.3(5) . . ? C26 N16 C29 121.2(7) . . ? C30 N17 C31 118.6(7) . . ? C30 N18 C33 117.5(7) . . ? C30 N18 Co3 116.4(5) . . ? C33 N18 Co3 126.0(5) . . ? C62 N19 C63 118.2(6) . . ? C62 N19 Co3 115.7(5) . . ? C63 N19 Co3 126.0(5) . . ? C62 N20 C65 121.2(8) . . ? C58 N21 C59 119.8(7) . . ? C58 N22 C60 118.2(7) . . ? C58 N22 Co1 114.6(5) . . ? C60 N22 Co1 125.6(5) . . ? C55 N23 C56 106.6(6) . . ? C55 N23 Co3 138.7(5) . . ? C56 N23 Co3 114.7(5) . . ? C55 N24 C57 107.1(6) . . ? C55 N24 Co1 139.0(5) . . ? C57 N24 Co1 113.6(5) . . ? C40 N25 C38 108.0(6) . . ? C40 N25 Co3 137.8(5) . . ? C38 N25 Co3 113.8(5) . . ? C40 N26 C39 107.8(6) . . ? C40 N26 Co4 138.1(6) . 7 ? C39 N26 Co4 114.1(5) . 7 ? C41 N27 C44 118.7(7) . . ? C41 N27 Co4 115.2(5) . 7 ? C44 N27 Co4 125.8(5) . 7 ? C41 N28 C42 117.8(7) . . ? C34 N29 C37 121.8(7) . . ? C34 N30 C35 118.7(6) . . ? C34 N30 Co3 114.7(5) . . ? C35 N30 Co3 125.5(5) . . ? C45 N31 C47 107.2(6) . . ? C45 N31 Co2 137.1(5) . . ? C47 N31 Co2 115.5(5) . . ? C45 N32 C46 107.4(6) . . ? C45 N32 Co4 137.1(5) . . ? C46 N32 Co4 115.3(5) . . ? C086 N33 C54 118.4(7) . . ? C086 N33 Co4 115.3(5) . . ? C54 N33 Co4 126.2(6) . . ? C086 N34 C52 118.7(11) . . ? C48 N35 C51 121.4(8) . . ? C48 N36 C49 119.5(7) . . ? C48 N36 Co2 115.0(6) . . ? C49 N36 Co2 125.2(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 55.09 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.531 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.090 # Attachment '- Compound 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 824170' #TrackingRef '- Compound 2.cif' _symmetry_space_group_name_hall '-P 2ac 2ab' #Added by publCIF _audit_update_record ; 2010-04-11 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H88 N32 Ni4 O16' _chemical_formula_weight 1700.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.3775(12) _cell_length_b 17.4940(12) _cell_length_c 24.6892(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7505.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 1.840 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9136 _exptl_absorpt_correction_T_max 0.9136 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23209 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 54.09 _reflns_number_total 3797 _reflns_number_gt 2186 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1250P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3797 _refine_ls_number_parameters 503 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1346 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2018 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Ni1 Ni 0.01731(8) 0.05165(8) 0.32087(5) 0.0384(6) Uani 1 1 d . . . Ni2 Ni 0.24761(8) -0.02143(9) 0.50838(5) 0.0350(5) Uani 1 1 d . . . O1 O 0.3308(3) -0.0170(5) 0.5733(2) 0.0442(18) Uani 1 1 d . . . O2 O 0.2706(4) 0.0857(3) 0.5487(2) 0.0424(18) Uani 1 1 d . . . O3 O 0.3492(4) 0.0903(4) 0.6174(3) 0.074(2) Uani 1 1 d . . . O5 O -0.0205(4) -0.0607(4) 0.2908(2) 0.0515(18) Uani 1 1 d . . . O4 O -0.0616(4) 0.0439(5) 0.2523(2) 0.050(2) Uani 1 1 d . . . O6 O -0.1080(4) -0.0665(4) 0.2274(3) 0.073(2) Uani 1 1 d . . . O7 O 0.5107(4) 0.1924(4) 0.4976(3) 0.064(2) Uani 1 1 d . . . C4 C 0.1763(7) 0.0427(5) 0.2962(3) 0.035(3) Uani 1 1 d . . . C3 C 0.1711(6) 0.0316(5) 0.3571(3) 0.035(3) Uani 1 1 d . . . C7 C 0.1134(5) 0.0688(6) 0.2138(3) 0.046(3) Uani 1 1 d . . . H7A H 0.0718 0.1048 0.2039 0.055 Uiso 1 1 calc R . . H7B H 0.1038 0.0199 0.1947 0.055 Uiso 1 1 calc R . . C12 C 0.1405(5) -0.1183(6) 0.5642(3) 0.035(3) Uani 1 1 d . . . C6 C 0.1918(5) 0.1019(6) 0.1954(3) 0.045(3) Uani 1 1 d . . . H6A H 0.1930 0.1067 0.1555 0.054 Uiso 1 1 calc R . . H6B H 0.1994 0.1534 0.2113 0.054 Uiso 1 1 calc R . . C1 C 0.1069(6) 0.0109(5) 0.4287(3) 0.036(2) Uani 1 1 d . . . H1 H 0.0647 0.0031 0.4525 0.043 Uiso 1 1 calc R . . C17 C -0.1226(5) 0.0087(5) 0.3978(3) 0.028(2) Uani 1 1 d . . . H17 H -0.1266 -0.0441 0.3893 0.034 Uiso 1 1 calc R . . C9 C 0.4150(5) 0.0051(5) 0.4614(3) 0.035(2) Uani 1 1 d . . . H9A H 0.4331 -0.0426 0.4788 0.042 Uiso 1 1 calc R . . H9B H 0.4257 0.0480 0.4865 0.042 Uiso 1 1 calc R . . C13 C 0.1748(6) -0.1653(6) 0.5216(3) 0.038(3) Uani 1 1 d . . . C2 C 0.2225(5) 0.0266(4) 0.3990(4) 0.031(2) Uani 1 1 d . . . C19 C -0.0389(6) 0.1888(7) 0.3707(3) 0.037(3) Uani 1 1 d . . . C10 C 0.4593(5) 0.0177(5) 0.4086(3) 0.042(3) Uani 1 1 d . . . H10A H 0.5143 0.0269 0.4169 0.050 Uiso 1 1 calc R . . H10B H 0.4559 -0.0289 0.3860 0.050 Uiso 1 1 calc R . . C16 C 0.2712(5) -0.1790(6) 0.4534(3) 0.044(3) Uani 1 1 d . . . H16A H 0.3272 -0.1686 0.4538 0.053 Uiso 1 1 calc R . . H16B H 0.2506 -0.1611 0.4183 0.053 Uiso 1 1 calc R . . C14 C 0.1723(5) -0.2798(5) 0.4655(3) 0.044(3) Uani 1 1 d . . . H14A H 0.1446 -0.2651 0.4320 0.053 Uiso 1 1 calc R . . H14B H 0.1634 -0.3349 0.4721 0.053 Uiso 1 1 calc R . . C20 C 0.0673(5) 0.2246(6) 0.3194(4) 0.052(3) Uani 1 1 d . . . H20A H 0.0486 0.2444 0.2842 0.062 Uiso 1 1 calc R . . H20B H 0.1190 0.2024 0.3134 0.062 Uiso 1 1 calc R . . C21 C 0.0740(6) 0.2900(5) 0.3585(3) 0.052(3) Uani 1 1 d . . . H21A H 0.0973 0.2717 0.3927 0.062 Uiso 1 1 calc R . . H21B H 0.1080 0.3298 0.3431 0.062 Uiso 1 1 calc R . . C11 C 0.4282(6) 0.0836(5) 0.3779(3) 0.047(3) Uani 1 1 d . . . H11A H 0.4389 0.1316 0.3978 0.057 Uiso 1 1 calc R . . H11B H 0.4534 0.0867 0.3420 0.057 Uiso 1 1 calc R . . C15 C 0.2579(6) -0.2650(6) 0.4586(4) 0.058(3) Uani 1 1 d . . . H15A H 0.2769 -0.2914 0.4257 0.070 Uiso 1 1 calc R . . H15B H 0.2864 -0.2851 0.4903 0.070 Uiso 1 1 calc R . . C8 C 0.3053(6) 0.0334(5) 0.4081(3) 0.033(3) Uani 1 1 d . . . C22 C -0.0023(6) 0.3228(6) 0.3696(4) 0.054(3) Uani 1 1 d . . . H22A H 0.0012 0.3589 0.4004 0.065 Uiso 1 1 calc R . . H22B H -0.0206 0.3514 0.3375 0.065 Uiso 1 1 calc R . . C5 C 0.2544(5) 0.0492(6) 0.2141(3) 0.045(3) Uani 1 1 d . . . H5A H 0.2509 0.0000 0.1944 0.054 Uiso 1 1 calc R . . H5B H 0.3053 0.0722 0.2065 0.054 Uiso 1 1 calc R . . C18 C 0.0863(5) -0.1279(6) 0.6055(3) 0.034(3) Uani 1 1 d . . . N16 N 0.8328(6) 0.2093(6) 0.7265(3) 0.073(3) Uani 1 1 d . . . O8 O 0.7693(4) 0.2937(5) 0.6728(3) 0.089(3) Uani 1 1 d . . . C27 C 0.7764(9) 0.2360(9) 0.7006(5) 0.094(5) Uani 1 1 d . . . H27 H 0.7311 0.2058 0.7029 0.112 Uiso 1 1 calc R . . C25 C 0.5613(7) 0.2016(7) 0.4625(5) 0.059(3) Uani 1 1 d . . . H25 H 0.5867 0.1571 0.4496 0.071 Uiso 1 1 calc R . . C24 C 0.5505(8) 0.3388(7) 0.4632(6) 0.135(6) Uani 1 1 d . . . H24A H 0.5079 0.3558 0.4402 0.203 Uiso 1 1 calc R . . H24B H 0.5907 0.3782 0.4638 0.203 Uiso 1 1 calc R . . H24C H 0.5317 0.3302 0.5002 0.203 Uiso 1 1 calc R . . C29 C 0.9055(12) 0.2500(11) 0.7179(8) 0.235(12) Uani 1 1 d . . . H29A H 0.8950 0.3044 0.7119 0.353 Uiso 1 1 calc R . . H29B H 0.9318 0.2288 0.6862 0.353 Uiso 1 1 calc R . . H29C H 0.9383 0.2441 0.7499 0.353 Uiso 1 1 calc R . . C23 C 0.6415(6) 0.2723(6) 0.3992(4) 0.088(4) Uani 1 1 d . . . H23A H 0.6632 0.2214 0.3927 0.132 Uiso 1 1 calc R . . H23B H 0.6823 0.3072 0.4107 0.132 Uiso 1 1 calc R . . H23C H 0.6181 0.2914 0.3657 0.132 Uiso 1 1 calc R . . N6 N 0.1122(4) 0.0556(4) 0.2734(2) 0.038(2) Uani 1 1 d . . . N7 N -0.0759(4) 0.0567(5) 0.3721(2) 0.033(2) Uani 1 1 d . . . N12 N 0.1633(4) -0.0428(5) 0.5629(2) 0.0307(19) Uani 1 1 d . . . N3 N 0.3316(4) 0.0001(4) 0.4517(2) 0.0314(19) Uani 1 1 d . . . N4 N 0.3457(5) 0.0738(5) 0.3713(3) 0.044(2) Uani 1 1 d D . . N1 N 0.0977(4) 0.0214(4) 0.3758(2) 0.035(2) Uani 1 1 d . . . N10 N 0.2340(4) -0.1360(4) 0.4977(2) 0.032(2) Uani 1 1 d . . . N8 N 0.0161(4) 0.1652(4) 0.3375(3) 0.037(2) Uani 1 1 d . . . N2 N 0.1799(4) 0.0121(4) 0.4457(2) 0.0327(19) Uani 1 1 d . . . N14 N 0.3184(5) 0.0538(7) 0.5807(3) 0.050(3) Uani 1 1 d . . . N13 N -0.0648(5) -0.0287(7) 0.2559(3) 0.052(3) Uani 1 1 d . . . N11 N 0.1432(4) -0.2352(5) 0.5111(3) 0.043(2) Uani 1 1 d . . . N5 N 0.2453(5) 0.0362(4) 0.2731(2) 0.042(2) Uani 1 1 d D . . N9 N -0.0570(5) 0.2616(6) 0.3827(3) 0.050(3) Uani 1 1 d . . . N15 N 0.5825(5) 0.2675(6) 0.4416(4) 0.077(3) Uani 1 1 d . . . C32 C 0.8348(8) 0.1447(8) 0.7582(6) 0.136(6) Uani 1 1 d . . . H32A H 0.8633 0.1554 0.7916 0.204 Uiso 1 1 calc R . . H32B H 0.8603 0.1034 0.7383 0.204 Uiso 1 1 calc R . . H32C H 0.7821 0.1292 0.7672 0.204 Uiso 1 1 calc R . . H100 H 0.320(7) 0.084(8) 0.341(4) 0.163 Uiso 1 1 d D . . H101 H -0.093(9) 0.273(9) 0.399(6) 0.163 Uiso 1 1 d . . . H102 H 0.099(8) -0.225(8) 0.512(6) 0.163 Uiso 1 1 d . . . H105 H 0.293(6) 0.024(8) 0.294(5) 0.163 Uiso 1 1 d 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 Ni1 0.0314(11) 0.0647(13) 0.0190(7) 0.0003(7) 0.0001(7) 0.0013(8) Ni2 0.0324(11) 0.0533(13) 0.0194(7) 0.0008(7) -0.0003(7) -0.0019(8) O1 0.039(5) 0.065(6) 0.029(3) 0.001(4) -0.008(3) 0.001(4) O2 0.042(5) 0.053(5) 0.033(3) 0.001(3) 0.001(3) -0.004(3) O3 0.080(6) 0.097(7) 0.044(4) -0.017(4) -0.004(4) -0.026(4) O5 0.051(5) 0.066(5) 0.038(4) -0.005(3) -0.002(4) 0.006(4) O4 0.051(5) 0.074(6) 0.024(3) 0.000(4) -0.002(3) 0.007(4) O6 0.049(5) 0.106(7) 0.065(4) -0.043(4) -0.017(4) 0.006(4) O7 0.052(5) 0.076(6) 0.065(5) 0.002(4) 0.001(4) -0.001(4) C4 0.027(8) 0.065(8) 0.013(4) 0.006(4) 0.015(5) -0.001(5) C3 0.032(8) 0.054(8) 0.020(5) 0.004(4) -0.008(5) -0.001(5) C7 0.022(7) 0.096(9) 0.019(4) 0.004(5) 0.003(5) 0.005(5) C12 0.029(7) 0.056(9) 0.020(5) -0.002(5) 0.001(5) 0.001(5) C6 0.039(8) 0.078(9) 0.018(4) 0.003(5) -0.005(5) 0.007(6) C1 0.028(7) 0.059(7) 0.020(5) -0.001(4) -0.002(5) 0.003(5) C17 0.027(7) 0.047(7) 0.011(4) 0.001(4) -0.007(5) -0.003(5) C9 0.027(7) 0.045(7) 0.034(5) -0.005(4) -0.006(5) 0.002(5) C13 0.040(8) 0.047(9) 0.028(5) -0.005(5) 0.008(5) -0.010(6) C2 0.014(7) 0.029(7) 0.049(6) -0.008(5) 0.001(6) 0.000(4) C19 0.038(8) 0.044(9) 0.028(5) 0.013(5) -0.011(5) -0.014(6) C10 0.020(6) 0.053(7) 0.052(6) 0.004(5) 0.013(5) 0.003(5) C16 0.035(7) 0.065(9) 0.033(5) -0.004(5) 0.009(5) 0.011(5) C14 0.018(7) 0.071(8) 0.043(6) -0.005(5) 0.006(5) -0.003(5) C20 0.047(8) 0.058(8) 0.051(6) 0.012(6) 0.010(6) -0.004(6) C21 0.060(9) 0.055(8) 0.041(6) 0.003(5) 0.018(6) -0.015(6) C11 0.051(9) 0.071(9) 0.019(5) 0.010(5) 0.008(5) -0.005(6) C15 0.087(11) 0.040(8) 0.048(6) -0.015(5) -0.004(6) 0.008(6) C8 0.033(8) 0.051(8) 0.015(5) -0.002(5) 0.010(5) -0.007(5) C22 0.056(8) 0.056(9) 0.051(6) 0.014(5) 0.010(6) -0.006(7) C5 0.038(7) 0.078(8) 0.018(4) -0.002(5) 0.000(5) -0.005(6) C18 0.047(7) 0.030(8) 0.025(5) -0.013(5) -0.010(5) 0.012(5) N16 0.082(9) 0.081(9) 0.055(5) 0.037(6) -0.031(6) -0.005(6) O8 0.080(6) 0.108(8) 0.079(5) 0.043(5) -0.001(5) 0.011(5) C27 0.126(14) 0.110(14) 0.045(7) 0.011(8) 0.009(8) 0.027(10) C25 0.050(9) 0.062(10) 0.066(8) -0.021(7) -0.013(7) 0.007(7) C24 0.177(16) 0.053(11) 0.176(14) 0.015(10) 0.089(13) 0.011(10) C29 0.24(2) 0.22(2) 0.24(2) 0.134(17) -0.128(19) -0.169(19) C23 0.081(10) 0.111(11) 0.071(8) -0.020(7) 0.035(7) -0.021(8) N6 0.023(6) 0.072(6) 0.020(4) 0.006(4) -0.005(4) 0.006(4) N7 0.021(5) 0.060(6) 0.017(4) 0.008(4) 0.006(3) 0.002(4) N12 0.032(5) 0.042(6) 0.018(4) -0.004(4) 0.002(4) 0.000(4) N3 0.030(6) 0.050(6) 0.014(4) 0.008(3) -0.003(4) -0.001(4) N4 0.027(7) 0.079(7) 0.025(4) 0.001(4) 0.001(4) -0.008(4) N1 0.016(6) 