# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jason Love' _publ_contact_author_email JASON.LOVE@ED.AC.UK _publ_section_title ; Tailoring dicobalt Pacman complexes of Schiff-base calixpyrroles towards dioxygen reduction catalysis ; _publ_requested_category FM loop_ _publ_author_name 'Jason Love' 'Elham Askarizadeh' 'Davar M. Boghaei' 'Alexandra M Z Slawin' 'Sahar Bani Yaghoob' # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'Co2_O2__L_.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-11-19 at 12:43:01 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : jl8017a a jl8017 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_jl8017a _database_code_depnum_ccdc_archive 'CCDC 749304' #TrackingRef 'Co2_O2__L_.cif' _audit_creation_date 2008-11-19T12:43:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H54 Co2 N10 O2, C19 H22 N O' _chemical_formula_sum 'C91 H76 Co2 N11 O3' _chemical_formula_weight 1489.49 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 14.4714(4) _cell_length_b 14.8327(4) _cell_length_c 18.8570(6) _cell_angle_alpha 78.571(2) _cell_angle_beta 75.865(2) _cell_angle_gamma 71.751(2) _cell_volume 3695.01(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 56.4 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.51 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.8445 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_unetI/netI 0.0951 _diffrn_reflns_number 43676 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 15079 _reflns_number_gt 12326 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; One molecule of PhMe was disordered was modelled isotripically over two sites with 55:45 occupancy Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+11.2333P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15079 _refine_ls_number_parameters 1010 _refine_ls_number_restraints 242 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.2066 _refine_ls_wR_factor_gt 0.1969 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.219 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.548 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.46091(5) 0.12407(5) 0.72596(4) 0.02105(17) Uani 1 1 d . . . Co2 Co 0.54988(5) 0.32959(4) 0.79168(3) 0.01675(16) Uani 1 1 d . . . O1 O 0.4112(2) 0.2443(2) 0.76327(19) 0.0272(8) Uani 1 1 d . . . O2 O 0.4620(2) 0.3131(2) 0.73516(18) 0.0206(7) Uani 1 1 d . . . O1S O 0.2230(3) 0.3750(4) 0.7908(3) 0.0536(12) Uani 1 1 d . . . N1 N 0.4812(3) 0.0656(3) 0.8290(2) 0.0229(9) Uani 1 1 d . . . N2 N 0.3348(3) 0.1057(3) 0.7646(2) 0.0235(9) Uani 1 1 d . . . N3 N 0.4142(3) 0.1836(3) 0.6396(2) 0.0237(9) Uani 1 1 d . . . N4 N 0.5842(3) 0.1518(3) 0.6688(2) 0.0204(9) Uani 1 1 d . . . N5 N 0.6602(3) 0.2816(3) 0.7113(2) 0.0178(8) Uani 1 1 d . . . N6 N 0.5442(3) 0.4470(3) 0.7304(2) 0.0172(8) Uani 1 1 d . . . N7 N 0.4382(3) 0.3947(3) 0.8545(2) 0.0182(8) Uani 1 1 d . . . N8 N 0.5342(3) 0.2174(3) 0.8661(2) 0.0206(9) Uani 1 1 d . . . N9 N 0.5132(3) -0.0062(3) 0.6862(2) 0.0264(10) Uani 1 1 d . . . N10 N 0.6470(3) 0.3524(3) 0.8454(2) 0.0201(9) Uani 1 1 d . . . C1 C 0.4005(4) 0.0473(3) 0.8704(3) 0.0219(10) Uani 1 1 d . . . H1 H 0.3979 0.0218 0.921 0.026 Uiso 1 1 calc R . . C2 C 0.3188(4) 0.0665(3) 0.8377(3) 0.0209(10) Uani 1 1 d . . . C3 C 0.2234(4) 0.0541(4) 0.8557(3) 0.0275(12) Uani 1 1 d . . . H3 H 0.1929 0.0272 0.9021 0.033 Uiso 1 1 calc R . . C4 C 0.1820(4) 0.0878(4) 0.7939(3) 0.0294(12) Uani 1 1 d . . . H4 H 0.1171 0.0899 0.7899 0.035 Uiso 1 1 calc R . . C5 C 0.2539(4) 0.1185(3) 0.7375(3) 0.0238(11) Uani 1 1 d . . . C6 C 0.2462(4) 0.1572(4) 0.6575(3) 0.0262(11) Uani 1 1 d . . . C7 C 0.2428(4) 0.0796(4) 0.6158(3) 0.0302(12) Uani 1 1 d . . . C8 C 0.3100(5) -0.0101(4) 0.6078(3) 0.0369(14) Uani 1 1 d . . . H8 H 0.3657 -0.0321 0.6313 0.044 Uiso 1 1 calc R . . C9 C 0.2926(5) -0.0672(5) 0.5638(4) 0.0474(17) Uani 1 1 d . . . H9 H 0.3375 -0.1288 0.5578 0.057 Uiso 1 1 calc R . . C10 C 0.2135(6) -0.0371(5) 0.5294(4) 0.0551(19) Uani 1 1 d . . . H10 H 0.2052 -0.0767 0.4989 0.066 Uiso 1 1 calc R . . C11 C 0.1450(6) 0.0516(6) 0.5391(4) 0.0554(19) Uani 1 1 d . . . H11 H 0.0889 0.0727 0.5161 0.066 Uiso 1 1 calc R . . C12 C 0.1602(5) 0.1097(5) 0.5834(3) 0.0402(14) Uani 1 1 d . . . C13 C 0.0990(4) 0.2022(5) 0.6063(3) 0.0386(14) Uani 1 1 d . . . C14 C 0.0050(5) 0.2588(6) 0.5934(4) 0.0529(18) Uani 1 1 d . . . H14 H -0.0285 0.2404 0.5635 0.064 Uiso 1 1 calc R . . C15 C -0.0369(5) 0.3421(5) 0.6257(4) 0.0523(18) Uani 1 1 d . . . H15 H -0.0999 0.3818 0.6172 0.063 Uiso 1 1 calc R . . C16 C 0.0106(5) 0.3691(5) 0.6698(4) 0.0476(17) Uani 1 1 d . . . H16 H -0.0202 0.4268 0.6912 0.057 Uiso 1 1 calc R . . C17 C 0.1024(4) 0.3131(4) 0.6833(3) 0.0359(13) Uani 1 1 d . . . H17 H 0.1354 0.3312 0.7137 0.043 Uiso 1 1 calc R . . C18 C 0.1447(4) 0.2298(4) 0.6510(3) 0.0267(11) Uani 1 1 d . . . C19 C 0.3311(4) 0.1987(4) 0.6153(3) 0.0231(11) Uani 1 1 d . . . C20 C 0.3394(4) 0.2505(3) 0.5450(3) 0.0238(11) Uani 1 1 d . . . H20 H 0.2902 0.272 0.5154 0.029 Uiso 1 1 calc R . . C21 C 0.4334(4) 0.2648(4) 0.5263(3) 0.0252(11) Uani 1 1 d . . . H21 H 