# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Shie-Ming Peng.' 'Yi-Lin Huang.' 'Rayyat H Ismayilov' 'Gene-Hsiang Lee.' 'Wen-Zhen Wang.' 'Rui-Ren Wang.' 'Chen-Yu Yeh.' _publ_contact_author_name 'Shie-Ming Peng' _publ_contact_author_email SMPENG@NTU.EDU.TW _publ_section_title ; First stable reduced form of [Co5]+10: Fine tuning of linear pentacobalt(II) complexes containing delocalized metal-metal bonds through ligand modification ; # Attachment 'ic11731.cif' data_ic11731 _database_code_depnum_ccdc_archive 'CCDC 694067' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H40 Cl14 Co5 N28' _chemical_formula_weight 1896.11 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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 22.6213(4) _cell_length_b 12.8225(2) _cell_length_c 24.5904(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7132.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 1.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47098 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8193 _reflns_number_gt 5467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+43.8804P] 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 8193 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.04695(3) 0.62194(6) 0.66747(3) 0.02767(18) Uani 1 1 d . . . Co2 Co 0.02276(3) 0.55923(5) 0.58332(3) 0.02141(16) Uani 1 1 d . . . Co3 Co 0.0000 0.5000 0.5000 0.0193(2) Uani 1 2 d S . . Cl1 Cl 0.07171(7) 0.68576(13) 0.75662(5) 0.0425(4) Uani 1 1 d . . . N1 N 0.12146(19) 0.6708(4) 0.63325(17) 0.0324(10) Uani 1 1 d . . . N3 N 0.02556(17) 0.6303(3) 0.46777(15) 0.0217(8) Uani 1 1 d . . . N5 N 0.02971(19) 0.4372(3) 0.30933(16) 0.0290(10) Uani 1 1 d . . . N8 N 0.0846(2) 0.4850(4) 0.67872(17) 0.0314(10) Uani 1 1 d . . . N10 N 0.07933(17) 0.4445(3) 0.49212(16) 0.0224(8) Uani 1 1 d . . . N12 N -0.0066(2) 0.2491(3) 0.35487(18) 0.0322(10) Uani 1 1 d . . . C7 C 0.0624(3) 0.8159(4) 0.4233(2) 0.0365(13) Uani 1 1 d . . . H7A H 0.0777 0.8787 0.4084 0.044 Uiso 0.50 1 calc PR A 1 H7'A H 0.0733 0.8814 0.4084 0.044 Uiso 0.50 1 d PR A 2 C20 C 0.1918(2) 0.3656(5) 0.4817(2) 0.0377(13) Uani 1 1 d . . . H20A H 0.2294 0.3332 0.4789 0.045 Uiso 0.50 1 calc PR B 1 H20B H 0.2311 0.3408 0.4775 0.045 Uiso 0.50 1 d PR B 2 N2 N 0.0736(4) 0.6625(7) 0.5498(3) 0.0262(18) Uiso 0.50 1 d P C 1 N4 N 0.0253(3) 0.5459(6) 0.3849(3) 0.0215(16) Uiso 0.50 1 d P . 1 N6 N 0.2304(6) 0.7170(11) 0.5879(6) 0.035(4) Uiso 0.50 1 d P C 1 N7 N 0.1421(7) 0.5327(13) 0.2816(6) 0.040(5) Uiso 0.50 1 d P D 1 N9 N 0.0891(3) 0.4655(6) 0.5854(3) 0.0233(17) Uiso 0.50 1 d P C 1 N11 N 0.0603(4) 0.4340(7) 0.4013(3) 0.0267(18) Uiso 0.50 1 d P . 1 N13 N 0.1456(6) 0.3012(11) 0.6945(6) 0.040(4) Uiso 0.50 1 d P C 1 N14 N 0.0447(7) 0.0652(12) 0.3867(6) 0.050(4) Uiso 0.50 1 d P E 1 N2' N 0.0198(4) 0.6978(7) 0.5540(3) 0.0283(19) Uiso 0.50 1 d P . 2 N4' N -0.0233(3) 0.5806(6) 0.3902(3) 0.0214(16) Uiso 0.50 1 d P . 2 N7' N 0.1332(7) 0.5232(12) 0.2736(6) 0.037(4) Uiso 0.50 1 d P F 2 N9' N 0.1035(3) 0.5490(6) 0.5648(3) 0.0235(17) Uiso 0.50 1 d P C 2 N6' N 0.2257(7) 0.7354(13) 0.5800(6) 0.043(5) Uiso 0.50 1 d P C 2 N11' N 0.0415(3) 0.3477(6) 0.4201(3) 0.0239(17) Uiso 0.50 1 d P . 2 N13' N 0.1329(6) 0.2823(10) 0.6941(5) 0.033(3) Uiso 0.50 1 d P C 2 N14' N 0.0615(6) 0.0735(10) 0.3882(5) 0.033(3) Uiso 0.50 1 d P G 2 C1 C 0.1563(5) 0.7402(11) 0.6568(5) 0.040(3) Uiso 0.50 1 d P C 1 H1A H 0.1439 0.7732 0.6895 0.048 Uiso 0.50 1 calc PR C 1 C2 C 0.2103(6) 0.7653(12) 0.6347(5) 0.045(3) Uiso 0.50 1 d P C 1 H2A H 0.2341 0.8166 0.6518 0.054 Uiso 0.50 1 calc PR C 1 C3 C 0.1933(5) 0.6562(10) 0.5644(5) 0.042(3) Uiso 0.50 1 d P C 1 H3A H 0.2024 0.6339 0.5285 0.050 Uiso 0.50 1 calc PR C 1 C4 C 0.1397(5) 0.6197(9) 0.5876(4) 0.030(2) Uiso 0.50 1 d P C 1 C5 C 0.0323(5) 0.7160(8) 0.5001(4) 0.027(2) Uiso 0.50 1 d P C 1 C6 C 0.0518(6) 0.8071(10) 0.4789(5) 0.035(3) Uiso 0.50 1 d P C 1 H6A H 0.0582 0.8654 0.5021 0.042 Uiso 0.50 1 calc PR C 1 C8 C 0.0508(6) 0.7348(10) 0.3913(5) 0.028(3) Uiso 0.50 1 d P C 1 H8A H 0.0532 0.7423 0.3529 0.033 Uiso 0.50 1 calc PR C 1 C9 C 0.0353(5) 0.6391(8) 0.4138(4) 0.024(2) Uiso 0.50 1 d P C 1 C10 C 0.0529(4) 0.5188(8) 0.3379(4) 0.024(2) Uiso 0.50 1 d P D 1 C11 C 0.1074(5) 0.5598(9) 0.3194(4) 0.032(2) Uiso 0.50 1 d P D 1 H11A H 0.1205 0.6191 0.3392 0.039 Uiso 0.50 1 calc PR D 1 C12 C 0.1086(5) 0.4473(10) 0.2485(5) 0.035(2) Uiso 0.50 1 d P D 1 H12A H 0.1257 0.4235 0.2154 0.042 Uiso 0.50 1 calc PR D 1 C13 C 0.0565(5) 0.4053(10) 0.2644(4) 0.031(2) Uiso 0.50 1 d P D 1 H13A H 0.0389 0.3520 0.2431 0.037 Uiso 0.50 1 calc PR D 1 C14 C 0.0979(5) 0.4458(9) 0.7280(5) 0.035(3) Uiso 0.50 1 d P C 1 H14A H 0.0887 0.4861 0.7593 0.042 Uiso 0.50 1 calc PR C 1 C15 C 0.1239(6) 0.3515(10) 0.7350(5) 0.041(3) Uiso 0.50 1 d P C 1 H15A H 0.1261 0.3222 0.7704 0.050 Uiso 0.50 1 calc PR C 1 C16 C 0.1325(5) 0.3285(10) 0.6457(5) 0.038(3) Uiso 0.50 1 d P C 1 H16A H 0.1406 0.2826 0.6163 0.046 Uiso 0.50 1 calc PR C 1 C17 C 0.1052(4) 0.4292(8) 0.6351(4) 0.027(2) Uiso 0.50 1 d P C 1 C18 C 0.1157(5) 0.4355(10) 0.5367(4) 0.026(2) Uiso 0.50 1 d P C 1 C19 C 0.1735(5) 0.3988(10) 0.5315(5) 0.024(3) Uiso 0.50 1 d P C 1 H19A H 0.1993 0.3969 0.5619 0.029 Uiso 0.50 1 calc PR C 1 C21 C 0.1586(5) 0.3767(10) 0.4355(5) 0.032(3) Uiso 0.50 1 d P C 1 C23 C -0.0003(5) 0.2274(9) 0.4097(5) 0.034(2) Uiso 0.50 1 d P E 1 H23A H -0.0162 0.2727 0.4365 0.040 Uiso 0.50 1 calc PR E 1 C24 C 0.0309(5) 0.1346(10) 0.4250(5) 0.041(3) Uiso 0.50 1 d P E 1 H24A H 0.0415 0.1228 0.4618 0.049 Uiso 0.50 1 calc PR E 1 C25 C 0.0496(6) 0.0910(11) 0.3389(5) 0.048(3) Uiso 0.50 1 d P E 1 H25A H 0.0731 0.0513 0.3145 0.057 Uiso 0.50 1 calc PR E 1 C26 C 0.0195(6) 0.1811(10) 0.3211(6) 0.048(3) Uiso 0.50 1 d P E 1 H26A H 0.0176 0.1943 0.2831 0.057 Uiso 0.50 1 calc PR E 1 C1' C 0.1718(5) 0.6897(9) 0.6608(5) 0.032(2) Uiso 0.50 1 d P C 2 H1'A H 0.1709 0.6850 0.6993 0.039 Uiso 0.50 1 calc PR C 2 C2' C 0.2240(6) 0.7154(11) 0.6364(5) 0.041(3) Uiso 0.50 1 d P C 2 H2'A H 0.2592 0.7198 0.6574 0.050 Uiso 0.50 1 calc PR C 2 C3' C 0.1784(5) 0.7119(9) 0.5537(4) 0.030(2) Uiso 0.50 1 d P C 2 H3'A H 0.1806 0.7119 0.5151 0.036 Uiso 0.50 1 calc PR C 2 C4' C 0.1234(5) 0.6861(8) 0.5773(4) 0.029(2) Uiso 0.50 1 d P C 2 C5' C 0.0624(5) 0.6959(8) 0.4975(4) 0.024(2) Uiso 0.50 1 d P C 2 C6' C 0.0778(5) 0.7928(9) 0.4763(4) 0.029(2) Uiso 0.50 1 d P C 2 H6'A H 0.0986 0.8421 0.4979 0.035 Uiso 0.50 1 calc PR C 2 C8' C 0.0314(6) 0.7458(10) 0.3914(5) 0.028(3) Uiso 0.50 1 d P C 2 H8'A H 0.0241 0.7597 0.3541 0.033 Uiso 0.50 1 calc PR C 2 C9' C 0.0112(5) 0.6542(8) 0.4157(4) 0.024(2) Uiso 0.50 1 d P C 2 C10' C 0.0762(4) 0.4523(8) 0.3466(4) 0.027(2) Uiso 0.50 1 d P F 2 H10A H 0.0718 0.4295 0.3831 0.032 Uiso 0.50 1 calc PR F 2 C11' C 0.1290(6) 0.5006(10) 0.3305(5) 0.043(3) Uiso 0.50 1 d P F 2 H11B H 0.1596 0.5172 0.3555 0.052 Uiso 0.50 1 calc PR F 2 C12' C 0.0970(7) 0.5030(13) 0.2427(6) 0.054(3) Uiso 0.50 1 d P F 2 H12B H 0.1036 0.5183 0.2054 0.065 Uiso 0.50 1 calc PR F 2 C13' C 0.0448(6) 0.4576(11) 0.2575(5) 0.040(3) Uiso 0.50 1 d P F 2 H13B H 0.0176 0.4396 0.2296 0.048 Uiso 0.50 1 calc PR F 2 C14' C 0.1269(6) 0.4725(10) 0.7139(5) 0.039(3) Uiso 0.50 1 d P C 2 H14B H 0.1397 0.5306 0.7348 0.047 Uiso 0.50 1 calc PR C 2 C15' C 0.1534(6) 0.3775(11) 0.7217(6) 0.048(3) Uiso 0.50 1 d P C 2 H15B H 0.1861 0.3730 0.7458 0.058 Uiso 0.50 1 calc PR C 2 C16' C 0.0905(5) 0.3019(9) 0.6601(5) 0.035(2) Uiso 0.50 1 d P C 2 H16B H 0.0762 0.2444 0.6395 0.042 Uiso 0.50 1 calc PR C 2 C17' C 0.0630(5) 0.4003(9) 0.6501(4) 0.030(2) Uiso 0.50 1 d P . 2 C18' C 0.1214(5) 0.4772(9) 0.5266(4) 0.026(2) Uiso 0.50 1 d P C 2 C19' C 0.1779(5) 0.4330(10) 0.5245(5) 0.029(3) Uiso 0.50 1 d P C 2 H19B H 0.2063 0.4486 0.5518 0.034 Uiso 0.50 1 calc PR C 2 C21' C 0.1468(5) 0.3340(10) 0.4443(5) 0.031(2) Uiso 0.50 1 d P C 2 C22 C 0.1005(4) 0.4198(8) 0.4422(4) 0.023(2) Uiso 0.50 1 d P C 2 C22' C 0.0900(4) 0.3712(9) 0.4523(4) 0.024(2) Uiso 0.50 1 d P C 2 C23' C 0.0358(5) 0.2528(8) 0.3938(4) 0.030(2) Uiso 0.50 1 d P . 2 C24' C 0.0658(5) 0.1607(9) 0.4074(5) 0.037(3) Uiso 0.50 1 d P G 2 H24B H 0.0938 0.1673 0.4361 0.045 Uiso 0.50 1 calc PR G 2 C25' C 0.0100(5) 0.0689(9) 0.3453(4) 0.034(2) Uiso 0.50 1 d P G 2 H25B H -0.0009 0.0044 0.3292 0.040 Uiso 0.50 1 calc PR G 2 C26' C -0.0184(5) 0.1571(9) 0.3315(5) 0.036(3) Uiso 0.50 1 d P G 2 H26B H -0.0480 0.1540 0.3042 0.044 Uiso 0.50 1 calc PR G 2 C1S C 0.1559(3) 0.4165(7) 0.0565(3) 0.069(2) Uani 1 1 d . . . H1SA H 0.1770 0.3496 0.0640 0.082 Uiso 1 1 calc R . . Cl1S Cl 0.17589(10) 0.4610(2) -0.00831(10) 0.0820(6) Uani 1 1 d . . . Cl2S Cl 0.08044(10) 0.3954(2) 0.06085(14) 0.1107(10) Uani 1 1 d . . . Cl3S Cl 0.17756(14) 0.5097(3) 0.10488(13) 0.1230(11) Uani 1 1 d . . . C2S C 0.2951(3) 0.3092(7) 0.3313(3) 0.068(2) Uani 1 1 d . . . H2SA H 0.3339 0.2895 0.3146 0.082 Uiso 1 1 calc R . . Cl4S Cl 0.27907(11) 0.2193(2) 0.38276(11) 0.0933(8) Uani 1 1 d . . . Cl5S Cl 0.30170(12) 0.4349(2) 0.35808(10) 0.0933(8) Uani 1 1 d . . . Cl6S Cl 0.24175(12) 0.3084(3) 0.28052(11) 0.1087(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0309(4) 0.0301(4) 0.0220(3) -0.0028(3) 0.0001(3) 0.0001(3) Co2 0.0222(3) 0.0218(3) 0.0202(3) -0.0006(3) 0.0016(3) 0.0010(3) Co3 0.0202(4) 0.0178(4) 0.0198(4) 0.0009(4) 0.0020(4) 0.0012(4) Cl1 0.0498(9) 0.0513(9) 0.0263(7) -0.0103(6) -0.0025(6) -0.0019(7) N1 0.032(2) 0.036(3) 0.030(2) -0.006(2) -0.0007(19) -0.004(2) N3 0.023(2) 0.0189(19) 0.023(2) 0.0011(16) 0.0036(16) -0.0002(17) N5 0.035(2) 0.033(2) 0.019(2) -0.0033(18) 0.0024(18) 0.003(2) N8 0.035(2) 0.037(3) 0.022(2) 0.0005(19) -0.0042(18) 0.005(2) N10 0.023(2) 0.020(2) 0.025(2) 0.0012(17) 0.0013(16) 0.0041(16) N12 0.042(3) 0.025(2) 0.030(2) -0.0073(19) 0.003(2) 0.000(2) C7 0.040(3) 0.025(3) 0.044(3) 0.012(2) 0.010(3) -0.001(2) C20 0.025(3) 0.044(3) 0.044(3) -0.002(3) 0.001(2) 0.012(2) C1S 0.045(4) 0.078(6) 0.083(6) 0.028(5) -0.001(4) -0.006(4) Cl1S 0.0794(15) 0.0856(16) 0.0811(15) 0.0193(12) 0.0056(12) -0.0060(12) Cl2S 0.0458(12) 0.108(2) 0.178(3) 0.024(2) 0.0206(15) -0.0055(12) Cl3S 0.101(2) 0.162(3) 0.106(2) -0.032(2) 0.0308(17) -0.025(2) C2S 0.054(4) 0.085(6) 0.067(5) -0.018(5) 0.009(4) -0.005(4) Cl4S 0.0886(16) 0.0862(17) 0.1051(18) 0.0040(14) 0.0484(14) 0.0240(13) Cl5S 0.0947(17) 0.0972(19) 0.0881(16) -0.0223(14) -0.0017(13) -0.0243(14) Cl6S 0.0847(17) 0.149(3) 0.0928(17) -0.0275(18) -0.0218(14) -0.0291(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 N12 1.967(5) 5_566 ? Co1 N8 1.970(5) . ? Co1 N5 1.977(4) 5_566 ? Co1 N1 1.985(4) . ? Co1 Co2 2.2865(9) . ? Co1 Cl1 2.4062(15) . ? Co2 N11' 1.883(8) 5_566 ? Co2 N9' 1.887(8) . ? Co2 N4 1.900(8) 5_566 ? Co2 N4' 1.908(8) 5_566 ? Co2 N2' 1.919(9) . ? Co2 N11 1.920(8) 