0.067(6) 0.022(4) -0.002(4) -0.003(4) -0.003(4) N10 0.029(5) 0.040(6) 0.026(4) 0.002(3) 0.007(4) 0.002(4) N8 0.023(5) 0.062(6) 0.024(4) 0.007(4) 0.008(4) -0.004(4) N2 0.025(6) 0.056(6) 0.018(4) -0.002(3) 0.001(4) 0.002(4) N14 0.046(7) 0.085(9) 0.018(4) -0.010(6) 0.010(5) -0.021(6) N13 0.026(6) 0.103(10) 0.027(5) -0.016(6) -0.001(4) 0.011(7) N11 0.042(6) 0.052(7) 0.034(4) -0.010(4) 0.011(4) 0.004(5) N5 0.031(6) 0.083(7) 0.014(4) 0.008(4) 0.003(4) 0.002(4) N9 0.062(8) 0.047(7) 0.040(5) 0.002(5) 0.008(5) -0.004(6) N15 0.085(8) 0.053(9) 0.093(7) 0.001(6) 0.027(6) -0.014(6) C32 0.132(13) 0.129(14) 0.148(13) 0.056(12) -0.053(10) -0.020(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.017(6) . ? Ni1 N6 2.024(7) . ? Ni1 N8 2.029(8) . ? Ni1 N7 2.057(7) . ? Ni1 O4 2.182(6) . ? Ni1 O5 2.202(6) . ? Ni2 N12 2.025(7) . ? Ni2 N2 2.030(7) . ? Ni2 N10 2.035(7) . ? Ni2 N3 2.057(6) . ? Ni2 O2 2.159(6) . ? Ni2 O1 2.161(6) . ? O1 N14 1.271(9) . ? O2 N14 1.274(9) . ? O3 N14 1.230(9) . ? O5 N13 1.283(9) . ? O4 N13 1.274(9) . ? O6 N13 1.223(9) . ? O7 C25 1.245(12) . ? C4 N6 1.270(10) . ? C4 N5 1.332(11) . ? C4 C3 1.518(10) . ? C3 N1 1.368(10) . ? C3 C2 1.369(11) . ? C7 N6 1.489(9) . ? C7 C6 1.548(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C12 N12 1.379(10) . ? C12 C18 1.397(11) . ? C12 C13 1.464(11) . ? C6 C5 1.498(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C1 N1 1.327(9) . ? C1 N2 1.337(9) . ? C1 H1 0.9500 . ? C17 N7 1.329(9) . ? C17 N12 1.339(9) 5_556 ? C17 H17 0.9500 . ? C9 N3 1.472(9) . ? C9 C10 1.530(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C13 N10 1.291(10) . ? C13 N11 1.365(12) . ? C2 N2 1.395(9) . ? C2 C8 1.462(12) . ? C19 N8 1.323(11) . ? C19 N9 1.346(12) . ? C19 C18 1.469(12) 5_556 ? C10 C11 1.481(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C16 N10 1.477(9) . ? C16 C15 1.527(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C14 N11 1.460(11) . ? C14 C15 1.519(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C20 N8 1.439(10) . ? C20 C21 1.502(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.471(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C11 N4 1.453(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C8 N3 1.307(9) . ? C8 N4 1.349(10) . ? C22 N9 1.466(12) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C5 N5 1.485(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C18 N7 1.375(10) 5_556 ? C18 C19 1.469(12) 5_556 ? N16 C27 1.261(14) . ? N16 C32 1.375(13) . ? N16 C29 1.465(16) . ? O8 C27 1.226(13) . ? C27 H27 0.9500 . ? C25 N15 1.316(12) . ? C25 H25 0.9500 . ? C24 N15 1.467(13) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C23 N15 1.468(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N7 C18 1.375(10) 5_556 ? N12 C17 1.339(9) 5_556 ? N4 H100 0.89(9) . ? N11 H102 0.79(14) . ? N5 H105 1.00(8) . ? N9 H101 0.77(14) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 Ni1 N6 80.5(3) . . ? N1 Ni1 N8 97.3(3) . . ? N6 Ni1 N8 95.3(3) . . ? N1 Ni1 N7 98.2(3) . . ? N6 Ni1 N7 174.9(3) . . ? N8 Ni1 N7 79.9(3) . . ? N1 Ni1 O4 160.1(3) . . ? N6 Ni1 O4 93.7(3) . . ? N8 Ni1 O4 102.2(3) . . ? N7 Ni1 O4 89.1(2) . . ? N1 Ni1 O5 101.5(3) . . ? N6 Ni1 O5 94.5(3) . . ? N8 Ni1 O5 160.0(3) . . ? N7 Ni1 O5 90.6(3) . . ? O4 Ni1 O5 59.7(3) . . ? N12 Ni2 N2 98.1(3) . . ? N12 Ni2 N10 79.7(3) . . ? N2 Ni2 N10 96.8(3) . . ? N12 Ni2 N3 178.8(3) . . ? N2 Ni2 N3 80.8(3) . . ? N10 Ni2 N3 100.1(3) . . ? N12 Ni2 O2 89.3(3) . . ? N2 Ni2 O2 102.0(3) . . ? N10 Ni2 O2 159.3(2) . . ? N3 Ni2 O2 91.4(2) . . ? N12 Ni2 O1 89.9(2) . . ? N2 Ni2 O1 160.5(3) . . ? N10 Ni2 O1 102.1(3) . . ? N3 Ni2 O1 91.3(2) . . ? O2 Ni2 O1 60.2(2) . . ? N14 O1 Ni2 91.6(5) . . ? N14 O2 Ni2 91.6(6) . . ? N13 O5 Ni1 90.9(6) . . ? N13 O4 Ni1 92.0(5) . . ? N6 C4 N5 127.9(7) . . ? N6 C4 C3 114.3(9) . . ? N5 C4 C3 117.8(9) . . ? N1 C3 C2 110.2(7) . . ? N1 C3 C4 114.0(8) . . ? C2 C3 C4 135.8(10) . . ? N6 C7 C6 111.1(7) . . ? N6 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N6 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N12 C12 C18 109.0(8) . . ? N12 C12 C13 113.8(8) . . ? C18 C12 C13 137.0(10) . . ? C5 C6 C7 108.6(8) . . ? C5 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? C5 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N1 C1 N2 114.9(8) . . ? N1 C1 H1 122.5 . . ? N2 C1 H1 122.5 . . ? N7 C17 N12 112.7(8) . 5_556 ? N7 C17 H17 123.6 . . ? N12 C17 H17 123.6 5_556 . ? N3 C9 C10 111.4(6) . . ? N3 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N3 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? N10 C13 N11 126.2(8) . . ? N10 C13 C12 115.4(9) . . ? N11 C13 C12 118.4(9) . . ? C3 C2 N2 106.9(7) . . ? C3 C2 C8 138.9(8) . . ? N2 C2 C8 114.2(8) . . ? N8 C19 N9 126.9(9) . . ? N8 C19 C18 115.3(10) . 5_556 ? N9 C19 C18 117.8(10) . 5_556 ? C11 C10 C9 111.3(7) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N10 C16 C15 111.9(7) . . ? N10 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? N10 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N11 C14 C15 109.6(7) . . ? N11 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N11 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N8 C20 C21 113.4(7) . . ? N8 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? N8 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 110.3(8) . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N4 C11 C10 109.0(8) . . ? N4 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? N4 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C14 C15 C16 109.0(8) . . ? C14 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? C14 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N3 C8 N4 127.4(9) . . ? N3 C8 C2 115.8(8) . . ? N4 C8 C2 116.8(8) . . ? N9 C22 C21 109.9(8) . . ? N9 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? N9 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N5 C5 C6 108.6(7) . . ? N5 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N5 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? N7 C18 C12 105.8(8) 5_556 . ? N7 C18 C19 115.0(9) 5_556 5_556 ? C12 C18 C19 139.3(10) . 5_556 ? C27 N16 C32 127.8(12) . . ? C27 N16 C29 114.6(12) . . ? C32 N16 C29 117.4(12) . . ? O8 C27 N16 131.9(15) . . ? O8 C27 H27 114.0 . . ? N16 C27 H27 114.0 . . ? O7 C25 N15 125.7(11) . . ? O7 C25 H25 117.2 . . ? N15 C25 H25 117.2 . . ? N15 C24 H24A 109.5 . . ? N15 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N15 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N16 C29 H29A 109.5 . . ? N16 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N16 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N15 C23 H23A 109.5 . . ? N15 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N15 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C4 N6 C7 117.0(7) . . ? C4 N6 Ni1 116.8(5) . . ? C7 N6 Ni1 126.1(6) . . ? C17 N7 C18 107.5(7) . 5_556 ? C17 N7 Ni1 138.4(7) . . ? C18 N7 Ni1 112.9(6) 5_556 . ? C17 N12 C12 105.0(7) 5_556 . ? C17 N12 Ni2 141.3(7) 5_556 . ? C12 N12 Ni2 113.6(6) . . ? C8 N3 C9 116.9(7) . . ? C8 N3 Ni2 113.2(6) . . ? C9 N3 Ni2 126.8(5) . . ? C8 N4 C11 119.9(7) . . ? C8 N4 H100 114(9) . . ? C11 N4 H100 124(9) . . ? C1 N1 C3 103.7(7) . . ? C1 N1 Ni1 141.3(7) . . ? C3 N1 Ni1 112.6(5) . . ? C13 N10 C16 118.9(8) . . ? C13 N10 Ni2 115.2(6) . . ? C16 N10 Ni2 123.1(6) . . ? C19 N8 C20 114.5(8) . . ? C19 N8 Ni1 116.0(7) . . ? C20 N8 Ni1 129.6(6) . . ? C1 N2 C2 104.2(7) . . ? C1 N2 Ni2 141.8(6) . . ? C2 N2 Ni2 112.0(6) . . ? O3 N14 O1 122.4(10) . . ? O3 N14 O2 120.9(10) . . ? O1 N14 O2 116.6(8) . . ? O6 N13 O4 121.7(9) . . ? O6 N13 O5 121.2(11) . . ? O4 N13 O5 117.1(9) . . ? C13 N11 C14 119.0(7) . . ? C13 N11 H102 101(10) . . ? C14 N11 H102 119(10) . . ? C4 N5 C5 120.2(7) . . ? C4 N5 H105 123(8) . . ? C5 N5 H105 116(8) . . ? C19 N9 C22 119.4(8) . . ? C19 N9 H101 123(10) . . ? C22 N9 H101 117(10) . . ? C25 N15 C24 119.8(10) . . ? C25 N15 C23 121.7(11) . . ? C24 N15 C23 118.4(10) . . ? N16 C32 H32A 109.5 . . ? N16 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N16 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 54.09 _diffrn_measured_fraction_theta_full 0.835 _refine_diff_density_max 0.732 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.099 # Attachment '- Compound 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 824171' _symmetry_space_group_name_hall '-P 2yn' #Added by publCIF _audit_update_record ; 2009-08-10 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H22 Cd N8 O4' _chemical_formula_weight 478.80 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.909(2) _cell_length_b 12.0710(19) _cell_length_c 12.950(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.858(2) _cell_angle_gamma 90.00 _cell_volume 1815.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5954 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.97 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8854 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.90 _reflns_number_total 3155 _reflns_number_gt 2805 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0491P)^2^+3.1048P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3155 _refine_ls_number_parameters 259 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.004 _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 Cd1 Cd 0.68190(2) 0.25978(2) 0.10653(2) 0.02278(13) Uani 1 1 d . . . C1 C 0.6007(3) 0.0583(3) -0.0558(3) 0.0184(7) Uani 1 1 d . . . O2 O 0.5404(2) 0.3953(2) 0.1490(3) 0.0373(7) Uani 1 1 d . . . O1 O 0.5871(3) 0.2311(2) 0.2203(3) 0.0349(7) Uani 1 1 d . . . C2 C 0.4369(3) 0.3058(3) -0.1464(3) 0.0217(8) Uani 1 1 d . . . N2 N 0.9450(3) 0.5066(3) 0.1571(3) 0.0278(8) Uani 1 1 d D . . N4 N 0.6869(2) 0.0868(3) 0.0405(3) 0.0229(7) Uani 1 1 d . . . N6 N 0.5263(3) 0.2469(2) -0.0719(3) 0.0219(7) Uani 1 1 d . . . N3 N 0.8721(3) 0.2490(2) 0.2555(3) 0.0225(7) Uani 1 1 d . . . N1 N 0.7684(3) 0.4173(3) 0.0985(3) 0.0229(7) Uani 1 1 d . . . C3 C 0.8770(3) 0.4282(3) 0.1699(3) 0.0205(8) Uani 1 1 d . . . C4 C 0.5192(3) 0.1458(3) -0.1246(3) 0.0200(8) Uani 1 1 d . . . O5 O 0.6863(3) 1.0080(3) 0.7230(3) 0.0440(8) Uani 1 1 d . . . N7 N 0.5300(3) 0.3212(3) 0.2094(3) 0.0357(9) Uani 1 1 d . . . N5 N 0.5830(3) -0.0483(3) -0.0881(3) 0.0288(8) Uani 1 1 d D . . C6 C 0.9253(3) 0.3506(3) 0.2679(3) 0.0196(8) Uani 1 1 d . . . C7 C 0.7869(5) 0.9839(4) 0.7855(5) 0.0436(12) Uani 1 1 d . . . O3 O 0.4669(3) 0.3307(3) 0.2581(4) 0.0677(12) Uani 1 1 d . . . C8 C 0.7559(3) -0.0080(4) 0.1054(4) 0.0335(10) Uani 1 1 d . . . H8A H 0.8321 0.0195 0.1613 0.040 Uiso 1 1 calc R . . H8B H 0.7176 -0.0415 0.1495 0.040 Uiso 1 1 calc R . . N8 N 0.8340(4) 0.8840(3) 0.7967(4) 0.0482(11) Uani 1 1 d . . . C10 C 0.8943(5) 0.5789(4) 0.0581(4) 0.0460(13) Uani 1 1 d . . . H10A H 0.9352 0.6508 0.0770 0.055 Uiso 1 1 calc R . . H10B H 0.9058 0.5457 -0.0061 0.055 Uiso 1 1 calc R . . C11 C 0.7240(4) 0.4949(4) 0.0015(4) 0.0469(13) Uani 1 1 d . . . H11A H 0.7319 0.4602 -0.0640 0.056 Uiso 1 1 calc R . . H11B H 0.6408 0.5062 -0.0218 0.056 Uiso 1 1 calc R . . C12 C 0.7772(5) 0.5978(5) 0.0220(5) 0.0618(16) Uani 1 1 d . . . H12A