0.4614 0.2961 0.481 0.03 Uiso 1 1 calc R . . C22 C 0.4784(4) 0.2243(3) 0.5868(3) 0.0192(10) Uani 1 1 d . . . C23 C 0.5717(4) 0.2031(3) 0.6058(3) 0.0223(11) Uani 1 1 d . . . H23 H 0.6238 0.2256 0.5736 0.027 Uiso 1 1 calc R . . C24 C 0.6804(3) 0.1219(3) 0.6866(3) 0.0215(10) Uani 1 1 d . . . C25 C 0.7379(4) 0.0269(4) 0.6858(3) 0.0342(13) Uani 1 1 d . . . H25 H 0.7108 -0.0183 0.675 0.041 Uiso 1 1 calc R . . C26 C 0.8325(4) -0.0037(4) 0.7000(3) 0.0345(13) Uani 1 1 d . . . C27 C 0.8923(5) -0.1071(4) 0.6967(5) 0.067(2) Uani 1 1 d . . . H27A H 0.8516 -0.1432 0.6866 0.101 Uiso 1 1 calc R . . H27B H 0.9128 -0.1348 0.744 0.101 Uiso 1 1 calc R . . H27C H 0.9512 -0.1105 0.6572 0.101 Uiso 1 1 calc R . . C28 C 0.9764(4) 0.0334(5) 0.7305(4) 0.0490(17) Uani 1 1 d . . . H28A H 0.9893 0.0886 0.7435 0.074 Uiso 1 1 calc R . . H28B H 1.0238 0.0126 0.686 0.074 Uiso 1 1 calc R . . H28C H 0.9837 -0.0191 0.7713 0.074 Uiso 1 1 calc R . . C29 C 0.8723(4) 0.0615(4) 0.7164(3) 0.0313(12) Uani 1 1 d . . . C30 C 0.8149(4) 0.1555(4) 0.7194(3) 0.0279(12) Uani 1 1 d . . . H30 H 0.8415 0.2003 0.7312 0.033 Uiso 1 1 calc R . . C31 C 0.7195(3) 0.1855(3) 0.7054(3) 0.0206(10) Uani 1 1 d . . . C32 C 0.6715(3) 0.3494(3) 0.6566(3) 0.0208(10) Uani 1 1 d . . . H32 H 0.7196 0.336 0.6129 0.025 Uiso 1 1 calc R . . C33 C 0.6098(3) 0.4430(3) 0.6649(3) 0.0193(10) Uani 1 1 d . . . C34 C 0.5932(4) 0.5339(3) 0.6244(3) 0.0253(11) Uani 1 1 d . . . H34 H 0.6281 0.5518 0.5767 0.03 Uiso 1 1 calc R . . C35 C 0.5155(4) 0.5929(3) 0.6678(3) 0.0247(11) Uani 1 1 d . . . H35 H 0.4873 0.6595 0.6552 0.03 Uiso 1 1 calc R . . C36 C 0.4858(3) 0.5367(3) 0.7338(3) 0.0195(10) Uani 1 1 d . . . C37 C 0.4063(4) 0.5670(3) 0.7999(3) 0.0208(10) Uani 1 1 d . . . C38 C 0.3157(4) 0.6404(3) 0.7736(3) 0.0227(11) Uani 1 1 d . . . C39 C 0.2534(4) 0.6270(4) 0.7349(3) 0.0295(12) Uani 1 1 d . . . H39 H 0.2587 0.5648 0.7257 0.035 Uiso 1 1 calc R . . C40 C 0.1823(4) 0.7063(4) 0.7094(3) 0.0365(14) Uani 1 1 d . . . H40 H 0.1388 0.6982 0.6822 0.044 Uiso 1 1 calc R . . C41 C 0.1745(4) 0.7966(4) 0.7231(3) 0.0402(15) Uani 1 1 d . . . H41 H 0.1275 0.8502 0.7033 0.048 Uiso 1 1 calc R . . C42 C 0.2329(4) 0.8106(4) 0.7646(3) 0.0349(14) Uani 1 1 d . . . H42 H 0.2254 0.8729 0.7751 0.042 Uiso 1 1 calc R . . C43 C 0.3046(4) 0.7307(3) 0.7916(3) 0.0242(11) Uani 1 1 d . . . C44 C 0.3769(4) 0.7230(3) 0.8358(3) 0.0254(11) Uani 1 1 d . . . C45 C 0.3905(4) 0.7899(4) 0.8709(3) 0.0328(13) Uani 1 1 d . . . H45 H 0.3475 0.8533 0.8693 0.039 Uiso 1 1 calc R . . C46 C 0.4679(5) 0.7628(4) 0.9085(3) 0.0350(14) Uani 1 1 d . . . H46 H 0.4779 0.808 0.9331 0.042 Uiso 1 1 calc R . . C47 C 0.5312(4) 0.6706(4) 0.9107(3) 0.0356(13) Uani 1 1 d . . . H47 H 0.5849 0.6538 0.9358 0.043 Uiso 1 1 calc R . . C48 C 0.5168(4) 0.6030(4) 0.8767(3) 0.0288(12) Uani 1 1 d . . . H48 H 0.5601 0.5398 0.8782 0.035 Uiso 1 1 calc R . . C49 C 0.4388(4) 0.6287(3) 0.8407(3) 0.0215(10) Uani 1 1 d . . . C50 C 0.3779(3) 0.4841(3) 0.8528(3) 0.0205(10) Uani 1 1 d . . . C51 C 0.2927(4) 0.4853(4) 0.9085(3) 0.0231(11) Uani 1 1 d . . . H51 H 0.2384 0.5396 0.9198 0.028 Uiso 1 1 calc R . . C52 C 0.3033(4) 0.3919(4) 0.9439(3) 0.0250(11) Uani 1 1 d . . . H52 H 0.2577 0.3705 0.9841 0.03 Uiso 1 1 calc R . . C53 C 0.3929(3) 0.3361(3) 0.9092(3) 0.0200(10) Uani 1 1 d . . . C54 C 0.4509(4) 0.2385(3) 0.9132(3) 0.0213(10) Uani 1 1 d . . . H54 H 0.4294 0.1906 0.9489 0.026 Uiso 1 1 calc R . . C55 C 0.5956(3) 0.1208(3) 0.8734(3) 0.0216(10) Uani 1 1 d . . . C56 C 0.6859(4) 0.1008(4) 0.8955(3) 0.0283(12) Uani 1 1 d . . . H56 H 0.7078 0.1523 0.9018 0.034 Uiso 1 1 calc R . . C57 C 0.7447(4) 0.0076(4) 0.9086(3) 0.0312(12) Uani 1 1 d . . . C58 C 0.8436(5) -0.0112(5) 0.9289(4) 0.0467(16) Uani 1 1 d . . . H58A H 0.8964 -0.0366 0.8884 0.07 Uiso 1 1 calc R . . H58B H 0.8479 -0.0579 0.9735 0.07 Uiso 1 1 calc R . . H58C H 0.851 0.0487 0.9381 0.07 Uiso 1 1 calc R . . C59 C 0.7723(5) -0.1711(4) 0.9140(4) 0.0552(19) Uani 1 1 d . . . H59A H 0.7403 -0.2132 0.901 0.083 Uiso 1 1 calc R . . H59B H 0.7752 -0.1866 0.9666 0.083 Uiso 1 1 calc R . . H59C H 0.8397 -0.1804 0.8846 0.083 Uiso 1 1 calc R . . C60 C 0.7130(4) -0.0677(4) 0.8984(3) 0.0343(13) Uani 1 1 d . . . C61 C 0.6258(4) -0.0470(4) 0.8730(3) 0.0347(13) Uani 1 1 d . . . H61 H 0.6056 -0.0985 0.8646 0.042 Uiso 1 1 calc R . . C62 C 0.5663(4) 0.0462(3) 0.8591(3) 0.0246(11) Uani 1 1 d . . . C63 C 0.5135(4) -0.0888(4) 0.7309(3) 0.0298(12) Uani 1 1 d . . . H63 H 0.4842 -0.0858 0.7817 0.036 Uiso 1 1 calc R . . C64 C 0.5541(4) -0.1780(4) 0.7072(3) 0.0361(14) Uani 1 1 d . . . H64 H 0.5539 -0.2347 0.7409 0.043 Uiso 1 1 calc R . . C65 C 0.5944(4) -0.1825(4) 0.6337(3) 0.0361(14) Uani 1 1 d . . . H65 H 0.6226 -0.2427 0.6158 0.043 Uiso 1 1 calc R . . C66 C 0.5938(5) -0.0984(4) 0.5861(3) 0.0357(14) Uani 1 1 d . . . H66 H 0.6218 -0.0998 0.5351 0.043 Uiso 1 1 calc R . . C67 C 0.5517(4) -0.0128(4) 0.6144(3) 0.0309(12) Uani 1 1 d . . . H67 H 0.5497 0.0448 0.5813 0.037 Uiso 1 1 calc R . . C68 C 0.7338(4) 0.3696(4) 0.8110(3) 0.0237(11) Uani 1 1 d . . . H68 H 0.7507 0.373 0.7588 0.028 Uiso 1 1 calc R . . C69 C 