5_566 ? Co2 N9 1.923(8) . ? Co2 N2 1.937(8) . ? Co2 Co3 2.2449(6) . ? Co3 N3 1.937(4) 5_566 ? Co3 N3 1.937(4) . ? Co3 N10 1.940(4) 5_566 ? Co3 N10 1.940(4) . ? Co3 Co2 2.2449(6) 5_566 ? N1 C1 1.322(13) . ? N1 C1' 1.347(12) . ? N1 C4 1.364(11) . ? N1 C4' 1.389(11) . ? N3 C9 1.351(11) . ? N3 C9' 1.355(11) . ? N3 C5 1.365(11) . ? N3 C5' 1.391(11) . ? N5 C13 1.324(12) . ? N5 C13' 1.345(13) . ? N5 C10 1.366(11) . ? N5 C10' 1.409(11) . ? N5 Co1 1.977(4) 5_566 ? N8 C14' 1.301(13) . ? N8 C14 1.346(12) . ? N8 C17 1.371(11) . ? N8 C17' 1.383(12) . ? N10 C18' 1.341(11) . ? N10 C22 1.354(10) . ? N10 C18 1.377(11) . ? N10 C22' 1.379(11) . ? N12 C26' 1.339(12) . ? N12 C26 1.341(14) . ? N12 C23' 1.357(11) . ? N12 C23 1.384(12) . ? N12 Co1 1.967(5) 5_566 ? C7 C8 1.329(13) . ? C7 C8' 1.382(13) . ? C7 C6' 1.382(12) . ? C7 C6 1.394(13) . ? C20 C19 1.361(12) . ? C20 C21 1.369(12) . ? C20 C19' 1.398(13) . ? C20 C21' 1.432(13) . ? N2 C5 1.685(13) . ? N2 C4 1.845(13) . ? N4 C10 1.360(12) . ? N4 C9 1.408(13) . ? N4 N11 1.687(11) . ? N4 Co2 1.900(8) 5_566 ? N6 C3 1.283(19) . ? N6 C2 1.38(2) . ? N7 C11 1.266(19) . ? N7 C12 1.560(19) . ? N9 C17 1.359(12) . ? N9 C18 1.393(13) . ? N11 C10 1.908(13) . ? N11 Co2 1.920(8) 5_566 ? N13 C15 1.283(18) . ? N13 C16 1.286(18) . ? N14 C25 1.224(19) . ? N14 C24 1.334(19) . ? N2' N11' 1.635(11) 5_566 ? N2' C5' 1.690(13) . ? N2' C23' 1.906(14) 5_566 ? N4' C17' 1.358(13) 5_566 ? N4' C9' 1.378(13) . ? N4' Co2 1.908(8) 5_566 ? N7' C12' 1.146(19) . ? N7' C11' 1.43(2) . ? N9' C18' 1.376(13) . ? N9' C4' 1.840(13) . ? N6' C3' 1.285(19) . ? N6' C2' 1.41(2) . ? N11' C23' 1.384(13) . ? N11' C22' 1.385(12) . ? N11' N2' 1.635(11) 5_566 ? N11' C22 1.712(13) . ? N11' Co2 1.883(8) 5_566 ? N13' C16' 1.298(16) . ? N13' C15' 1.471(19) . ? N14' C24' 1.218(16) . ? N14' C25' 1.573(17) . ? C1 C2 1.375(17) . ? C3 C4 1.420(16) . ? C5 C6 1.353(16) . ? C8 C9 1.391(16) . ? C10 C11 1.415(14) . ? C12 C13 1.354(16) . ? C14 C15 1.356(17) . ? C16 C17 1.455(16) . ? C18 C19 1.394(15) . ? C23 C24 1.433(16) . ? C25 C26 1.412(18) . ? C1' C2' 1.365(17) . ? C3' C4' 1.412(15) . ? C5' C6' 1.392(15) . ? C8' C9' 1.394(16) . ? C10' C11' 1.402(16) . ? C12' C13' 1.367(19) . ? C14' C15' 1.371(18) . ? C16' C17' 1.429(15) . ? C17' N4' 1.358(13) 5_566 ? C18' C19' 1.400(16) . ? C21' C22' 1.385(15) . ? C21' C22 1.519(15) . ? C22 C22' 0.711(11) . ? C23' C24' 1.403(16) . ? C23' N2' 1.906(14) 5_566 ? C25' C26' 1.344(16) . ? C1S Cl2S 1.731(7) . ? C1S Cl1S 1.751(8) . ? C1S Cl3S 1.756(9) . ? C2S Cl6S 1.737(8) . ? C2S Cl5S 1.748(9) . ? C2S Cl4S 1.750(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 N12 Co1 N8 171.33(18) 5_566 . ? N12 Co1 N5 89.77(19) 5_566 5_566 ? N8 Co1 N5 89.80(19) . 5_566 ? N12 Co1 N1 90.58(19) 5_566 . ? N8 Co1 N1 88.52(19) . . ? N5 Co1 N1 171.18(17) 5_566 . ? N12 Co1 Co2 86.09(13) 5_566 . ? N8 Co1 Co2 85.24(12) . . ? N5 Co1 Co2 85.21(12) 5_566 . ? N1 Co1 Co2 86.02(13) . . ? N12 Co1 Cl1 94.39(14) 5_566 . ? N8 Co1 Cl1 94.28(13) . . ? N5 Co1 Cl1 94.10(13) 5_566 . ? N1 Co1 Cl1 94.66(13) . . ? Co2 Co1 Cl1 179.16(6) . . ? N11' Co2 N9' 141.3(4) 5_566 . ? N11' Co2 N4 91.5(3) 5_566 5_566 ? N9' Co2 N4 127.2(3) . 5_566 ? N11' Co2 N4' 128.0(3) 5_566 5_566 ? N9' Co2 N4' 90.6(3) . 5_566 ? N4 Co2 N4' 36.6(3) 5_566 5_566 ? N11' Co2 N2' 50.9(3) 5_566 . ? N9' Co2 N2' 90.4(4) . . ? N4 Co2 N2' 142.3(3) 5_566 . ? N4' Co2 N2' 177.4(3) 5_566 . ? N11' Co2 N11 39.1(3) 5_566 5_566 ? N9' Co2 N11 177.1(3) . 5_566 ? N4 Co2 N11 52.4(3) 5_566 5_566 ? N4' Co2 N11 88.9(3) 5_566 5_566 ? N2' Co2 N11 89.9(4) . 5_566 ? N11' Co2 N9 178.7(4) 5_566 . ? N9' Co2 N9 37.6(3) . . ? N4 Co2 N9 89.6(3) 5_566 . ? N4' Co2 N9 53.0(3) 5_566 . ? N2' Co2 N9 128.0(3) . . ? N11 Co2 N9 141.9(3) 5_566 . ? N11' Co2 N2 90.3(4) 5_566 . ? N9' Co2 N2 51.0(3) . . ? N4 Co2 N2 178.0(3) 5_566 . ? N4' Co2 N2 141.6(3) 5_566 . ? N2' Co2 N2 39.4(3) . . ? N11 Co2 N2 129.3(4) 5_566 . ? N9 Co2 N2 88.6(3) . . ? N11' Co2 Co3 89.8(2) 5_566 . ? N9' Co2 Co3 88.8(2) . . ? N4 Co2 Co3 90.2(2) 5_566 . ? N4' Co2 Co3 89.8(2) 5_566 . ? N2' Co2 Co3 87.8(3) . . ? N11 Co2 Co3 88.3(2) 5_566 . ? N9 Co2 Co3 89.5(2) . . ? N2 Co2 Co3 88.8(2) . . ? N11' Co2 Co1 90.1(2) 5_566 . ? N9' Co2 Co1 90.6(2) . . ? N4 Co2 Co1 90.8(2) 5_566 . ? N4' Co2 Co1 91.1(2) 5_566 . ? N2' Co2 Co1 91.3(3) . . ? N11 Co2 Co1 92.3(2) 5_566 . ? N9 Co2 Co1 90.5(2) . . ? N2 Co2 Co1 90.1(2) . . ? Co3 Co2 Co1 178.95(4) . . ? N3 Co3 N3 180.0(2) 5_566 . ? N3 Co3 N10 89.95(16) 5_566 5_566 ? N3 Co3 N10 90.05(16) . 5_566 ? N3 Co3 N10 90.05(16) 5_566 . ? N3 Co3 N10 89.95(16) . . ? N10 Co3 N10 180.0(2) 5_566 . ? N3 Co3 Co2 89.24(12) 5_566 . ? N3 Co3 Co2 90.76(12) . . ? N10 Co3 Co2 89.82(12) 5_566 . ? N10 Co3 Co2 90.18(12) . . ? N3 Co3 Co2 90.76(12) 5_566 5_566 ? N3 Co3 Co2 89.24(12) . 5_566 ? N10 Co3 Co2 90.18(12) 5_566 5_566 ? N10 Co3 Co2 89.82(12) . 5_566 ? Co2 Co3 Co2 180.0 . 5_566 ? C1 N1 C1' 32.3(6) . . ? C1 N1 C4 120.3(8) . . ? C1' N1 C4 104.1(7) . . ? C1 N1 C4' 108.7(8) . . ? C1' N1 C4' 116.4(7) . . ? C4 N1 C4' 40.9(6) . . ? C1 N1 Co1 122.2(6) . . ? C1' N1 Co1 124.2(6) . . ? C4 N1 Co1 117.0(5) . . ? C4' N1 Co1 119.4(5) . . ? C9 N3 C9' 24.7(5) . . ? C9 N3 C5 119.2(7) . . ? C9' N3 C5 113.2(7) . . ? C9 N3 C5' 111.7(7) . . ? C9' N3 C5' 120.2(7) . . ? C5 N3 C5' 30.8(5) . . ? C9 N3 Co3 121.5(5) . . ? C9' N3 Co3 120.7(5) . . ? C5 N3 Co3 119.3(5) . . ? C5' N3 Co3 119.0(5) . . ? C13 N5 C13' 32.3(6) . . ? C13 N5 C10 119.3(7) . . ? C13' N5 C10 103.9(8) . . ? C13 N5 C10' 104.0(7) . . ? C13' N5 C10' 113.6(7) . . ? C10 N5 C10' 43.4(6) . . ? C13 N5 Co1 121.6(6) . 5_566 ? C13' N5 Co1 124.8(6) . 5_566 ? C10 N5 Co1 118.9(5) . 5_566 ? C10' N5 Co1 121.3(5) . 5_566 ? C14' N8 C14 35.8(6) . . ? C14' N8 C17 101.9(7) . . ? C14 N8 C17 115.6(7) . . ? C14' N8 C17' 120.1(8) . . ? C14 N8 C17' 104.1(7) . . ? C17 N8 C17' 46.6(6) . . ? C14' N8 Co1 121.4(6) . . ? C14 N8 Co1 123.8(6) . . ? C17 N8 Co1 120.1(5) . . ? C17' N8 Co1 118.4(5) . . ? C18' N10 C22 113.3(7) . . ? C18' N10 C18 25.6(5) . . ? C22 N10 C18 119.4(7) . . ? C18' N10 C22' 122.6(7) . . ? C22 N10 C22' 30.1(5) . . ? C18 N10 C22' 113.9(7) . . ? C18' N10 Co3 118.6(5) . . ? C22 N10 Co3 120.2(5) . . ? C18 N10 Co3 120.3(5) . . ? C22' N10 Co3 118.8(5) . . ? C26' N12 C26 41.3(7) . . ? C26' N12 C23' 118.3(8) . . ? C26 N12 C23' 98.6(8) . . ? C26' N12 C23 105.1(8) . . ? C26 N12 C23 115.3(8) . . ? C23' N12 C23 41.1(6) . . ? C26' N12 Co1 121.9(6) . 5_566 ? C26 N12 Co1 125.3(7) . 5_566 ? C23' N12 Co1 119.7(5) . 5_566 ? C23 N12 Co1 119.3(5) . 5_566 ? C8 C7 C8' 19.4(7) . . ? C8 C7 C6' 116.1(8) . . ? C8' C7 C6' 121.5(8) . . ? C8 C7 C6 118.9(8) . . ? C8' C7 C6 114.6(8) . . ? C6' C7 C6 25.8(6) . . ? C19 C20 C21 123.1(8) . . ? C19 C20 C19' 20.1(6) . . ? C21 C20 C19' 115.9(8) . . ? C19 C20 C21' 116.8(8) . . ? C21 C20 C21' 26.6(6) . . ? C19' C20 C21' 120.0(8) . . ? C5 N2 C4 159.4(7) . . ? C5 N2 Co2 104.9(6) . . ? C4 N2 Co2 93.7(5) . . ? C10 N4 C9 124.9(8) . . ? C10 N4 N11 76.7(6) . . ? C9 N4 N11 121.9(7) . . ? C10 N4 Co2 115.6(6) . 5_566 ? C9 N4 Co2 119.1(6) . 5_566 ? N11 N4 Co2 64.4(4) . 5_566 ? C3 N6 C2 115.5(13) . . ? C11 N7 C12 106.0(12) . . ? C17 N9 C18 124.2(9) . . ? C17 N9 Co2 116.6(6) . . ? C18 N9 Co2 119.2(7) . . ? N4 N11 C10 43.9(4) . . ? N4 N11 Co2 63.2(4) . 5_566 ? C10 N11 Co2 92.8(5) . 5_566 ? C15 N13 C16 119.9(13) . . ? C25 N14 C24 121.2(15) . . ? N11' N2' C5' 143.0(7) 5_566 . ? N11' N2' C23' 45.2(5) 5_566 5_566 ? C5' N2' C23' 159.1(7) . 5_566 ? N11' N2' Co2 63.4(4) 5_566 . ? C5' N2' Co2 106.0(6) . . ? C23' N2' Co2 94.4(5) 5_566 . ? C17' N4' C9' 125.7(9) 5_566 . ? C17' N4' Co2 115.0(7) 5_566 5_566 ? C9' N4' Co2 119.0(7) . 5_566 ? C12' N7' C11' 123.6(16) . . ? C18' N9' C4' 133.0(8) . . ? C18' N9' Co2 119.7(7) . . ? C4' N9' Co2 97.4(5) . . ? C3' N6' C2' 115.3(14) . . ? C23' N11' C22' 122.2(9) . . ? C23' N11' N2' 77.8(7) . 5_566 ? C22' N11' N2' 121.8(7) . 5_566 ? C23' N11' C22 134.1(8) . . ? C22' N11' C22 23.6(5) . . ? N2' N11' C22 136.9(7) 5_566 . ? C23' N11' Co2 117.7(7) . 5_566 ? C22' N11' Co2 119.9(7) . 5_566 ? N2' N11' Co2 65.7(4) 5_566 5_566 ? C22 N11' Co2 105.9(5) . 5_566 ? C16' N13' C15' 111.7(11) . . ? C24' N14' C25' 110.8(11) . . ? N1 C1 C2 120.8(12) . . ? C1 C2 N6 121.2(13) . . ? N6 C3 C4 125.3(12) . . ? N1 C4 C3 115.5(9) . . ? N1 C4 N2 91.4(6) . . ? C3 C4 N2 113.1(9) . . ? C6 C5 N3 120.5(9) . . ? C6 C5 N2 116.7(9) . . ? N3 C5 N2 99.0(7) . . ? C5 C6 C7 120.2(10) . . ? C7 C8 C9 120.3(10) . . ? N3 C9 C8 120.3(9) . . ? N3 C9 N4 113.5(8) . . ? C8 C9 N4 126.1(10) . . ? N4 C10 N5 117.2(8) . . ? N4 C10 C11 125.3(9) . . ? N5 C10 C11 117.0(8) . . ? N4 C10 N11 59.4(5) . . ? N5 C10 N11 90.9(6) . . ? C11 C10 N11 113.4(8) . . ? N7 C11 C10 132.4(12) . . ? C13 C12 N7 123.4(11) . . ? N5 C13 C12 121.2(10) . . ? N8 C14 C15 123.1(11) . . ? N13 C15 C14 121.0(13) . . ? N13 C16 C17 120.5(12) . . ? N9 C17 N8 115.7(8) . . ? N9 C17 C16 125.4(9) . . ? N8 C17 C16 117.8(9) . . ? N10 C18 N9 113.7(8) . . ? N10 C18 C19 121.0(9) . . ? N9 C18 C19 125.3(10) . . ? C20 C19 C18 118.3(10) . . ? N12 C23 C24 118.3(10) . . ? N14 C24 C23 119.0(12) . . ? N14 C25 C26 118.5(14) . . ? N12 C26 C25 123.5(12) . . ? N1 C1' C2' 123.7(10) . . ? C1' C2' N6' 119.9(12) . . ? N6' C3' C4' 125.6(12) . . ? N1 C4' C3' 117.9(9) . . ? N1 C4' N9' 91.3(6) . . ? C3' C4' N9' 111.7(8) . . ? N3 C5' C6' 119.5(9) . . ? N3 C5' N2' 95.7(7) . . ? C6' C5' N2' 115.9(9) . . ? C7 C6' C5' 118.8(9) . . ? C7 C8' C9' 118.1(10) . . ? N3 C9' N4' 114.3(8) . . ? N3 C9' C8' 121.1(9) . . ? N4' C9' C8' 124.6(10) . . ? C11' C10' N5 120.9(9) . . ? C10' C11' N7' 114.9(12) . . ? N7' C12' C13' 122.6(16) . . ? N5 C13' C12' 123.6(12) . . ? N8 C14' C15' 121.7(12) . . ? C14' C15' N13' 122.3(12) . . ? N13' C16' C17' 127.1(11) . . ? N4' C17' N8 117.5(9) 5_566 . ? N4' C17' C16' 124.9(10) 5_566 . ? N8 C17' C16' 116.9(9) . . ? N10 C18' N9' 115.7(8) . . ? N10 C18' C19' 119.9(9) . . ? N9' C18' C19' 124.3(10) . . ? C20 C19' C18' 118.9(10) . . ? C22' C21' C20 118.1(9) . . ? C22' C21' C22 27.8(5) . . ? C20 C21' C22 107.8(9) . . ? C22' C22 N10 76.8(12) . . ? C22' C22 C21' 65.5(13) . . ? N10 C22 C21' 112.5(8) . . ? C22' C22 N11' 51.4(11) . . ? N10 C22 N11' 98.0(7) . . ? C21' C22 N11' 99.0(8) . . ? C22 C22' N10 73.0(12) . . ? C22 C22' N11' 105.0(14) . . ? N10 C22' N11' 114.6(8) . . ? C22 C22' C21' 86.6(14) . . ? N10 C22' C21' 119.8(9) . . ? N11' C22' C21' 125.3(9) . . ? N12 C23' N11' 115.2(8) . . ? N12 C23' C24' 118.8(9) . . ? N11' C23' C24' 125.7(10) . . ? N12 C23' N2' 91.1(6) . 5_566 ? N11' C23' N2' 57.0(6) . 5_566 ? C24' C23' N2' 116.0(9) . 5_566 ? N14' C24' C23' 129.9(12) . . ? C26' C25' N14' 119.5(10) . . ? N12 C26' C25' 122.6(10) . . ? Cl2S C1S Cl1S 111.3(5) . . ? Cl2S C1S Cl3S 109.9(5) . . ? Cl1S C1S Cl3S 108.8(4) . . ? Cl6S C2S Cl5S 109.6(5) . . ? Cl6S C2S Cl4S 111.8(5) . . ? Cl5S C2S Cl4S 110.