H 0.7642 0.6378 0.0820 0.074 Uiso 1 1 calc R . . H12B H 0.7458 0.6430 -0.0489 0.074 Uiso 1 1 calc R . . C15 C 0.9551(6) 0.8675(7) 0.8750(7) 0.096(3) Uani 1 1 d . . . H15A H 0.9906 0.9392 0.9063 0.144 Uiso 1 1 calc R . . H15B H 0.9948 0.8337 0.8334 0.144 Uiso 1 1 calc R . . H15C H 0.9612 0.8187 0.9378 0.144 Uiso 1 1 calc R . . C16 C 0.7731(8) 0.7901(6) 0.7333(8) 0.096(3) Uani 1 1 d . . . H16A H 0.6902 0.8043 0.7013 0.144 Uiso 1 1 calc R . . H16B H 0.7923 0.7255 0.7841 0.144 Uiso 1 1 calc R . . H16C H 0.7947 0.7758 0.6708 0.144 Uiso 1 1 calc R . . C14 C 0.6686(5) -0.1273(5) -0.0238(6) 0.0671(19) Uani 1 1 d . . . H14A H 0.6427 -0.1656 0.0284 0.080 Uiso 1 1 calc R . . H14B H 0.6718 -0.1835 -0.0780 0.080 Uiso 1 1 calc R . . H2 H 0.417(3) 0.376(3) -0.141(3) 0.013(9) Uiso 1 1 d . . . H1 H 1.018(3) 0.500(3) 0.196(3) 0.015 Uiso 1 1 d D . . C17 C 0.7730(7) -0.0915(6) 0.0375(6) 0.081(2) Uani 1 1 d . . . H17A H 0.8069 -0.0606 -0.0117 0.097 Uiso 1 1 calc R . . H17B H 0.8234 -0.1513 0.0858 0.097 Uiso 1 1 calc R . . H9 H 0.853(6) 1.042(6) 0.835(6) 0.097 Uiso 1 1 d . . . H11 H 0.535(5) -0.073(6) -0.151(5) 0.097 Uiso 1 1 d 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 Cd1 0.01750(18) 0.02574(19) 0.01670(19) -0.00403(11) -0.00035(13) -0.00167(10) C1 0.0161(17) 0.0233(19) 0.0149(18) 0.0007(14) 0.0059(15) -0.0004(14) O2 0.0349(16) 0.0288(16) 0.0399(19) -0.0040(14) 0.0086(14) 0.0006(13) O1 0.0338(17) 0.0333(17) 0.0375(18) 0.0029(13) 0.0154(15) 0.0032(13) C2 0.0186(19) 0.018(2) 0.021(2) -0.0012(15) 0.0014(16) 0.0010(14) N2 0.0216(17) 0.036(2) 0.0177(17) 0.0061(14) 0.0013(14) -0.0045(15) N4 0.0168(15) 0.0265(17) 0.0179(16) 0.0006(13) 0.0005(13) 0.0020(13) N6 0.0200(17) 0.0215(17) 0.0173(17) -0.0019(12) 0.0017(14) -0.0018(12) N3 0.0179(16) 0.0224(18) 0.0191(18) -0.0011(12) 0.0007(14) -0.0028(12) N1 0.0208(16) 0.0232(17) 0.0154(16) 0.0017(12) -0.0008(13) 0.0035(12) C3 0.0210(19) 0.0197(19) 0.0176(19) -0.0006(14) 0.0055(16) 0.0026(14) C4 0.0181(18) 0.0222(19) 0.0170(19) -0.0006(15) 0.0052(15) 0.0000(14) O5 0.0279(17) 0.061(2) 0.0404(19) 0.0071(16) 0.0125(15) 0.0062(15) N7 0.0276(19) 0.038(2) 0.041(2) -0.0061(18) 0.0142(17) -0.0032(16) N5 0.036(2) 0.0194(17) 0.0257(19) -0.0018(14) 0.0080(16) -0.0021(14) C6 0.0160(17) 0.0203(19) 0.0194(19) -0.0001(15) 0.0048(15) 0.0020(14) C7 0.049(3) 0.047(3) 0.045(3) 0.007(2) 0.030(3) 0.002(2) O3 0.062(2) 0.073(3) 0.096(3) 0.001(2) 0.061(3) 0.008(2) C8 0.026(2) 0.038(2) 0.033(2) 0.0136(19) 0.0095(19) 0.0094(18) N8 0.054(3) 0.037(2) 0.069(3) 0.017(2) 0.042(2) 0.016(2) C10 0.080(4) 0.030(2) 0.030(3) 0.0104(19) 0.025(3) 0.016(2) C11 0.054(3) 0.051(3) 0.032(3) 0.021(2) 0.015(2) 0.034(2) C12 0.074(4) 0.058(4) 0.044(3) 0.006(3) 0.018(3) 0.011(3) C15 0.077(5) 0.107(6) 0.123(6) 0.044(5) 0.062(5) 0.049(4) C16 0.148(8) 0.049(4) 0.138(7) -0.016(4) 0.105(7) -0.024(4) C14 0.049(3) 0.055(4) 0.118(5) 0.050(4) 0.056(4) 0.032(3) C17 0.091(5) 0.076(5) 0.079(5) 0.029(4) 0.040(4) 0.027(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 Cd1 N1 2.230(3) . ? Cd1 N4 2.268(3) . ? Cd1 N6 2.313(3) . ? Cd1 O1 2.316(3) . ? Cd1 N3 2.374(3) . ? C1 N4 1.305(5) . ? C1 N5 1.342(5) . ? C1 C4 1.482(5) . ? O2 N7 1.234(5) . ? O1 N7 1.287(5) . ? C2 N6 1.341(5) . ? C2 N3 1.351(5) 4_565 ? N2 C3 1.349(5) . ? N2 C10 1.450(5) . ? N4 C8 1.468(5) . ? N6 C4 1.382(5) . ? N3 C2 1.351(5) 4_666 ? N3 C6 1.381(5) . ? N1 C3 1.307(5) . ? N1 C11 1.468(5) . ? C3 C6 1.478(5) . ? C4 C6 1.392(5) 4_565 ? O5 C7 1.228(6) . ? N7 O3 1.234(5) . ? N5 C14 1.421(6) . ? C6 C4 1.392(5) 4_666 ? C7 N8 1.330(6) . ? C8 C17 1.418(8) . ? N8 C16 1.419(8) . ? N8 C15 1.458(8) . ? C10 C12 1.392(8) . ? C11 C12 1.388(8) . ? C14 C17 1.304(9) . ? 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 Cd1 N4 132.09(11) . . ? N1 Cd1 N6 104.18(11) . . ? N4 Cd1 N6 73.53(10) . . ? N1 Cd1 O1 124.84(11) . . ? N4 Cd1 O1 102.25(11) . . ? N6 Cd1 O1 98.98(11) . . ? N1 Cd1 N3 73.95(10) . . ? N4 Cd1 N3 93.81(10) . . ? N6 Cd1 N3 161.44(12) . . ? O1 Cd1 N3 96.92(12) . . ? N4 C1 N5 120.6(3) . . ? N4 C1 C4 118.2(3) . . ? N5 C1 C4 121.1(3) . . ? N7 O1 Cd1 103.9(2) . . ? N6 C2 N3 113.7(3) . 4_565 ? C3 N2 C10 117.7(4) . . ? C1 N4 C8 113.2(3) . . ? C1 N4 Cd1 116.8(2) . . ? C8 N4 Cd1 127.7(3) . . ? C2 N6 C4 105.2(3) . . ? C2 N6 Cd1 141.6(2) . . ? C4 N6 Cd1 113.2(2) . . ? C2 N3 C6 104.7(3) 4_666 . ? C2 N3 Cd1 142.0(3) 4_666 . ? C6 N3 Cd1 109.3(2) . . ? C3 N1 C11 116.1(4) . . ? C3 N1 Cd1 117.2(2) . . ? C11 N1 Cd1 124.6(3) . . ? N1 C3 N2 122.6(3) . . ? N1 C3 C6 117.6(3) . . ? N2 C3 C6 119.8(3) . . ? N6 C4 C6 107.9(3) . 4_565 ? N6 C4 C1 117.1(3) . . ? C6 C4 C1 134.7(3) 4_565 . ? O2 N7 O3 122.4(4) . . ? O2 N7 O1 117.8(3) . . ? O3 N7 O1 119.8(4) . . ? C1 N5 C14 118.5(4) . . ? N3 C6 C4 108.4(3) . 4_666 ? N3 C6 C3 117.5(3) . . ? C4 C6 C3 134.1(3) 4_666 . ? O5 C7 N8 126.0(5) . . ? C17 C8 N4 114.8(4) . . ? C7 N8 C16 123.3(6) . . ? C7 N8 C15 120.0(5) . . ? C16 N8 C15 116.7(6) . . ? C12 C10 N2 113.6(4) . . ? C12 C11 N1 115.5(5) . . ? C11 C12 C10 107.0(5) . . ? C17 C14 N5 117.9(6) . . ? C14 C17 C8 102.3(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.90 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.793 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.102 # Attachment '- Compound 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 824172' #TrackingRef '- Compound 4.cif' _publ_section_comment ; Structure contains several disordered water solvent molecules ; _symmetry_space_group_name_hall '-R 3' #Added by publCIF _refine_ls_number_constraints ? #Added by publCIF _audit_update_record ; 2009-08-08 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H126 In8 N84 O39.67' _chemical_formula_weight 4442.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 28.1055(4) _cell_length_b 28.1055(4) _cell_length_c 19.1669(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13111.9(5) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _exptl_crystal_description '0.1 0.1 0.1' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6646 _exptl_absorpt_coefficient_mu 9.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2628 _exptl_absorpt_correction_T_max 0.2628 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8639 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 54.19 _reflns_number_total 3368 _reflns_number_gt 2389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0696P)^2^+157.5448P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3368 _refine_ls_number_parameters 465 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.81110(3) 0.00800(3) 0.60045(3) 0.0543(3) Uani 1 1 d . . . In2 In 1.0000 0.0000 0.79223(5) 0.0683(4) Uani 1 3 d S . . C1 C 0.9103(4) -0.0048(4) 0.6755(4) 0.057(2) Uani 1 1 d . . . H1 H 0.9120 -0.0292 0.6428 0.068 Uiso 1 1 calc R . . C2 C 0.9300(5) 0.0508(4) 0.7615(5) 0.065(3) Uani 1 1 d . . . C3 C 0.8852(5) 0.0468(4) 0.7286(5) 0.062(3) Uani 1 1 d . . . C4 C 0.8476(4) 0.0685(4) 0.7397(5) 0.065(3) Uani 1 1 d . . . C5 C 1.0363(6) 0.1012(7) 0.9039(7) 0.109(5) Uani 1 1 d . . . C6 C 0.9673(5) 0.0855(5) 0.8194(5) 0.076(3) Uani 1 1 d . . . C7 C 0.9239(4) 0.0972(4) 0.5120(4) 0.049(2) Uani 1 1 d . . . H7 H 0.9507 0.0940 0.5386 0.058 Uiso 1 1 calc R . . C8 C 0.8460(4) 0.0860(4) 0.4762(4) 0.053(2) Uani 1 1 d . . . C9 C 0.7860(4) 0.0651(4) 0.4854(5) 0.060(3) Uani 1 1 d . . . C10 C 0.7044(5) 0.0691(6) 0.4528(7) 0.095(4) Uani 1 1 d . . . H10A H 0.6996 0.0978 0.4765 0.115 Uiso 1 1 calc R . . H10B H 0.6883 0.0637 0.4055 0.115 Uiso 1 1 calc R . . C11 C 0.6765(6) 0.0197(9) 0.4904(8) 0.151(8) Uani 1 1 d U . . H11A H 0.6644 -0.0107 0.4563 0.181 Uiso 1 1 calc R . . H11B H 0.6428 0.0176 0.5098 0.181 Uiso 1 1 calc R . . C12 C 0.8876(5) 0.1488(5) 0.3657(5) 0.070(3) Uani 1 1 d . . . C13 C 0.8860(4) 0.1209(4) 0.4318(4) 0.048(2) Uani 1 1 d . . . C14 C 0.9376(5) 0.2215(6) 0.2813(6) 0.107(5) Uani 1 1 d . . . C16 C 0.8396(6) 0.1503(7) 0.2582(6) 0.123(6) Uani 1 1 d . . . C17 C 0.8104(6) 0.1088(6) 0.8171(7) 0.099(4) Uani 1 1 d . . . H17A H 0.8278 0.1394 0.8509 0.119 Uiso 1 1 calc R . . H17B H 0.7765 0.0791 0.8386 0.119 Uiso 1 1 calc R . . C18 C 0.7964(6) 0.1278(5) 0.7536(7) 0.097(4) Uani 1 1 d . . . H18A H 0.8288 0.1622 0.7375 0.117 Uiso 1 1 calc R . . H18B H 0.7665 0.1358 0.7638 0.117 Uiso 1 1 calc R . . C19 C 0.7777(5) 0.0845(5) 0.6955(6) 0.083(4) Uani 1 1 d . . . H19A H 0.7407 0.0535 0.7067 0.100 Uiso 1 1 calc R . . H19B H 0.7753 0.1009 0.6509 0.100 Uiso 1 1 calc R . . C20 C 1.0145(8) 0.1746(8) 0.8803(11) 0.173(10) Uani 1 1 d . . . C21 C 0.7027(5) 0.0080(5) 0.5463(6) 0.082(3) Uani 1 1 d . . . H21A H 0.6838 -0.0323 0.5536 0.099 Uiso 1 1 calc R . . H21B H 0.6987 0.0249 0.5897 0.099 Uiso 1 1 calc R . . C22 C 0.8802(7) 0.2099(8) 0.2607(9) 0.113(7) Uani 0.80 1 d P . . H22A H 0.8676 0.2278 0.2948 0.136 Uiso 0.80 1 calc PR . . H22B H 0.8820 0.2262 0.2143 0.136 Uiso 0.80 1 calc PR . . C23 C 1.0634(10) 0.1637(9) 0.8801(12) 0.157(9) Uani 0.80 1 d P . . H23A H 1.0923 0.1883 0.9132 0.189 Uiso 0.80 1 calc PR . . H23B H 1.0796 0.1690 0.8328 0.189 Uiso 0.80 1 calc PR . . C220 C 0.900(3) 0.167(3) 0.226(3) 0.12(3) Uani 0.20 1 d PU . . H22C H 0.9033 0.1779 0.1768 0.147 Uiso 0.20 1 calc PR . . H22D H 0.9084 0.1369 0.2320 0.147 Uiso 0.20 1 calc PR . . C230 C 1.013(3) 0.124(2) 0.943(2) 0.10(2) Uani 0.20 1 d PU . . H23C H 1.0354 0.1419 0.9855 0.122 Uiso 0.20 1 calc PR . . H23D H 0.9753 0.0965 0.9575 0.122 Uiso 0.20 1 calc PR . . H300 H 0.952(5) 0.144(5) 0.796(7) 0.122 Uiso 1 1 d . . . H555 H 0.855(5) 0.079(5) 0.849(7) 0.122 Uiso 1 1 d . . . H800 H 0.778(6) 0.109(6) 0.423(8) 0.122 Uiso 1 1 d . . . N1 N 0.9953(4) 0.0658(4) 0.8500(4) 0.081(3) Uani 1 1 d . . . N2 N 0.9446(3) 0.0166(3) 0.7287(4) 0.060(2) Uani 1 1 d . . . N3 N 0.8737(3) 0.0111(3) 0.6724(3) 0.059(2) Uani 1 1 d . . . N4 N 0.8162(3) 0.0635(3) 0.6875(4) 0.058(2) Uani 1 1 d . . . N5 N 0.8473(4) 0.0887(4) 0.8024(5) 0.086(3) Uani 1 1 d . . . N6 N 0.8703(3) 0.0705(3) 0.5265(3) 0.0450(18) Uani 1 1 d . . . N7 N 0.7614(3) 0.0285(3) 0.5335(4) 0.060(2) Uani 1 1 d . . . N8 N 0.7625(4) 0.0873(4) 0.4472(5) 0.079(3) Uani 1 1 d . . . N9 N 0.9354(3) 0.1291(3) 0.4556(3) 0.0502(19) Uani 1 1 d . . . N10 N 0.9338(4) 0.1928(4) 0.3489(4) 0.068(2) Uani 1 1 d . . . N11 N 0.8406(4) 0.1252(5) 0.3277(4) 0.091(3) Uani 1 1 d . . . N13 N 0.9718(5) 0.1332(5) 0.8313(6) 0.111(4) Uani 1 1 d . . . N31 N 0.6815(7) 0.1271(8) 0.6457(9) 0.138(5) Uiso 1 1 d . . . N41 N 0.701(2) 0.138(2) 0.282(2) 0.265(19) Uiso 0.83 1 d P . . N51 N 0.0000 0.0000 0.5000 0.158(13) Uiso 1 6 d S . . O31 O 0.7223(10) 0.1514(13) 0.6031(14) 0.074(9) Uiso 0.46 1 d P . . O32 O 0.6578(9) 0.0883(10) 0.6755(11) 0.073(6) Uiso 0.46 1 d P . . O33 O 0.6581(11) 0.1629(10) 0.6575(13) 0.120(8) Uiso 0.46 1 d P . . O41 O 0.644(2) 0.0894(18) 0.295(2) 0.097(11) Uiso 0.27 1 d P . . O42 O 0.7375(17) 0.1591(16) 0.3274(19) 0.115(11) Uiso 0.27 1 d P . . O43 O 0.7025(19) 0.1119(18) 0.227(2) 0.120(13) Uiso 0.27 1 d P . . O51 O 0.0415(9) 0.0401(10) 0.4667(11) 0.153(8) Uiso 0.50 1 d P . . O52 O 0.7823(9) 0.1898(11) 0.3767(11) 0.133(7) Uiso 0.52 1 d P . . O53 O 0.6451(14) 0.0870(14) 0.6142(19) 0.080(9) Uiso 0.25 1 d P . . O54 O 0.6864(19) 0.1208(19) 0.712(2) 0.123(13) Uiso 0.25 1 d P . . O55 O 0.7722(17) 0.2632(17) 0.3962(15) 0.084(10) Uiso 0.25 1 d P . . O57 O 0.671(3) 0.112(3) 0.266(3) 0.120(15) Uiso 0.25 1 d P . . O58 O 0.792(3) 0.231(4) 0.395(3) 0.18(2) Uiso 0.25 1 d P . . O59 O 0.697(2) 0.098(2) 0.274(3) 0.129(15) Uiso 0.25 1 d P . . O60 O 0.628(3) 0.086(3) 0.572(4) 0.010(17) Uiso 0.05 1 d P . . O61 O 0.638(4) 0.162(3) 0.268(4) 0.087(19) Uiso 0.17 1 d P . . O62 O 0.704(4) 0.182(4) 0.310(4) 0.15(2) Uiso 0.17 1 d P . . O63 O 0.612(5) 0.138(5) 0.270(4) 0.12(3) Uiso 0.17 1 d P . . O64 O 0.651(3) 0.152(4) 0.244(5) 0.12(3) Uiso 0.17 1 d P . . O65 O 0.658(3) 0.145(3) 0.282(3) 0.100(18) Uiso 0.17 1 d P . . O66 O 0.675(6) 0.129(6) 0.223(7) 0.22(5) Uiso 0.17 1 d P . . O67 O 0.613(4) 0.083(3) 0.295(4) 0.14(3) Uiso 0.17 1 d P . . O68 O 0.719(2) 0.133(3) 0.605(3) 0.066(18) Uiso 0.17 1 d P . . O69 O 0.7285(15) 0.154(2) 0.6242(19) 0.027(10) Uiso 0.17 1 d P . . O71 O 0.650(2) 0.070(2) 0.656(3) 0.079(18) Uiso 0.17 1 d P . . O338 O 0.679(4) 0.162(4) 0.675(4) 0.08(2) Uiso 0.10 1 d P . . O339 O 0.622(6) 0.121(6) 0.596(7) 0.19(5) Uiso 0.10 1 d P . . 