0.7998(4) 0.3829(4) 0.8471(3) 0.0346(13) Uani 1 1 d . . . H69 H 0.8607 0.394 0.8201 0.042 Uiso 1 1 calc R . . C70 C 0.7768(4) 0.3798(4) 0.9225(3) 0.0327(13) Uani 1 1 d . . . H70 H 0.821 0.3887 0.9487 0.039 Uiso 1 1 calc R . . C71 C 0.6875(4) 0.3634(4) 0.9591(3) 0.0296(12) Uani 1 1 d . . . H71 H 0.6685 0.3617 1.0111 0.036 Uiso 1 1 calc R . . C72 C 0.6262(4) 0.3496(3) 0.9193(3) 0.0249(11) Uani 1 1 d . . . H72 H 0.5655 0.3372 0.9455 0.03 Uiso 1 1 calc R . . N1S N 0.2845(5) 0.6348(4) 0.5205(3) 0.0546(15) Uani 1 1 d . . . C1S C 0.2078(6) 0.5943(6) 0.5418(4) 0.060(2) Uani 1 1 d . . . H1S H 0.1466 0.6287 0.527 0.072 Uiso 1 1 calc R . . C2S C 0.2145(6) 0.5071(5) 0.5832(4) 0.0553(19) Uani 1 1 d . . . H2S H 0.1597 0.4808 0.5951 0.066 Uiso 1 1 calc R . . C3S C 0.3011(6) 0.4568(5) 0.6079(4) 0.0498(17) Uani 1 1 d . . . H3S H 0.3067 0.3968 0.6382 0.06 Uiso 1 1 calc R . . C4S C 0.3769(5) 0.4961(5) 0.5873(4) 0.0444(15) Uani 1 1 d . . . H4S H 0.4382 0.4633 0.6024 0.053 Uiso 1 1 calc R . . C5S C 0.3659(5) 0.5838(5) 0.5445(4) 0.0480(17) Uani 1 1 d . . . H5S H 0.4212 0.6095 0.5313 0.058 Uiso 1 1 calc R . . C10S C 0.9022(6) 0.1390(6) 0.0516(5) 0.078(3) Uani 1 1 d . . . H10A H 0.9098 0.1146 0.1027 0.116 Uiso 1 1 calc R . . H10B H 0.934 0.0873 0.0209 0.116 Uiso 1 1 calc R . . H10C H 0.8315 0.163 0.0496 0.116 Uiso 1 1 calc R . . C11S C 0.9492(5) 0.2173(5) 0.0239(4) 0.0512(18) Uani 1 1 d . . . C12S C 0.9399(5) 0.2854(5) 0.0668(4) 0.0503(17) Uani 1 1 d . . . H12S H 0.9021 0.2832 0.1157 0.06 Uiso 1 1 calc R . . C13S C 0.9859(6) 0.3574(6) 0.0385(6) 0.076(3) Uani 1 1 d . . . H13S H 0.9793 0.4058 0.0672 0.091 Uiso 1 1 calc R . . C14S C 1.0429(6) 0.3575(7) -0.0337(7) 0.083(3) Uani 1 1 d . . . H14S H 1.0753 0.4061 -0.0543 0.1 Uiso 1 1 calc R . . C15S C 1.0512(6) 0.2882(7) -0.0735(6) 0.080(3) Uani 1 1 d . . . H15S H 1.0903 0.2883 -0.1219 0.096 Uiso 1 1 calc R . . C16S C 1.0055(6) 0.2191(6) -0.0463(4) 0.064(2) Uani 1 1 d . . . H16S H 1.012 0.1714 -0.0756 0.077 Uiso 1 1 calc R . . C21S C 0.8965(10) 0.6303(10) 0.7334(9) 0.101(6) Uani 0.55 1 d PGDU A 1 C22S C 0.9415(9) 0.6413(12) 0.6594(10) 0.090(6) Uani 0.55 1 d PGU A 1 H22S H 1.0023 0.6581 0.6454 0.107 Uiso 0.55 1 calc PR A 1 C23S C 0.8976(10) 0.6278(11) 0.6060(7) 0.093(7) Uani 0.55 1 d PGU A 1 H23S H 0.9284 0.6353 0.5554 0.112 Uiso 0.55 1 calc PR A 1 C24S C 0.8087(9) 0.6033(8) 0.6265(7) 0.069(4) Uani 0.55 1 d PGU A 1 H24S H 0.7787 0.5941 0.59 0.083 Uiso 0.55 1 calc PR A 1 C25S C 0.7636(7) 0.5923(9) 0.7006(8) 0.082(6) Uani 0.55 1 d PGU A 1 H25S H 0.7029 0.5755 0.7146 0.098 Uiso 0.55 1 calc PR A 1 C26S C 0.8075(10) 0.6057(11) 0.7540(7) 0.088(6) Uani 0.55 1 d PGU A 1 H26S H 0.7768 0.5982 0.8046 0.106 Uiso 0.55 1 calc PR A 1 C20S C 0.9462(19) 0.613(2) 0.7984(13) 0.136(9) Uani 0.55 1 d PDU A 1 H20A H 1.0069 0.5597 0.7919 0.204 Uiso 0.55 1 calc PR A 1 H20B H 0.9011 0.5968 0.8438 0.204 Uiso 0.55 1 calc PR A 1 H20C H 0.963 0.6708 0.8017 0.204 Uiso 0.55 1 calc PR A 1 C31S C 0.8651(13) 0.6257(11) 0.6616(8) 0.087(6) Uani 0.45 1 d PGDU B 2 C32S C 0.7795(10) 0.6203(13) 0.7132(11) 0.100(8) Uani 0.45 1 d PGU B 2 H32S H 0.7223 0.6192 0.6975 0.12 Uiso 0.45 1 calc PR B 2 C33S C 0.7775(11) 0.6164(14) 0.7878(10) 0.108(8) Uani 0.45 1 d PGU B 2 H33S H 0.719 0.6127 0.8231 0.129 Uiso 0.45 1 calc PR B 2 C34S C 0.8612(14) 0.6179(13) 0.8108(8) 0.107(7) Uani 0.45 1 d PGU B 2 H34S H 0.8598 0.6153 0.8618 0.129 Uiso 0.45 1 calc PR B 2 C35S C 0.9468(11) 0.6234(16) 0.7592(10) 0.130(10) Uani 0.45 1 d PGU B 2 H35S H 1.004 0.6245 0.7749 0.155 Uiso 0.45 1 calc PR B 2 C36S C 0.9488(10) 0.6273(15) 0.6846(9) 0.069(6) Uani 0.45 1 d PGU B 2 H36S H 1.0073 0.631 0.6493 0.083 Uiso 0.45 1 calc PR B 2 C30S C 0.869(2) 0.628(2) 0.5818(11) 0.112(10) Uani 0.45 1 d PDU B 2 H30A H 0.8345 0.5834 0.5757 0.168 Uiso 0.45 1 calc PR B 2 H30B H 0.9387 0.608 0.5563 0.168 Uiso 0.45 1 calc PR B 2 H30C H 0.8374 0.6926 0.5607 0.168 Uiso 0.45 1 calc PR B 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 0.0194(3) 0.0167(3) 0.0254(4) 0.0010(3) -0.0054(3) -0.0043(3) Co2 0.0156(3) 0.0106(3) 0.0207(3) -0.0005(2) -0.0022(3) -0.0010(2) O1 0.0200(18) 0.029(2) 0.031(2) 0.0035(16) -0.0023(15) -0.0121(15) O2 0.0188(17) 0.0137(16) 0.0291(19) 0.0003(14) -0.0062(14) -0.0053(13) O1S 0.035(3) 0.067(3) 0.058(3) -0.014(2) -0.008(2) -0.008(2) N1 0.024(2) 0.014(2) 0.030(2) 0.0028(17) -0.0086(18) -0.0045(17) N2 0.024(2) 0.021(2) 0.027(2) -0.0025(17) -0.0042(18) -0.0079(18) N3 0.025(2) 0.019(2) 0.024(2) -0.0002(17) -0.0006(18) -0.0059(18) N4 0.018(2) 0.0142(19) 0.028(2) -0.0055(17) -0.0019(17) -0.0031(16) N5 0.0144(19) 0.0123(19) 0.025(2) -0.0044(16) -0.0021(16) -0.0010(15) N6 0.020(2) 0.0108(18) 0.0172(19) 0.0031(15) -0.0009(16) -0.0042(16) N7 0.020(2) 0.0113(19) 0.019(2) -0.0012(15) -0.0013(16) -0.0010(16) N8 0.023(2) 0.0104(19) 0.027(2) 0.0031(16) -0.0074(18) -0.0037(16) N9 0.026(2) 0.016(2) 0.034(3) -0.0004(18) -0.0046(19) -0.0058(18) N10 0.022(2) 0.016(2) 0.021(2) -0.0015(16) -0.0042(17) -0.0032(16) C1 0.030(3) 0.011(2) 0.024(3) -0.0027(19) -0.005(2) -0.006(2) C2 0.024(3) 0.014(2) 0.021(2) -0.0008(19) -0.002(2) -0.0033(19) C3 