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.898 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.128 # Attachment 'ic12447.cif' data_ic12447 _database_code_depnum_ccdc_archive 'CCDC 694068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H44 Cl8 Co5 N30 S2' _chemical_formula_weight 1803.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.2216(8) _cell_length_b 21.3254(15) _cell_length_c 26.4776(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6900.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used total _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour dark-purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3620 _exptl_absorpt_coefficient_mu 1.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27749 _diffrn_reflns_av_R_equivalents 0.1089 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6079 _reflns_number_gt 3278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6079 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1383 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Co1 Co 0.19994(6) 0.09402(3) 0.10650(3) 0.0239(2) Uani 1 1 d . . . Co2 Co 0.09983(6) 0.09537(3) 0.17912(3) 0.0230(2) Uani 1 1 d . . . Co3 Co 0.0000 0.09555(5) 0.2500 0.0218(3) Uani 1 2 d S . . S1 S 0.36861(16) 0.03956(10) -0.04716(6) 0.0613(6) Uani 1 1 d . . . N1 N 0.2919(4) 0.1575(2) 0.13927(15) 0.0248(11) Uani 1 1 d . . . N2 N 0.2226(4) 0.1260(2) 0.21617(15) 0.0248(11) Uani 1 1 d . . . N3 N 0.1338(3) 0.09536(19) 0.28910(15) 0.0205(11) Uani 1 1 d . . . N4 N 0.0264(4) 0.0652(2) 0.35617(15) 0.0246(12) Uani 1 1 d . . . N5 N -0.0964(4) 0.0292(2) 0.41624(15) 0.0242(11) Uani 1 1 d . . . N6 N 0.4181(5) 0.2509(2) 0.18497(18) 0.0460(15) Uani 1 1 d . . . N7 N 0.0454(4) -0.0690(2) 0.44289(17) 0.0339(13) Uani 1 1 d . . . N8 N 0.1005(4) 0.16084(19) 0.08339(16) 0.0241(11) Uani 1 1 d . . . N9 N 0.0551(4) 0.1800(2) 0.16665(16) 0.0272(12) Uani 1 1 d . . . N10 N 0.0000 0.1863(3) 0.2500 0.0225(16) Uani 1 2 d S . . N11 N -0.0410(4) 0.2556(2) 0.04989(18) 0.0385(13) Uani 1 1 d . . . N12 N 0.2885(4) 0.0285(2) 0.13941(15) 0.0258(12) Uani 1 1 d . . . N13 N 0.1437(4) 0.0112(2) 0.19314(15) 0.0235(11) Uani 1 1 d . . . N14 N 0.0000 0.0046(3) 0.2500 0.0217(16) Uani 1 2 d S . . N15 N 0.4171(4) -0.0594(2) 0.19054(18) 0.0384(14) Uani 1 1 d . . . N16 N 0.2896(4) 0.0922(2) 0.04152(17) 0.0286(12) Uani 1 1 d . . . C1 C 0.3513(5) 0.1984(3) 0.1119(2) 0.0320(16) Uani 1 1 d . . . H1 H 0.3496 0.1957 0.0761 0.038 Uiso 1 1 calc R . . C2 C 0.4145(5) 0.2439(3) 0.1344(2) 0.0458(19) Uani 1 1 d . . . H2 H 0.4568 0.2711 0.1137 0.055 Uiso 1 1 calc R . . C3 C 0.3586(5) 0.2119(3) 0.2117(2) 0.0338(16) Uani 1 1 d . . . H3 H 0.3600 0.2160 0.2475 0.041 Uiso 1 1 calc R . . C4 C 0.2924(5) 0.1638(3) 0.1906(2) 0.0288(15) Uani 1 1 d . . . C5 C 0.2313(5) 0.1113(2) 0.2672(2) 0.0247(14) Uani 1 1 d . . . C6 C 0.3286(5) 0.1090(3) 0.2953(2) 0.0310(15) Uani 1 1 d . . . H6 H 0.3969 0.1181 0.2799 0.037 Uiso 1 1 calc R . . C7 C 0.3229(5) 0.0932(3) 0.3453(2) 0.0338(16) Uani 1 1 d . . . H7 H 0.3881 0.0925 0.3648 0.041 Uiso 1 1 calc R . . C8 C 0.2246(5) 0.0783(2) 0.3680(2) 0.0266(14) Uani 1 1 d . . . H8 H 0.2216 0.0681 0.4029 0.032 Uiso 1 1 calc R . . C9 C 0.1304(5) 0.0786(2) 0.3389(2) 0.0238(14) Uani 1 1 d . . . C10 C 0.0046(5) 0.0243(3) 0.3948(2) 0.0259(14) Uani 1 1 d . . . C11 C 0.0745(5) -0.0259(3) 0.4097(2) 0.0321(15) Uani 1 1 d . . . H11 H 0.1452 -0.0285 0.3950 0.039 Uiso 1 1 calc R . . C12 C -0.0541(5) -0.0630(3) 0.4635(2) 0.0313(15) Uani 1 1 d . . . H12 H -0.0775 -0.0930 0.4877 0.038 Uiso 1 1 calc R . . C13 C -0.1234(5) -0.0148(3) 0.45068(19) 0.0269(14) Uani 1 1 d . . . H13 H -0.1929 -0.0124 0.4667 0.032 Uiso 1 1 calc R . . C14 C 0.0855(5) 0.1733(3) 0.0340(2) 0.0308(15) Uani 1 1 d . . . H14 H 0.1250 0.1498 0.0096 0.037 Uiso 1 1 calc R . . C15 C 0.0154(5) 0.2186(3) 0.0180(2) 0.0332(16) Uani 1 1 d . . . H15 H 0.0059 0.2245 -0.0173 0.040 Uiso 1 1 calc R . . C16 C -0.0249(5) 0.2443(3) 0.0988(2) 0.0332(16) Uani 1 1 d . . . H16 H -0.0625 0.2696 0.1227 0.040 Uiso 1 1 calc R . . C17 C 0.0455(5) 0.1966(3) 0.1172(2) 0.0265(14) Uani 1 1 d . . . C18 C 0.0278(5) 0.2189(3) 0.2072(2) 0.0274(15) Uani 1 1 d . . . C19 C 0.0340(4) 0.2834(2) 0.2077(2) 0.0273(15) Uani 1 1 d . . . H19 H 0.0614 0.3055 0.1793 0.033 Uiso 1 1 calc R . . C20 C 0.0000 0.3154(4) 0.2500 0.031(2) Uani 1 2 d S . . H20 H 0.0000 0.3600 0.2500 0.037 Uiso 1 2 calc SR . . C21 C 0.3937(5) 0.0176(3) 0.1266(2) 0.0320(15) Uani 1 1 d . . . H21 H 0.4254 0.0401 0.0994 0.038 Uiso 1 1 calc R . . C22 C 0.4557(5) -0.0256(3) 0.1523(2) 0.0358(16) Uani 1 1 d . . . H22 H 0.5296 -0.0316 0.1423 0.043 Uiso 1 1 calc R . . C23 C 0.3146(5) -0.0497(3) 0.2023(2) 0.0348(16) Uani 1 1 d . . . H23 H 0.2837 -0.0743 0.2286 0.042 Uiso 1 1 calc R . . C24 C 0.2464(5) -0.0047(3) 0.1783(2) 0.0270(14) Uani 1 1 d . . . C25 C 0.0741(5) -0.0273(3) 0.22075(19) 0.0256(14) Uani 1 1 d . . . C26 C 0.0714(5) -0.0925(3) 0.2189(2) 0.0322(15) Uani 1 1 d . . . H26 H 0.1181 -0.1148 0.1965 0.039 Uiso 1 1 calc R . . C27 C 0.0000 -0.1242(4) 0.2500 0.037(2) Uani 1 2 d S . . H27 H 0.0000 -0.1688 0.2500 0.044 Uiso 1 2 calc SR . . C28 C 0.3233(5) 0.0713(3) 0.0045(2) 0.0352(16) Uani 1 1 d . . . C29 C 0.7221(8) 0.3314(4) 0.1197(4) 0.118(4) Uani 1 1 d . . . H29A H 0.6513 0.3501 0.1095 0.141 Uiso 1 1 calc R . . H29B H 0.7714 0.3325 0.0900 0.141 Uiso 1 1 calc R . . Cl1 Cl 0.77904(19) 0.37662(11) 0.16810(8) 0.0828(7) Uani 1 1 d . . . Cl2 Cl 0.70082(18) 0.25392(10) 0.13697(10) 0.0953(8) Uani 1 1 d . . . C30 C 0.1275(6) 0.3757(3) 0.0334(2) 0.066(2) Uani 1 1 d . . . H30A H 0.0503 0.3623 0.0369 0.080 Uiso 1 1 calc R . . H30B H 0.1287 0.4221 0.0315 0.080 Uiso 1 1 calc R . . Cl3 Cl 0.20071(18) 0.35152(10) 0.08609(8) 0.0802(7) Uani 1 1 d . . . Cl4 Cl 0.1811(2) 0.34501(12) -0.02180(8) 0.1151(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0287(5) 0.0216(4) 0.0215(4) -0.0007(4) 0.0027(4) -0.0027(4) Co2 0.0270(5) 0.0206(4) 0.0214(4) -0.0015(4) 0.0028(4) -0.0009(4) Co3 0.0259(7) 0.0184(6) 0.0212(6) 0.000 0.0017(5) 0.000 S1 0.0527(13) 0.0906(16) 0.0406(10) -0.0258(11) 0.0127(10) -0.0011(12) N1 0.027(3) 0.026(3) 0.021(3) -0.002(2) 0.003(2) -0.002(2) N2 0.030(3) 0.024(3) 0.020(3) -0.001(2) 0.004(2) -0.005(2) N3 0.020(3) 0.024(3) 0.018(2) 0.001(2) 0.002(2) 0.002(2) N4 0.023(3) 0.029(3) 0.021(3) 0.004(2) 0.001(2) 0.006(2) N5 0.035(3) 0.022(3) 0.016(2) -0.002(2) 0.002(2) 0.005(2) N6 0.059(4) 0.045(3) 0.034(3) -0.004(3) 0.010(3) -0.024(3) N7 0.039(4) 0.029(3) 0.034(3) 0.006(3) 0.003(3) 0.007(3) N8 0.028(3) 0.025(3) 0.019(3) 0.000(2) 0.007(2) -0.001(2) N9 0.032(3) 0.022(3) 0.027(3) 0.003(2) 0.002(2) 0.001(2) N10 0.030(4) 0.021(4) 0.017(3) 0.000 -0.003(3) 0.000 N11 0.040(4) 0.036(3) 0.040(3) 0.003(3) -0.005(3) 0.001(3) N12 0.038(3) 0.020(3) 0.019(2) 0.000(2) 0.009(2) 0.000(2) N13 0.024(3) 0.021(3) 0.025(3) 0.003(2) 0.003(2) 0.001(2) N14 0.029(4) 0.021(4) 0.016(3) 0.000 -0.001(3) 0.000 N15 0.040(4) 0.036(3) 0.039(3) 0.010(3) 0.011(3) 0.009(3) N16 0.034(3) 0.027(3) 0.024(3) -0.003(2) 0.005(2) -0.004(3) C1 0.037(4) 0.034(4) 0.024(3) -0.002(3) 0.008(3) -0.008(3) C2 0.062(5) 0.046(4) 0.029(4) -0.003(3) 0.008(4) -0.027(4) C3 0.039(4) 0.037(4) 0.025(3) 0.002(3) -0.002(3) -0.010(3) C4 0.032(4) 0.027(4) 0.027(3) -0.005(3) 0.006(3) 0.000(3) C5 0.027(4) 0.016(3) 0.031(3) 0.001(3) 0.006(3) 0.003(3) C6 0.019(4) 0.038(4) 0.037(4) 0.002(3) 0.001(3) -0.004(3) C7 0.034(4) 0.036(4) 0.032(4) 0.003(3) -0.009(3) -0.001(3) C8 0.024(4) 0.034(4) 0.022(3) 0.009(3) -0.004(3) -0.002(3) C9 0.023(4) 0.017(3) 0.031(3) -0.006(3) 0.003(3) 0.005(3) C10 0.032(4) 0.023(3) 0.023(3) -0.003(3) -0.002(3) -0.001(3) C11 0.030(4) 0.033(4) 0.032(3) 0.008(3) 0.005(3) 0.002(3) C12 0.035(4) 0.028(4) 0.032(3) 0.007(3) 0.006(3) 0.000(3) C13 0.029(4) 0.029(3) 0.022(3) 0.001(3) 0.003(3) 0.005(3) C14 0.040(4) 0.027(3) 0.025(3) -0.005(3) 0.004(3) -0.007(3) C15 0.045(4) 0.031(4) 0.023(3) 0.002(3) -0.004(3) 0.002(3) C16 0.037(4) 0.036(4) 0.027(4) 0.000(3) 0.005(3) 0.004(3) C17 0.028(4) 0.024(3) 0.028(3) 0.003(3) -0.001(3) -0.009(3) C18 0.032(4) 0.024(3) 0.026(3) -0.002(3) 0.003(3) 0.004(3) C19 0.038(4) 0.017(3) 0.027(3) 0.005(3) 0.003(3) -0.002(3) C20 0.040(6) 0.021(5) 0.032(5) 0.000 0.000(4) 0.000 C21 0.037(4) 0.034(4) 0.025(3) -0.003(3) 0.012(3) -0.003(3) C22 0.029(4) 0.037(4) 0.041(4) 0.006(3) 0.003(3) 0.009(3) C23 0.041(5) 0.035(4) 0.029(3) 0.011(3) 0.006(3) 0.004(3) C24 0.030(4) 0.020(3) 0.031(3) -0.005(3) -0.001(3) 0.000(3) C25 0.033(4) 0.022(3) 0.022(3) -0.001(3) 0.000(3) 0.006(3) C26 0.042(4) 0.024(3) 0.031(3) -0.006(3) 0.009(3) -0.003(3) C27 0.047(6) 0.020(5) 0.044(5) 0.000 0.014(5) 0.000 C28 0.031(4) 0.034(4) 0.040(4) 0.006(3) -0.002(3) -0.007(3) C29 0.139(9) 0.053(6) 0.161(9) 0.012(6) -0.098(8) 0.010(6) Cl1 0.0907(18) 0.0868(16) 0.0710(13) -0.0046(12) -0.0143(13) -0.0050(14) Cl2 0.0642(16) 0.0657(14) 0.156(2) -0.0015(15) 0.0247(15) -0.0037(12) C30 0.081(6) 0.045(4) 0.074(5) 0.013(4) 0.024(5) -0.005(4) Cl3 0.0807(17) 0.0802(15) 0.0797(14) 0.0156(12) 0.0015(13) -0.0195(13) Cl4 0.180(3) 0.0992(18) 0.0662(14) -0.0046(13) 0.0505(17) -0.0460(19) _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 1.962(4) . ? Co1 N5 1.969(4) 3 ? Co1 N12 1.970(4) . ? Co1 N8 1.971(4) . ? Co1 N16 2.040(5) . ? Co1 Co2 2.2793(10) . ? Co2 N2 1.908(4) . ? Co2 N13 1.909(4) . ? Co2 N4 1.915(4) 3 ? Co2 N9 1.915(4) . ? Co2 Co3 2.2385(7) . ? Co3 N10 1.935(6) . ? Co3 N3 1.936(4) 3 ? Co3 N3 1.936(4) . ? Co3 N14 1.940(6) . ? Co3 Co2 2.2385(7) 3 ? S1 C28 1.622(7) . ? N1 C1 1.346(6) . ? N1 C4 1.366(6) . ? N2 C4 1.355(7) . ? N2 C5 1.392(6) . ? N3 C9 1.367(6) . ? N3 C5 1.368(6) . ? N4 C10 1.371(6) . ? N4 C9 1.381(7) . ? N4 Co2 1.915(4) 3 ? N5 C13 1.349(6) . ? N5 C10 1.362(7) . ? N5 Co1 1.969(4) 3 ? N6 C3 1.313(7) . ? N6 C2 1.349(6) . ? N7 C11 1.322(6) . ? N7 C12 1.338(7) . ? N8 C14 1.348(6) . ? N8 C17 1.354(6) . ? N9 C17 1.363(6) . ? N9 C18 1.397(6) . ? N10 C18 1.373(6) . ? N10 C18 1.373(6) 3 ? N11 C16 1.332(6) . ? N11 C15 1.345(7) . ? N12 C21 1.351(7) . ? N12 C24 1.351(6) . ? N13 C24 1.358(7) . ? N13 C25 1.390(7) . ? N14 C25 1.371(6) 3 ? N14 C25 1.371(6) . ? N15 C23 1.308(7) . ? N15 C22 1.330(7) . ? N16 C28 1.155(7) . ? C1 C2 1.376(8) . ? C3 C4 1.421(7) . ? C5 C6 1.402(7) . ? C6 C7 1.368(7) . ? C7 C8 1.380(7) . ? C8 C9 1.385(7) . ? C10 C11 1.424(7) . ? C12 C13 1.375(7) . ? C14 C15 1.358(7) . ? C16 C17 1.417(8) . ? C18 C19 1.377(7) . ? C19 C20 1.375(6) . ? C20 C19 1.375(6) 3 ? C21 C22 1.371(8) . ? C23 C24 1.422(8) . ? C25 C26 1.393(7) . ? C26 C27 1.377(6) . ? C27 C26 1.377(6) 3 ? C29 Cl2 1.733(8) . ? C29 Cl1 1.749(8) . ? C30 Cl4 1.730(7) . ? C30 Cl3 1.736(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 N5 171.17(18) . 