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 In1 0.0542(5) 0.0460(5) 0.0573(4) -0.0008(3) 0.0087(3) 0.0211(4) In2 0.0779(7) 0.0779(7) 0.0490(6) 0.000 0.000 0.0390(3) C1 0.057(7) 0.058(7) 0.059(5) 0.001(4) 0.005(5) 0.033(6) C2 0.068(8) 0.074(8) 0.058(5) -0.007(5) 0.001(5) 0.039(7) C3 0.075(8) 0.052(7) 0.058(5) 0.004(5) 0.009(5) 0.032(6) C4 0.058(7) 0.060(7) 0.071(7) -0.008(5) 0.008(5) 0.025(6) C5 0.127(13) 0.114(12) 0.093(8) -0.053(9) -0.054(8) 0.066(11) C6 0.090(9) 0.082(9) 0.067(6) -0.022(6) -0.018(6) 0.050(8) C7 0.051(7) 0.050(6) 0.048(5) -0.002(4) -0.003(4) 0.027(5) C8 0.045(6) 0.043(6) 0.061(5) -0.004(4) -0.005(5) 0.015(5) C9 0.057(7) 0.058(7) 0.069(6) -0.005(5) -0.009(5) 0.032(6) C10 0.054(9) 0.091(10) 0.142(11) 0.022(8) 0.001(7) 0.037(8) C11 0.064(10) 0.24(2) 0.127(11) 0.075(13) 0.009(8) 0.060(13) C12 0.050(7) 0.082(9) 0.069(6) 0.008(6) -0.004(5) 0.028(7) C13 0.043(6) 0.047(6) 0.050(5) 0.002(4) -0.004(4) 0.020(5) C14 0.055(8) 0.148(13) 0.094(8) 0.065(8) -0.008(6) 0.034(9) C16 0.085(11) 0.166(16) 0.082(8) 0.044(9) -0.015(7) 0.035(11) C17 0.094(11) 0.098(11) 0.100(9) -0.026(8) 0.021(7) 0.044(9) C18 0.110(11) 0.086(10) 0.109(9) -0.016(7) 0.014(8) 0.059(9) C19 0.084(9) 0.062(8) 0.096(8) -0.011(6) 0.017(6) 0.030(7) C20 0.168(19) 0.167(18) 0.24(2) -0.131(16) -0.136(16) 0.129(17) C21 0.058(8) 0.054(8) 0.128(9) 0.009(6) 0.014(7) 0.023(6) C22 0.071(12) 0.114(16) 0.109(12) 0.059(11) -0.022(9) 0.013(12) C23 0.16(2) 0.11(2) 0.17(2) -0.058(15) -0.068(17) 0.050(18) C220 0.13(6) 0.14(6) 0.05(3) 0.05(3) -0.01(3) 0.04(5) C230 0.16(6) 0.05(3) 0.03(2) -0.02(2) -0.03(3) 0.01(4) N1 0.090(7) 0.101(8) 0.056(5) -0.023(5) -0.014(4) 0.051(7) N2 0.067(6) 0.065(6) 0.052(4) -0.004(4) -0.010(4) 0.035(5) N3 0.057(6) 0.069(6) 0.049(4) -0.013(4) -0.005(3) 0.031(5) N4 0.062(6) 0.048(5) 0.072(5) -0.006(4) 0.010(4) 0.032(5) N5 0.082(7) 0.106(8) 0.073(5) -0.026(5) 0.012(5) 0.050(7) N6 0.039(5) 0.033(4) 0.052(4) 0.000(3) 0.005(3) 0.010(4) N7 0.045(5) 0.058(6) 0.080(5) 0.008(4) 0.007(4) 0.029(5) N8 0.053(7) 0.078(8) 0.109(8) 0.011(5) -0.002(5) 0.035(6) N9 0.041(5) 0.053(5) 0.048(4) 0.004(3) 0.006(3) 0.018(4) N10 0.053(6) 0.085(7) 0.066(5) 0.022(4) -0.002(4) 0.034(6) N11 0.061(7) 0.121(9) 0.074(5) 0.018(5) -0.018(5) 0.031(6) N13 0.144(11) 0.104(9) 0.114(8) -0.062(7) -0.060(7) 0.084(9) _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 In1 N7 2.175(8) . ? In1 N3 2.204(8) . ? In1 N6 2.223(7) . ? In1 N4 2.240(7) . ? In1 N9 2.249(7) 12_546 ? In1 N10 2.251(8) 12_546 ? In2 N2 2.203(7) 2_645 ? In2 N2 2.203(7) . ? In2 N2 2.203(8) 3_765 ? In2 N1 2.215(9) 3_765 ? In2 N1 2.215(9) . ? In2 N1 2.215(9) 2_645 ? C1 N3 1.309(12) . ? C1 N2 1.323(11) . ? C2 C3 1.363(14) . ? C2 N2 1.371(12) . ? C2 C6 1.502(14) . ? C3 N3 1.396(12) . ? C3 C4 1.473(14) . ? C4 N4 1.295(12) . ? C4 N5 1.332(12) . ? C5 C230 1.35(7) . ? C5 N1 1.497(14) . ? C5 C23 1.59(3) . ? C6 N13 1.303(14) . ? C6 N1 1.306(14) . ? C7 N6 1.334(11) . ? C7 N9 1.337(10) . ? C8 C13 1.359(12) . ? C8 N6 1.373(11) . ? C8 C9 1.492(13) . ? C9 N7 1.295(12) . ? C9 N8 1.333(13) . ? C10 C11 1.407(18) . ? C10 N8 1.451(15) . ? C11 C21 1.428(17) . ? C12 N10 1.308(13) . ? C12 N11 1.357(13) . ? C12 C13 1.479(13) . ? C13 N9 1.368(11) . ? C14 N10 1.501(12) . ? C14 C22 1.529(19) . ? C14 C220 1.73(8) . ? C16 C22 1.48(2) . ? C16 N11 1.513(14) . ? C16 C220 1.63(8) . ? C17 N5 1.435(15) . ? C17 C18 1.462(17) . ? C18 C19 1.536(15) . ? C19 N4 1.474(13) . ? C20 N13 1.510(17) . ? C20 C23 1.55(3) . ? C20 C230 1.86(6) . ? C21 N7 1.471(13) . ? N9 In1 2.249(7) 11_666 ? N10 In1 2.251(8) 11_666 ? N31 O32 1.11(2) . ? N31 O338 1.17(8) . ? N31 O69 1.22(4) . ? N31 O53 1.23(3) . ? N31 O68 1.25(6) . ? N31 O31 1.29(3) . ? N31 O54 1.29(4) . ? N31 O71 1.40(6) . ? N31 O33 1.47(3) . ? N41 O57 0.86(7) . ? N41 O59 1.08(6) . ? N41 O42 1.24(5) . ? N41 O62 1.30(8) . ? N41 O65 1.30(8) . ? N41 O66 1.31(14) . ? N41 O43 1.31(6) . ? N41 O41 1.52(7) . ? N41 O64 1.79(10) . ? N51 O51 1.31(2) 11_556 ? N51 O51 1.31(2) 10_556 ? N51 O51 1.31(2) 3 ? N51 O51 1.31(2) 2 ? N51 O51 1.31(2) . ? N51 O51 1.31(2) 12_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 In1 N3 164.7(3) . . ? N7 In1 N6 75.0(3) . . ? N3 In1 N6 95.8(3) . . ? N7 In1 N4 94.6(3) . . ? N3 In1 N4 74.6(3) . . ? N6 In1 N4 99.4(3) . . ? N7 In1 N9 101.7(3) . 12_546 ? N3 In1 N9 91.1(3) . 12_546 ? N6 In1 N9 95.4(2) . 12_546 ? N4 In1 N9 160.3(3) . 12_546 ? N7 In1 N10 96.8(3) . 12_546 ? N3 In1 N10 94.5(3) . 12_546 ? N6 In1 N10 165.9(3) . 12_546 ? N4 In1 N10 92.6(3) . 12_546 ? N9 In1 N10 74.8(3) 12_546 12_546 ? N2 In2 N2 92.4(3) 2_645 . ? N2 In2 N2 92.4(3) 2_645 3_765 ? N2 In2 N2 92.4(3) . 3_765 ? N2 In2 N1 96.0(3) 2_645 3_765 ? N2 In2 N1 165.8(3) . 3_765 ? N2 In2 N1 75.9(3) 3_765 3_765 ? N2 In2 N1 165.8(3) 2_645 . ? N2 In2 N1 75.9(3) . . ? N2 In2 N1 96.0(3) 3_765 . ? N1 In2 N1 97.2(3) 3_765 . ? N2 In2 N1 75.9(3) 2_645 2_645 ? N2 In2 N1 96.0(3) . 2_645 ? N2 In2 N1 165.8(3) 3_765 2_645 ? N1 In2 N1 97.2(3) 3_765 2_645 ? N1 In2 N1 97.2(3) . 2_645 ? N3 C1 N2 113.5(8) . . ? C3 C2 N2 108.5(8) . . ? C3 C2 C6 135.3(10) . . ? N2 C2 C6 116.0(10) . . ? C2 C3 N3 106.7(9) . . ? C2 C3 C4 136.3(9) . . ? N3 C3 C4 116.9(9) . . ? N4 C4 N5 126.4(11) . . ? N4 C4 C3 115.9(8) . . ? N5 C4 C3 117.7(10) . . ? C230 C5 N1 108(3) . . ? C230 C5 C23 74(3) . . ? N1 C5 C23 108.6(12) . . ? N13 C6 N1 126.1(11) . . ? N13 C6 C2 118.3(11) . . ? N1 C6 C2 115.4(11) . . ? N6 C7 N9 111.8(8) . . ? C13 C8 N6 107.7(8) . . ? C13 C8 C9 136.2(9) . . ? N6 C8 C9 115.9(8) . . ? N7 C9 N8 124.8(10) . . ? N7 C9 C8 116.5(8) . . ? N8 C9 C8 118.6(9) . . ? C11 C10 N8 111.0(11) . . ? C10 C11 C21 121.0(14) . . ? N10 C12 N11 126.4(9) . . ? N10 C12 C13 117.8(9) . . ? N11 C12 C13 115.8(10) . . ? C8 C13 N9 108.5(7) . . ? C8 C13 C12 135.6(9) . . ? N9 C13 C12 115.8(8) . . ? N10 C14 C22 108.9(9) . . ? N10 C14 C220 102(2) . . ? C22 C14 C220 62(3) . . ? C22 C16 N11 108.4(11) . . ? C22 C16 C220 66(3) . . ? N11 C16 C220 102(2) . . ? N5 C17 C18 111.2(10) . . ? C17 C18 C19 111.2(11) . . ? N4 C19 C18 111.4(10) . . ? N13 C20 C23 106.7(13) . . ? N13 C20 C230 96.4(19) . . ? C23 C20 C230 62(3) . . ? C11 C21 N7 113.0(10) . . ? C16 C22 C14 112.5(15) . . ? C20 C23 C5 103.6(19) . . ? C16 C220 C14 97(5) . . ? C5 C230 C20 100(3) . . ? C6 N1 C5 117.1(11) . . ? C6 N1 In2 115.4(7) . . ? C5 N1 In2 123.5(8) . . ? C1 N2 C2 105.5(8) . . ? C1 N2 In2 139.6(7) . . ? C2 N2 In2 112.7(6) . . ? C1 N3 C3 105.8(8) . . ? C1 N3 In1 139.6(6) . . ? C3 N3 In1 113.8(7) . . ? C4 N4 C19 118.3(8) . . ? C4 N4 In1 116.9(7) . . ? C19 N4 In1 123.5(7) . . ? C4 N5 C17 120.3(11) . . ? C7 N6 C8 106.1(7) . . ? C7 N6 In1 140.0(6) . . ? C8 N6 In1 113.8(6) . . ? C9 N7 C21 118.6(8) . . ? C9 N7 In1 118.1(6) . . ? C21 N7 In1 122.8(7) . . ? C9 N8 C10 122.0(10) . . ? C7 N9 C13 105.7(7) . . ? C7 N9 In1 140.1(6) . 11_666 ? C13 N9 In1 113.5(5) . 11_666 ? C12 N10 C14 119.4(8) . . ? C12 N10 In1 113.4(6) . 11_666 ? C14 N10 In1 122.0(7) . 11_666 ? C12 N11 C16 118.9(10) . . ? C6 N13 C20 122.1(12) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 54.19 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.352 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.099 # Attachment '- Compound1b.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 824173' #TrackingRef '- Compound1b.cif' _publ_section_comment ; The structure contains two disordered methylene atoms (C100-C101) and (C102-C103) and several disordered water solvent molecules. ; #Added by publCIF _audit_update_record ; 2010-02-27 # Formatted by publCIF ; _symmetry_space_group_name_hall '-P 2yn' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C135 H175 Co8 N73 O56 S6' _chemical_formula_weight 4380.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.3067(9) _cell_length_b 18.7195(8) _cell_length_c 24.9104(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.1820(10) _cell_angle_gamma 90.00 _cell_volume 9454.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 6.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3420 _exptl_absorpt_correction_T_max 0.5483 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31450 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 53.42 _reflns_number_total 9187 _reflns_number_gt 5597 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1146P)^2^+22.3075P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9187 _refine_ls_number_parameters 1292 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.83991(7) 0.44273(7) 0.33845(6) 0.0344(5) Uani 1 1 d . . . Co2 Co 0.89007(7) 0.67659(7) 0.62352(6) 0.0324(5) Uani 1 1 d . . . Co3 Co 0.94365(7) 0.73111(7) 0.39685(5) 0.0300(5) Uani 1 1 d . . . Co4 Co 0.78863(7) 0.38824(7) 0.56668(6) 0.0335(5) Uani 1 1 d . . . S1 S 0.0884(3) 0.5829(3) 0.1510(2) 0.1193(16) Uani 1 1 d D . . S2 S 0.90672(19) 0.1666(2) 0.07190(14) 0.0720(10) Uani 1 1 d . . . S3 S 0.16207(16) 0.94008(15) 0.59371(11) 0.0458(8) Uani 1 1 d . . . C1 C 0.8250(4) 0.4370(5) 0.4568(4) 0.031(3) Uani 1 1 d . . . H1 H 0.8330 0.4860 0.4646 0.037 Uiso 1 1 calc R . . C2 C 0.8132(5) 0.3359(5) 0.4132(4) 0.033(3) Uani 1 1 d . . . C3 C 0.8021(5) 0.3232(5) 0.4668(4) 0.032(3) Uani 1 1 d . . . C4 C 0.7818(5) 0.2663(6) 0.5038(4) 0.037(3) Uani 1 1 d . . . C5 C 0.7618(6) 0.1429(6) 0.5268(5) 0.060(3) Uani 1 1 d . . . H5A H 0.7849 0.0976 0.5196 0.072 Uiso 1 1 calc R A 3 H5B H 0.7138 0.1340 0.5216 0.072 Uiso 1 1 calc R A 3 C7 C 0.7462(5) 0.2381(5) 0.5909(4) 0.052(3) Uani 1 1 d . . . H7A H 0.6976 0.2326 0.5878 0.062 Uiso 1 1 calc R B 3 H7B H 0.7583 0.2570 0.6273 0.062 Uiso 1 1 calc R B 3 C8 C 0.8079(5) 0.3007(6) 0.3600(4) 0.040(3) Uani 1 1 d . . . C9 C 0.8134(5) 0.3165(5) 0.2652(4) 0.047(3) Uani 1 1 d . . . H9A H 0.7718 0.3322 0.2461 0.056 Uiso 1 1 calc R . . H9B H 0.8506 0.3360 0.2457 0.056 Uiso 1 1 calc R . . C10 C 0.8166(10) 0.2388(8) 0.2654(5) 0.133(7) Uani 1 1 d . . . H10A H 0.7977 0.2228 0.2300 0.160 Uiso 1 1 calc R . . H10B H 0.8640 0.2261 