0.025(3) 0.024(3) 0.031(3) -0.001(2) 0.001(2) -0.010(2) C4 0.017(3) 0.036(3) 0.033(3) -0.005(2) -0.003(2) -0.006(2) C5 0.026(3) 0.020(2) 0.025(3) -0.003(2) -0.006(2) -0.005(2) C6 0.027(3) 0.026(3) 0.028(3) -0.004(2) -0.006(2) -0.011(2) C7 0.039(3) 0.036(3) 0.022(3) -0.001(2) -0.006(2) -0.022(3) C8 0.045(4) 0.031(3) 0.042(3) -0.005(3) -0.008(3) -0.019(3) C9 0.060(4) 0.044(4) 0.042(4) -0.016(3) 0.003(3) -0.024(3) C10 0.072(5) 0.062(5) 0.050(4) -0.024(4) -0.013(4) -0.034(4) C11 0.059(5) 0.070(5) 0.053(4) -0.010(4) -0.024(4) -0.029(4) C12 0.043(4) 0.048(4) 0.038(3) -0.004(3) -0.010(3) -0.023(3) C13 0.033(3) 0.048(4) 0.037(3) 0.004(3) -0.010(3) -0.017(3) C14 0.040(4) 0.072(5) 0.054(4) 0.001(4) -0.028(3) -0.017(4) C15 0.023(3) 0.061(5) 0.066(5) 0.003(4) -0.014(3) -0.005(3) C16 0.034(3) 0.043(4) 0.054(4) 0.003(3) 0.000(3) -0.007(3) C17 0.032(3) 0.032(3) 0.037(3) 0.002(2) -0.004(3) -0.007(2) C18 0.021(3) 0.031(3) 0.030(3) 0.003(2) -0.008(2) -0.010(2) C19 0.022(3) 0.025(3) 0.025(3) -0.002(2) -0.008(2) -0.009(2) C20 0.028(3) 0.019(2) 0.027(3) -0.001(2) -0.010(2) -0.007(2) C21 0.026(3) 0.021(3) 0.025(3) -0.003(2) -0.002(2) -0.005(2) C22 0.022(2) 0.013(2) 0.023(2) -0.0027(18) -0.001(2) -0.0075(19) C23 0.022(3) 0.016(2) 0.026(3) -0.007(2) 0.004(2) -0.004(2) C24 0.017(2) 0.018(2) 0.027(3) -0.002(2) -0.004(2) -0.0020(19) C25 0.022(3) 0.021(3) 0.060(4) -0.011(3) -0.011(3) -0.001(2) C26 0.025(3) 0.020(3) 0.054(4) -0.003(2) -0.009(3) 0.002(2) C27 0.043(4) 0.018(3) 0.139(8) -0.014(4) -0.034(5) 0.008(3) C28 0.029(3) 0.040(4) 0.076(5) -0.015(3) -0.027(3) 0.011(3) C29 0.022(3) 0.028(3) 0.037(3) -0.002(2) -0.009(2) 0.004(2) C30 0.027(3) 0.024(3) 0.036(3) -0.010(2) -0.011(2) -0.004(2) C31 0.018(2) 0.017(2) 0.022(2) -0.0016(19) -0.001(2) -0.0010(19) C32 0.016(2) 0.022(2) 0.025(3) -0.004(2) -0.004(2) -0.0041(19) C33 0.018(2) 0.016(2) 0.023(2) -0.0048(19) -0.0035(19) -0.0027(19) C34 0.027(3) 0.021(3) 0.020(3) -0.001(2) 0.000(2) -0.001(2) C35 0.030(3) 0.015(2) 0.025(3) 0.0009(19) -0.005(2) -0.003(2) C36 0.020(2) 0.013(2) 0.026(3) -0.0063(19) -0.007(2) -0.0017(19) C37 0.021(3) 0.014(2) 0.022(2) -0.0036(19) -0.003(2) 0.0010(19) C38 0.018(2) 0.017(2) 0.023(3) 0.0021(19) 0.002(2) 0.0020(19) C39 0.024(3) 0.031(3) 0.028(3) -0.006(2) -0.005(2) 0.000(2) C40 0.027(3) 0.043(4) 0.032(3) -0.003(3) -0.008(2) 0.001(3) C41 0.029(3) 0.036(3) 0.043(3) 0.001(3) -0.013(3) 0.011(3) C42 0.035(3) 0.012(2) 0.041(3) -0.001(2) 0.003(3) 0.008(2) C43 0.026(3) 0.014(2) 0.025(3) -0.0037(19) 0.004(2) -0.001(2) C44 0.032(3) 0.016(2) 0.024(3) -0.004(2) 0.004(2) -0.007(2) C45 0.043(3) 0.021(3) 0.033(3) -0.011(2) 0.005(3) -0.011(2) C46 0.059(4) 0.024(3) 0.029(3) -0.011(2) 0.001(3) -0.025(3) C47 0.039(3) 0.042(3) 0.030(3) -0.003(3) -0.007(3) -0.018(3) C48 0.031(3) 0.024(3) 0.032(3) -0.004(2) -0.006(2) -0.009(2) C49 0.027(3) 0.016(2) 0.018(2) -0.0025(19) 0.000(2) -0.003(2) C50 0.017(2) 0.020(2) 0.022(2) -0.0063(19) -0.0045(19) 0.0001(19) C51 0.020(2) 0.023(3) 0.024(3) -0.007(2) -0.004(2) -0.001(2) C52 0.024(3) 0.028(3) 0.020(2) -0.001(2) 0.002(2) -0.009(2) C53 0.015(2) 0.024(3) 0.022(2) 0.001(2) -0.0023(19) -0.0084(19) C54 0.023(3) 0.019(2) 0.023(3) 0.0034(19) -0.009(2) -0.008(2) C55 0.018(2) 0.016(2) 0.022(2) 0.0025(19) -0.0021(19) 0.0029(19) C56 0.032(3) 0.023(3) 0.032(3) -0.003(2) -0.014(2) -0.007(2) C57 0.026(3) 0.024(3) 0.036(3) 0.005(2) -0.011(2) 0.001(2) C58 0.038(4) 0.037(3) 0.063(4) -0.003(3) -0.026(3) 0.004(3) C59 0.051(4) 0.022(3) 0.087(5) -0.003(3) -0.034(4) 0.011(3) C60 0.037(3) 0.024(3) 0.038(3) 0.005(2) -0.015(3) -0.003(2) C61 0.043(3) 0.016(3) 0.045(3) 0.003(2) -0.019(3) -0.005(2) C62 0.025(3) 0.016(2) 0.030(3) 0.001(2) -0.007(2) -0.002(2) C63 0.035(3) 0.019(3) 0.032(3) -0.006(2) 0.001(2) -0.008(2) C64 0.046(4) 0.019(3) 0.038(3) -0.006(2) 0.003(3) -0.009(2) C65 0.038(3) 0.020(3) 0.051(4) -0.009(3) -0.008(3) -0.007(2) C66 0.048(4) 0.027(3) 0.029(3) -0.008(2) 0.005(3) -0.013(3) C67 0.038(3) 0.017(3) 0.037(3) -0.001(2) -0.005(3) -0.010(2) C68 0.025(3) 0.026(3) 0.021(3) -0.005(2) -0.003(2) -0.008(2) C69 0.028(3) 0.044(3) 0.037(3) -0.006(3) -0.005(2) -0.018(3) C70 0.031(3) 0.035(3) 0.035(3) -0.004(2) -0.013(2) -0.009(2) C71 0.036(3) 0.030(3) 0.022(3) -0.003(2) -0.008(2) -0.007(2) C72 0.026(3) 0.021(3) 0.028(3) 0.000(2) -0.005(2) -0.009(2) N1S 0.065(4) 0.061(4) 0.035(3) -0.003(3) -0.003(3) -0.021(3) C1S 0.050(4) 0.078(6) 0.041(4) -0.009(4) -0.007(3) -0.005(4) C2S 0.056(5) 0.061(5) 0.052(4) -0.007(4) 0.001(4) -0.030(4) C3S 0.068(5) 0.042(4) 0.043(4) -0.019(3) -0.003(3) -0.018(4) C4S 0.047(4) 0.044(4) 0.048(4) -0.016(3) -0.006(3) -0.015(3) C5S 0.057(4) 0.058(4) 0.041(4) -0.003(3) -0.012(3) -0.032(4) C10S 0.052(5) 0.082(6) 0.097(7) -0.028(5) -0.011(5) -0.009(4) C11S 0.035(4) 0.047(4) 0.061(5) 0.009(3) -0.015(3) -0.002(3) C12S 0.039(4) 0.052(4) 0.049(4) -0.007(3) -0.010(3) 0.004(3) C13S 0.050(5) 0.055(5) 0.121(8) 0.000(5) -0.037(5) -0.002(4) C14S 0.035(4) 0.057(5) 0.138(9) 0.036(6) -0.017(5) -0.015(4) C15S 0.044(5) 0.071(6) 0.088(7) 0.022(5) -0.003(4) 0.006(4) C16S 0.050(5) 0.065(5) 