3 ? N1 Co1 N12 88.80(18) . . ? N5 Co1 N12 89.44(18) 3 . ? N1 Co1 N8 89.52(18) . . ? N5 Co1 N8 90.95(18) 3 . ? N12 Co1 N8 171.46(18) . . ? N1 Co1 N16 94.49(18) . . ? N5 Co1 N16 94.26(18) 3 . ? N12 Co1 N16 93.73(18) . . ? N8 Co1 N16 94.75(18) . . ? N1 Co1 Co2 85.73(13) . . ? N5 Co1 Co2 85.52(13) 3 . ? N12 Co1 Co2 86.02(13) . . ? N8 Co1 Co2 85.50(13) . . ? N16 Co1 Co2 179.67(13) . . ? N2 Co2 N13 90.05(19) . . ? N2 Co2 N4 178.11(19) . 3 ? N13 Co2 N4 90.31(19) . 3 ? N2 Co2 N9 89.46(19) . . ? N13 Co2 N9 178.70(18) . . ? N4 Co2 N9 90.14(19) 3 . ? N2 Co2 Co3 89.84(13) . . ? N13 Co2 Co3 89.53(13) . . ? N4 Co2 Co3 88.31(13) 3 . ? N9 Co2 Co3 89.27(13) . . ? N2 Co2 Co1 90.91(13) . . ? N13 Co2 Co1 90.08(13) . . ? N4 Co2 Co1 90.95(13) 3 . ? N9 Co2 Co1 91.14(13) . . ? Co3 Co2 Co1 179.16(5) . . ? N10 Co3 N3 90.12(12) . 3 ? N10 Co3 N3 90.12(12) . . ? N3 Co3 N3 179.8(2) 3 . ? N10 Co3 N14 180.000(1) . . ? N3 Co3 N14 89.88(12) 3 . ? N3 Co3 N14 89.88(12) . . ? N10 Co3 Co2 90.10(3) . . ? N3 Co3 Co2 90.69(12) 3 . ? N3 Co3 Co2 89.31(12) . . ? N14 Co3 Co2 89.90(3) . . ? N10 Co3 Co2 90.10(3) . 3 ? N3 Co3 Co2 89.31(12) 3 3 ? N3 Co3 Co2 90.69(12) . 3 ? N14 Co3 Co2 89.90(3) . 3 ? Co2 Co3 Co2 179.80(6) . 3 ? C1 N1 C4 117.9(5) . . ? C1 N1 Co1 121.2(4) . . ? C4 N1 Co1 120.7(4) . . ? C4 N2 C5 124.9(5) . . ? C4 N2 Co2 116.2(3) . . ? C5 N2 Co2 118.8(4) . . ? C9 N3 C5 120.0(5) . . ? C9 N3 Co3 119.4(4) . . ? C5 N3 Co3 120.6(3) . . ? C10 N4 C9 123.9(5) . . ? C10 N4 Co2 114.9(4) . 3 ? C9 N4 Co2 120.7(4) . 3 ? C13 N5 C10 116.8(5) . . ? C13 N5 Co1 122.5(4) . 3 ? C10 N5 Co1 120.6(4) . 3 ? C3 N6 C2 116.6(5) . . ? C11 N7 C12 116.6(5) . . ? C14 N8 C17 117.5(5) . . ? C14 N8 Co1 121.9(4) . . ? C17 N8 Co1 120.6(4) . . ? C17 N9 C18 124.4(5) . . ? C17 N9 Co2 115.8(4) . . ? C18 N9 Co2 119.7(3) . . ? C18 N10 C18 119.1(6) . 3 ? C18 N10 Co3 120.5(3) . . ? C18 N10 Co3 120.5(3) 3 . ? C16 N11 C15 115.3(5) . . ? C21 N12 C24 117.5(5) . . ? C21 N12 Co1 122.4(4) . . ? C24 N12 Co1 120.0(4) . . ? C24 N13 C25 124.8(5) . . ? C24 N13 Co2 116.0(4) . . ? C25 N13 Co2 119.0(4) . . ? C25 N14 C25 120.6(6) 3 . ? C25 N14 Co3 119.7(3) 3 . ? C25 N14 Co3 119.7(3) . . ? C23 N15 C22 115.8(5) . . ? C28 N16 Co1 156.3(5) . . ? N1 C1 C2 121.9(5) . . ? N6 C2 C1 121.7(6) . . ? N6 C3 C4 124.1(5) . . ? N2 C4 N1 115.8(5) . . ? N2 C4 C3 126.2(5) . . ? N1 C4 C3 117.8(5) . . ? N3 C5 N2 113.6(5) . . ? N3 C5 C6 120.3(5) . . ? N2 C5 C6 125.9(5) . . ? C7 C6 C5 118.6(5) . . ? C6 C7 C8 121.4(5) . . ? C7 C8 C9 118.7(5) . . ? N3 C9 N4 113.7(5) . . ? N3 C9 C8 120.8(5) . . ? N4 C9 C8 125.5(5) . . ? N5 C10 N4 116.0(5) . . ? N5 C10 C11 119.1(5) . . ? N4 C10 C11 124.6(5) . . ? N7 C11 C10 123.1(5) . . ? N7 C12 C13 122.1(5) . . ? N5 C13 C12 122.4(5) . . ? N8 C14 C15 121.9(5) . . ? N11 C15 C14 123.0(5) . . ? N11 C16 C17 123.6(5) . . ? N8 C17 N9 116.5(5) . . ? N8 C17 C16 118.6(5) . . ? N9 C17 C16 124.6(5) . . ? N10 C18 C19 120.7(5) . . ? N10 C18 N9 113.1(5) . . ? C19 C18 N9 126.0(5) . . ? C20 C19 C18 119.2(6) . . ? C19 C20 C19 120.4(7) . 3 ? N12 C21 C22 121.2(5) . . ? N15 C22 C21 123.0(6) . . ? N15 C23 C24 124.2(6) . . ? N12 C24 N13 116.2(5) . . ? N12 C24 C23 118.2(5) . . ? N13 C24 C23 125.5(5) . . ? N14 C25 N13 114.1(5) . . ? N14 C25 C26 120.0(5) . . ? N13 C25 C26 125.8(5) . . ? C27 C26 C25 119.0(6) . . ? C26 C27 C26 121.2(8) . 3 ? N16 C28 S1 178.0(6) . . ? Cl2 C29 Cl1 113.1(5) . . ? Cl4 C30 Cl3 111.8(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.668 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.111 # Attachment 'ic12532.cif' data_ic12532 _database_code_depnum_ccdc_archive 'CCDC 694069' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H64 Cl6 Co5 N28 O2 P' _chemical_formula_weight 1963.89 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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 16.3673(7) _cell_length_b 27.5890(14) _cell_length_c 17.3331(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.231(3) _cell_angle_gamma 90.00 _cell_volume 7825.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used total _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6750 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14150 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6830 _reflns_number_gt 5218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+95.4591P] 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 6830 _refine_ls_number_parameters 552 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2313 _refine_ls_wR_factor_gt 0.2129 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.006 _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 0.5000 0.03017(4) 0.7500 0.0254(3) Uani 1 2 d S . . Co2 Co 0.5000 0.11313(4) 0.7500 0.0228(3) Uani 1 2 d S . . Co3 Co 0.5000 0.19575(4) 0.7500 0.0213(3) Uani 1 2 d S . . Co4 Co 0.5000 0.27819(4) 0.7500 0.0235(3) Uani 1 2 d S . . Co5 Co 0.5000 0.36108(4) 0.7500 0.0285(3) Uani 1 2 d S . . Cl1 Cl 0.5000 -0.05862(8) 0.7500 0.0374(5) Uani 1 2 d S . . Cl2 Cl 0.5000 0.45111(8) 0.7500 0.0443(6) Uani 1 2 d S . . N1 N 0.5332(3) 0.03577(18) 0.6419(3) 0.0281(11) Uani 1 1 d . . . N2 N 0.4842(3) 0.11444(17) 0.6400(3) 0.0253(11) Uani 1 1 d . . . N3 N 0.4499(3) 0.19607(17) 0.6472(3) 0.0244(10) Uani 1 1 d . . . N4 N 0.4202(3) 0.27754(17) 0.6670(3) 0.0261(11) Uani 1 1 d . . . N5 N 0.3900(3) 0.35588(19) 0.7037(3) 0.0309(12) Uani 1 1 d . . . N6 N 0.5930(3) 0.0458(2) 0.4926(3) 0.0375(13) Uani 1 1 d . . . N7 N 0.2341(4) 0.3501(2) 0.6347(4) 0.0452(15) Uani 1 1 d . . . N8 N 0.6147(3) 0.03563(18) 0.7834(3) 0.0278(11) Uani 1 1 d . . . N9 N 0.6161(3) 0.11410(17) 0.7371(3) 0.0247(10) Uani 1 1 d . . . N10 N 0.6068(3) 0.19550(17) 0.7033(3) 0.0235(10) Uani 1 1 d . . . N11 N 0.5862(3) 0.27703(18) 0.6762(3) 0.0255(11) Uani 1 1 d . . . N12 N 0.5477(3) 0.35550(19) 0.6467(3) 0.0337(12) Uani 1 1 d . . . N13 N 0.7799(3) 0.0413(2) 0.8270(3) 0.0417(14) Uani 1 1 d . . . N14 N 0.6061(4) 0.3472(2) 0.4968(3) 0.0486(16) Uani 1 1 d . . . C1 C 0.5757(4) 0.0003(2) 0.6063(4) 0.0327(14) Uani 1 1 d . . . H1A H 0.5856 -0.0292 0.6333 0.039 Uiso 1 1 calc R . . C2 C 0.6046(4) 0.0051(3) 0.5337(4) 0.0390(16) Uani 1 1 d . . . H2A H 0.6337 -0.0211 0.5116 0.047 Uiso 1 1 calc R . . C3 C 0.5505(4) 0.0804(2) 0.5253(3) 0.0322(14) Uani 1 1 d . . . H3A H 0.5402 0.1092 0.4966 0.039 Uiso 1 1 calc R . . C4 C 0.5192(4) 0.0772(2) 0.6012(3) 0.0257(12) Uani 1 1 d . . . C5 C 0.4498(4) 0.1543(2) 0.6040(3) 0.0250(12) Uani 1 1 d . . . C6 C 0.4130(4) 0.1546(2) 0.5309(3) 0.0304(14) Uani 1 1 d . . . H6A H 0.4063 0.1251 0.5032 0.036 Uiso 1 1 calc R . . C7 C 0.3866(4) 0.1972(2) 0.4986(4) 0.0334(15) Uani 1 1 d . . . H7A H 0.3653 0.1975 0.4471 0.040 Uiso 1 1 calc R . . C8 C 0.3906(4) 0.2399(2) 0.5405(3) 0.0308(14) Uani 1 1 d . . . H8A H 0.3750 0.2699 0.5174 0.037 Uiso 1 1 calc R . . C9 C 0.4180(3) 0.2381(2) 0.6171(3) 0.0251(12) Uani 1 1 d . . . C10 C 0.3675(4) 0.3151(2) 0.6632(3) 0.0297(13) Uani 1 1 d . . . C11 C 0.2884(4) 0.3150(2) 0.6273(4) 0.0354(15) Uani 1 1 d . . . H11A H 0.2737 0.2880 0.5960 0.042 Uiso 1 1 calc R . . C12 C 0.2579(5) 0.3888(3) 0.6779(4) 0.0490(19) Uani 1 1 d . . . H12A H 0.2205 0.4147 0.6853 0.059 Uiso 1 1 calc R . . C13 C 0.3341(5) 0.3917(2) 0.7111(4) 0.0406(16) Uani 1 1 d . . . H13A H 0.3485 0.4197 0.7403 0.049 Uiso 1 1 calc R . . C14 C 0.6521(4) -0.0003(2) 0.8241(3) 0.0337(14) Uani 1 1 d . . . H14A H 0.6217 -0.0282 0.8381 0.040 Uiso 1 1 calc R . . C15 C 0.7331(4) 0.0029(3) 0.8455(4) 0.0432(17) Uani 1 1 d . . . H15A H 0.7572 -0.0229 0.8744 0.052 Uiso 1 1 calc R . . C16 C 0.7434(4) 0.0764(2) 0.7885(4) 0.0366(15) Uani 1 1 d . . . H16A H 0.7752 0.1037 0.7743 0.044 Uiso 1 1 calc R . . C17 C 0.6592(4) 0.0761(2) 0.7668(3) 0.0266(13) Uani 1 1 d . . . C18 C 0.6517(4) 0.1534(2) 0.7011(3) 0.0256(13) Uani 1 1 d . . . C19 C 0.7246(4) 0.1520(2) 0.6601(4) 0.0311(14) Uani 1 1 d . . . H19A H 0.7521 0.1221 0.6526 0.037 Uiso 1 1 calc R . . C20 C 0.7561(4) 0.1944(2) 0.6308(4) 0.0358(15) Uani 1 1 d . . . H20A H 0.8069 0.1941 0.6054 0.043 Uiso 1 1 calc R . . C21 C 0.7135(4) 0.2373(2) 0.6384(4) 0.0323(14) Uani 1 1 d . . . H21A H 0.7369 0.2669 0.6219 0.039 Uiso 1 1 calc R . . C22 C 0.6356(4) 0.2369(2) 0.6704(3) 0.0247(12) Uani 1 1 d . . . C23 C 0.5858(4) 0.3143(2) 0.6248(3) 0.0281(13) Uani 1 1 d . . . C24 C 0.6145(4) 0.3121(2) 0.5482(4) 0.0361(15) Uani 1 1 d . . . H24A H 0.6415 0.2833 0.5328 0.043 Uiso 1 1 calc R . . C25 C 0.5677(6) 0.3876(3) 0.5212(4) 0.055(2) Uani 1 1 d . . . H25A H 0.5606 0.4140 0.4864 0.066 Uiso 1 1 calc R . . C26 C 0.5391(5) 0.3917(3) 0.5936(4) 0.0448(18) Uani 1 1 d . . . H26A H 0.5122 0.4207 0.6079 0.054 Uiso 1 1 calc R . . P1 P 0.5000 -0.24581(9) 0.7500 0.0394(6) Uani 1 2 d S . . C27 C 0.5574(4) -0.2086(2) 0.8167(4) 0.0376(15) Uani 1 1 d . . . C28 C 0.5995(4) -0.1684(3) 0.7885(5) 0.0437(17) Uani 1 1 d . . . H28A H 0.5943 -0.1596 0.7356 0.052 Uiso 1 1 calc R . . C29 C 0.6491(5) -0.1414(3) 0.8387(5) 0.0487(19) Uani 1 1 d . . . H29A H 0.6773 -0.1139 0.8199 0.058 Uiso 1 1 calc R . . C30 C 0.6576(4) -0.1543(3) 0.9151(5) 0.0465(19) Uani 1 1 d . . . H30A H 0.6934 -0.1365 0.9484 0.056 Uiso 1 1 calc R . . C31 C 0.6140(5) -0.1930(3) 0.9433(5) 0.0498(19) Uani 1 1 d . . . H31A H 0.6177 -0.2007 0.9967 0.060 Uiso 1 1 calc R . . C32 C 0.5650(4) -0.2208(3) 0.8943(5) 0.0452(18) Uani 1 1 d . . . H32A H 0.5366 -0.2481 0.9137 0.054 Uiso 1 1 calc R . . C33 C 0.5689(4) -0.2839(3) 0.6970(4) 0.0415(16) Uani 1 1 d . . . C34 C 0.6512(4) -0.2729(3) 0.6940(4) 0.0419(16) Uani 1 1 d . . . H34A H 0.6731 -0.2467 0.7232 0.050 Uiso 1 1 calc R . . C35 C 0.7017(5) -0.3009(3) 0.6477(5) 0.0484(19) Uani 1 1 d . . . H35A H 0.7584 -0.2938 0.6456 0.058 Uiso 1 1 calc R . . C36 C 0.6700(5) -0.3381(3) 0.6058(5) 0.053(2) Uani 1 1 d . . . H36A H 0.7046 -0.3564 0.5735 0.064 Uiso 1 1 calc R . . C37 C 0.5893(6) -0.3497(3) 0.6093(6) 0.066(3) Uani 1 1 d . . . H37A H 0.5685 -0.3765 0.5806 0.080 Uiso 1 1 calc R . . C38 C 0.5373(5) -0.3229(3) 0.6542(6) 0.059(2) Uani 1 1 d . . . H38A H 0.4809 -0.3308 0.6560 0.070 Uiso 1 1 calc R . . Cl3 Cl 0.6814(2) 0.56205(12) 0.47800(18) 0.1014(10) Uani 1 1 d D . . C39 C 0.6326(6) 0.5102(4) 0.4444(9) 0.087(5) Uani 0.70 1 d PD A 1 H39A H 0.6136 0.4918 0.4897 0.104 Uiso 0.70 1 d PR A 1 H39B H 0.5840 0.5193 0.4127 0.104 Uiso 0.70 1 d PR A 1 Cl4A Cl 0.6859(4) 0.4782(2) 0.3744(4) 0.0611(15) Uiso 0.35 1 d PD A 1 Cl4B Cl 0.7041(5) 0.4670(3) 0.4173(5) 0.0759(19) Uiso 0.35 1 d PD A 1 C39' C 0.6028(17) 0.5295(11) 0.5230(12) 0.082(10) Uiso 0.30 1 d PD A 2 H39C H 0.6206 0.4956 0.5154 0.098 Uiso 0.30 1 calc PR A 2 H39D H 0.5566 0.5339 0.4858 0.098 Uiso 0.30 1 calc PR A 2 Cl4' Cl 0.5512(5) 0.5253(3) 0.6117(5) 0.076(2) Uani 0.30 1 d PD A 2 O1 O 