0.2667 0.160 Uiso 1 1 calc R . . C11 C 0.7890(7) 0.1985(6) 0.3022(5) 0.078(4) Uani 1 1 d . . . H11A H 0.8101 0.1508 0.3032 0.094 Uiso 1 1 calc R . . H11B H 0.7416 0.1920 0.2920 0.094 Uiso 1 1 calc R . . C12 C 0.9137(5) 0.6816(5) 0.5066(4) 0.029(3) Uani 1 1 d . . . H12 H 0.8903 0.6395 0.4962 0.035 Uiso 1 1 calc R . . C13 C 0.9583(4) 0.7662(5) 0.5552(4) 0.028(2) Uani 1 1 d . . . C14 C 0.9712(4) 0.7791(5) 0.5017(4) 0.026(2) Uani 1 1 d . . . C15 C 0.9670(5) 0.7974(5) 0.6099(4) 0.032(3) Uani 1 1 d . . . C16 C 0.9338(5) 0.7919(5) 0.7007(4) 0.046(3) Uani 1 1 d . . . H16A H 0.9668 0.7643 0.7227 0.055 Uiso 1 1 calc R C 4 H16B H 0.8903 0.7856 0.7163 0.055 Uiso 1 1 calc R C 4 C18 C 1.0124(6) 0.8846(5) 0.6746(4) 0.047(3) Uani 1 1 d . . . H18A H 1.0503 0.8622 0.6948 0.057 Uiso 1 1 calc R D 4 H18B H 1.0206 0.9367 0.6728 0.057 Uiso 1 1 calc R D 4 C19 C 0.9991(5) 0.8322(5) 0.4677(4) 0.029(3) Uani 1 1 d . . . C20 C 1.0555(5) 0.9462(5) 0.4526(4) 0.050(3) Uani 1 1 d . . . H20A H 1.1033 0.9401 0.4483 0.060 Uiso 1 1 calc R . . H20B H 1.0485 0.9935 0.4692 0.060 Uiso 1 1 calc R . . C21 C 1.0194(6) 0.9429(6) 0.3993(4) 0.057(3) Uani 1 1 d . . . H21A H 1.0425 0.9734 0.3738 0.069 Uiso 1 1 calc R . . H21B H 0.9746 0.9627 0.4024 0.069 Uiso 1 1 calc R . . C22 C 1.0137(5) 0.8685(5) 0.3768(4) 0.042(3) Uani 1 1 d . . . H22A H 0.9843 0.8688 0.3437 0.050 Uiso 1 1 calc R . . H22B H 1.0577 0.8515 0.3672 0.050 Uiso 1 1 calc R . . C23 C 0.9047(5) 0.7654(5) 0.2817(4) 0.041(3) Uani 1 1 d . . . H23A H 0.8856 0.8102 0.2952 0.049 Uiso 1 1 calc R . . H23B H 0.8686 0.7300 0.2768 0.049 Uiso 1 1 calc R . . C24 C 0.9337(6) 0.7796(6) 0.2279(4) 0.060(3) Uani 1 1 d . . . H24A H 0.8978 0.7935 0.2014 0.071 Uiso 1 1 calc R . . H24B H 0.9650 0.8201 0.2317 0.071 Uiso 1 1 calc R . . C25 C 0.9686(6) 0.7157(6) 0.2076(4) 0.068(4) Uani 1 1 d . . . H25A H 0.9365 0.6778 0.1969 0.081 Uiso 1 1 calc R . . H25B H 0.9934 0.7286 0.1758 0.081 Uiso 1 1 calc R . . C26 C 1.0045(6) 0.7032(5) 0.3037(4) 0.036(3) Uani 1 1 d . . . C27 C 1.0518(6) 0.6781(5) 0.3457(4) 0.033(3) Uani 1 1 d . . . C28 C 1.0723(6) 0.6637(5) 0.4313(4) 0.028(3) Uani 1 1 d . . . H28 H 1.0673 0.6640 0.4690 0.033 Uiso 1 1 calc R . . C29 C 0.9726(7) 0.5977(5) 0.6952(4) 0.034(3) Uani 1 1 d . . . C30 C 0.9119(6) 0.6083(5) 0.7224(4) 0.043(3) Uani 1 1 d . . . C31 C 0.8408(7) 0.5925(7) 0.7978(5) 0.080(4) Uani 1 1 d . . . H31A H 0.8511 0.5964 0.8370 0.096 Uiso 1 1 calc R . . H31B H 0.8102 0.5519 0.7913 0.096 Uiso 1 1 calc R . . C32 C 0.8102(6) 0.6585(7) 0.7777(5) 0.084(4) Uani 1 1 d . . . H32A H 0.8365 0.6996 0.7919 0.100 Uiso 1 1 calc R . . H32B H 0.7656 0.6624 0.7917 0.100 Uiso 1 1 calc R . . C33 C 0.8042(5) 0.6632(5) 0.7178(4) 0.040(3) Uani 1 1 d . . . H33A H 0.7713 0.6279 0.7036 0.048 Uiso 1 1 calc R . . H33B H 0.7884 0.7114 0.7069 0.048 Uiso 1 1 calc R . . C34 C 0.7631(6) 0.6759(6) 0.5757(4) 0.039(3) Uani 1 1 d . . . C35 C 0.6847(8) 0.7713(7) 0.5548(5) 0.075(4) Uani 1 1 d . . . H35A H 0.6610 0.7845 0.5204 0.090 Uiso 1 1 calc R E 1 H35B H 0.6537 0.7769 0.5838 0.090 Uiso 1 1 calc R E 1 C38 C 0.7895(6) 0.7941(5) 0.6050(4) 0.045(3) Uani 1 1 d . . . H38A H 0.8292 0.8224 0.5977 0.053 Uiso 1 1 calc R F 1 H38B H 0.7762 0.8062 0.6415 0.053 Uiso 1 1 calc R F 1 C39 C 0.6929(5) 0.4350(5) 0.3191(4) 0.048(3) Uani 1 1 d . . . H39A H 0.6962 0.3898 0.3398 0.057 Uiso 1 1 calc R . . H39B H 0.6921 0.4229 0.2804 0.057 Uiso 1 1 calc R . . C40 C 0.6297(6) 0.4725(6) 0.3310(5) 0.069(4) Uani 1 1 d . . . H40A H 0.5918 0.4458 0.3143 0.083 Uiso 1 1 calc R . . H40B H 0.6250 0.4736 0.3703 0.083 Uiso 1 1 calc R . . C41 C 0.6293(5) 0.5472(5) 0.3096(4) 0.053(3) Uani 1 1 d . . . H41A H 0.6298 0.5464 0.2699 0.064 Uiso 1 1 calc R . . H41B H 0.5889 0.5723 0.3197 0.064 Uiso 1 1 calc R . . C42 C 0.7438(6) 0.5472(6) 0.3433(4) 0.031(3) Uani 1 1 d . . . C43 C 0.8067(7) 0.7231(5) 0.3870(3) 0.028(3) Uani 1 1 d . . . C44 C 0.7213(5) 0.8148(5) 0.3934(4) 0.047(3) Uani 1 1 d . . . H44A H 0.7118 0.8238 0.4314 0.056 Uiso 1 1 calc R . . H44B H 0.6803 0.8231 0.3709 0.056 Uiso 1 1 calc R . . C45 C 0.7743(5) 0.8646(5) 0.3767(4) 0.040(3) Uani 1 1 d . . . H45A H 0.7633 0.9141 0.3872 0.048 Uiso 1 1 calc R . . H45B H 0.7765 0.8633 0.3371 0.048 Uiso 1 1 calc R . . C46 C 0.8403(5) 0.8441(5) 0.4028(4) 0.032(3) Uani 1 1 d . . . H46A H 0.8750 0.8747 0.3886 0.038 Uiso 1 1 calc R . . H46B H 0.8399 0.8523 0.4421 0.038 Uiso 1 1 calc R . . C47 C 0.8297(6) 0.6511(5) 0.3776(3) 0.025(2) Uani 1 1 d U . . C48 C 0.8042(5) 0.5841(5) 0.3625(3) 0.028(3) Uani 1 1 d . . . C49 C 0.9107(5) 0.5749(6) 0.3754(3) 0.028(3) Uani 1 1 d . . . H49 H 0.9538 0.5551 0.3781 0.034 Uiso 1 1 calc R . . C50 C 0.9210(7) 0.4621(5) 0.2539(4) 0.042(3) Uani 1 1 d . . . C51 C 0.9642(6) 0.4298(5) 0.2963(4) 0.039(3) Uani 1 1 d . . . C52 C 0.8998(9) 0.5113(8) 0.1644(5) 0.113(6) Uani 1 1 d . . . H52A H 0.9224 0.5500 0.1456 0.135 Uiso 1 1 calc R . . H52B H 0.8878 0.4736 0.1378 0.135 Uiso 1 1 calc R . . C53 C 0.8429(8) 0.5383(12) 0.1851(7) 0.157(9) Uani 1 1 d . . . H53A H 0.8095 0.5428 0.1548 0.189 Uiso 1 1 calc R . . H53B H 0.8529 0.5873 0.1981 0.189 Uiso 1 1 calc R . . C54 C 0.8129(5) 0.5021(5) 0.2266(4) 0.049(3) Uani 1 1 d . . . H54A H 0.7840 0.4641 0.2107 0.059 Uiso 1 1 calc R . . H54B H 0.7846 0.5361 0.2453 0.059 Uiso 1 1 calc R . . C55 C 0.7609(6) 0.5343(6) 0.5599(4) 0.034(3) Uani 1 1 d . . . C56 C 0.7847(6) 0.6012(5) 0.5733(4) 0.033(3) Uani 1 1 d . . . C57 C 0.8614(5) 0.5234(6) 0.5947(3) 0.026(2) Uani 1 1 d . . . H57 H 0.9023 0.5031 0.6073 0.031 Uiso 1 1 calc R . . C58 C 0.6994(6) 0.4975(7) 0.5424(4) 0.043(3) Uani 1 1 d . . . C59 C 0.6457(5) 0.3835(5) 0.5288(4) 0.046(3) Uani 1 1 d . . . H59A H 0.6601 0.3458 0.5041 0.056 Uiso 1 1 calc R . . H59B H 0.6285 0.3595 0.5606 0.056 Uiso 1 1 calc R . . C60 C 0.5926(6) 0.4245(7) 0.5017(6) 0.098(5) Uani 1 1 d . . . H60A H 0.5998 0.4238 0.4627 0.117 Uiso 1 1 calc R . . H60B H 0.5508 0.3987 0.5068 0.117 Uiso 1 1 calc R . . C61 C 0.5834(6) 0.4953(7) 0.5165(6) 0.084(4) Uani 1 1 d . . . H61A H 0.5577 0.4965 0.5491 0.101 Uiso 1 1 calc R . . H61B H 0.5573 0.5199 0.4874 0.101 Uiso 1 1 calc R . . C62 C 0.7114(5) 0.4016(5) 0.6660(4) 0.046(3) Uani 1 1 d . . . H62A H 0.6784 0.3635 0.6581 0.055 Uiso 1 1 calc R . . H62B H 0.6943 0.4463 0.6492 0.055 Uiso 1 1 calc R . . C64 C 0.7628(8) 0.3743(9) 0.7543(5) 0.104(6) Uani 1 1 d . . . H64A H 0.7422 0.3284 0.7638 0.125 Uiso 1 1 calc R . . H64B H 0.7733 0.4007 0.7881 0.125 Uiso 1 1 calc R . . C65 C 0.8241(6) 0.3653(5) 0.6751(5) 0.037(3) Uani 1 1 d . . . C66 C 0.8849(6) 0.3490(5) 0.6462(4) 0.034(3) Uani 1 1 d . . . C67 C 0.9727(6) 0.3825(5) 0.3764(4) 0.027(3) Uani 1 1 d . . . H67 H 0.9622 0.3672 0.4112 0.032 Uiso 1 1 calc R . . C100 C 0.7332(15) 0.8134(13) 0.563(2) 0.080(15) Uani 0.58(5) 1 d P G 1 H10X H 0.7151 0.8600 0.5744 0.096 Uiso 0.58(5) 1 calc PR G 1 H10Y H 0.7534 0.8212 0.5286 0.096 Uiso 0.58(5) 1 calc PR G 1 C101 C 0.7201(15) 0.8079(13) 0.6053(16) 0.022(11) Uani 0.42(5) 1 d PU G 2 H10E H 0.7120 0.8601 0.6043 0.026 Uiso 0.42(5) 1 calc PR G 2 H10F H 0.7025 0.7886 0.6386 0.026 Uiso 0.42(5) 1 calc PR G 2 C102 C 0.7778(18) 0.1651(9) 0.5852(9) 0.057(11) Uani 0.57(3) 1 d P H 3 H10G H 0.7592 0.1304 0.6103 0.068 Uiso 0.57(3) 1 calc PR H 3 H10H H 0.8261 0.1680 0.5928 0.068 Uiso 0.57(3) 1 calc PR H 3 C103 C 0.7174(19) 0.1715(11) 0.5647(10) 0.033(11) Uani 0.43(3) 1 d P H 4 H10I H 0.7096 0.1353 0.5926 0.040 Uiso 0.43(3) 1 calc PR H 4 H10J H 0.6745 0.1830 0.5459 0.040 Uiso 0.43(3) 1 calc PR H 4 C104 C 0.9526(7) 0.8714(6) 0.7020(4) 0.071(4) Uani 1 1 d . I 4 H10C H 0.9161 0.8997 0.6848 0.085 Uiso 1 1 calc R I 4 H10D H 0.9589 0.8872 0.7399 0.085 Uiso 1 1 calc R I 4 C106 C 0.7199(8) 0.4116(12) 0.7243(6) 0.147(8) Uani 1 1 d . . . H63A H 0.7309 0.4626 0.7304 0.176 Uiso 1 1 calc R . . H63B H 0.6762 0.4037 0.7390 0.176 Uiso 1 1 calc R . . H701 H 0.681(7) 0.665(7) 0.536(6) 0.176 Uiso 1 1 d D . . H702 H 1.045(8) 0.894(9) 0.523(4) 0.176 Uiso 1 1 d D . . H703 H 1.043(6) 0.863(9) 0.598(6) 0.176 Uiso 1 1 d D . . H704 H 0.721(9) 0.703(9) 0.391(7) 0.176 Uiso 1 1 d . . . H705 H 0.687(8) 0.619(7) 0.355(6) 0.176 Uiso 1 1 d D . . N1 N 1.0260(4) 0.6851(4) 0.3954(3) 0.029(2) Uani 1 1 d . . . N2 N 0.9542(4) 0.7385(4) 0.3214(3) 0.033(2) Uani 1 1 d . . . N3 N 1.0138(5) 0.6909(5) 0.2513(4) 0.055(3) Uani 1 1 d D . . N4 N 0.8600(5) 0.4697(4) 0.2663(3) 0.035(2) Uani 1 1 d . . . N5 N 0.9458(5) 0.4810(6) 0.2070(4) 0.080(3) Uani 1 1 d . . . N6 N 0.9306(4) 0.4166(4) 0.3418(3) 0.029(2) Uani 1 1 d . . . N7 N 0.8972(4) 0.6439(4) 0.3847(3) 0.029(2) Uani 1 1 d . . . N8 N 0.8567(5) 0.5376(4) 0.3619(3) 0.026(2) Uani 1 1 d . . . N9 N 0.7512(4) 0.4793(4) 0.3331(3) 0.036(2) Uani 1 1 d . . . N10 N 0.6877(5) 0.5843(4) 0.3323(3) 0.045(2) Uani 1 1 d D . . N11 N 0.7431(5) 0.7397(4) 0.3872(3) 0.041(3) Uani 1 1 d . . . N12 N 0.8556(4) 0.7693(4) 0.3928(3) 0.028(2) Uani 1 1 d . . . N13 N 0.8271(3) 0.4081(4) 0.4080(3) 0.029(2) Uani 1 1 d . . . N14 N 0.8101(3) 0.3874(4) 0.4939(3) 0.032(2) Uani 1 1 d . . . N15 N 0.7660(4) 0.2905(4) 0.5505(4) 0.035(2) Uani 1 1 d . H . N16 N 0.7812(4) 0.1973(4) 0.4879(3) 0.045(2) Uani 1 1 d . H . N17 N 0.7962(5) 0.2309(5) 0.3555(3) 0.063(3) Uani 1 1 d . . . N18 N 0.8165(4) 0.3446(4) 0.3203(3) 0.036(2) Uani 1 1 d . . . N19 N 0.8483(4) 0.5930(4) 0.5950(3) 0.027(2) Uani 1 1 d . . . N20 N 0.8102(4) 0.4858(4) 0.5746(3) 0.029(2) Uani 1 1 d . . . N21 N 0.7030(4) 0.4268(5) 0.5464(3) 0.036(2) Uani 1 1 d . . . N22 N 0.6453(5) 0.5340(5) 0.5274(4) 0.065(3) Uani 1 1 d U . . N23 N 0.7053(5) 0.6966(4) 0.5523(4) 0.054(3) Uani 1 1 d D G . N24 N 0.8052(4) 0.7177(4) 0.6025(3) 0.033(2) Uani 1 1 d . G . N25 N 0.9216(4) 0.7037(4) 0.5569(3) 0.031(2) Uani 1 1 d . . . N26 N 0.9419(4) 0.7247(4) 0.4719(3) 0.028(2) Uani 1 1 d . . . N27 N 0.9307(4) 0.7650(4) 0.6453(3) 0.032(2) Uani 1 1 d . I . N28 N 1.0059(4) 0.8547(4) 0.6197(3) 0.037(2) Uani 1 1 d D I . N30 N 0.9870(4) 0.8202(4) 0.4167(3) 0.031(2) Uani 1 1 d . . . N31 N 0.9697(5) 0.6269(4) 0.6441(3) 0.031(2) Uani 1 1 d . . . N32 N 0.8677(5) 0.6493(4) 0.6946(3) 0.037(2) Uani 1 1 d . . . N33 N 0.9012(5) 0.5804(5) 0.7702(4) 0.065(3) Uani 1 1 d . . . N34 N 0.7734(5) 0.3822(4) 0.6427(3) 0.032(2) Uani 1 1 d . . . N35 N 0.8244(5) 0.3593(5) 0.7283(4) 0.071(3) Uani 1 1 d . . . N36 N 0.8739(4) 0.3581(4) 0.5912(3) 0.026(2) Uani 1 1 d . . . N206 N 1.0319(4) 0.8898(4) 0.4876(3) 0.038(2) Uani 1 1 d D . . O1 O 0.1353(4) 0.9953(3) 0.5587(3) 0.064(2) Uani 1 1 d . . . O2 O 0.2328(4) 0.9290(4) 0.5866(3) 0.088(3) Uani 1 1 d . . . O3 O 0.1509(4) 0.9550(4) 0.6496(3) 0.063(2) Uani 1 1 d . . . O4 O 0.1282(3) 0.8713(3) 0.5774(2) 0.0452(19) Uani 1 1 d . . . O5 O 0.9354(5) 0.2217(7) 0.0407(4) 0.145(5) Uani 1 1 d . . . O6 O 0.9499(4) 0.1054(5) 0.0783(3) 0.115(4) Uani 1 1 d . . . O7 O 0.8411(4) 0.1455(4) 0.0478(3) 0.061(2) Uani 1 1 d . . . O8 O 0.8927(3) 0.1940(4) 0.1265(3) 0.064(2) Uani 1 1 d . . . O10 O 0.0690(4) 0.5661(4) 0.2064(4) 0.090(3) Uani 1 1 d . . . O11 O 0.1540(6) 0.5504(6) 0.1398(5) 0.160(5) Uani 1 1 d . . . O12 O 0.0513(9) 0.5235(10) 0.1244(8) 0.183(8) Uani 0.67 1 d PDU . . O13 O 0.1078(8) 0.6569(6) 0.1660(7) 