0.061(5) -0.008(4) -0.010(4) 0.006(4) C21S 0.071(11) 0.070(10) 0.159(15) -0.023(11) -0.030(11) -0.005(9) C22S 0.075(12) 0.051(10) 0.138(15) 0.001(12) -0.018(11) -0.023(9) C23S 0.078(13) 0.083(11) 0.094(13) 0.025(12) -0.024(11) -0.004(10) C24S 0.050(8) 0.041(7) 0.114(12) 0.008(8) -0.034(8) -0.007(6) C25S 0.059(9) 0.028(8) 0.145(14) 0.019(8) -0.030(9) -0.004(7) C26S 0.039(9) 0.051(9) 0.160(16) -0.013(10) -0.017(10) 0.007(7) C20S 0.117(19) 0.107(18) 0.19(2) -0.035(17) -0.037(18) -0.029(15) C31S 0.061(11) 0.051(10) 0.129(15) 0.026(11) -0.034(12) -0.001(9) C32S 0.047(10) 0.050(12) 0.162(16) 0.028(12) -0.008(12) 0.007(9) C33S 0.044(11) 0.070(12) 0.175(17) 0.004(13) 0.008(12) -0.003(9) C34S 0.077(12) 0.055(10) 0.167(16) -0.020(12) 0.016(12) -0.014(10) C35S 0.080(14) 0.082(13) 0.182(19) 0.012(16) 0.011(15) -0.006(13) C36S 0.057(11) 0.056(11) 0.071(11) 0.019(9) 0.017(9) -0.022(9) C30S 0.075(16) 0.113(18) 0.13(2) 0.047(16) -0.060(15) -0.009(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.865(4) . ? Co1 N2 1.876(4) . ? Co1 O1 1.908(4) . ? Co1 N4 1.965(4) . ? Co1 N1 2.015(4) . ? Co1 N9 2.062(4) . ? Co2 N7 1.868(4) . ? Co2 N6 1.881(4) . ? Co2 O2 1.942(3) . ? Co2 N5 1.971(4) . ? Co2 N8 1.986(4) . ? Co2 N10 2.060(4) . ? O1 O2 1.389(4) . ? N1 C1 1.311(6) . ? N1 C62 1.406(6) . ? N2 C5 1.334(6) . ? N2 C2 1.379(6) . ? N3 C19 1.330(6) . ? N3 C22 1.371(6) . ? N4 C23 1.299(6) . ? N4 C24 1.424(6) . ? N5 C32 1.307(6) . ? N5 C31 1.425(6) . ? N6 C36 1.338(6) . ? N6 C33 1.361(6) . ? N7 C50 1.339(6) . ? N7 C53 1.386(6) . ? N8 C54 1.300(6) . ? N8 C55 1.430(6) . ? N9 C63 1.342(6) . ? N9 C67 1.342(7) . ? N10 C68 1.343(6) . ? N10 C72 1.346(6) . ? C1 C2 1.391(7) . ? C1 H1 0.95 . ? C2 C3 1.401(7) . ? C3 C4 1.375(7) . ? C3 H3 0.95 . ? C4 C5 1.409(7) . ? C4 H4 0.95 . ? C5 C6 1.522(7) . ? C6 C19 1.525(7) . ? C6 C7 1.537(7) . ? C6 C18 1.542(7) . ? C7 C12 1.384(8) . ? C7 C8 1.391(8) . ? C8 C9 1.409(8) . ? C8 H8 0.95 . ? C9 C10 1.363(10) . ? C9 H9 0.95 . ? C10 C11 1.392(10) . ? C10 H10 0.95 . ? C11 C12 1.408(9) . ? C11 H11 0.95 . ? C12 C13 1.464(9) . ? C13 C18 1.375(8) . ? C13 C14 1.408(9) . ? C14 C15 1.384(10) . ? C14 H14 0.95 . ? C15 C16 1.382(10) . ? C15 H15 0.95 . ? C16 C17 1.382(8) . ? C16 H16 0.95 . ? C17 C18 1.383(8) . ? C17 H17 0.95 . ? C19 C20 1.393(7) . ? C20 C21 1.391(7) . ? C20 H20 0.95 . ? C21 C22 1.390(7) . ? C21 H21 0.95 . ? C22 C23 1.405(7) . ? C23 H23 0.95 . ? C24 C31 1.379(7) . ? C24 C25 1.395(7) . ? C25 C26 1.376(8) . ? C25 H25 0.95 . ? C26 C29 1.385(8) . ? C26 C27 1.512(8) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.507(8) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C30 1.385(7) . ? C30 C31 1.385(7) . ? C30 H30 0.95 . ? C32 C33 1.411(7) . ? C32 H32 0.95 . ? C33 C34 1.392(6) . ? C34 C35 1.385(7) . ? C34 H34 0.95 . ? C35 C36 1.407(7) . ? C35 H35 0.95 . ? C36 C37 1.509(7) . ? C37 C50 1.519(6) . ? C37 C38 1.536(6) . ? C37 C49 1.542(7) . ? C38 C39 1.369(7) . ? C38 C43 1.398(7) . ? C39 C40 1.390(7) . ? C39 H39 0.95 . ? C40 C41 1.379(9) . ? C40 H40 0.95 . ? C41 C42 1.366(9) . ? C41 H41 0.95 . ? C42 C43 1.410(7) . ? C42 H42 0.95 . ? C43 C44 1.456(8) . ? C44 C45 1.381(7) . ? C44 C49 1.405(7) . ? C45 C46 1.383(8) . ? C45 H45 0.95 . ? C46 C47 1.386(8) . ? C46 H46 0.95 . ? C47 C48 1.383(8) . ? C47 H47 0.95 . ? C48 C49 1.371(7) . ? C48 H48 0.95 . ? C50 C51 1.408(7) . ? C51 C52 1.392(7) . ? C51 H51 0.95 . ? C52 C53 1.386(7) . ? C52 H52 0.95 . ? C53 C54 1.425(7) . ? C54 H54 0.95 . ? C55 C56 1.394(7) . ? C55 C62 1.395(7) . ? C56 C57 1.388(7) . ? C56 H56 0.95 . ? C57 C60 1.396(8) . ? C57 C58 1.498(8) . ? C58 H58A 0.98 . ? C58 H58B 0.98 . ? C58 H58C 0.98 . ? C59 C60 1.515(7) . ? C59 H59A 0.98 . ? C59 H59B 0.98 . ? C59 H59C 0.98 . ? C60 C61 1.381(8) . ? C61 C62 1.394(7) . ? C61 H61 0.95 . ? C63 C64 1.384(7) . ? C63 H63 0.95 . ? C64 C65 1.371(8) . ? C64 H64 0.95 . ? C65 C66 1.383(8) . ? C65 H65 0.95 . ? C66 C67 1.377(7) . ? C66 H66 0.95 . ? C67 H67 0.95 . ? C68 C69 1.380(7) . ? C68 H68 0.95 . ? C69 C70 1.374(8) . ? C69 H69 0.95 . ? C70 C71 1.378(8) . ? C70 H70 0.95 . ? C71 C72 1.376(7) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? N1S C5S 1.316(9) . ? N1S C1S 1.364(9) . ? C1S C2S 1.360(10) . ? C1S H1S 0.95 . ? C2S C3S 1.380(10) . ? C2S H2S 0.95 . ? C3S C4S 1.341(9) . ? C3S H3S 0.95 . ? C4S C5S 1.373(9) . ? C4S H4S 0.95 . ? C5S H5S 0.95 . ? C10S C11S 1.472(11) . ? C10S H10A 0.98 . ? C10S H10B 0.98 . ? C10S H10C 0.98 . ? C11S C12S 1.371(10) . ? C11S C16S 1.374(10) . ? C12S C13S 1.384(11) . ? C12S H12S 0.95 . ? C13S C14S 1.409(13) . ? C13S H13S 0.95 . ? C14S C15S 1.348(14) . ? C14S H14S 0.95 . ? C15S C16S 1.342(12) . ? C15S H15S 0.95 . ? C16S H16S 0.95 . ? C21S C22S 1.39 . ? C21S C26S 1.39 . ? C21S C20S 1.508(17) . ? C22S C23S 1.39 . ? C22S H22S 0.95 . ? C23S C24S 1.39 . ? C23S H23S 0.95 . ? C24S C25S 1.39 . ? C24S H24S 0.95 . ? C25S C26S 1.39 . ? C25S H25S 0.95 . ? C26S H26S 0.95 . ? C20S H20A 0.98 . ? C20S H20B 0.98 . ? C20S H20C 0.98 . ? C31S C32S 1.39 . ? C31S C36S 1.39 . ? C31S C30S 1.487(17) . ? C32S C33S 1.39 . ? C32S H32S 0.95 . ? C33S C34S 1.39 . ? C33S H33S 