0.5793(9) 0.4247(5) 0.3171(9) 0.196(6) Uiso 1 1 d . . . H1B H 0.6116 0.4409 0.3460 0.293 Uiso 1 1 d R . . H1C H 0.5959 0.3976 0.3248 0.293 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0324(6) 0.0247(6) 0.0191(6) 0.000 -0.0002(4) 0.000 Co2 0.0278(6) 0.0246(6) 0.0160(6) 0.000 0.0003(4) 0.000 Co3 0.0246(6) 0.0248(6) 0.0146(6) 0.000 -0.0002(4) 0.000 Co4 0.0287(6) 0.0245(6) 0.0173(6) 0.000 -0.0011(4) 0.000 Co5 0.0380(7) 0.0250(6) 0.0224(6) 0.000 -0.0012(5) 0.000 Cl1 0.0499(14) 0.0269(11) 0.0353(12) 0.000 -0.0017(10) 0.000 Cl2 0.0650(16) 0.0277(12) 0.0403(13) 0.000 0.0032(11) 0.000 N1 0.034(3) 0.025(3) 0.025(3) -0.005(2) -0.003(2) -0.001(2) N2 0.031(3) 0.026(3) 0.019(2) -0.0026(19) 0.002(2) 0.000(2) N3 0.025(3) 0.027(3) 0.020(2) 0.0003(19) 0.0007(19) -0.001(2) N4 0.033(3) 0.025(3) 0.020(3) 0.0029(19) -0.001(2) 0.001(2) N5 0.037(3) 0.031(3) 0.024(3) 0.003(2) -0.002(2) 0.002(2) N6 0.045(3) 0.038(3) 0.030(3) -0.002(2) 0.008(2) 0.000(3) N7 0.046(4) 0.042(3) 0.047(4) -0.002(3) -0.014(3) 0.015(3) N8 0.035(3) 0.025(3) 0.023(3) -0.003(2) -0.004(2) 0.004(2) N9 0.024(2) 0.030(3) 0.020(2) -0.0013(19) 0.0010(19) 0.000(2) N10 0.025(2) 0.028(3) 0.017(2) -0.0015(19) -0.0008(19) -0.002(2) N11 0.028(3) 0.029(3) 0.019(2) -0.001(2) 0.003(2) -0.003(2) N12 0.046(3) 0.027(3) 0.028(3) 0.000(2) -0.002(2) -0.005(2) N13 0.041(3) 0.039(3) 0.045(3) 0.003(3) -0.014(3) -0.001(3) N14 0.074(5) 0.043(4) 0.029(3) 0.008(3) 0.010(3) -0.005(3) C1 0.034(3) 0.031(3) 0.033(3) -0.004(3) 0.001(3) 0.004(3) C2 0.047(4) 0.037(4) 0.033(4) -0.005(3) 0.008(3) 0.005(3) C3 0.041(4) 0.035(3) 0.021(3) 0.000(3) 0.004(3) -0.002(3) C4 0.028(3) 0.026(3) 0.023(3) -0.003(2) -0.004(2) -0.004(2) C5 0.027(3) 0.027(3) 0.021(3) -0.001(2) 0.004(2) -0.006(2) C6 0.035(3) 0.035(4) 0.021(3) -0.006(2) -0.002(3) -0.006(3) C7 0.034(3) 0.047(4) 0.019(3) 0.001(3) -0.005(3) 0.001(3) C8 0.033(3) 0.038(4) 0.021(3) 0.005(3) -0.003(2) 0.002(3) C9 0.025(3) 0.031(3) 0.019(3) 0.005(2) 0.000(2) -0.003(2) C10 0.036(3) 0.031(3) 0.022(3) 0.003(2) -0.001(3) 0.003(3) C11 0.039(4) 0.033(3) 0.034(4) 0.002(3) -0.003(3) 0.004(3) C12 0.059(5) 0.039(4) 0.048(5) 0.000(3) -0.015(4) 0.018(3) C13 0.055(4) 0.027(3) 0.039(4) 0.002(3) -0.006(3) 0.009(3) C14 0.048(4) 0.029(3) 0.024(3) 0.002(3) -0.001(3) 0.005(3) C15 0.049(4) 0.039(4) 0.041(4) 0.005(3) -0.009(3) 0.007(3) C16 0.039(4) 0.036(4) 0.035(4) -0.001(3) -0.007(3) 0.000(3) C17 0.035(3) 0.028(3) 0.017(3) -0.005(2) 0.001(2) 0.004(2) C18 0.032(3) 0.027(3) 0.018(3) -0.004(2) -0.002(2) -0.001(2) C19 0.032(3) 0.034(4) 0.027(3) -0.003(3) 0.001(3) 0.002(3) C20 0.033(3) 0.044(4) 0.030(3) 0.002(3) 0.006(3) -0.003(3) C21 0.033(3) 0.036(4) 0.028(3) 0.002(3) 0.001(3) -0.005(3) C22 0.026(3) 0.031(3) 0.017(3) -0.003(2) -0.001(2) -0.005(2) C23 0.032(3) 0.027(3) 0.026(3) -0.002(2) 0.001(2) -0.005(2) C24 0.046(4) 0.034(4) 0.028(3) 0.003(3) 0.005(3) -0.001(3) C25 0.098(7) 0.031(4) 0.036(4) 0.007(3) 0.016(4) 0.002(4) C26 0.071(5) 0.029(4) 0.035(4) 0.008(3) 0.003(3) 0.003(3) P1 0.0326(13) 0.0330(13) 0.0525(16) 0.000 -0.0026(11) 0.000 C27 0.030(3) 0.030(3) 0.053(4) -0.002(3) 0.001(3) 0.005(3) C28 0.038(4) 0.036(4) 0.056(5) 0.000(3) -0.002(3) 0.003(3) C29 0.042(4) 0.032(4) 0.073(6) -0.011(4) 0.007(4) -0.002(3) C30 0.038(4) 0.039(4) 0.063(5) -0.015(3) 0.000(3) 0.010(3) C31 0.051(5) 0.047(5) 0.052(5) -0.014(4) -0.003(4) 0.012(4) C32 0.039(4) 0.043(4) 0.054(5) -0.003(3) 0.002(3) 0.006(3) C33 0.039(4) 0.035(4) 0.050(4) -0.002(3) -0.005(3) 0.004(3) C34 0.046(4) 0.037(4) 0.043(4) 0.006(3) -0.005(3) 0.002(3) C35 0.046(4) 0.044(4) 0.056(5) 0.015(4) 0.006(4) 0.009(3) C36 0.063(5) 0.044(5) 0.054(5) 0.007(4) 0.004(4) 0.017(4) C37 0.081(7) 0.041(5) 0.077(7) -0.021(4) -0.008(5) 0.006(4) C38 0.047(5) 0.044(5) 0.085(7) -0.011(4) -0.001(4) 0.000(4) Cl3 0.136(3) 0.088(2) 0.081(2) -0.0070(16) 0.0088(18) -0.0061(19) C39 0.063(9) 0.066(9) 0.132(15) -0.013(9) 0.026(9) -0.017(7) Cl4' 0.074(5) 0.083(6) 0.072(5) 0.017(4) -0.011(4) -0.020(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 Co1 N8 1.958(5) . ? Co1 N8 1.958(5) 2_656 ? Co1 N1 1.969(5) 2_656 ? Co1 N1 1.969(5) . ? Co1 Co2 2.2888(15) . ? Co1 Cl1 2.450(2) . ? Co2 N9 1.918(5) 2_656 ? Co2 N9 1.918(5) . ? Co2 N2 1.918(5) 2_656 ? Co2 N2 1.918(5) . ? Co2 Co3 2.2793(15) . ? Co3 N10 1.943(5) 2_656 ? Co3 N10 1.943(5) . ? Co3 N3 1.946(5) 2_656 ? Co3 N3 1.946(5) . ? Co3 Co4 2.2745(15) . ? Co4 N4 1.923(5) 2_656 ? Co4 N4 1.923(5) . ? Co4 N11 1.924(5) 2_656 ? Co4 N11 1.924(5) . ? Co4 Co5 2.2867(15) . ? Co5 N5 1.961(5) 2_656 ? Co5 N5 1.961(5) . ? Co5 N12 1.974(5) 2_656 ? Co5 N12 1.974(5) . ? Co5 Cl2 2.484(3) . ? N1 C1 1.355(8) . ? N1 C4 1.359(8) . ? N2 C4 1.362(8) . ? N2 C5 1.379(8) . ? N3 C9 1.370(7) . ? N3 C5 1.373(7) . ? N4 C10 1.347(8) . ? N4 C9 1.390(8) . ? N5 C13 1.354(9) . ? N5 C10 1.372(8) . ? N6 C3 1.315(8) . ? N6 C2 1.342(9) . ? N7 C11 1.322(9) . ? N7 C12 1.358(10) . ? N8 C14 1.356(8) . ? N8 C17 1.367(8) . ? N9 C17 1.358(8) . ? N9 C18 1.385(8) . ? N10 C22 1.364(7) . ? N10 C18 1.376(7) . ? N11 C23 1.360(8) . ? N11 C22 1.377(8) . ? N12 C23 1.355(8) . ? N12 C26 1.363(8) . ? N13 C16 1.313(9) . ? N13 C15 1.351(9) . ? N14 C24 1.321(9) . ? N14 C25 1.352(10) . ? C1 C2 1.361(9) . ? C3 C4 1.425(8) . ? C5 C6 1.392(8) . ? C6 C7 1.368(9) . ? C7 C8 1.385(9) . ? C8 C9 1.394(8) . ? C10 C11 1.425(9) . ? C12 C13 1.365(10) . ? C14 C15 1.372(10) . ? C16 C17 1.422(9) . ? C18 C19 1.402(9) . ? C19 C20 1.380(9) . ? C20 C21 1.381(9) . ? C21 C22 1.402(9) . ? C23 C24 1.419(9) . ? C25 C26 1.354(10) . ? P1 C27 1.797(7) . ? P1 C27 1.797(7) 2_656 ? P1 C33 1.807(7) 2_656 ? P1 C33 1.807(7) . ? C27 C32 1.389(11) . ? C27 C28 1.400(10) . ? C28 C29 1.393(11) . ? C29 C30 1.375(12) . ? C30 C31 1.381(11) . ? C31 C32 1.388(11) . ? C33 C34 1.382(10) . ? C33 C38 1.399(11) . ? C34 C35 1.397(11) . ? C35 C36 1.355(12) . ? C36 C37 1.362(13) . ? C37 C38 1.380(12) . ? Cl3 C39 1.734(8) . ? Cl3 C39' 1.766(10) . ? C39 Cl4B 1.741(8) . ? C39 Cl4A 1.749(8) . ? Cl4A Cl4B 0.853(8) . ? C39' Cl4' 1.773(10) . ? 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 N8 Co1 N8 171.2(3) . 2_656 ? N8 Co1 N1 89.7(2) . 2_656 ? N8 Co1 N1 89.6(2) 2_656 2_656 ? N8 Co1 N1 89.6(2) . . ? N8 Co1 N1 89.7(2) 2_656 . ? N1 Co1 N1 171.0(3) 2_656 . ? N8 Co1 Co2 85.59(14) . . ? N8 Co1 Co2 85.59(15) 2_656 . ? N1 Co1 Co2 85.50(14) 2_656 . ? N1 Co1 Co2 85.50(14) . . ? N8 Co1 Cl1 94.41(14) . . ? N8 Co1 Cl1 94.41(15) 2_656 . ? N1 Co1 Cl1 94.50(14) 2_656 . ? N1 Co1 Cl1 94.50(14) . . ? Co2 Co1 Cl1 180.0 . . ? N9 Co2 N9 178.4(3) 2_656 . ? N9 Co2 N2 89.8(2) 2_656 2_656 ? N9 Co2 N2 90.2(2) . 2_656 ? N9 Co2 N2 90.2(2) 2_656 . ? N9 Co2 N2 89.8(2) . . ? N2 Co2 N2 177.8(3) 2_656 . ? N9 Co2 Co3 89.20(15) 2_656 . ? N9 Co2 Co3 89.20(15) . . ? N2 Co2 Co3 88.92(14) 2_656 . ? N2 Co2 Co3 88.92(14) . . ? N9 Co2 Co1 90.80(15) 2_656 . ? N9 Co2 Co1 90.80(15) . . ? N2 Co2 Co1 91.08(14) 2_656 . ? N2 Co2 Co1 91.08(14) . . ? Co3 Co2 Co1 180.0 . . ? N10 Co3 N10 179.6(3) 2_656 . ? N10 Co3 N3 89.0(2) 2_656 2_656 ? N10 Co3 N3 91.0(2) . 2_656 ? N10 Co3 N3 91.0(2) 2_656 . ? N10 Co3 N3 89.0(2) . . ? N3 Co3 N3 179.5(3) 2_656 . ? N10 Co3 Co4 90.21(14) 2_656 . ? N10 Co3 Co4 90.21(14) . . ? N3 Co3 Co4 89.74(14) 2_656 . ? N3 Co3 Co4 89.74(14) . . ? N10 Co3 Co2 89.79(14) 2_656 . ? N10 Co3 Co2 89.79(14) . . ? N3 Co3 Co2 90.26(14) 2_656 . ? N3 Co3 Co2 90.26(14) . . ? Co4 Co3 Co2 180.0 . . ? N4 Co4 N4 178.9(3) 2_656 . ? N4 Co4 N11 89.9(2) 2_656 2_656 ? N4 Co4 N11 90.1(2) . 2_656 ? N4 Co4 N11 90.1(2) 2_656 . ? N4 Co4 N11 89.9(2) . . ? N11 Co4 N11 178.1(3) 2_656 . ? N4 Co4 Co3 89.46(15) 2_656 . ? N4 Co4 Co3 89.46(15) . . ? N11 Co4 Co3 89.04(15) 2_656 . ? N11 Co4 Co3 89.04(15) . . ? N4 Co4 Co5 90.54(15) 2_656 . ? N4 Co4 Co5 90.54(15) . . ? N11 Co4 Co5 90.96(15) 2_656 . ? N11 Co4 Co5 90.96(15) . . ? Co3 Co4 Co5 180.0 . . ? N5 Co5 N5 171.6(3) 2_656 . ? N5 Co5 N12 90.0(2) 2_656 2_656 ? N5 Co5 N12 89.3(2) . 2_656 ? N5 Co5 N12 89.3(2) 2_656 . ? N5 Co5 N12 90.0(2) . . ? N12 Co5 N12 171.1(3) 2_656 . ? N5 Co5 Co4 85.81(16) 2_656 . ? N5 Co5 Co4 85.81(16) . . ? N12 Co5 Co4 85.53(15) 2_656 . ? N12 Co5 Co4 85.53(15) . . ? N5 Co5 Cl2 94.19(16) 2_656 . ? N5 Co5 Cl2 94.19(16) . . ? N12 Co5 Cl2 94.47(15) 2_656 . ? N12 Co5 Cl2 94.47(15) . . ? Co4 Co5 Cl2 180.0 . . ? C1 N1 C4 117.0(5) . . ? C1 N1 Co1 122.0(4) . . ? C4 N1 Co1 120.8(4) . . ? C4 N2 C5 123.4(5) . . ? C4 N2 Co2 115.4(4) . . ? C5 N2 Co2 120.6(4) . . ? C9 N3 C5 120.5(5) . . ? C9 N3 Co3 120.1(4) . . ? C5 N3 Co3 119.4(4) . . ? C10 N4 C9 124.3(5) . . ? C10 N4 Co4 116.9(4) . . ? C9 N4 Co4 118.7(4) . . ? C13 N5 C10 118.2(6) . . ? C13 N5 Co5 121.6(5) . . ? C10 N5 Co5 120.2(4) . . ? C3 N6 C2 116.6(6) . . ? C11 N7 C12 116.4(6) . . ? C14 N8 C17 118.1(5) . . ? C14 N8 Co1 121.1(4) . . ? C17 N8 Co1 120.8(4) . . ? C17 N9 C18 123.7(5) . . ? C17 N9 Co2 116.9(4) . . ? C18 N9 Co2 119.4(4) . . ? C22 N10 C18 120.4(5) . . ? C22 N10 Co3 119.5(4) . . ? C18 N10 Co3 120.0(4) . . ? C23 N11 C22 123.7(5) . . ? C23 N11 Co4 115.5(4) . . ? C22 N11 Co4 120.1(4) . . ? C23 N12 C26 117.8(6) . . ? C23 N12 Co5 120.9(4) . . ? C26 N12 Co5 121.2(5) . . ? C16 N13 C15 116.5(6) . . ? C24 N14 C25 115.9(6) . . ? N1 C1 C2 122.9(6) . . ? N6 C2 C1 121.6(6) . . ? N6 C3 C4 123.8(6) . . ? N1 C4 N2 116.5(5) . . ? N1 C4 C3 118.1(5) . . ? N2 C4 C3 125.0(5) . . ? N3 C5 N2 115.3(5) . . ? N3 C5 C6 119.1(5) . . ? N2 C5 C6 125.6(5) . . ? C7 C6 C5 120.3(6) . . ? C6 C7 C8 120.4(6) . . ? C7 C8 C9 118.6(6) . . ? N3 C9 N4 114.9(5) . . ? N3 C9 C8 120.4(5) . . ? N4 C9 C8 124.6(5) . . ? N4 C10 N5 116.2(5) . . ? N4 C10 C11 126.5(6) . . ? N5 C10 C11 117.0(6) . . ? N7 C11 C10 124.3(6) . . ? N7 C12 C13 121.8(7) . . ? N5 C13 C12 122.1(7) . . ? N8 C14 C15 121.1(6) . . ? N13 C15 C14 122.4(6) . . ? N13 C16 C17 123.9(6) . . ? N9 C17 N8 115.8(5) . . ? N9 C17 C16 126.1(6) . . ? N8 C17 C16 117.8(5) . . ? N10 C18 N9 114.7(5) . . ? N10 C18 C19 119.9(5) . . ? N9 C18 C19 125.3(5) . . ? C20 C19 C18 119.4(6) . . ? C19 C20 C21 119.9(6) . . ? C20 C21 C22 119.7(6) . . ? N10 C22 N11 115.8(5) . . ? N10 C22 C21 119.8(5) . . ? N11 C22 C21 124.3(5) . . ? N12 C23 N11 116.5(5) . . ? N12 C23 C24 117.5(6) . . ? N11 C23 C24 125.7(6) . . ? N14 C24 C23 124.6(6) . . ? N14 C25 C26 122.1(7) . . ? C25 C26 N12 122.1(7) . . ? C27 P1 C27 110.3(5) . 2_656 ? C27 P1 C33 109.2(3) . 