0.140(7) Uani 0.67 1 d PDU . . N600 N 0.5994(9) 0.2032(9) 0.4324(6) 0.052(5) Uiso 0.50 1 d P . . O300 O 0.6499(7) 0.2907(8) 0.3932(5) 0.059(4) Uiso 0.50 1 d P . . C600 C 0.5435(14) 0.2460(15) 0.4422(11) 0.106(10) Uiso 0.50 1 d P . . H60C H 0.5419 0.2548 0.4809 0.160 Uiso 0.50 1 calc PR . . H60D H 0.5033 0.2210 0.4292 0.160 Uiso 0.50 1 calc PR . . H60E H 0.5467 0.2916 0.4232 0.160 Uiso 0.50 1 calc PR . . C601 C 0.5958(12) 0.1337(12) 0.4507(9) 0.078(8) Uiso 0.50 1 d P . . H60F H 0.5512 0.1152 0.4429 0.117 Uiso 0.50 1 calc PR . . H60G H 0.6063 0.1326 0.4896 0.117 Uiso 0.50 1 calc PR . . H60H H 0.6276 0.1041 0.4325 0.117 Uiso 0.50 1 calc PR . . C701 C 0.6455(11) 0.2279(12) 0.4066(8) 0.059(6) Uiso 0.50 1 d P . . H730 H 0.6792 0.1960 0.3968 0.070 Uiso 0.50 1 calc PR . . O100 O 0.0773(12) 0.6263(13) 0.9382(11) 0.157(9) Uiso 0.50 1 d P . . O101 O 0.0697(17) 0.6284(18) 0.9863(16) 0.111(12) Uiso 0.27 1 d P . . O102 O 0.1061(4) 0.0646(4) 0.7047(3) 0.049(2) Uiso 0.75 1 d P . . O103 O 0.2085(6) 0.0190(6) 0.3682(4) 0.122(4) Uiso 1 1 d . . . O104 O 0.242(3) 0.002(3) 0.384(2) 0.023(16) Uiso 0.10 1 d P . . O109 O 0.0766(6) 0.2101(7) 0.1709(6) 0.120(4) Uiso 0.80 1 d P . . O110 O 0.074(2) 0.234(3) 0.127(2) 0.185(18) Uiso 0.30 1 d P . . O111 O 0.0655(7) 0.2665(8) 0.0733(6) 0.124(5) Uiso 0.70 1 d P . . O112 O 0.3530(19) -0.031(2) 0.4405(16) 0.155(14) Uiso 0.30 1 d P . . O113 O 0.3507(15) 0.0337(16) 0.4827(12) 0.103(10) Uiso 0.30 1 d P . . O114 O 0.3055(8) 0.0334(9) 0.5290(7) 0.160(6) Uiso 0.75 1 d P . . O115 O 0.2845(10) 0.5513(9) 0.0195(7) 0.084(7) Uiso 0.50 1 d P . . O116 O 0.3187(9) 0.5629(9) 0.0279(7) 0.069(6) Uiso 0.50 1 d P . . O119 O 0.9622(6) 0.9322(7) 0.8414(4) 0.084(4) Uiso 0.75 1 d P . . O120 O 0.9508(14) 0.8843(17) 0.8435(11) 0.153(11) Uiso 0.45 1 d P . . O121 O 0.9830(8) 0.6048(9) 0.8904(7) 0.170(6) Uiso 0.75 1 d P . . O122 O 0.9611(5) 0.2944(5) 0.1880(4) 0.114(3) Uiso 1 1 d . . . O500 O 0.091(3) 0.919(3) 0.150(2) 0.20(2) Uiso 0.30 1 d P . . O501 O 0.1217(13) 0.8164(15) 0.2095(13) 0.134(9) Uiso 0.50 1 d P . . O502 O 0.0117(7) 0.9671(8) 0.2447(6) 0.046(4) Uiso 0.50 1 d P . . O503 O 0.0988(16) 0.8928(18) 0.2032(13) 0.072(9) Uiso 0.25 1 d P . . O504 O 0.1357(9) 0.9363(9) 0.3012(9) 0.097(6) Uiso 0.60 1 d P . . O505 O 0.166(3) 0.897(3) 0.326(2) 0.109(16) Uiso 0.20 1 d P . . O506 O 0.1083(10) 0.8580(13) 0.1612(9) 0.115(7) Uiso 0.50 1 d P . . O507 O 0.0554(16) 0.8435(18) 0.1173(13) 0.218(13) Uiso 0.50 1 d P . . O508 O 0.1734(15) 0.9311(14) 0.1908(12) 0.178(10) Uiso 0.50 1 d P . . O509 O 0.058(4) 0.945(3) 0.261(3) 0.12(3) Uiso 0.20 1 d P . . O510 O 0.1493(15) 0.8165(15) 0.2518(13) 0.232(12) Uiso 0.60 1 d P . . O511 O 0.122(4) 0.786(5) 0.185(4) 0.08(3) Uiso 0.10 1 d P . . O512 O 0.064(3) 0.958(3) 0.214(3) 0.29(3) Uiso 0.40 1 d P . . O514 O 0.131(6) 0.932(6) 0.270(5) 0.26(6) Uiso 0.20 1 d P . . O517 O 0.1348(19) 0.9213(15) 0.1599(12) 0.024(8) Uiso 0.20 1 d P . . O518 O 0.027(4) 0.939(3) 0.268(2) 0.011(17) Uiso 0.10 1 d P . . H706 H 1.046(3) 0.662(4) 0.250(3) 0.013 Uiso 1 1 d D . . O14 O 0.0485(9) 0.6209(14) 0.1141(8) 0.189(11) Uani 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0403(13) 0.0261(10) 0.0356(10) -0.0028(7) -0.0082(8) 0.0014(8) Co2 0.0400(12) 0.0259(10) 0.0314(10) -0.0024(7) 0.0021(8) 0.0036(8) Co3 0.0328(12) 0.0241(9) 0.0329(10) -0.0010(7) -0.0007(8) 0.0013(8) Co4 0.0312(12) 0.0277(10) 0.0419(11) -0.0017(8) 0.0043(8) -0.0015(8) S1 0.141(5) 0.099(4) 0.123(4) 0.006(3) 0.051(4) 0.027(3) S2 0.056(3) 0.094(3) 0.065(3) 0.006(2) -0.004(2) 0.009(2) S3 0.046(3) 0.043(2) 0.048(2) -0.0136(15) -0.0040(16) -0.0015(16) C1 0.030(7) 0.019(6) 0.044(7) 0.001(6) -0.002(5) 0.001(5) C2 0.037(7) 0.021(7) 0.041(8) -0.006(6) -0.009(5) -0.006(5) C3 0.038(7) 0.012(6) 0.046(7) 0.001(6) 0.003(6) 0.003(5) C4 0.029(7) 0.034(8) 0.046(8) 0.000(7) 0.002(6) -0.002(5) C5 0.067(9) 0.035(8) 0.080(10) 0.008(7) 0.033(8) 0.006(7) C7 0.062(9) 0.037(8) 0.056(8) -0.002(6) 0.005(6) -0.018(7) C8 0.041(8) 0.039(8) 0.040(7) -0.001(7) -0.006(6) 0.006(6) C9 0.069(9) 0.030(8) 0.041(7) -0.007(5) -0.007(6) 0.005(6) C10 0.30(2) 0.063(12) 0.035(9) -0.018(8) -0.002(11) -0.045(12) C11 0.152(13) 0.038(8) 0.042(8) -0.001(7) -0.020(8) -0.010(8) C12 0.036(7) 0.012(6) 0.039(7) -0.001(6) -0.008(6) 0.009(5) C13 0.024(7) 0.022(6) 0.037(7) -0.007(5) 0.000(5) 0.006(5) C14 0.025(7) 0.023(6) 0.029(6) 0.000(5) 0.001(5) 0.002(5) C15 0.030(8) 0.028(7) 0.038(7) -0.004(6) -0.007(6) 0.007(6) C16 0.066(9) 0.027(7) 0.044(7) -0.003(5) 0.008(6) 0.004(6) C18 0.048(9) 0.053(8) 0.042(7) 0.001(6) 0.005(7) -0.006(6) C19 0.033(7) 0.024(7) 0.031(7) 0.001(6) 0.001(5) -0.003(5) C20 0.063(9) 0.036(7) 0.050(7) -0.006(6) -0.002(7) -0.012(6) C21 0.070(9) 0.046(8) 0.055(8) 0.019(6) -0.003(7) -0.020(6) C22 0.041(8) 0.038(7) 0.046(7) 0.000(6) -0.003(6) -0.008(5) C23 0.049(8) 0.038(7) 0.034(7) 0.000(5) -0.007(6) 0.004(6) C24 0.076(9) 0.057(8) 0.044(8) 0.003(6) -0.014(7) 0.027(7) C25 0.081(10) 0.081(10) 0.041(7) 0.005(7) 0.004(7) 0.026(8) C26 0.049(10) 0.032(7) 0.027(7) 0.009(5) -0.007(7) -0.010(6) C27 0.024(9) 0.043(7) 0.033(7) 0.011(5) 0.011(6) -0.001(6) C28 0.022(8) 0.030(6) 0.032(6) 0.004(5) 0.011(7) 0.005(5) C29 0.043(10) 0.039(7) 0.020(7) -0.003(5) 0.004(7) 0.004(6) C30 0.056(10) 0.038(7) 0.035(7) -0.012(6) 0.006(8) 0.006(7) C31 0.094(12) 0.087(11) 0.063(9) 0.031(8) 0.035(9) 0.028(9) C32 0.085(11) 0.104(12) 0.066(10) 0.026(8) 0.032(8) 0.013(9) C33 0.045(9) 0.036(7) 0.040(7) 0.003(5) 0.008(6) 0.004(6) C34 0.040(9) 0.036(8) 0.043(7) -0.002(6) 0.011(6) 0.002(7) C35 0.103(13) 0.052(10) 0.067(9) -0.026(7) -0.027(8) 0.037(9) C38 0.056(11) 0.040(8) 0.037(7) 0.001(5) 0.007(6) 0.006(6) C39 0.040(9) 0.020(6) 0.080(8) -0.005(5) -0.024(6) 0.001(6) C40 0.040(9) 0.045(9) 0.120(11) -0.016(8) -0.012(7) 0.004(7) C41 0.048(9) 0.030(8) 0.079(9) 0.002(6) -0.016(7) 0.010(6) C42 0.020(9) 0.033(8) 0.039(6) 0.007(5) -0.006(6) 0.006(7) C43 0.027(9) 0.023(8) 0.031(6) 0.000(5) -0.008(5) -0.001(7) C44 0.051(9) 0.035(8) 0.055(7) -0.006(6) -0.009(6) 0.014(7) C45 0.049(9) 0.025(6) 0.045(7) -0.001(5) -0.003(6) -0.001(6) C46 0.020(7) 0.031(7) 0.044(6) -0.002(5) -0.001(5) 0.000(5) C47 0.033(9) 0.008(7) 0.034(6) -0.005(5) 0.001(5) -0.006(5) C48 0.015(8) 0.032(7) 0.036(6) 0.006(5) -0.008(5) 0.007(7) C49 0.032(9) 0.025(7) 0.027(6) 0.011(5) 0.000(5) 0.021(6) C50 0.059(11) 0.035(7) 0.031(8) -0.010(6) -0.014(8) 0.020(7) C51 0.045(10) 0.029(7) 0.044(8) -0.006(5) 0.006(7) 0.012(6) C52 0.117(14) 0.179(16) 0.042(8) 0.029(9) 0.005(9) 0.096(12) C53 0.072(13) 0.29(3) 0.111(14) 0.113(16) 0.016(11) 0.054(15) C54 0.069(9) 0.046(7) 0.030(7) -0.005(6) -0.017(7) 0.008(6) C55 0.010(9) 0.047(8) 0.043(7) -0.004(6) -0.004(6) 0.000(7) C56 0.027(9) 0.030(8) 0.041(7) -0.008(5) 0.001(6) 0.002(6) C57 0.015(8) 0.034(8) 0.030(6) 0.004(5) 0.002(5) 0.005(6) C58 0.018(10) 0.054(9) 0.057(8) 0.002(6) -0.001(6) 0.015(8) C59 0.026(8) 0.046(7) 0.068(8) -0.001(6) 0.003(6) -0.004(7) C60 0.026(9) 0.066(11) 0.197(16) -0.002(10) -0.037(9) -0.002(8) C61 0.032(10) 0.058(10) 0.159(14) 0.014(9) -0.024(8) 0.012(8) C62 0.024(8) 0.044(7) 0.073(9) -0.002(6) 0.024(7) -0.005(6) C64 0.078(13) 0.177(16) 0.061(10) 0.045(10) 0.032(10) 0.055(11) C65 0.032(10) 0.028(6) 0.054(9) 0.005(6) 0.013(8) 0.000(5) C66 0.036(10) 0.030(6) 0.038(8) 0.014(5) 0.011(7) -0.002(6) C67 0.025(8) 0.027(6) 0.027(6) 0.004(5) -0.007(6) 0.004(5) C100 0.08(2) 0.027(16) 0.13(4) -0.001(18) 0.00(2) 0.010(14) C101 0.03(2) 0.022(15) 0.019(19) -0.002(12) 0.005(14) 0.013(12) C102 0.08(3) 0.030(14) 0.057(17) 0.003(10) 0.005(16) 0.008(12) C103 0.04(3) 0.013(14) 0.048(17) -0.005(12) -0.012(16) -0.004(12) C104 0.111(13) 0.059(10) 0.042(7) -0.015(6) 0.004(8) -0.005(8) C106 0.066(12) 0.33(3) 0.053(11) -0.003(13) 0.026(9) 0.059(15) N1 0.024(6) 0.026(5) 0.038(6) 0.004(4) 0.003(5) 0.000(4) N2 0.028(6) 0.032(5) 0.036(5) 0.000(4) -0.002(5) 0.008(4) N3 0.050(8) 0.070(7) 0.047(7) 0.012(6) 0.003(6) 0.033(5) N4 0.041(7) 0.030(5) 0.034(5) -0.008(4) -0.013(5) 0.012(5) N5 0.094(9) 0.119(9) 0.028(6) 0.019(6) 0.006(6) 0.052(7) N6 0.034(6) 0.020(5) 0.034(5) -0.005(4) 0.004(5) 0.003(4) N7 0.023(7) 0.031(6) 0.032(5) -0.002(4) -0.002(4) -0.004(4) N8 0.021(6) 0.025(5) 0.029(5) 0.002(4) -0.018(4) -0.009(5) N9 0.038(7) 0.019(6) 0.051(6) -0.005(4) -0.006(4) 0.001(5) N10 0.031(7) 0.038(6) 0.063(7) -0.004(5) -0.017(5) -0.007(6) N11 0.023(8) 0.033(7) 0.065(6) -0.010(5) -0.007(5) 0.007(5) N12 0.036(6) 0.010(5) 0.039(5) -0.003(4) -0.002(4) 0.003(5) N13 0.035(6) 0.025(5) 0.025(5) -0.012(4) -0.001(4) 0.003(4) N14 0.025(6) 0.023(5) 0.046(5) 0.000(5) -0.004(4) 0.002(4) N15 0.033(6) 0.027(5) 0.046(6) 0.002(5) 0.009(5) -0.004(4) N16 0.063(7) 0.019(6) 0.054(6) 0.001(5) 0.006(5) -0.011(4) N17 0.119(9) 0.024(6) 0.047(6) -0.015(5) -0.002(6) -0.015(5) N18 0.042(6) 0.030(5) 0.033(5) 0.003(5) -0.013(4) 0.001(4) N19 0.029(7) 0.022(6) 0.031(5) -0.001(4) 0.004(4) 0.000(4) N20 0.015(6) 0.038(6) 0.035(5) -0.008(4) 0.004(4) -0.001(5) N21 0.022(6) 0.031(6) 0.055(6) 0.000(4) -0.001(4) -0.003(5) N22 0.006(7) 0.042(6) 0.143(9) 0.002(6) -0.024(6) -0.008(6) N23 0.053(8) 0.026(7) 0.080(7) -0.010(5) -0.017(6) 0.021(5) N24 0.044(6) 0.011(5) 0.044(5) -0.004(4) 0.007(5) 0.002(4) N25 0.046(6) 0.020(5) 0.026(5) -0.008(4) 0.001(4) 0.004(4) N26 0.030(6) 0.013(5) 0.040(5) 0.005(4) 0.000(4) 0.005(4) N27 0.045(6) 0.032(5) 0.020(5) 0.000(4) 0.007(4) -0.001(4) N28 0.047(7) 0.028(5) 0.035(6) -0.007(4) -0.012(4) -0.009(5) N30 0.031(6) 0.031(5) 0.029(5) 0.007(4) 0.001(4) 0.004(4) N31 0.034(7) 0.027(5) 0.032(6) 0.003(4) -0.001(5) 0.002(4) N32 0.038(7) 0.031(5) 0.044(6) -0.005(4) 0.008(5) 0.008(5) N33 0.071(8) 0.090(8) 0.037(6) 0.022(5) 0.030(6) 0.026(6) N34 0.020(7) 0.031(5) 0.047(6) -0.004(4) 0.010(6) -0.004(4) N35 0.055(8) 0.129(9) 0.033(6) 0.029(6) 0.034(6) 0.027(6) N36 0.019(6) 0.027(5) 0.031(5) 0.002(4) 0.007(5) -0.003(4) N206 0.050(6) 0.029(6) 0.035(5) 0.001(5) 0.006(5) -0.011(5) O1 0.094(6) 0.034(5) 0.063(5) -0.001(4) -0.006(4) -0.004(4) O2 0.029(6) 0.126(7) 0.108(7) -0.065(6) -0.002(5) 0.004(5) O3 0.077(6) 0.068(5) 0.044(5) -0.011(4) 0.002(4) -0.002(4) O4 0.055(5) 0.029(4) 0.051(4) -0.009(3) -0.002(4) -0.008(4) O5 0.094(8) 0.235(13) 0.107(8) 0.071(9) 0.004(6) -0.059(8) O6 0.094(8) 0.156(9) 0.092(7) -0.034(6) -0.032(6) 0.082(7) O7 0.042(6) 0.063(5) 0.076(6) 0.006(4) -0.020(4) 0.004(4) O8 0.063(6) 0.059(5) 0.068(6) 0.002(4) 0.000(4) -0.004(4) O10 0.106(7) 0.088(7) 0.079(7) -0.001(5) 0.018(6) 0.014(5) O11 0.102(9) 0.167(11) 0.219(13) -0.021(9) 0.081(9) 0.040(8) O12 0.20(2) 0.21(2) 0.139(17) -0.048(16) 0.015(14) -0.004(18) O13 0.188(19) 0.089(13) 0.153(16) 0.021(11) 0.089(14) 0.046(12) O14 0.125(16) 0.28(3) 0.164(18) 0.142(19) 0.002(13) 0.096(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N13 1.882(7) . ? Co1 N8 1.894(8) . ? Co1 N6 1.903(8) . ? Co1 N9 1.925(8) . ? Co1 N4 1.932(8) . ? Co1 N18 1.945(8) . ? Co2 N25 1.881(8) . ? Co2 N19 1.899(8) . ? Co2 N31 1.911(9) . ? Co2 N27 1.915(8) . ? Co2 N32 1.922(8) . ? Co2 N24 1.933(8) . ? Co3 N26 1.876(8) . ? Co3 N1 1.883(8) . ? Co3 N7 1.901(8) . ? Co3 N2 1.907(8) . ? Co3 N12 1.922(8) . ? Co3 