0.95 . ? C34S C35S 1.39 . ? C34S H34S 0.95 . ? C35S C36S 1.39 . ? C35S H35S 0.95 . ? C36S H36S 0.95 . ? C30S H30A 0.98 . ? C30S H30B 0.98 . ? C30S H30C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N2 87.05(18) . . ? N3 Co1 O1 89.10(17) . . ? N2 Co1 O1 87.42(16) . . ? N3 Co1 N4 82.71(17) . . ? N2 Co1 N4 169.70(18) . . ? O1 Co1 N4 93.54(15) . . ? N3 Co1 N1 168.10(17) . . ? N2 Co1 N1 81.77(17) . . ? O1 Co1 N1 86.37(16) . . ? N4 Co1 N1 108.53(17) . . ? N3 Co1 N9 90.94(18) . . ? N2 Co1 N9 91.96(17) . . ? O1 Co1 N9 179.38(16) . . ? N4 Co1 N9 87.07(16) . . ? N1 Co1 N9 93.48(17) . . ? N7 Co2 N6 87.40(16) . . ? N7 Co2 O2 88.64(16) . . ? N6 Co2 O2 85.39(15) . . ? N7 Co2 N5 169.21(16) . . ? N6 Co2 N5 82.40(16) . . ? O2 Co2 N5 87.02(15) . . ? N7 Co2 N8 82.95(16) . . ? N6 Co2 N8 170.28(17) . . ? O2 Co2 N8 93.18(15) . . ? N5 Co2 N8 107.15(16) . . ? N7 Co2 N10 93.11(17) . . ? N6 Co2 N10 91.29(16) . . ? O2 Co2 N10 176.17(15) . . ? N5 Co2 N10 90.67(16) . . ? N8 Co2 N10 90.41(16) . . ? O2 O1 Co1 118.7(3) . . ? O1 O2 Co2 118.8(2) . . ? C1 N1 C62 119.9(4) . . ? C1 N1 Co1 111.4(3) . . ? C62 N1 Co1 128.7(3) . . ? C5 N2 C2 109.0(4) . . ? C5 N2 Co1 135.3(4) . . ? C2 N2 Co1 115.7(3) . . ? C19 N3 C22 109.1(4) . . ? C19 N3 Co1 135.8(3) . . ? C22 N3 Co1 115.1(3) . . ? C23 N4 C24 119.0(4) . . ? C23 N4 Co1 111.6(3) . . ? C24 N4 Co1 129.3(3) . . ? C32 N5 C31 120.0(4) . . ? C32 N5 Co2 111.8(3) . . ? C31 N5 Co2 128.1(3) . . ? C36 N6 C33 109.5(4) . . ? C36 N6 Co2 134.8(3) . . ? C33 N6 Co2 115.7(3) . . ? C50 N7 C53 108.4(4) . . ? C50 N7 Co2 135.5(3) . . ? C53 N7 Co2 114.7(3) . . ? C54 N8 C55 117.6(4) . . ? C54 N8 Co2 111.3(3) . . ? C55 N8 Co2 131.1(3) . . ? C63 N9 C67 116.7(4) . . ? C63 N9 Co1 121.8(4) . . ? C67 N9 Co1 121.5(3) . . ? C68 N10 C72 115.6(4) . . ? C68 N10 Co2 123.7(3) . . ? C72 N10 Co2 120.7(3) . . ? N1 C1 C2 117.6(4) . . ? N1 C1 H1 121.2 . . ? C2 C1 H1 121.2 . . ? N2 C2 C1 113.4(4) . . ? N2 C2 C3 107.7(4) . . ? C1 C2 C3 138.8(5) . . ? C4 C3 C2 107.4(5) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? C3 C4 C5 107.1(5) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N2 C5 C4 108.8(4) . . ? N2 C5 C6 123.6(4) . . ? C4 C5 C6 127.6(5) . . ? C5 C6 C19 113.1(4) . . ? C5 C6 C7 111.5(4) . . ? C19 C6 C7 108.3(4) . . ? C5 C6 C18 111.9(4) . . ? C19 C6 C18 111.2(4) . . ? C7 C6 C18 100.1(4) . . ? C12 C7 C8 120.8(5) . . ? C12 C7 C6 110.8(5) . . ? C8 C7 C6 128.4(5) . . ? C7 C8 C9 117.6(6) . . ? C7 C8 H8 121.2 . . ? C9 C8 H8 121.2 . . ? C10 C9 C8 122.3(7) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 119.9(6) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 118.9(7) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C7 C12 C11 120.5(6) . . ? C7 C12 C13 108.7(5) . . ? C11 C12 C13 130.8(6) . . ? C18 C13 C14 119.8(6) . . ? C18 C13 C12 109.2(5) . . ? C14 C13 C12 130.9(6) . . ? C15 C14 C13 117.6(6) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C16 C15 C14 121.8(6) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C17 C16 C15 120.7(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 117.7(6) . . ? C16 C17 H17 121.1 . . ? C18 C17 H17 121.1 . . ? C13 C18 C17 122.4(5) . . ? C13 C18 C6 110.8(5) . . ? C17 C18 C6 126.8(5) . . ? N3 C19 C20 109.0(4) . . ? N3 C19 C6 123.4(4) . . ? C20 C19 C6 127.4(5) . . ? C21 C20 C19 107.0(5) . . ? C21 C20 H20 126.5 . . ? C19 C20 H20 126.5 . . ? C22 C21 C20 106.7(4) . . ? C22 C21 H21 126.6 . . ? C20 C21 H21 126.6 . . ? N3 C22 C21 108.1(4) . . ? N3 C22 C23 112.2(4) . . ? C21 C22 C23 139.1(5) . . ? N4 C23 C22 117.8(4) . . ? N4 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C31 C24 C25 117.9(5) . . ? C31 C24 N4 121.2(4) . . ? C25 C24 N4 120.9(4) . . ? C26 C25 C24 122.4(5) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C29 119.2(5) . . ? C25 C26 C27 120.1(5) . . ? C29 C26 C27 120.7(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 C30 118.9(5) . . ? C26 C29 C28 121.9(5) . . ? C30 C29 C28 119.1(5) . . ? C31 C30 C29 121.5(5) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C24 C31 C30 120.0(4) . . ? C24 C31 N5 119.2(4) . . ? C30 C31 N5 120.7(4) . . ? N5 C32 C33 117.7(4) . . ? N5 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? N6 C33 C34 108.9(4) . . ? N6 C33 C32 112.4(4) . . ? C34 C33 C32 138.7(5) . . ? C35 C34 C33 106.0(4) . . ? C35 C34 H34 127 . . ? C33 C34 H34 127 . . ? C34 C35 C36 108.0(4) . . ? C34 C35 H35 126 . . ? C36 C35 H35 126 . . ? N6 C36 C35 107.6(4) . . ? N6 C36 C37 123.3(4) . . ? C35 C36 C37 129.0(4) . . ? C36 C37 C50 113.9(4) . . ? C36 C37 C38 109.3(4) . . ? C50 C37 C38 111.8(4) . . ? C36 C37 C49 109.7(4) . . ? C50 C37 C49 110.5(4) . . ? C38 C37 C49 100.8(4) . . ? C39 C38 C43 121.1(5) . . ? C39 C38 C37 128.4(5) . . ? C43 C38 C37 110.4(4) . . ? C38 C39 C40 118.8(5) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? C41 C40 C39 120.5(6) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 121.5(5) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C43 118.6(5) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C38 C43 C42 119.4(5) . . ? C38 C43 C44 109.4(4) . . ? C42 C43 C44 131.2(5) . . ? C45 