2_656 ? C27 P1 C33 109.6(3) 2_656 2_656 ? C27 P1 C33 109.6(3) . . ? C27 P1 C33 109.2(3) 2_656 . ? C33 P1 C33 108.9(5) 2_656 . ? C32 C27 C28 119.8(7) . . ? C32 C27 P1 121.3(5) . . ? C28 C27 P1 118.8(6) . . ? C29 C28 C27 119.3(7) . . ? C30 C29 C28 120.6(7) . . ? C29 C30 C31 119.9(7) . . ? C30 C31 C32 120.4(8) . . ? C31 C32 C27 119.8(7) . . ? C34 C33 C38 119.9(7) . . ? C34 C33 P1 120.7(6) . . ? C38 C33 P1 119.3(6) . . ? C33 C34 C35 119.3(7) . . ? C36 C35 C34 120.1(8) . . ? C35 C36 C37 121.0(8) . . ? C36 C37 C38 120.6(8) . . ? C37 C38 C33 119.1(8) . . ? C39 Cl3 C39' 52.6(8) . . ? Cl3 C39 Cl4B 110.3(6) . . ? Cl3 C39 Cl4A 114.6(6) . . ? Cl4B C39 Cl4A 28.3(3) . . ? Cl4B Cl4A C39 75.4(7) . . ? Cl4A Cl4B C39 76.3(7) . . ? Cl3 C39' Cl4' 141.4(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.430 _refine_diff_density_min -1.731 _refine_diff_density_rms 0.140 # Attachment 'ic13154.cif' data_ic13154 _database_code_depnum_ccdc_archive 'CCDC 694070' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H64 Cl8 Co5 N30 P S2' _chemical_formula_weight 2142.97 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' P P 0.1023 0.0942 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8060(4) _cell_length_b 16.8778(4) _cell_length_c 17.7166(5) _cell_angle_alpha 98.6556(15) _cell_angle_beta 93.3470(14) _cell_angle_gamma 90.8523(16) _cell_volume 4368.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour deep-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65266 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19869 _reflns_number_gt 10995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+18.2139P] 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 19869 _refine_ls_number_parameters 1147 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1405 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.1868 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.015 _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 0.76165(5) 0.23746(5) 0.66658(4) 0.02639(19) Uani 1 1 d . . . Co2 Co 0.75325(5) 0.26651(4) 0.54464(4) 0.02268(18) Uani 1 1 d . . . Co3 Co 0.74398(5) 0.29625(4) 0.42439(4) 0.02144(17) Uani 1 1 d . . . Co4 Co 0.73448(5) 0.32607(4) 0.30417(4) 0.02268(18) Uani 1 1 d . . . Co5 Co 0.72436(5) 0.35592(5) 0.18268(4) 0.02547(19) Uani 1 1 d . . . S1 S 0.7681(2) 0.17101(17) 0.92306(13) 0.0935(10) Uani 1 1 d . . . S2 S 0.70679(13) 0.44351(13) -0.06655(10) 0.0516(5) Uani 1 1 d . . . N1 N 0.6932(3) 0.1384(3) 0.6240(3) 0.0323(11) Uani 1 1 d . . . N2 N 0.6493(3) 0.1971(3) 0.5183(3) 0.0254(10) Uani 1 1 d . . . N3 N 0.6191(3) 0.2582(3) 0.4121(3) 0.0250(10) Uani 1 1 d . . . N4 N 0.6056(3) 0.3241(3) 0.3069(3) 0.0250(10) Uani 1 1 d . . . N5 N 0.6049(3) 0.3991(3) 0.2082(3) 0.0253(10) Uani 1 1 d . . . N6 N 0.6049(4) -0.0057(3) 0.5601(3) 0.0490(15) Uani 1 1 d . . . N7 N 0.4375(3) 0.4633(3) 0.2486(3) 0.0337(12) Uani 1 1 d . . . N8 N 0.8288(3) 0.3399(3) 0.6930(3) 0.0264(10) Uani 1 1 d . . . N9 N 0.8575(3) 0.3369(3) 0.5662(3) 0.0247(10) Uani 1 1 d . . . N10 N 0.8689(3) 0.3330(3) 0.4367(3) 0.0238(10) Uani 1 1 d . . . N11 N 0.8648(3) 0.3255(3) 0.3049(3) 0.0258(10) Uani 1 1 d . . . N12 N 0.8419(3) 0.3038(3) 0.1734(3) 0.0278(11) Uani 1 1 d . . . N13 N 0.9253(4) 0.4860(3) 0.7339(3) 0.0371(12) Uani 1 1 d . . . N14 N 0.9937(3) 0.2088(3) 0.1593(3) 0.0392(13) Uani 1 1 d . . . N15 N 0.6461(3) 0.2917(3) 0.6773(3) 0.0299(11) Uani 1 1 d . . . N16 N 0.6751(3) 0.3535(3) 0.5735(3) 0.0243(10) Uani 1 1 d . . . N17 N 0.7041(3) 0.4023(3) 0.4621(2) 0.0225(10) Uani 1 1 d . . . N18 N 0.7379(3) 0.4373(3) 0.3461(3) 0.0252(10) Uani 1 1 d . . . N19 N 0.7810(3) 0.4603(3) 0.2281(3) 0.0281(11) Uani 1 1 d . . . N20 N 0.4695(3) 0.3510(3) 0.6801(3) 0.0398(13) Uani 1 1 d . . . N21 N 0.8599(4) 0.6096(3) 0.2922(3) 0.0399(13) Uani 1 1 d . . . N22 N 0.8758(3) 0.1857(3) 0.6381(3) 0.0294(11) Uani 1 1 d . . . N23 N 0.8304(3) 0.1793(3) 0.5108(3) 0.0262(10) Uani 1 1 d . . . N24 N 0.7821(3) 0.1887(3) 0.3860(3) 0.0259(10) Uani 1 1 d . . . N25 N 0.7284(3) 0.2135(3) 0.2670(3) 0.0254(10) Uani 1 1 d . . . N26 N 0.6684(3) 0.2486(3) 0.1537(3) 0.0276(11) Uani 1 1 d . . . N27 N 1.0427(4) 0.1209(4) 0.6011(3) 0.0446(14) Uani 1 1 d . . . N28 N 0.5762(4) 0.1005(3) 0.1160(3) 0.0390(13) Uani 1 1 d . . . N29 N 0.7714(3) 0.2104(3) 0.7790(3) 0.0300(11) Uani 1 1 d . . . N30 N 0.7154(3) 0.3847(3) 0.0717(3) 0.0288(11) Uani 1 1 d . . . C1 C 0.6926(5) 0.0737(4) 0.6599(4) 0.0438(17) Uani 1 1 d . . . H1 H 0.7242 0.0766 0.7085 0.053 Uiso 1 1 calc R . . C2 C 0.6481(6) 0.0041(4) 0.6287(4) 0.054(2) Uani 1 1 d . . . H2 H 0.6481 -0.0393 0.6572 0.065 Uiso 1 1 calc R . . C3 C 0.6034(4) 0.0574(4) 0.5235(4) 0.0384(15) Uani 1 1 d . . . H3 H 0.5726 0.0525 0.4744 0.046 Uiso 1 1 calc R . . C4 C 0.6459(4) 0.1318(4) 0.5548(3) 0.0301(13) Uani 1 1 d . . . C5 C 0.5867(4) 0.2108(3) 0.4609(3) 0.0256(12) Uani 1 1 d . . . C6 C 0.4971(4) 0.1857(4) 0.4547(4) 0.0312(13) Uani 1 1 d . . . H6 H 0.4738 0.1564 0.4913 0.037 Uiso 1 1 calc R . . C7 C 0.4414(4) 0.2040(4) 0.3938(3) 0.0321(14) Uani 1 1 d . . . H7 H 0.3799 0.1861 0.3883 0.039 Uiso 1 1 calc R . . C8 C 0.4749(4) 0.2481(3) 0.3413(3) 0.0291(13) Uani 1 1 d . . . H8 H 0.4382 0.2580 0.2981 0.035 Uiso 1 1 calc R . . C9 C 0.5633(4) 0.2774(3) 0.3533(3) 0.0257(12) Uani 1 1 d . . . C10 C 0.5598(4) 0.3744(3) 0.2665(3) 0.0249(12) Uani 1 1 d . . . C11 C 0.4764(4) 0.4092(4) 0.2845(3) 0.0299(13) Uani 1 1 d . . . H11 H 0.4464 0.3923 0.3255 0.036 Uiso 1 1 calc R . . C12 C 0.4836(4) 0.4861(4) 0.1910(4) 0.0364(15) Uani 1 1 d . . . H12 H 0.4581 0.5250 0.1630 0.044 Uiso 1 1 calc R . . C13 C 0.5649(4) 0.4551(4) 0.1720(3) 0.0302(13) Uani 1 1 d . . . H13 H 0.5946 0.4738 0.1317 0.036 Uiso 1 1 calc R . . C14 C 0.8340(4) 0.3799(4) 0.7661(3) 0.0318(14) Uani 1 1 d . . . H14 H 0.8032 0.3583 0.8042 0.038 Uiso 1 1 calc R . . C15 C 0.8820(5) 0.4498(4) 0.7857(4) 0.0387(15) Uani 1 1 d . . . H15 H 0.8856 0.4744 0.8377 0.046 Uiso 1 1 calc R . . C16 C 0.9189(4) 0.4488(4) 0.6638(3) 0.0302(13) Uani 1 1 d . . . H16 H 0.9479 0.4729 0.6262 0.036 Uiso 1 1 calc R . . C17 C 0.8716(4) 0.3748(4) 0.6397(3) 0.0294(13) Uani 1 1 d . . . C18 C 0.9115(4) 0.3487(3) 0.5072(3) 0.0254(12) Uani 1 1 d . . . C19 C 1.0037(4) 0.3688(4) 0.5167(3) 0.0321(14) Uani 1 1 d . . . H19 H 1.0342 0.3759 0.5660 0.038 Uiso 1 1 calc R . . C20 C 1.0496(4) 0.3782(4) 0.4529(3) 0.0322(14) Uani 1 1 d . . . H20 H 1.1118 0.3937 0.4586 0.039 Uiso 1 1 calc R . . C21 C 1.0060(4) 0.3652(4) 0.3809(4) 0.0311(13) Uani 1 1 d . . . H21 H 1.0374 0.3731 0.3372 0.037 Uiso 1 1 calc R . . C22 C 0.9156(4) 0.3403(3) 0.3732(3) 0.0255(12) Uani 1 1 d . . . C23 C 0.8973(4) 0.2965(3) 0.2368(3) 0.0276(12) Uani 1 1 d . . . C24 C 0.9754(4) 0.2494(4) 0.2257(4) 0.0355(14) Uani 1 1 d . . . H24 H 1.0165 0.2471 0.2685 0.043 Uiso 1 1 calc R . . C25 C 0.9361(4) 0.2151(4) 0.0988(4) 0.0362(15) Uani 1 1 d . . . H25 H 0.9471 0.1856 0.0502 0.043 Uiso 1 1 calc R . . C26 C 0.8623(4) 0.2629(4) 0.1056(3) 0.0315(13) Uani 1 1 d . . . H26 H 0.8245 0.2673 0.0613 0.038 Uiso 1 1 calc R . . C27 C 0.5864(4) 0.2737(4) 0.7291(4) 0.0366(15) Uani 1 1 d . . . H27 H 0.6049 0.2400 0.7652 0.044 Uiso 1 1 calc R . . C28 C 0.5017(4) 0.3032(4) 0.7297(4) 0.0414(16) Uani 1 1 d . . . H28 H 0.4630 0.2894 0.7668 0.050 Uiso 1 1 calc R . . C29 C 0.5269(4) 0.3697(4) 0.6314(4) 0.0342(14) Uani 1 1 d . . . H29 H 0.5071 0.4038 0.5960 0.041 Uiso 1 1 calc R . . C30 C 0.6167(4) 0.3421(3) 0.6286(3) 0.0272(12) Uani 1 1 d . . . C31 C 0.6700(4) 0.4171(3) 0.5332(3) 0.0245(12) Uani 1 1 d . . . C32 C 0.6391(4) 0.4919(3) 0.5607(3) 0.0283(13) Uani 1 1 d . . . H32 H 0.6198 0.5028 0.6113 0.034 Uiso 1 1 calc R . . C33 C 0.6361(4) 0.5515(4) 0.5143(3) 0.0314(13) Uani 1 1 d . . . H33 H 0.6122 0.6023 0.5322 0.038 Uiso 1 1 calc R . . C34 C 0.6686(4) 0.5360(3) 0.4407(3) 0.0293(13) Uani 1 1 d . . . H34 H 0.6659 0.5755 0.4078 0.035 Uiso 1 1 calc R . . C35 C 0.7048(4) 0.4616(3) 0.4175(3) 0.0258(12) Uani 1 1 d . . . C36 C 0.7758(4) 0.4887(3) 0.3037(3) 0.0277(13) Uani 1 1 d . . . C37 C 0.8163(4) 0.5647(4) 0.3330(4) 0.0323(14) Uani 1 1 d . . . H37 H 0.8115 0.5844 0.3858 0.039 Uiso 1 1 calc R . . C38 C 0.8635(4) 0.5797(4) 0.2172(4) 0.0389(15) Uani 1 1 d . . . H38 H 0.8930 0.6105 0.1848 0.047 Uiso 1 1 calc R . . C39 C 0.8265(4) 0.5073(4) 0.1867(4) 0.0335(14) Uani 1 1 d . . . H39 H 0.8328 0.4886 0.1340 0.040 Uiso 1 1 calc R . . C40 C 0.9426(4) 0.1776(4) 0.6924(4) 0.0390(16) Uani 1 1 d . . . H40 H 0.9321 0.1944 0.7447 0.047 Uiso 1 1 calc R . . C41 C 1.0235(5) 0.1462(4) 0.6740(4) 0.0476(18) Uani 1 1 d . . . H41 H 1.0682 0.1420 0.7138 0.057 Uiso 1 1 calc R . . C42 C 0.9791(4) 0.1288(4) 0.5481(4) 0.0392(16) Uani 1 1 d . . . H42 H 0.9912 0.1114 0.4962 0.047 Uiso 1 1 calc R . . C43 C 0.8928(4) 0.1619(4) 0.5639(3) 0.0297(13) Uani 1 1 d . . . C44 C 0.8224(4) 0.1436(3) 0.4358(3) 0.0276(13) Uani 1 1 d . . . C45 C 0.8456(4) 0.0645(4) 0.4090(4) 0.0358(15) Uani 1 1 d . . . H45 H 0.8706 0.0314 0.4433 0.043 Uiso 1 1 calc R . . C46 C 0.8316(5) 0.0358(4) 0.3325(4) 0.0414(16) Uani 1 1 d . . . H46 H 0.8485 -0.0173 0.3139 0.050 Uiso 1 1 calc R . . C47 C 0.7933(4) 0.0827(4) 0.2818(4) 0.0360(15) Uani 1 1 d . . . H47 H 0.7857 0.0630 0.2287 0.043 Uiso 1 1 calc R . . C48 C 0.7664(4) 0.1592(3) 0.3108(3) 0.0281(13) Uani 1 1 d . . . C49 C 0.6776(4) 0.1917(3) 0.2009(3) 0.0284(13) Uani 1 1 d . . . C50 C 0.6278(4) 0.1187(4) 0.1803(4) 0.0332(14) Uani 1 1 d . . . H50 H 0.6316 0.0805 0.2145 0.040 Uiso 1 1 calc R . . C51 C 0.5726(5) 0.1567(4) 0.0696(4) 0.0418(16) Uani 1 1 d . . . H51 H 0.5375 0.1458 0.0224 0.050 Uiso 1 1 calc R . . C52 C 0.6175(4) 0.2289(4) 0.0880(3) 0.0336(14) Uani 1 1 d . . . H52 H 0.6126 0.2665 0.0531 0.040 Uiso 1 1 calc R . . C53 C 0.7692(5) 0.1946(4) 0.8360(4) 0.0452(17) Uani 1 1 d . . . C54 C 0.7122(4) 0.4079(4) 0.0153(4) 0.0335(14) Uani 1 1 d . . . P1 P 0.21504(11) 0.26711(10) 0.05072(9) 0.0334(4) Uani 1 1 d . . . C55 C 0.1081(4) 0.3016(4) 0.0176(4) 0.0351(14) Uani 1 1 d . . . C56 C 0.0683(4) 0.3677(4) 0.0593(4) 0.0458(17) Uani 1 1 d . . . H56 H 0.0954 0.3925 0.1071 0.055 Uiso 1 1 calc R . . C57 C -0.0118(5) 0.3966(5) 0.0296(5) 0.053(2) Uani 1 1 d . . . H57 H -0.0382 0.4426 0.0566 0.064 Uiso 1 1 calc R . . C58 C -0.0521(5) 0.3602(5) -0.0367(5) 0.057(2) Uani 1 1 d . . . H58 H -0.1075 0.3798 -0.0555 0.069 Uiso 1 1 calc R . . C59 C -0.0139(5) 0.2949(6) -0.0777(4) 0.058(2) Uani 1 1 d . . . H59 H -0.0429 0.2705 -0.1248 0.070 Uiso 1 1 calc R . . C60 C 0.0660(5) 0.2642(5) -0.0513(4) 0.0481(18) Uani 1 1 d . . . H60 H 0.0917 0.2185 -0.0796 0.058 Uiso 1 1 calc R . . C61 C 0.3030(4) 0.3177(4) 0.0096(4) 0.0341(14) Uani 1 1 d . . . C62 C 0.2863(4) 0.3400(4) -0.0625(4) 0.0415(16) Uani 1 1 d . . . H62 H 0.2267 0.3353 -0.0859 0.050 Uiso 1 1 calc R . . C63 C 0.3561(5) 0.3688(5) -0.0998(4) 0.0496(19) Uani 1 1 d . . . H63 H 0.3454 0.3822 -0.1497 0.060 Uiso 1 1 calc R . . C64 C 0.4417(5) 0.3777(4) -0.0640(4) 0.0496(18) Uani 1 1 d . . . H64 H 0.4897 0.3979 -0.0895 0.060 Uiso 1 1 calc R . . C65 C 0.4585(4) 0.3583(4) 0.0072(4) 0.0446(17) Uani 1 1 d . . . H65 H 0.5176 0.3660 0.0313 0.053 Uiso 1 1 calc R . . C66 C 0.3888(4) 0.3270(4) 0.0452(4) 0.0401(16) Uani 1 1 d . . . H66 H 0.4005 0.3124 0.0945 