N30 1.937(7) . ? Co4 N20 1.885(8) . ? Co4 N14 1.889(8) . ? Co4 N36 1.890(8) . ? Co4 N21 1.924(8) . ? Co4 N15 1.925(8) . ? Co4 N34 1.939(8) . ? S1 O14 1.387(14) . ? S1 O12 1.480(10) . ? S1 O13 1.483(9) . ? S1 O10 1.489(9) . ? S1 O11 1.506(10) . ? S2 O5 1.433(10) . ? S2 O6 1.446(8) . ? S2 O7 1.484(7) . ? S2 O8 1.495(7) . ? S3 O1 1.440(7) . ? S3 O3 1.450(7) . ? S3 O2 1.471(8) . ? S3 O4 1.505(6) . ? C1 N13 1.333(10) . ? C1 N14 1.356(10) . ? C1 H1 0.9500 . ? C2 C3 1.386(12) . ? C2 N13 1.388(11) . ? C2 C8 1.479(13) . ? C3 N14 1.382(10) . ? C3 C4 1.483(13) . ? C4 N15 1.304(11) . ? C4 N16 1.350(11) . ? C5 C103 1.44(3) . ? C5 N16 1.475(12) . ? C5 C102 1.53(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 N15 1.478(12) . ? C7 C103 1.51(2) . ? C7 C102 1.52(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N18 1.306(11) . ? C8 N17 1.331(12) . ? C9 C10 1.456(15) . ? C9 N18 1.466(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.334(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N17 1.459(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N25 1.321(10) . ? C12 N26 1.334(10) . ? C12 H12 0.9500 . ? C13 N25 1.389(11) . ? C13 C14 1.393(12) . ? C13 C15 1.484(12) . ? C14 N26 1.377(10) . ? C14 C19 1.443(12) . ? C15 N27 1.327(11) . ? C15 N28 1.346(11) . ? C16 N27 1.466(11) . ? C16 C104 1.535(13) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C104 1.448(13) . ? C18 N28 1.477(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N30 1.302(10) . ? C19 N206 1.347(11) . ? C20 N206 1.466(12) . ? C20 C21 1.483(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.503(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N30 1.469(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N2 1.460(11) . ? C23 C24 1.518(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.494(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N3 1.459(13) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N2 1.314(12) . ? C26 N3 1.349(12) . ? C26 C27 1.458(13) . ? C27 N1 1.377(11) . ? C27 C66 1.386(13) 3_766 ? C28 N36 1.321(10) 3_766 ? C28 N1 1.324(10) . ? C28 H28 0.9500 . ? C29 N31 1.383(11) . ? C29 C51 1.389(13) 3_766 ? C29 C30 1.453(15) . ? C30 N33 1.330(12) . ? C30 N32 1.343(12) . ? C31 N33 1.457(13) . ? C31 C32 1.460(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.494(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N32 1.465(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 N24 1.314(11) . ? C34 N23 1.338(13) . ? C34 C56 1.468(13) . ? C35 C100 1.27(2) . ? C35 N23 1.462(13) . ? C35 C101 1.57(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C38 C101 1.43(3) . ? C38 N24 1.467(11) . ? C38 C100 1.54(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N9 1.470(11) . ? C39 C40 1.507(13) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.497(13) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N10 1.462(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N9 1.307(11) . ? C42 N10 1.348(12) . ? C42 C48 1.465(13) . ? C43 N12 1.318(11) . ? C43 N11 1.330(12) . ? C43 C47 1.449(13) . ? C44 N11 1.483(12) . ? C44 C45 1.500(12) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.507(12) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N12 1.460(10) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 N7 1.380(11) . ? C47 C48 1.401(12) . ? C48 N8 1.377(11) . ? C49 N8 1.327(10) . ? C49 N7 1.344(10) . ? C49 H49 0.9500 . ? C50 N4 1.303(12) . ? C50 N5 1.343(13) . ? C50 C51 1.466(14) . ? C51 N6 1.376(11) . ? C51 C29 1.389(13) 3_766 ? C52 C53 1.387(17) . ? C52 N5 1.487(13) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.403(16) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 N4 1.467(11) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.377(13) . ? C55 N20 1.386(11) . ? C55 C58 1.471(14) . ? C56 N19 1.380(11) . ? C57 N19 1.329(10) . ? C57 N20 1.331(10) . ? C57 H57 0.9500 . ? C58 N21 1.328(12) . ? C58 N22 1.330(12) . ? C59 C60 1.459(14) . ? C59 N21 1.465(11) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.391(15) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 N22 1.463(13) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 N34 1.462(11) . ? C62 C106 1.466(16) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C64 C106 1.317(16) . ? C64 N35 1.467(14) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N34 1.311(11) . ? C65 N35 1.329(12) . ? C65 C66 1.495(15) . ? C66 C27 1.386(13) 3_766 ? C66 N36 1.386(11) . ? C67 N31 1.313(11) 3_766 ? C67 N6 1.341(10) . ? C67 H67 0.9500 . ? C100 H10X 0.9900 . ? C100 H10Y 0.9900 . ? C101 H10E 0.9900 . ? C101 H10F 0.9900 . ? C102 H10G 0.9900 . ? C102 H10H 0.9900 . ? C103 H10I 0.9900 . ? C103 H10J 0.9900 . ? C104 H10C 0.9900 . ? C104 H10D 0.9900 . ? C106 H63A 0.9900 . ? C106 H63B 0.9900 . ? N3 H706 0.85(6) . ? N10 H705 0.86(9) . ? N11 H704 0.83(17) . ? N23 H701 0.86(9) . ? N28 H703 0.96(7) . ? N31 C67 1.313(11) 3_766 ? N36 C28 1.321(10) 3_766 ? N206 H702 0.90(9) . ? N600 C701 1.25(2) . ? N600 C601 1.38(2) . ? N600 C600 1.42(3) . ? O300 C701 1.23(2) . ? C600 H60C 0.9800 . ? C600 H60D 0.9800 . ? C600 H60E 0.9800 . ? C601 H60F 0.9800 . ? C601 H60G 0.9800 . ? C601 H60H 0.9800 . ? C701 H730 0.9500 . ? O100 O101 1.22(4) . ? O103 O104 0.84(6) . ? O109 O110 1.17(5) . ? O110 O111 1.48(5) . ? O112 O113 1.61(4) . ? O113 O114 1.51(3) . ? O115 O116 0.75(2) . ? O119 O120 0.93(3) . ? O500 O517 0.91(5) . ? O500 O506 1.23(6) . ? O500 O503 1.42(6) . ? O500 O507 1.77(6) . ? O501 O511 0.83(9) . ? O501 O510 1.17(3) . ? O501 O506 1.44(3) . ? O501 O503 1.51(4) . ? O502 O518 0.82(6) . ? O502 O509 1.08(7) . ? O502 O512 1.35(6) . ? O503 O506 1.26(3) . ? O503 O517 1.44(4) . ? O503 O512 1.45(6) . ? O503 O508 1.72(4) . ? O504 O514 0.78(12) . ? O504 O505 1.11(5) . ? O505 O514 1.65(12) . ? O506 O517 1.30(3) . ? O506 O511 1.50(9) . ? O506 O507 1.51(3) . ? O508 O517 1.08(3) . ? O509 O518 0.67(9) . ? O509 O512 1.22(7) . ? O509 O514 1.52(11) . ? O510 O511 1.81(10) . ? O512 O518 1.62(9) . ? 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 N13 Co1 N8 94.1(3) . . ? N13 Co1 N6 93.1(3) . . ? N8 Co1 N6 94.0(4) . . ? N13 Co1 N9 90.6(3) . . ? N8 Co1 N9 80.8(4) . . ? N6 Co1 N9 173.8(3) . . ? N13 Co1 N4 173.6(4) . . ? N8 Co1 N4 89.9(3) . . ? N6 Co1 N4 81.6(4) . . ? N9 Co1 N4 95.0(4) . . ? N13 Co1 N18 81.0(3) . . ? N8 Co1 N18 174.1(4) . . ? N6 Co1 N18 89.5(3) . . ? N9 Co1 N18 95.9(3) . . ? N4 Co1 N18 95.3(3) . . ? N25 Co2 N19 93.4(3) . . ? N25 Co2 N31 92.5(4) . . ? N19 Co2 N31 93.0(3) . . ? N25 Co2 N27 81.6(3) . . ? N19 Co2 N27 174.3(3) . . ? N31 Co2 N27 90.0(3) . . ? N25 Co2 N32 173.7(4) . . ? N19 Co2 N32 90.1(3) . . ? N31 Co2 N32 82.1(4) . . ? N27 Co2 N32 95.1(3) . . ? N25 Co2 N24 89.7(3) . . ? N19 Co2 N24 81.6(4) . . ? N31 Co2 N24 174.3(3) . . ? N27 Co2 N24 95.5(3) . . ? N32 Co2 N24 95.9(4) . . ? N26 Co3 N1 93.2(3) . . ? N26 Co3 N7 93.8(3) . . ? N1 Co3 N7 92.1(4) . . ? N26 Co3 N2 174.7(4) . . ? N1 Co3 N2 82.3(4) . . ? N7 Co3 N2 89.3(3) . . ? N26 Co3 N12 90.4(3) . . ? N1 Co3 N12 173.2(3) . . ? N7 Co3 N12 81.9(4) . . ? N2 Co3 N12 94.3(3) . . ? N26 Co3 N30 80.5(3) . . ? N1 Co3 N30 90.4(3) . . ? N7 Co3 N30 173.9(3) . . ? N2 Co3 N30 96.6(3) . . ? N12 Co3 N30 95.8(3) . . ? N20 Co4 N14 92.5(3) . . ? N20 Co4 N36 93.0(4) . . ? N14 Co4 N36 93.0(3) . . ? N20 Co4 N21 82.3(4) . . ? N14 Co4 N21 90.2(3) . . ? N36 Co4 N21 174.4(3) . . ? N20 Co4 N15 173.9(4) . . ? N14 Co4 N15 81.7(4) . . ? N36 Co4 N15 89.3(3) . . ? N21 Co4 N15 95.8(3) . . ? N20 Co4 N34 90.2(3) . . ? N14 Co4 N34 174.3(4) . . ? N36 Co4 N34 81.9(4) . . ? N21 Co4 N34 95.0(4) . . ? N15 Co4 N34 95.8(3) . . ? O14 S1 O12 79.9(14) . . ? O14 S1 O13 80.0(13) . . ? O12 S1 O13 159.6(12) . . ? O14 S1 O10 123.3(9) . . ? O12 S1 O10 95.9(9) . . ? O13 S1 O10 92.5(8) . . ? O14 S1 O11 124.9(10) . . ? O12 S1 O11 92.6(10) . . ? O13 S1 O11 101.5(9) . . ? O10 S1 O11 111.7(7) . . ? O5 S2 O6 111.5(7) . . ? O5 S2 O7 110.8(5) . . ? O6 S2 O7 111.0(5) . . ? O5 S2 O8 110.5(6) . . ? O6 S2 O8 108.5(5) . . ? O7 S2 O8 104.3(4) . . ? O1 S3 O3 111.6(4) . . ? O1 S3 O2 111.5(5) . . ? O3 S3 O2 110.4(4) . . ? O1 S3 O4 107.4(4) . . ? O3 S3 O4 109.3(4) . . ? O2 S3 O4 106.3(4) . . ? N13 C1 N14 111.3(8) . . ? N13 C1 H1 124.4 . . ? N14 C1 H1 124.4 . . ? C3 C2 N13 107.5(8) . . ? C3 C2 C8 141.2(10) . . ? N13 C2 C8 110.8(9) . . ? N14 C3 C2 107.5(8) . . ? N14 C3 C4 110.5(9) . . ? C2 C3 C4 141.9(10) . . ? N15 C4 N16 126.5(9) . . ? N15 C4 C3 113.3(9) . . ? N16 C4 C3 120.3(10) . . ? C103 C5 N16 111.9(12) . . ? C103 C5 C102 52.0(11) . . ? N16 C5 C102 112.7(11) . . ? C103 C5 H5A 139.0 . . ? N16 C5 H5A 109.1 . . ? C102 C5 H5A 109.1 . . ? C103 C5 H5B 60.2 . . ? N16 C5 H5B 109.1 . . ? C102 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N15 C7 C103 111.5(12) . . ? N15 C7 C102 113.6(11) . . ? C103 C7 C102 51.1(11) . . ? N15 C7 H7A 108.8 . . ? C103 C7 H7A 61.3 . . ? C102 C7 H7A 108.8 . . ? N15 C7 H7B 108.8 . . ? C103 C7 H7B 139.6 . . ? C102 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N18 C8 N17 125.8(9) . . ? N18 C8 C2 113.1(10) . . ? N17 C8 C2 121.1(10) . . ? C10 C9 N18 110.8(8) . . ? C10 C9 H9A 109.5 . . ? N18 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? N18 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 123.2(13) . . ? C11 C10 H10A 106.5 . . ? C9 C10 H10A 106.5 . . ? C11 C10 H10B 106.5 . . ? C9 C10 H10B 106.5 . . ? H10A C10 H10B 106.5 . . ? C10 C11 N17 111.5(10) . . ? C10 C11 H11A 109.3 . . ? N17 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? N17 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N25 C12 N26 113.0(8) . . ? N25 C12 H12 123.5 . . ? N26 C12 H12 123.5 . . ? N25 C13 C14 107.7(8) . . ? N25 C13 C15 109.9(9) . . ? C14 C13 C15 142.3(10) . . ? N26 C14 C13 106.9(8) . . ? N26 C14 C19 111.4(8) . . ? C13 C14 C19 141.4(9) . . ? N27 C15 N28 125.9(9) . . ? N27 C15 C13 112.8(9) . . ? N28 C15 C13 121.1(10) . . ? N27 C16 C104 110.5(8) . . ? N27 C16 H16A 109.5 . . ? C104 C16 H16A 109.5 . . ? N27 C16 H16B 109.5 . . ? C104 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C104 C18 N28 109.8(9) . . ? C104 C18 H18A 109.7 . . ? N28 C18 H18A 109.7 . . ? C104 C18 H18B 109.7 . . ? N28 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N30 C19 N206 124.1(9) . . ? N30 C19 C14 113.3(9) . . ? N206 C19 C14 122.6(9) . . ? N206 C20 C21 110.0(8) . . ? N206 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? N206 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 C21 C22 113.3(8) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N30 C22 C21 110.1(8) . . ? N30 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? N30 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.2 . . ? N2 C23 C24 111.9(8) . . ? N2 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? N2 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 112.0(9) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N3 C25 C24 107.0(9) . . ? N3 C25 H25A 110.3 . . ? C24 C25 H25A 110.3 . . ? N3 C25 H25B 110.3 . . ? C24 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? N2 C26 N3 124.3(9) . . ? N2 C26 C27 114.4(10) . . ? N3 C26 C27 121.2(11) . . ? N1 C27 C66 107.4(9) . 