0.048 Uiso 1 1 calc R . . C67 C 0.2224(4) 0.1620(4) 0.0179(4) 0.0372(15) Uani 1 1 d . . . C68 C 0.2955(5) 0.1332(4) -0.0232(4) 0.0465(17) Uani 1 1 d . . . H68 H 0.3404 0.1694 -0.0350 0.056 Uiso 1 1 calc R . . C69 C 0.3026(6) 0.0512(5) -0.0468(5) 0.058(2) Uani 1 1 d . . . H69 H 0.3530 0.0312 -0.0739 0.069 Uiso 1 1 calc R . . C70 C 0.2360(5) -0.0014(4) -0.0307(4) 0.0499(18) Uani 1 1 d . . . H70 H 0.2406 -0.0573 -0.0473 0.060 Uiso 1 1 calc R . . C71 C 0.1636(5) 0.0272(5) 0.0092(4) 0.0515(19) Uani 1 1 d . . . H71 H 0.1186 -0.0092 0.0205 0.062 Uiso 1 1 calc R . . C72 C 0.1553(5) 0.1091(4) 0.0331(4) 0.0407(16) Uani 1 1 d . . . H72 H 0.1043 0.1287 0.0596 0.049 Uiso 1 1 calc R . . C73 C 0.2289(4) 0.2880(4) 0.1529(4) 0.0365(15) Uani 1 1 d . . . C74 C 0.2188(4) 0.2268(4) 0.1975(4) 0.0417(16) Uani 1 1 d . . . H74 H 0.2090 0.1728 0.1736 0.050 Uiso 1 1 calc R . . C75 C 0.2232(4) 0.2450(6) 0.2752(4) 0.052(2) Uani 1 1 d . . . H75 H 0.2172 0.2034 0.3053 0.063 Uiso 1 1 calc R . . C76 C 0.2361(4) 0.3234(6) 0.3107(4) 0.052(2) Uani 1 1 d . . . H76 H 0.2370 0.3353 0.3649 0.063 Uiso 1 1 calc R . . C77 C 0.2476(4) 0.3839(5) 0.2685(4) 0.0491(19) Uani 1 1 d . . . H77 H 0.2573 0.4376 0.2932 0.059 Uiso 1 1 calc R . . C78 C 0.2450(4) 0.3661(5) 0.1886(4) 0.0442(17) Uani 1 1 d . . . H78 H 0.2542 0.4076 0.1589 0.053 Uiso 1 1 calc R . . C79 C 0.5883(6) 0.0209(5) 0.8738(6) 0.074(3) Uani 1 1 d . . . H79A H 0.5540 0.0020 0.9142 0.089 Uiso 1 1 calc R . . H79B H 0.6373 0.0578 0.8992 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.6363(2) -0.0614(2) 0.81984(16) 0.0993(9) Uani 1 1 d . . . Cl2 Cl 0.5161(2) 0.07350(19) 0.8191(2) 0.1093(10) Uani 1 1 d . . . C80 C 0.2812(8) 0.1945(8) 0.6898(8) 0.134(5) Uani 1 1 d D . . H80A H 0.3029 0.2504 0.6906 0.160 Uiso 1 1 calc R . . H80B H 0.2222 0.1873 0.6600 0.160 Uiso 1 1 calc R . . Cl3 Cl 0.2677(3) 0.1780(3) 0.7796(2) 0.1608(17) Uani 1 1 d . . . Cl4 Cl 0.3601(3) 0.1274(3) 0.6451(3) 0.1726(19) Uani 1 1 d D . . C81 C 0.2104(9) 0.1256(7) 0.4826(7) 0.109(4) Uiso 1 1 d . . . H81A H 0.2726 0.1052 0.4787 0.131 Uiso 1 1 calc R . . H81B H 0.1868 0.1094 0.5293 0.131 Uiso 1 1 calc R . . Cl5 Cl 0.2176(4) 0.2297(3) 0.4955(3) 0.221(3) Uani 1 1 d . . . Cl6 Cl 0.1467(4) 0.0792(4) 0.4071(3) 0.198(2) Uiso 1 1 d . . . C82 C 1.0336(7) 1.0312(9) 0.2105(6) 0.151(6) Uani 1 1 d D . . H82A H 1.0264 1.0845 0.1944 0.181 Uiso 0.67 1 calc PR A 1 H82B H 1.0148 1.0350 0.2637 0.181 Uiso 0.67 1 calc PR A 1 H82C H 1.0822 1.0408 0.1767 0.181 Uiso 0.33 1 calc PR A 2 H82D H 0.9973 1.0802 0.2146 0.181 Uiso 0.33 1 calc PR A 2 Cl7 Cl 0.9662(3) 0.9648(3) 0.15383(17) 0.1288(13) Uani 1 1 d . B . Cl8 Cl 1.1408(3) 1.0072(3) 0.2087(2) 0.0962(13) Uani 0.67 1 d PD B 1 Cl8' Cl 1.0877(6) 1.0407(5) 0.2937(5) 0.091(2) Uiso 0.33 1 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0272(4) 0.0292(4) 0.0240(4) 0.0085(3) -0.0008(3) 0.0015(3) Co2 0.0210(4) 0.0260(4) 0.0218(4) 0.0066(3) 0.0000(3) 0.0019(3) Co3 0.0189(4) 0.0249(4) 0.0211(4) 0.0054(3) 0.0003(3) 0.0025(3) Co4 0.0201(4) 0.0274(4) 0.0210(4) 0.0051(3) 0.0005(3) 0.0029(3) Co5 0.0227(4) 0.0327(5) 0.0218(4) 0.0067(3) 0.0006(3) 0.0038(3) S1 0.146(3) 0.099(2) 0.0368(12) 0.0312(13) -0.0216(14) -0.0634(19) S2 0.0484(11) 0.0763(14) 0.0365(10) 0.0260(9) 0.0071(8) 0.0171(9) N1 0.037(3) 0.028(3) 0.033(3) 0.009(2) -0.003(2) -0.001(2) N2 0.022(2) 0.028(3) 0.026(3) 0.007(2) -0.0002(19) -0.0037(19) N3 0.019(2) 0.031(3) 0.025(3) 0.006(2) 0.0000(19) 0.0036(19) N4 0.019(2) 0.035(3) 0.021(2) 0.007(2) 0.0003(18) 0.0045(19) N5 0.023(2) 0.030(3) 0.022(2) 0.004(2) 0.0000(19) 0.0043(19) N6 0.067(4) 0.032(3) 0.048(4) 0.016(3) -0.015(3) -0.012(3) N7 0.024(3) 0.038(3) 0.042(3) 0.017(2) 0.001(2) 0.007(2) N8 0.024(2) 0.031(3) 0.025(3) 0.009(2) -0.0036(19) 0.002(2) N9 0.020(2) 0.033(3) 0.023(2) 0.009(2) -0.0013(18) 0.0026(19) N10 0.021(2) 0.028(3) 0.024(2) 0.008(2) 0.0007(19) 0.0020(19) N11 0.023(2) 0.032(3) 0.024(2) 0.008(2) 0.0006(19) 0.001(2) N12 0.024(2) 0.034(3) 0.026(3) 0.008(2) 0.002(2) 0.000(2) N13 0.041(3) 0.036(3) 0.033(3) 0.003(2) 0.001(2) -0.002(2) N14 0.030(3) 0.052(3) 0.036(3) 0.007(3) 0.003(2) 0.008(2) N15 0.027(3) 0.037(3) 0.028(3) 0.010(2) 0.005(2) 0.003(2) N16 0.024(2) 0.027(3) 0.023(2) 0.007(2) 0.0035(19) 0.0036(19) N17 0.022(2) 0.026(2) 0.020(2) 0.0048(19) -0.0007(18) 0.0041(19) N18 0.024(2) 0.025(3) 0.026(3) 0.006(2) -0.0017(19) -0.0007(19) N19 0.024(2) 0.034(3) 0.028(3) 0.011(2) 0.000(2) 0.001(2) N20 0.029(3) 0.050(3) 0.043(3) 0.013(3) 0.012(2) 0.004(2) N21 0.040(3) 0.041(3) 0.040(3) 0.011(3) 0.006(2) -0.009(2) N22 0.032(3) 0.029(3) 0.028(3) 0.009(2) 0.000(2) 0.004(2) N23 0.024(2) 0.030(3) 0.026(3) 0.009(2) -0.0010(19) 0.002(2) N24 0.022(2) 0.027(3) 0.029(3) 0.007(2) 0.0017(19) 0.0039(19) N25 0.025(2) 0.030(3) 0.021(2) 0.003(2) -0.0022(19) 0.004(2) N26 0.023(2) 0.036(3) 0.023(3) 0.002(2) 0.0007(19) 0.003(2) N27 0.036(3) 0.057(4) 0.042(3) 0.012(3) -0.006(3) 0.021(3) N28 0.040(3) 0.037(3) 0.039(3) 0.002(3) -0.004(2) 0.000(2) N29 0.034(3) 0.036(3) 0.019(3) 0.001(2) 0.000(2) -0.003(2) N30 0.028(3) 0.040(3) 0.020(3) 0.009(2) -0.001(2) 0.003(2) C1 0.059(4) 0.038(4) 0.038(4) 0.021(3) -0.008(3) -0.005(3) C2 0.076(5) 0.035(4) 0.053(5) 0.021(4) -0.019(4) -0.011(4) C3 0.036(4) 0.038(4) 0.042(4) 0.011(3) -0.008(3) -0.004(3) C4 0.029(3) 0.034(3) 0.030(3) 0.013(3) 0.003(2) 0.002(3) C5 0.025(3) 0.024(3) 0.027(3) 0.005(2) 0.001(2) 0.001(2) C6 0.027(3) 0.031(3) 0.037(3) 0.013(3) 0.000(3) -0.005(2) C7 0.022(3) 0.034(3) 0.039(4) 0.007(3) -0.003(3) -0.002(2) C8 0.027(3) 0.031(3) 0.030(3) 0.007(3) -0.002(2) 0.003(2) C9 0.024(3) 0.029(3) 0.024(3) 0.002(2) 0.001(2) 0.003(2) C10 0.026(3) 0.026(3) 0.021(3) 0.002(2) -0.002(2) 0.000(2) C11 0.029(3) 0.033(3) 0.028(3) 0.006(3) 0.002(2) 0.005(2) C12 0.033(3) 0.044(4) 0.035(3) 0.015(3) -0.004(3) 0.013(3) C13 0.031(3) 0.035(3) 0.026(3) 0.009(3) 0.001(2) 0.008(3) C14 0.034(3) 0.037(4) 0.025(3) 0.007(3) 0.002(3) 0.007(3) C15 0.051(4) 0.039(4) 0.024(3) 0.000(3) -0.001(3) -0.002(3) C16 0.028(3) 0.032(3) 0.031(3) 0.007(3) -0.003(2) 0.001(2) C17 0.027(3) 0.032(3) 0.032(3) 0.015(3) -0.002(2) 0.006(2) C18 0.023(3) 0.029(3) 0.026(3) 0.007(2) 0.000(2) 0.005(2) C19 0.026(3) 0.040(4) 0.031(3) 0.006(3) -0.003(2) 0.000(3) C20 0.017(3) 0.043(4) 0.035(3) 0.004(3) 0.001(2) -0.002(2) C21 0.023(3) 0.037(4) 0.035(3) 0.009(3) 0.007(2) 0.000(2) C22 0.026(3) 0.026(3) 0.025(3) 0.008(2) -0.001(2) 0.001(2) C23 0.023(3) 0.031(3) 0.029(3) 0.006(3) 0.001(2) -0.003(2) C24 0.028(3) 0.048(4) 0.032(3) 0.008(3) 0.002(3) 0.007(3) C25 0.033(3) 0.043(4) 0.032(3) 0.004(3) 0.005(3) 0.004(3) C26 0.031(3) 0.038(4) 0.027(3) 0.006(3) 0.005(2) 0.003(3) C27 0.031(3) 0.045(4) 0.036(4) 0.013(3) 0.005(3) 0.001(3) C28 0.031(3) 0.059(4) 0.038(4) 0.015(3) 0.014(3) 0.001(3) C29 0.030(3) 0.040(4) 0.034(3) 0.010(3) 0.006(3) 0.005(3) C30 0.024(3) 0.032(3) 0.024(3) 0.002(2) 0.000(2) -0.001(2) C31 0.025(3) 0.028(3) 0.020(3) 0.004(2) -0.005(2) 0.000(2) C32 0.029(3) 0.035(3) 0.021(3) 0.004(2) -0.001(2) 0.002(2) C33 0.035(3) 0.032(3) 0.028(3) 0.005(3) 0.002(3) 0.009(3) C34 0.031(3) 0.026(3) 0.032(3) 0.010(3) -0.002(3) 0.001(2) C35 0.022(3) 0.031(3) 0.025(3) 0.006(2) -0.003(2) 0.001(2) C36 0.023(3) 0.031(3) 0.031(3) 0.013(3) -0.002(2) 0.002(2) C37 0.029(3) 0.033(3) 0.034(3) 0.006(3) -0.004(3) -0.004(3) C38 0.031(3) 0.043(4) 0.046(4) 0.016(3) 0.003(3) -0.006(3) C39 0.029(3) 0.044(4) 0.030(3) 0.015(3) 0.000(3) 0.000(3) C40 0.043(4) 0.041(4) 0.034(4) 0.011(3) -0.008(3) 0.011(3) C41 0.039(4) 0.061(5) 0.042(4) 0.008(3) -0.011(3) 0.021(3) C42 0.037(4) 0.051(4) 0.032(3) 0.010(3) 0.002(3) 0.013(3) C43 0.027(3) 0.034(3) 0.030(3) 0.011(3) 0.000(2) 0.005(2) C44 0.026(3) 0.033(3) 0.027(3) 0.012(3) 0.003(2) 0.005(2) C45 0.042(4) 0.029(3) 0.038(4) 0.010(3) -0.001(3) 0.009(3) C46 0.054(4) 0.031(4) 0.038(4) 0.002(3) -0.001(3) 0.015(3) C47 0.041(4) 0.036(4) 0.029(3) 0.001(3) -0.001(3) 0.007(3) C48 0.026(3) 0.033(3) 0.027(3) 0.009(3) 0.001(2) 0.007(2) C49 0.025(3) 0.031(3) 0.029(3) 0.003(3) 0.007(2) 0.007(2) C50 0.036(3) 0.027(3) 0.034(3) -0.002(3) -0.003(3) 0.003(3) C51 0.042(4) 0.050(4) 0.031(4) 0.001(3) -0.010(3) 0.007(3) C52 0.037(3) 0.037(4) 0.025(3) 0.002(3) -0.001(3) 0.006(3) C53 0.054(5) 0.038(4) 0.039(4) -0.001(3) -0.007(3) -0.013(3) C54 0.025(3) 0.039(4) 0.036(4) 0.002(3) 0.005(3) 0.005(3) P1 0.0272(8) 0.0397(10) 0.0335(9) 0.0069(7) -0.0012(7) 0.0044(7) C55 0.030(3) 0.042(4) 0.035(4) 0.012(3) 0.001(3) 0.003(3) C56 0.028(3) 0.046(4) 0.063(5) 0.010(4) -0.001(3) 0.004(3) C57 0.036(4) 0.053(5) 0.076(6) 0.020(4) 0.009(4) 0.015(3) C58 0.034(4) 0.088(6) 0.060(5) 0.043(5) 0.003(4) 0.016(4) C59 0.035(4) 0.107(7) 0.036(4) 0.021(4) -0.003(3) 0.006(4) C60 0.035(4) 0.072(5) 0.037(4) 0.011(4) 0.004(3) 0.002(3) C61 0.030(3) 0.039(4) 0.033(3) 0.005(3) 0.004(3) 0.005(3) C62 0.033(4) 0.047(4) 0.046(4) 0.013(3) 0.000(3) 0.005(3) C63 0.044(4) 0.063(5) 0.048(4) 0.028(4) 0.004(3) 0.005(4) C64 0.044(4) 0.051(5) 0.056(5) 0.016(4) 0.011(4) 0.000(3) C65 0.026(3) 0.055(4) 0.053(4) 0.010(4) 0.001(3) 0.005(3) C66 0.033(4) 0.046(4) 0.043(4) 0.013(3) 0.003(3) 0.005(3) C67 0.037(4) 0.042(4) 0.032(3) 0.006(3) 0.001(3) 0.005(3) C68 0.045(4) 0.045(4) 0.051(4) 0.008(3) 0.010(3) 0.008(3) C69 0.061(5) 0.051(5) 0.063(5) 0.007(4) 0.018(4) 0.017(4) C70 0.064(5) 0.037(4) 0.051(5) 0.007(3) 0.012(4) 0.007(3) C71 0.064(5) 0.049(5) 0.044(4) 0.013(4) 0.010(4) -0.006(4) C72 0.039(4) 0.044(4) 0.040(4) 0.005(3) 0.005(3) 0.002(3) C73 0.023(3) 0.051(4) 0.034(3) 0.000(3) 0.001(3) 0.007(3) C74 0.030(3) 0.055(4) 0.039(4) 0.007(3) -0.005(3) 0.007(3) C75 0.031(4) 0.096(7) 0.031(4) 0.015(4) 0.002(3) 0.003(4) C76 0.021(3) 0.100(7) 0.035(4) 0.007(4) 0.000(3) 0.007(4) C77 0.025(3) 0.073(5) 0.044(4) -0.009(4) -0.001(3) 0.001(3) C78 0.032(4) 0.061(5) 0.039(4) 0.004(3) 0.002(3) 0.002(3) C79 0.060(6) 0.069(6) 0.096(7) 0.021(5) 0.005(5) -0.008(5) Cl1 0.099(2) 0.124(2) 0.0785(18) 0.0216(17) 0.0136(15) 0.0373(18) Cl2 0.0838(19) 0.103(2) 0.156(3) 0.065(2) 0.0100(18) 0.0091(16) C80 0.097(10) 0.180(15) 0.115(11) -0.006(10) 0.005(8) -0.027(10) Cl3 0.153(4) 0.221(5) 0.096(3) 0.002(3) -0.020(2) -0.045(3) Cl4 0.174(4) 0.200(5) 0.133(4) -0.006(3) 0.020(3) -0.049(4) Cl5 0.285(6) 0.231(5) 0.206(5) 0.154(4) 0.168(5) 0.180(5) C82 0.158(14) 0.165(14) 0.116(11) -0.004(10) -0.050(10) 0.063(11) Cl7 0.126(3) 0.184(4) 0.0680(18) 0.003(2) -0.0061(18) -0.041(3) Cl8 0.085(3) 0.136(4) 0.078(3) 0.049(3) 0.010(2) 0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N15 1.958(5) . ? Co1 N8 1.961(5) . ? Co1 N1 1.967(5) . ? Co1 N22 1.971(5) . ? Co1 N29 2.106(5) . ? Co1 Co2 2.2830(10) . ? Co2 N16 1.911(4) . ? Co2 N2 1.912(5) . ? Co2 N9 1.919(5) . ? Co2 N23 1.922(5) . ? Co2 Co3 2.2582(10) . ? Co3 N17 1.929(4) . ? Co3 N10 