3_766 ? N1 C27 C26 110.2(10) . . ? C66 C27 C26 142.3(11) 3_766 . ? N36 C28 N1 112.3(9) 3_766 . ? N36 C28 H28 123.9 3_766 . ? N1 C28 H28 123.9 . . ? N31 C29 C51 106.2(10) . 3_766 ? N31 C29 C30 112.4(11) . . ? C51 C29 C30 141.4(10) 3_766 . ? N33 C30 N32 123.2(11) . . ? N33 C30 C29 123.3(11) . . ? N32 C30 C29 113.5(10) . . ? N33 C31 C32 108.9(10) . . ? N33 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? N33 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? C31 C32 C33 113.7(10) . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32B 108.8 . . ? C33 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? N32 C33 C32 111.0(8) . . ? N32 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? N32 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? N24 C34 N23 125.4(10) . . ? N24 C34 C56 113.5(10) . . ? N23 C34 C56 121.0(10) . . ? C100 C35 N23 112.3(16) . . ? C100 C35 C101 43.8(19) . . ? N23 C35 C101 109.4(12) . . ? C100 C35 H35A 109.1 . . ? N23 C35 H35A 109.1 . . ? C101 C35 H35A 139.7 . . ? C100 C35 H35B 109.1 . . ? N23 C35 H35B 109.1 . . ? C101 C35 H35B 69.5 . . ? H35A C35 H35B 107.9 . . ? C101 C38 N24 113.1(13) . . ? C101 C38 C100 43.1(12) . . ? N24 C38 C100 110.8(12) . . ? C101 C38 H38A 135.7 . . ? N24 C38 H38A 109.5 . . ? C100 C38 H38A 109.5 . . ? C101 C38 H38B 68.6 . . ? N24 C38 H38B 109.5 . . ? C100 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? N9 C39 C40 112.0(8) . . ? N9 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? N9 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C41 C40 C39 110.7(10) . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? N10 C41 C40 108.6(8) . . ? N10 C41 H41A 110.0 . . ? C40 C41 H41A 110.0 . . ? N10 C41 H41B 110.0 . . ? C40 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? N9 C42 N10 124.5(10) . . ? N9 C42 C48 114.7(9) . . ? N10 C42 C48 120.3(10) . . ? N12 C43 N11 124.9(9) . . ? N12 C43 C47 112.4(11) . . ? N11 C43 C47 122.7(10) . . ? N11 C44 C45 109.7(9) . . ? N11 C44 H44A 109.7 . . ? C45 C44 H44A 109.7 . . ? N11 C44 H44B 109.7 . . ? C45 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? C44 C45 C46 110.8(8) . . ? C44 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? N12 C46 C45 111.4(7) . . ? N12 C46 H46A 109.4 . . ? C45 C46 H46A 109.4 . . ? N12 C46 H46B 109.4 . . ? C45 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? N7 C47 C48 107.3(8) . . ? N7 C47 C43 113.3(9) . . ? C48 C47 C43 139.4(11) . . ? N8 C48 C47 107.2(9) . . ? N8 C48 C42 109.5(9) . . ? C47 C48 C42 143.1(10) . . ? N8 C49 N7 112.1(9) . . ? N8 C49 H49 123.9 . . ? N7 C49 H49 123.9 . . ? N4 C50 N5 125.8(10) . . ? N4 C50 C51 114.3(11) . . ? N5 C50 C51 119.9(13) . . ? N6 C51 C29 107.7(9) . 3_766 ? N6 C51 C50 111.4(11) . . ? C29 C51 C50 140.6(12) 3_766 . ? C53 C52 N5 112.2(11) . . ? C53 C52 H52A 109.2 . . ? N5 C52 H52A 109.2 . . ? C53 C52 H52B 109.2 . . ? N5 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C52 C53 C54 120.2(15) . . ? C52 C53 H53A 107.3 . . ? C54 C53 H53A 107.3 . . ? C52 C53 H53B 107.3 . . ? C54 C53 H53B 107.3 . . ? H53A C53 H53B 106.9 . . ? C53 C54 N4 113.7(10) . . ? C53 C54 H54A 108.8 . . ? N4 C54 H54A 108.8 . . ? C53 C54 H54B 108.8 . . ? N4 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C56 C55 N20 107.1(9) . . ? C56 C55 C58 141.2(11) . . ? N20 C55 C58 111.1(10) . . ? C55 C56 N19 107.5(8) . . ? C55 C56 C34 140.7(11) . . ? N19 C56 C34 111.5(9) . . ? N19 C57 N20 111.6(8) . . ? N19 C57 H57 124.2 . . ? N20 C57 H57 124.2 . . ? N21 C58 N22 125.0(11) . . ? N21 C58 C55 113.7(10) . . ? N22 C58 C55 121.2(11) . . ? C60 C59 N21 113.6(9) . . ? C60 C59 H59A 108.8 . . ? N21 C59 H59A 108.8 . . ? C60 C59 H59B 108.8 . . ? N21 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C61 C60 C59 119.0(11) . . ? C61 C60 H60A 107.6 . . ? C59 C60 H60A 107.6 . . ? C61 C60 H60B 107.6 . . ? C59 C60 H60B 107.6 . . ? H60A C60 H60B 107.0 . . ? C60 C61 N22 113.2(10) . . ? C60 C61 H61A 108.9 . . ? N22 C61 H61A 108.9 . . ? C60 C61 H61B 108.9 . . ? N22 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? N34 C62 C106 111.6(9) . . ? N34 C62 H62A 109.3 . . ? C106 C62 H62A 109.3 . . ? N34 C62 H62B 109.3 . . ? C106 C62 H62B 109.3 . . ? H62A C62 H62B 108.0 . . ? C106 C64 N35 113.8(12) . . ? C106 C64 H64A 108.8 . . ? N35 C64 H64A 108.8 . . ? C106 C64 H64B 108.8 . . ? N35 C64 H64B 108.8 . . ? H64A C64 H64B 107.7 . . ? N34 C65 N35 126.4(11) . . ? N34 C65 C66 113.2(10) . . ? N35 C65 C66 120.4(11) . . ? C27 C66 N36 106.7(9) 3_766 . ? C27 C66 C65 142.0(10) 3_766 . ? N36 C66 C65 111.0(10) . . ? N31 C67 N6 111.4(9) 3_766 . ? N31 C67 H67 124.3 3_766 . ? N6 C67 H67 124.3 . . ? C35 C100 C38 120(3) . . ? C35 C100 H10X 107.2 . . ? C38 C100 H10X 107.2 . . ? C35 C100 H10Y 107.2 . . ? C38 C100 H10Y 107.2 . . ? H10X C100 H10Y 106.8 . . ? C38 C101 C35 109(2) . . ? C38 C101 H10E 109.9 . . ? C35 C101 H10E 109.9 . . ? C38 C101 H10F 109.9 . . ? C35 C101 H10F 109.9 . . ? H10E C101 H10F 108.3 . . ? C7 C102 C5 105.4(18) . . ? C7 C102 H10G 110.7 . . ? C5 C102 H10G 110.7 . . ? C7 C102 H10H 110.7 . . ? C5 C102 H10H 110.7 . . ? H10G C102 H10H 108.8 . . ? C5 C103 C7 110(2) . . ? C5 C103 H10I 109.6 . . ? C7 C103 H10I 109.6 . . ? C5 C103 H10J 109.6 . . ? C7 C103 H10J 109.6 . . ? H10I C103 H10J 108.1 . . ? C18 C104 C16 111.7(10) . . ? C18 C104 H10C 109.3 . . ? C16 C104 H10C 109.3 . . ? C18 C104 H10D 109.3 . . ? C16 C104 H10D 109.3 . . ? H10C C104 H10D 107.9 . . ? C64 C106 C62 122.2(15) . . ? C64 C106 H63A 106.8 . . ? C62 C106 H63A 106.8 . . ? C64 C106 H63B 106.8 . . ? C62 C106 H63B 106.8 . . ? H63A C106 H63B 106.6 . . ? C28 N1 C27 106.7(8) . . ? C28 N1 Co3 136.3(8) . . ? C27 N1 Co3 116.4(7) . . ? C26 N2 C23 117.7(8) . . ? C26 N2 Co3 115.3(7) . . ? C23 N2 Co3 125.6(7) . . ? C26 N3 C25 123.5(9) . . ? C26 N3 H706 108(5) . . ? C25 N3 H706 128(5) . . ? C50 N4 C54 118.6(9) . . ? C50 N4 Co1 116.4(7) . . ? C54 N4 Co1 124.8(8) . . ? C50 N5 C52 118.0(11) . . ? C67 N6 C51 106.7(9) . . ? C67 N6 Co1 137.0(8) . . ? C51 N6 Co1 116.1(7) . . ? C49 N7 C47 106.4(8) . . ? C49 N7 Co3 138.6(8) . . ? C47 N7 Co3 114.7(6) . . ? C49 N8 C48 107.1(8) . . ? C49 N8 Co1 134.7(8) . . ? C48 N8 Co1 118.0(7) . . ? C42 N9 C39 119.7(9) . . ? C42 N9 Co1 116.7(7) . . ? C39 N9 Co1 123.6(6) . . ? C42 N10 C41 119.4(8) . . ? C42 N10 H705 108(10) . . ? C41 N10 H705 124(10) . . ? C43 N11 C44 121.2(8) . . ? C43 N11 H704 110(10) . . ? C44 N11 H704 127(10) . . ? C43 N12 C46 118.8(8) . . ? C43 N12 Co3 117.0(7) . . ? C46 N12 Co3 123.7(6) . . ? C1 N13 C2 107.0(8) . . ? C1 N13 Co1 135.4(7) . . ? C2 N13 Co1 117.4(6) . . ? C1 N14 C3 106.7(8) . . ? C1 N14 Co4 136.1(7) . . ? C3 N14 Co4 116.7(7) . . ? C4 N15 C7 117.9(8) . . ? C4 N15 Co4 116.7(7) . . ? C7 N15 Co4 124.0(7) . . ? C4 N16 C5 117.8(9) . . ? C8 N17 C11 119.5(9) . . ? C8 N18 C9 118.9(8) . . ? C8 N18 Co1 117.3(7) . . ? C9 N18 Co1 123.6(6) . . ? C57 N19 C56 106.9(8) . . ? C57 N19 Co2 136.4(8) . . ? C56 N19 Co2 116.3(7) . . ? C57 N20 C55 106.9(8) . . ? C57 N20 Co4 136.4(8) . . ? C55 N20 Co4 116.6(7) . . ? C58 N21 C59 119.4(8) . . ? C58 N21 Co4 116.0(7) . . ? C59 N21 Co4 124.1(7) . . ? C58 N22 C61 119.1(9) . . ? C34 N23 C35 120.3(9) . . ? C34 N23 H701 119(10) . . ? C35 N23 H701 121(10) . . ? C34 N24 C38 117.7(9) . . ? C34 N24 Co2 116.5(7) . . ? C38 N24 Co2 124.7(7) . . ? C12 N25 C13 105.8(8) . . ? C12 N25 Co2 136.2(7) . . ? C13 N25 Co2 117.6(6) . . ? C12 N26 C14 106.6(8) . . ? C12 N26 Co3 135.9(7) . . ? C14 N26 Co3 117.3(6) . . ? C15 N27 C16 118.1(8) . . ? C15 N27 Co2 117.0(6) . . ? C16 N27 Co2 124.0(6) . . ? C15 N28 C18 119.3(8) . . ? C15 N28 H703 120(10) . . ? C18 N28 H703 115(10) . . ? C19 N30 C22 119.8(8) . . ? C19 N30 Co3 117.2(6) . . ? C22 N30 Co3 122.5(6) . . ? C67 N31 C29 108.1(9) 3_766 . ? C67 N31 Co2 136.0(7) 3_766 . ? C29 N31 Co2 115.6(9) . . ? C30 N32 C33 118.5(9) . . ? C30 N32 Co2 116.1(7) . . ? C33 N32 Co2 125.0(7) . . ? C30 N33 C31 123.1(10) . . ? C65 N34 C62 118.7(9) . . ? C65 N34 Co4 117.0(7) . . ? C62 N34 Co4 124.1(7) . . ? C65 N35 C64 117.9(10) . . ? C28 N36 C66 106.8(8) 3_766 . ? C28 N36 Co4 136.1(7) 3_766 . ? C66 N36 Co4 116.8(8) . . ? C19 N206 C20 122.0(8) . . ? C19 N206 H702 122(10) . . ? C20 N206 H702 115(10) . . ? C701 N600 C601 125(2) . . ? C701 N600 C600 120(2) . . ? C601 N600 C600 115(2) . . ? N600 C600 H60C 109.5 . . ? N600 C600 H60D 109.5 . . ? H60C C600 H60D 109.5 . . ? N600 C600 H60E 109.5 . . ? H60C C600 H60E 109.5 . . ? H60D C600 H60E 109.5 . . ? N600 C601 H60F 109.5 . . ? N600 C601 H60G 109.5 . . ? H60F C601 H60G 109.5 . . ? N600 C601 H60H 109.5 . . ? H60F C601 H60H 109.5 . . ? H60G C601 H60H 109.5 . . ? O300 C701 N600 124(2) . . ? O300 C701 H730 118.0 . . ? N600 C701 H730 118.0 . . ? O109 O110 O111 176(4) . . ? O114 O113 O112 122(3) . . ? O517 O500 O506 74(5) . . ? O517 O500 O503 73(5) . . ? O506 O500 O503 56(3) . . ? O517 O500 O507 122(6) . . ? O506 O500 O507 57(3) . . ? O503 O500 O507 100(4) . . ? O511 O501 O510 129(8) . . ? O511 O501 O506 77(7) . . ? O510 O501 O506 144(3) . . ? O511 O501 O503 126(8) . . ? O510 O501 O503 103(3) . . ? O506 O501 O503 50.3(16) . . ? O518 O502 O509 38(5) . . ? O518 O502 O512 93(6) . . ? O509 O502 O512 59(4) . . ? O506 O503 O500 54(3) . . ? O506 O503 O517 57(2) . . ? O500 O503 O517 37(2) . . ? O506 O503 O512 134(4) . . ? O500 O503 O512 81(4) . . ? O517 O503 O512 96(3) . . ? O506 O503 O501 62(2) . . ? O500 O503 O501 116(4) . . ? O517 O503 O501 105(3) . . ? O512 O503 O501 159(4) . . ? O506 O503 O508 84(2) . . ? O500 O503 O508 75(3) . . ? O517 O503 O508 38.9(15) . . ? O512 O503 O508 97(3) . . ? O501 O503 O508 98(2) . . ? O514 O504 O505 120(10) . . ? O504 O505 O514 24(5) . . ? O500 O506 O503 70(3) . . ? O500 O506 O517 42(3) . . ? O503 O506 O517 68(2) . . ? O500 O506 O501 137(4) . . ? O503 O506 O501 67(2) . . ? O517 O506 O501 117(2) . . ? O500 O506 O511 168(5) . . ? O503 O506 O511 100(4) . . ? O517 O506 O511 140(4) . . ? O501 O506 O511 33(3) . . ? O500 O506 O507 79(3) . . ? O503 O506 O507 124(3) . . ? O517 O506 O507 115(3) . . ? O501 O506 O507 127(2) . . ? O511 O506 O507 104(4) . . ? O506 O507 O500 43(2) . . ? O517 O508 O503 57(2) . . ? O518 O509 O502 50(8) . . ? O518 O509 O512 114(10) . . ? O502 O509 O512 72(5) . . ? O518 O509 O514 151(10) . . ? O502 O509 O514 159(9) . . ? O512 O509 O514 91(7) . . ? O501 O510 O511 21(3) . . ? O501 O511 O506 70(7) . . ? O501 O511 O510 30(5) . . ? O506 O511 O510 97(5) . . ? O509 O512 O502 49(4) . . ? O509 O512 O503 95(6) . . ? O502 O512 O503 128(5) . . ? O509 O512 O518 22(4) . . ? O502 O512 O518 31(3) . . ? O503 O512 O518 103(5) . . ? O504 O514 O509 101(10) . . ? O504 O514 O505 36(7) . . ? O509 O514 O505 124(9) . . ? O500 O517 O508 149(6) . . ? O500 O517 O506 64(4) . . ? O508 O517 O506 115(3) . . ? O500 O517 O503 70(4) . . ? O508 O517 O503 85(3) . . ? O506 O517 O503 54.2(17) . . ? O509 O518 O502 93(10) . . ? O509 O518 O512 44(8) . . ? O502 O518 O512 57(4) . . ? _diffrn_measured_fraction_theta_max 0.821 _diffrn_reflns_theta_full 53.42 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.613 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.085