1.932(4) . ? Co3 N3 1.937(4) . ? Co3 N24 1.944(5) . ? Co3 Co4 2.2582(10) . ? Co4 N18 1.911(5) . ? Co4 N4 1.912(4) . ? Co4 N25 1.915(5) . ? Co4 N11 1.929(4) . ? Co4 Co5 2.2803(10) . ? Co5 N26 1.964(5) . ? Co5 N12 1.966(5) . ? Co5 N5 1.975(4) . ? Co5 N19 1.976(5) . ? Co5 N30 2.093(5) . ? S1 C53 1.651(8) . ? S2 C54 1.649(7) . ? N1 C1 1.344(7) . ? N1 C4 1.364(7) . ? N2 C4 1.359(7) . ? N2 C5 1.384(7) . ? N3 C5 1.366(7) . ? N3 C9 1.371(7) . ? N4 C10 1.356(7) . ? N4 C9 1.390(7) . ? N5 C13 1.346(7) . ? N5 C10 1.373(7) . ? N6 C2 1.327(9) . ? N6 C3 1.327(8) . ? N7 C11 1.312(7) . ? N7 C12 1.358(8) . ? N8 C14 1.365(7) . ? N8 C17 1.366(7) . ? N9 C17 1.364(7) . ? N9 C18 1.389(7) . ? N10 C18 1.354(7) . ? N10 C22 1.373(7) . ? N11 C23 1.351(7) . ? N11 C22 1.376(7) . ? N12 C26 1.345(7) . ? N12 C23 1.374(7) . ? N13 C16 1.302(8) . ? N13 C15 1.362(8) . ? N14 C24 1.314(8) . ? N14 C25 1.349(8) . ? N15 C30 1.359(7) . ? N15 C27 1.372(7) . ? N16 C30 1.374(7) . ? N16 C31 1.375(7) . ? N17 C35 1.366(7) . ? N17 C31 1.374(7) . ? N18 C36 1.365(7) . ? N18 C35 1.391(7) . ? N19 C39 1.357(7) . ? N19 C36 1.360(7) . ? N20 C29 1.315(8) . ? N20 C28 1.352(8) . ? N21 C37 1.311(8) . ? N21 C38 1.354(8) . ? N22 C43 1.355(7) . ? N22 C40 1.361(7) . ? N23 C43 1.347(7) . ? N23 C44 1.371(7) . ? N24 C48 1.355(7) . ? N24 C44 1.367(7) . ? N25 C49 1.353(7) . ? N25 C48 1.391(7) . ? N26 C52 1.345(7) . ? N26 C49 1.368(7) . ? N27 C42 1.314(8) . ? N27 C41 1.346(9) . ? N28 C50 1.328(8) . ? N28 C51 1.345(8) . ? N29 C53 1.085(8) . ? N30 C54 1.125(7) . ? C1 C2 1.365(10) . ? C3 C4 1.417(9) . ? C5 C6 1.379(8) . ? C6 C7 1.395(8) . ? C7 C8 1.383(8) . ? C8 C9 1.386(8) . ? C10 C11 1.407(8) . ? C12 C13 1.360(8) . ? C14 C15 1.356(9) . ? C16 C17 1.418(8) . ? C18 C19 1.396(8) . ? C19 C20 1.379(8) . ? C20 C21 1.382(8) . ? C21 C22 1.390(8) . ? C23 C24 1.418(8) . ? C25 C26 1.368(8) . ? C27 C28 1.356(9) . ? C29 C30 1.416(8) . ? C31 C32 1.378(8) . ? C32 C33 1.391(8) . ? C33 C34 1.404(8) . ? C34 C35 1.386(8) . ? C36 C37 1.419(8) . ? C38 C39 1.353(9) . ? C40 C41 1.355(9) . ? C42 C43 1.428(8) . ? C44 C45 1.403(8) . ? C45 C46 1.371(9) . ? C46 C47 1.386(8) . ? C47 C48 1.390(8) . ? C49 C50 1.414(8) . ? C51 C52 1.365(9) . ? P1 C67 1.789(7) . ? P1 C73 1.790(6) . ? P1 C55 1.792(6) . ? P1 C61 1.796(6) . ? C55 C60 1.395(9) . ? C55 C56 1.400(9) . ? C56 C57 1.393(9) . ? C57 C58 1.343(11) . ? C58 C59 1.373(11) . ? C59 C60 1.384(10) . ? C61 C66 1.381(9) . ? C61 C62 1.393(9) . ? C62 C63 1.380(9) . ? C63 C64 1.379(10) . ? C64 C65 1.360(10) . ? C65 C66 1.402(9) . ? C67 C72 1.390(9) . ? C67 C68 1.392(9) . ? C68 C69 1.392(10) . ? C69 C70 1.386(11) . ? C70 C71 1.373(10) . ? C71 C72 1.393(10) . ? C73 C78 1.384(10) . ? C73 C74 1.404(9) . ? C74 C75 1.362(9) . ? C75 C76 1.381(11) . ? C76 C77 1.368(11) . ? C77 C78 1.400(9) . ? C79 Cl2 1.742(9) . ? C79 Cl1 1.749(10) . ? C80 Cl3 1.678(14) . ? C80 Cl4 1.775(8) . ? C81 Cl6 1.676(13) . ? C81 Cl5 1.739(13) . ? Cl6 Cl8' 2.147(10) 1_445 ? C82 Cl8' 1.619(8) . ? C82 Cl8 1.645(8) . ? C82 Cl7 1.664(13) . ? Cl8' Cl6 2.147(10) 1_665 ? 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 N15 Co1 N8 91.2(2) . . ? N15 Co1 N1 88.2(2) . . ? N8 Co1 N1 171.22(19) . . ? N15 Co1 N22 170.59(19) . . ? N8 Co1 N22 88.8(2) . . ? N1 Co1 N22 90.4(2) . . ? N15 Co1 N29 95.04(19) . . ? N8 Co1 N29 94.38(19) . . ? N1 Co1 N29 94.40(19) . . ? N22 Co1 N29 94.35(19) . . ? N15 Co1 Co2 85.71(14) . . ? N8 Co1 Co2 85.33(13) . . ? N1 Co1 Co2 85.89(14) . . ? N22 Co1 Co2 84.90(14) . . ? N29 Co1 Co2 179.20(14) . . ? N16 Co2 N2 89.3(2) . . ? N16 Co2 N9 90.9(2) . . ? N2 Co2 N9 177.39(19) . . ? N16 Co2 N23 177.35(19) . . ? N2 Co2 N23 90.0(2) . . ? N9 Co2 N23 89.7(2) . . ? N16 Co2 Co3 88.52(13) . . ? N2 Co2 Co3 88.82(14) . . ? N9 Co2 Co3 88.59(13) . . ? N23 Co2 Co3 88.92(14) . . ? N16 Co2 Co1 90.91(13) . . ? N2 Co2 Co1 91.16(14) . . ? N9 Co2 Co1 91.44(13) . . ? N23 Co2 Co1 91.66(14) . . ? Co3 Co2 Co1 179.42(5) . . ? N17 Co3 N10 91.03(19) . . ? N17 Co3 N3 89.56(19) . . ? N10 Co3 N3 179.38(19) . . ? N17 Co3 N24 179.05(19) . . ? N10 Co3 N24 89.92(19) . . ? N3 Co3 N24 89.50(19) . . ? N17 Co3 Co2 90.25(13) . . ? N10 Co3 Co2 89.94(13) . . ? N3 Co3 Co2 89.83(13) . . ? N24 Co3 Co2 89.84(14) . . ? N17 Co3 Co4 89.69(13) . . ? N10 Co3 Co4 90.13(13) . . ? N3 Co3 Co4 90.10(13) . . ? N24 Co3 Co4 90.22(14) . . ? Co2 Co3 Co4 179.91(5) . . ? N18 Co4 N4 90.0(2) . . ? N18 Co4 N25 177.0(2) . . ? N4 Co4 N25 88.6(2) . . ? N18 Co4 N11 90.8(2) . . ? N4 Co4 N11 177.63(19) . . ? N25 Co4 N11 90.5(2) . . ? N18 Co4 Co3 88.92(14) . . ? N4 Co4 Co3 88.83(13) . . ? N25 Co4 Co3 88.39(14) . . ? N11 Co4 Co3 88.93(14) . . ? N18 Co4 Co5 91.19(14) . . ? N4 Co4 Co5 90.97(13) . . ? N25 Co4 Co5 91.50(14) . . ? N11 Co4 Co5 91.26(14) . . ? Co3 Co4 Co5 179.78(5) . . ? N26 Co5 N12 87.00(19) . . ? N26 Co5 N5 89.64(19) . . ? N12 Co5 N5 169.90(19) . . ? N26 Co5 N19 171.21(19) . . ? N12 Co5 N19 92.7(2) . . ? N5 Co5 N19 89.17(19) . . ? N26 Co5 N30 94.97(19) . . ? N12 Co5 N30 95.56(19) . . ? N5 Co5 N30 94.22(18) . . ? N19 Co5 N30 93.80(19) . . ? N26 Co5 Co4 85.68(14) . . ? N12 Co5 Co4 84.62(14) . . ? N5 Co5 Co4 85.63(13) . . ? N19 Co5 Co4 85.54(14) . . ? N30 Co5 Co4 179.33(15) . . ? C1 N1 C4 116.9(5) . . ? C1 N1 Co1 122.2(4) . . ? C4 N1 Co1 120.9(4) . . ? C4 N2 C5 123.5(5) . . ? C4 N2 Co2 115.9(4) . . ? C5 N2 Co2 120.4(4) . . ? C5 N3 C9 119.6(5) . . ? C5 N3 Co3 120.2(4) . . ? C9 N3 Co3 120.2(4) . . ? C10 N4 C9 122.7(5) . . ? C10 N4 Co4 116.8(4) . . ? C9 N4 Co4 120.3(3) . . ? C13 N5 C10 116.7(5) . . ? C13 N5 Co5 122.6(4) . . ? C10 N5 Co5 120.6(4) . . ? C2 N6 C3 116.6(6) . . ? C11 N7 C12 115.6(5) . . ? C14 N8 C17 116.9(5) . . ? C14 N8 Co1 121.0(4) . . ? C17 N8 Co1 122.1(4) . . ? C17 N9 C18 124.1(5) . . ? C17 N9 Co2 116.5(4) . . ? C18 N9 Co2 119.3(4) . . ? C18 N10 C22 119.9(5) . . ? C18 N10 Co3 120.4(4) . . ? C22 N10 Co3 119.7(4) . . ? C23 N11 C22 124.9(5) . . ? C23 N11 Co4 114.2(4) . . ? C22 N11 Co4 119.9(4) . . ? C26 N12 C23 118.2(5) . . ? C26 N12 Co5 119.5(4) . . ? C23 N12 Co5 121.4(4) . . ? C16 N13 C15 115.8(5) . . ? C24 N14 C25 117.4(5) . . ? C30 N15 C27 116.6(5) . . ? C30 N15 Co1 121.7(4) . . ? C27 N15 Co1 121.3(4) . . ? C30 N16 C31 123.2(5) . . ? C30 N16 Co2 115.3(4) . . ? C31 N16 Co2 120.8(4) . . ? C35 N17 C31 119.6(5) . . ? C35 N17 Co3 120.9(4) . . ? C31 N17 Co3 119.4(4) . . ? C36 N18 C35 123.5(5) . . ? C36 N18 Co4 116.9(4) . . ? C35 N18 Co4 119.6(4) . . ? C39 N19 C36 116.4(5) . . ? C39 N19 Co5 122.7(4) . . ? C36 N19 Co5 120.9(4) . . ? C29 N20 C28 115.5(5) . . ? C37 N21 C38 115.6(6) . . ? C43 N22 C40 117.9(5) . . ? C43 N22 Co1 121.2(4) . . ? C40 N22 Co1 120.7(4) . . ? C43 N23 C44 125.4(5) . . ? C43 N23 Co2 115.1(4) . . ? C44 N23 Co2 119.4(3) . . ? C48 N24 C44 121.2(5) . . ? C48 N24 Co3 119.5(4) . . ? C44 N24 Co3 119.2(4) . . ? C49 N25 C48 123.9(5) . . ? C49 N25 Co4 115.3(4) . . ? C48 N25 Co4 120.5(4) . . ? C52 N26 C49 117.4(5) . . ? C52 N26 Co5 121.5(4) . . ? C49 N26 Co5 121.0(4) . . ? C42 N27 C41 116.6(6) . . ? C50 N28 C51 115.9(6) . . ? C53 N29 Co1 174.2(5) . . ? C54 N30 Co5 173.1(5) . . ? N1 C1 C2 122.0(6) . . ? N6 C2 C1 122.7(6) . . ? N6 C3 C4 122.6(6) . . ? N2 C4 N1 116.0(5) . . ? N2 C4 C3 124.8(5) . . ? N1 C4 C3 119.0(5) . . ? N3 C5 C6 120.9(5) . . ? N3 C5 N2 113.8(5) . . ? C6 C5 N2 125.1(5) . . ? C5 C6 C7 119.0(5) . . ? C8 C7 C6 120.5(5) . . ? C7 C8 C9 118.4(5) . . ? N3 C9 C8 121.3(5) . . ? N3 C9 N4 113.6(5) . . ? C8 C9 N4 125.0(5) . . ? N4 C10 N5 115.4(5) . . ? N4 C10 C11 125.6(5) . . ? N5 C10 C11 118.5(5) . . ? N7 C11 C10 124.4(6) . . ? N7 C12 C13 122.3(5) . . ? N5 C13 C12 122.4(6) . . ? C15 C14 N8 121.8(6) . . ? C14 C15 N13 122.6(6) . . ? N13 C16 C17 124.5(6) . . ? N9 C17 N8 115.0(5) . . ? N9 C17 C16 126.3(5) . . ? N8 C17 C16 118.4(5) . . ? N10 C18 N9 114.2(5) . . ? N10 C18 C19 121.1(5) . . ? N9 C18 C19 124.5(5) . . ? C20 C19 C18 118.6(5) . . ? C19 C20 C21 120.8(5) . . ? C20 C21 C22 118.9(5) . . ? N10 C22 N11 114.8(5) . . ? N10 C22 C21 120.5(5) . . ? N11 C22 C21 124.6(5) . . ? N11 C23 N12 115.7(5) . . ? N11 C23 C24 126.0(5) . . ? N12 C23 C24 117.6(5) . . ? N14 C24 C23 123.4(6) . . ? N14 C25 C26 121.5(6) . . ? N12 C26 C25 121.7(6) . . ? C28 C27 N15 121.3(6) . . ? N20 C28 C27 123.4(6) . . ? N20 C29 C30 123.9(6) . . ? N15 C30 N16 115.0(5) . . ? N15 C30 C29 119.3(5) . . ? N16 C30 C29 125.2(5) . . ? N17 C31 N16 114.3(5) . . ? N17 C31 C32 120.5(5) . . ? N16 C31 C32 125.2(5) . . ? C31 C32 C33 120.0(5) . . ? C32 C33 C34 119.6(5) . . ? C35 C34 C33 118.3(5) . . ? N17 C35 C34 121.7(5) . . ? N17 C35 N18 113.3(5) . . ? C34 C35 N18 124.7(5) . . ? N19 C36 N18 115.6(5) . . ? N19 C36 C37 118.5(5) . . ? N18 C36 C37 125.6(5) . . ? N21 C37 C36 124.4(6) . . ? C39 C38 N21 122.2(6) . . ? C38 C39 N19 122.9(6) . . ? C41 C40 N22 121.9(6) . . ? N27 C41 C40 122.2(6) . . ? N27 C42 C43 123.8(6) . . ? N23 C43 N22 116.9(5) . . ? N23 C43 C42 125.1(5) . . ? N22 C43 C42 117.6(5) . . ? N24 C44 N23 115.3(5) . . ? N24 C44 C45 119.3(5) . . ? N23 C44 C45 125.2(5) . . ? C46 C45 C44 119.0(5) . . ? C45 C46 C47 121.4(6) . . ? C46 C47 C48 118.3(6) . . ? N24 C48 C47 120.7(5) . . ? N24 C48 N25 114.4(5) . . ? C47 C48 N25 124.8(5) . . ? N25 C49 N26 116.2(5) . . ? N25 C49 C50 125.5(5) . . ? N26 C49 C50 118.1(5) . . ? N28 C50 C49 123.9(6) . . ? N28 C51 C52 122.3(6) . . ? N26 C52 C51 122.2(6) . . ? N29 C53 S1 178.8(7) . . ? N30 C54 S2 178.9(6) . . ? C67 P1 C73 110.9(3) . . ? C67 P1 C55 109.4(3) . . ? C73 P1 C55 110.6(3) . . ? C67 P1 C61 107.9(3) . . ? C73 P1 C61 109.7(3) . . ? C55 P1 C61 108.3(3) . . ? C60 C55 C56 119.9(6) . . ? C60 C55 P1 119.8(5) . . ? C56 C55 P1 120.2(5) . . ? C57 C56 C55 119.1(7) . . ? C58 C57 C56 120.7(7) . . ? C57 C58 C59 120.7(7) . . ? C58 C59 C60 121.1(7) . . ? C59 C60 C55 118.6(7) . . ? C66 C61 C62 120.3(6) . . ? C66 C61 P1 120.3(5) . . ? C62 C61 P1 119.1(5) . . ? C63 C62 C61 120.1(6) . . ? C64 C63 C62 119.3(7) . . ? C65 C64 C63 121.2(7) . . ? C64 C65 C66 120.3(6) . . ? C61 C66 C65 118.8(6) . . ? C72 C67 C68 120.0(6) . . ? C72 C67 P1 120.2(5) . . ? C68 C67 P1 119.8(5) . . ? C67 C68 C69 119.8(7) . . ? C70 C69 C68 120.0(7) . . ? C71 C70 C69 120.1(7) . . ? C70 C71 C72 120.7(7) . . ? C67 C72 C71 119.4(6) . . ? C78 C73 C74 119.5(6) . . ? C78 C73 P1 119.7(5) . . ? C74 C73 P1 120.7(5) . . ? C75 C74 C73 119.7(7) . . ? C74 C75 C76 120.8(8) . . ? C77 C76 C75 120.5(7) . . ? C76 C77 C78 119.5(7) . . ? C73 C78 C77 119.9(7) . . ? Cl2 C79 Cl1 113.1(6) . . ? Cl3 C80 Cl4 110.8(8) . . ? Cl6 C81 Cl5 117.7(8) . . ? C81 Cl6 Cl8' 163.9(6) . 1_445 ? Cl8' C82 Cl8 65.3(5) . . ? Cl8' C82 Cl7 139.1(11) . . ? Cl8 C82 Cl7 112.6(8) . . ? C82 Cl8' Cl6 167.4(7) . 1_665 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.710 _refine_diff_density_min -1.815 _refine_diff_density_rms 0.129