C44 C49 120.2(5) . . ? C45 C44 C43 131.1(5) . . ? C49 C44 C43 108.7(4) . . ? C44 C45 C46 118.6(5) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.7 . . ? C45 C46 C47 120.9(5) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 120.6(6) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C49 C48 C47 118.9(5) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C44 120.7(5) . . ? C48 C49 C37 128.9(4) . . ? C44 C49 C37 110.4(4) . . ? N7 C50 C51 108.9(4) . . ? N7 C50 C37 122.0(4) . . ? C51 C50 C37 129.0(4) . . ? C52 C51 C50 107.1(4) . . ? C52 C51 H51 126.4 . . ? C50 C51 H51 126.4 . . ? C53 C52 C51 106.9(4) . . ? C53 C52 H52 126.5 . . ? C51 C52 H52 126.5 . . ? N7 C53 C52 108.6(4) . . ? N7 C53 C54 112.1(4) . . ? C52 C53 C54 139.3(4) . . ? N8 C54 C53 117.7(4) . . ? N8 C54 H54 121.2 . . ? C53 C54 H54 121.2 . . ? C56 C55 C62 119.5(4) . . ? C56 C55 N8 119.6(5) . . ? C62 C55 N8 121.0(4) . . ? C57 C56 C55 121.7(5) . . ? C57 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C56 C57 C60 119.0(5) . . ? C56 C57 C58 120.4(5) . . ? C60 C57 C58 120.6(5) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 C57 119.0(5) . . ? C61 C60 C59 119.6(5) . . ? C57 C60 C59 121.4(5) . . ? C60 C61 C62 122.7(5) . . ? C60 C61 H61 118.6 . . ? C62 C61 H61 118.6 . . ? C61 C62 C55 118.0(5) . . ? C61 C62 N1 121.5(5) . . ? C55 C62 N1 120.5(4) . . ? N9 C63 C64 123.5(5) . . ? N9 C63 H63 118.3 . . ? C64 C63 H63 118.3 . . ? C65 C64 C63 118.5(5) . . ? C65 C64 H64 120.8 . . ? C63 C64 H64 120.8 . . ? C64 C65 C66 119.3(5) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? C67 C66 C65 118.4(5) . . ? C67 C66 H66 120.8 . . ? C65 C66 H66 120.8 . . ? N9 C67 C66 123.6(5) . . ? N9 C67 H67 118.2 . . ? C66 C67 H67 118.2 . . ? N10 C68 C69 123.8(5) . . ? N10 C68 H68 118.1 . . ? C69 C68 H68 118.1 . . ? C70 C69 C68 119.5(5) . . ? C70 C69 H69 120.3 . . ? C68 C69 H69 120.3 . . ? C69 C70 C71 117.9(5) . . ? C69 C70 H70 121 . . ? C71 C70 H70 121 . . ? C72 C71 C70 119.2(5) . . ? C72 C71 H71 120.4 . . ? C70 C71 H71 120.4 . . ? N10 C72 C71 124.0(5) . . ? N10 C72 H72 118 . . ? C71 C72 H72 118 . . ? C5S N1S C1S 114.8(6) . . ? C2S C1S N1S 123.2(7) . . ? C2S C1S H1S 118.4 . . ? N1S C1S H1S 118.4 . . ? C1S C2S C3S 119.8(7) . . ? C1S C2S H2S 120.1 . . ? C3S C2S H2S 120.1 . . ? C4S C3S C2S 117.3(7) . . ? C4S C3S H3S 121.3 . . ? C2S C3S H3S 121.3 . . ? C3S C4S C5S 120.0(7) . . ? C3S C4S H4S 120 . . ? C5S C4S H4S 120 . . ? N1S C5S C4S 124.8(6) . . ? N1S C5S H5S 117.6 . . ? C4S C5S H5S 117.6 . . ? C11S C10S H10A 109.5 . . ? C11S C10S H10B 109.5 . . ? H10A C10S H10B 109.5 . . ? C11S C10S H10C 109.5 . . ? H10A C10S H10C 109.5 . . ? H10B C10S H10C 109.5 . . ? C12S C11S C16S 120.4(7) . . ? C12S C11S C10S 121.6(7) . . ? C16S C11S C10S 117.9(8) . . ? C11S C12S C13S 119.5(8) . . ? C11S C12S H12S 120.2 . . ? C13S C12S H12S 120.2 . . ? C12S C13S C14S 118.7(9) . . ? C12S C13S H13S 120.7 . . ? C14S C13S H13S 120.7 . . ? C15S C14S C13S 119.6(8) . . ? C15S C14S H14S 120.2 . . ? C13S C14S H14S 120.2 . . ? C16S C15S C14S 121.6(9) . . ? C16S C15S H15S 119.2 . . ? C14S C15S H15S 119.2 . . ? C15S C16S C11S 120.1(9) . . ? C15S C16S H16S 120 . . ? C11S C16S H16S 120 . . ? C22S C21S C26S 120 . . ? C22S C21S C20S 126.2(14) . . ? C26S C21S C20S 111.3(14) . . ? C23S C22S C21S 120 . . ? C23S C22S H22S 120 . . ? C21S C22S H22S 120 . . ? C22S C23S C24S 120 . . ? C22S C23S H23S 120 . . ? C24S C23S H23S 120 . . ? C25S C24S C23S 120 . . ? C25S C24S H24S 120 . . ? C23S C24S H24S 120 . . ? C26S C25S C24S 120 . . ? C26S C25S H25S 120 . . ? C24S C25S H25S 120 . . ? C25S C26S C21S 120 . . ? C25S C26S H26S 120 . . ? C21S C26S H26S 120 . . ? C32S C31S C36S 120 . . ? C32S C31S C30S 120.7(16) . . ? C36S C31S C30S 119.3(16) . . ? C31S C32S C33S 120 . . ? C31S C32S H32S 120 . . ? C33S C32S H32S 120 . . ? C32S C33S C34S 120 . . ? C32S C33S H33S 120 . . ? C34S C33S H33S 120 . . ? C35S C34S C33S 120 . . ? C35S C34S H34S 120 . . ? C33S C34S H34S 120 . . ? C34S C35S C36S 120 . . ? C34S C35S H35S 120 . . ? C36S C35S H35S 120 . . ? C35S C36S C31S 120 . . ? C35S C36S H36S 120 . . ? C31S C36S H36S 120 . . ? C31S C30S H30A 109.5 . . ? C31S C30S H30B 109.5 . . ? H30A C30S H30B 109.5 . . ? C31S C30S H30C 109.5 . . ? H30A C30S H30C 109.5 . . ? H30B C30S H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Co1 O1 O2 -74.5(3) . . . . ? N2 Co1 O1 O2 -161.6(3) . . . . ? N4 Co1 O1 O2 8.2(3) . . . . ? N1 Co1 O1 O2 116.5(3) . . . . ? N9 Co1 O1 O2 -17E1(8) . . . . ? Co1 O1 O2 Co2 -100.3(3) . . . . ? N7 Co2 O2 O1 -76.4(3) . . . . ? N6 Co2 O2 O1 -163.9(3) . . . . ? N5 Co2 O2 O1 113.5(3) . . . . ? N8 Co2 O2 O1 6.5(3) . . . . ? N10 Co2 O2 O1 166(2) . . . . ? N3 Co1 N1 C1 18.3(10) . . . . ? N2 Co1 N1 C1 -1.8(3) . . . . ? O1 Co1 N1 C1 86.1(3) . . . . ? N4 Co1 N1 C1 178.7(3) . . . . ? N9 Co1 N1 C1 -93.3(3) . . . . ? N3 Co1 N1 C62 -160.0(7) . . . . ? N2 Co1 N1 C62 179.9(4) . . . . ? O1 Co1 N1 C62 -92.2(4) . . . . ? N4 Co1 N1 C62 0.3(4) . . . . ? N9 Co1 N1 C62 88.4(4) . . . . ? N3 Co1 N2 C5 7.9(5) . . . . ? O1 Co1 N2 C5 97.1(5) . . . . ? N4 Co1 N2 C5 1.5(13) . . . . ? N1 Co1 N2 C5 -176.2(5) . . . . ? N9 Co1 N2 C5 -83.0(5) . . . . ? N3 Co1 N2 C2 -175.0(4) . . . . ? O1 Co1 N2 C2 -85.8(3) . . . . ? N4 Co1 N2 C2 178.6(8) . . . . ? N1 Co1 N2 C2 0.9(3) . . . . ? N9 Co1 N2 C2 94.1(4) . . . . ? N2 Co1 N3 C19 -4.6(5) . . . . ? O1 Co1 N3 C19 -92.1(5) . . . . ? N4 Co1 N3 C19 174.2(5) . . . . ? N1 Co1 N3 C19 -24.5(12) . . . . ? N9 Co1 N3 C19 87.3(5) . . . . ? N2 Co1 N3 C22 174.1(4) . . . . ? O1 Co1 N3 C22 86.6(3) . . . . ? N4 Co1 N3 C22 -7.1(3) . . . . ? N1 Co1 N3 C22 154.2(7) . . . . ? N9 Co1 N3 C22 -94.0(3) . . . . ? N3 Co1 N4 C23 6.1(3) . . . . ? N2 Co1 N4 C23 12.5(11) . . . . ? O1 Co1 N4 C23 -82.5(3) . . . . ? N1 Co1 N4 C23 -169.9(3) . . . . ? N9 Co1 N4 C23 97.4(3) . . . . ? N3 Co1 N4 C24 -172.1(4) . . . . ? N2 Co1 N4 C24 -165.7(8) . . . . ? O1 Co1 N4 C24 99.2(4) . . . . ? N1 Co1 N4 C24 11.9(4) . . . . ? N9 Co1 N4 C24 -80.8(4) . . . . ? N7 Co2 N5 C32 16.3(11) . . . . ? N6 Co2 N5 C32 -3.0(3) . . . . ? O2 Co2 N5 C32 82.7(3) . . . . ? N8 Co2 N5 C32 175.1(3) . . . . ? N10 Co2 N5 C32 -94.2(3) . . . . ? N7 Co2 N5 C31 -158.9(8) . . . . ? N6 Co2 N5 C31 -178.2(4) . . . . ? O2 Co2 N5 C31 -92.5(4) . . . . ? N8 Co2 N5 C31 -0.1(4) . . . . ? N10 Co2 N5 C31 90.6(4) . . . . ? N7 Co2 N6 C36 1.6(5) . . . . ? O2 Co2 N6 C36 90.5(5) . . . . ? N5 Co2 N6 C36 178.1(5) . . . . ? N8 Co2 N6 C36 8.6(13) . . . . ? N10 Co2 N6 C36 -91.4(5) . . . . ? N7 Co2 N6 C33 -174.2(4) . . . . ? O2 Co2 N6 C33 -85.4(3) . . . . ? N5 Co2 N6 C33 2.2(3) . . . . ? N8 Co2 N6 C33 -167.3(9) . . . . ? N10 Co2 N6 C33 92.7(3) . . . . ? N6 Co2 N7 C50 4.1(5) . . . . ? O2 Co2 N7 C50 -81.4(5) . . . . ? N5 Co2 N7 C50 -15.1(12) . . . . ? N8 Co2 N7 C50 -174.7(5) . . . . ? N10 Co2 N7 C50 95.2(5) . . . . ? N6 Co2 N7 C53 168.4(3) . . . . ? O2 Co2 N7 C53 82.9(3) . . . . ? N5 Co2 N7 C53 149.2(8) . . . . ? N8 Co2 N7 C53 -10.5(3) . . . . ? N10 Co2 N7 C53 -100.5(3) . . . . ? N7 Co2 N8 C54 9.5(3) . . . . ? N6 Co2 N8 C54 2.5(12) . . . . ? O2 Co2 N8 C54 -78.7(3) . . . . ? N5 Co2 N8 C54 -166.6(3) . . . . ? N10 Co2 N8 C54 102.6(3) . . . . ? N7 Co2 N8 C55 -173.5(5) . . . . ? N6 Co2 N8 C55 18E1(5) . . . . ? O2 Co2 N8 C55 98.3(4) . . . . ? N5 Co2 N8 C55 10.5(5) . . . . ? N10 Co2 N8 C55 -80.4(4) . . . . ? N3 Co1 N9 C63 -146.5(4) . . . . ? N2 Co1 N9 C63 -59.4(4) . . . . ? O1 Co1 N9 C63 -53(17) . . . . ? N4 Co1 N9 C63 130.9(4) . . . . ? N1 Co1 N9 C63 22.5(4) . . . . ? N3 Co1 N9 C67 35.7(4) . . . . ? N2 Co1 N9 C67 122.7(4) . . . . ? O1 Co1 N9 C67 129(16) . . . . ? N4 Co1 N9 C67 -47.0(4) . . . . ? N1 Co1 N9 C67 -155.4(4) . . . . ? N7 Co2 N10 C68 -143.3(4) . . . . ? N6 Co2 N10 C68 -55.8(4) . . . . ? O2 Co2 N10 C68 -26(2) . . . . ? N5 Co2 N10 C68 26.6(4) . . . . ? N8 Co2 N10 C68 133.7(4) . . . . ? N7 Co2 N10 C72 37.4(4) . . . . ? N6 Co2 N10 C72 124.9(4) . . . . ? O2 Co2 N10 C72 155(2) . . . . ? N5 Co2 N10 C72 -152.7(4) . . . . ? N8 Co2 N10 C72 -45.6(4) . . . . ? C62 N1 C1 C2 -179.1(4) . . . . ? Co1 N1 C1 C2 2.4(5) . . . . ? C5 N2 C2 C1 177.9(4) . . . . ? Co1 N2 C2 C1 0.1(5) . . . . ? C5 N2 C2 C3 0.6(5) . . . . ? Co1 N2 C2 C3 -177.3(3) . . . . ? N1 C1 C2 N2 -1.7(6) . . . . ? N1 C1 C2 C3 174.5(6) . . . . ? N2 C2 C3 C4 -1.3(6) . . . . ? C1 C2 C3 C4 -177.6(6) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? C2 N2 C5 C4 0.4(6) . . . . ? Co1 N2 C5 C4 177.6(4) . . . . ? C2 N2 C5 C6 -177.7(4) . . . . ? Co1 N2 C5 C6 -0.5(8) . . . . ? C3 C4 C5 N2 -1.2(6) . . . . ? C3 C4 C5 C6 176.8(5) . . . . ? N2 C5 C6 C19 -11.7(7) . . . . ? C4 C5 C6 C19 170.6(5) . . . . ? N2 C5 C6 C7 110.7(5) . . . . ? C4 C5 C6 C7 -67.1(7) . . . . ? N2 C5 C6 C18 -138.2(5) . . . . ? C4 C5 C6 C18 44.1(7) . . . . ? C5 C6 C7 C12 125.4(5) . . . . ? C19 C6 C7 C12 -109.6(5) . . . . ? C18 C6 C7 C12 6.8(5) . . . . ? C5 C6 C7 C8 -55.1(7) . . . . ? C19 C6 C7 C8 69.9(7) . . . . ? C18 C6 C7 C8 -173.7(5) . . . . ? C12 C7 C8 C9 2.2(8) . . . . ? C6 C7 C8 C9 -177.3(5) . . . . ? C7 C8 C9 C10 0.2(9) . . . . ? C8 C9 C10 C11 -1.9(11) . . . . ? C9 C10 C11 C12 1.3(11) . . . . ? C8 C7 C12 C11 -2.8(9) . . . . ? C6 C7 C12 C11 176.7(5) . . . . ? C8 C7 C12 C13 175.0(5) . . . . ? C6 C7 C12 C13 -5.5(6) . . . . ? C10 C11 C12 C7 1.1(10) . . . . ? C10 C11 C12 C13 -176.2(7) . . . . ? C7 C12 C13 C18 1.4(7) . . . . ? C11 C12 C13 C18 178.9(6) . . . . ? C7 C12 C13 C14 -174.6(6) . . . . ? C11 C12 C13 C14 2.9(11) . . . . ? C18 C13 C14 C15 1.3(9) . . . . ? C12 C13 C14 C15 177.0(6) . . . . ? C13 C14 C15 C16 -0.7(10) . . . . ? C14 C15 C16 C17 0.0(10) . . . . ? C15 C16 C17 C18 0.1(9) . . . . ? C14 C13 C18 C17 -1.1(9) . . . . ? C12 C13 C18 C17 -177.7(5) . . . . ? C14 C13 C18 C6 179.7(5) . . . . ? C12 C13 C18 C6 3.2(6) . . . . ? C16 C17 C18 C13 0.4(8) . . . . ? C16 C17 C18 C6 179.4(5) . . . . ? C5 C6 C18 C13 -124.2(5) . . . . ? C19 C6 C18 C13 108.3(5) . . . . ? C7 C6 C18 C13 -5.9(5) . . . . ? C5 C6 C18 C17 56.7(7) . . . . ? C19 C6 C18 C17 -70.8(7) . . . . ? C7 C6 C18 C17 175.0(5) . . . . ? C22 N3 C19 C20 0.0(6) . . . . ? Co1 N3 C19 C20 178.7(4) . . . . ? C22 N3 C19 C6 175.5(4) . . . . ? Co1 N3 C19 C6 -5.8(8) . . . . ? C5 C6 C19 N3 14.5(7) . . . . ? C7 C6 C19 N3 -109.6(6) . . . . ? C18 C6 C19 N3 141.4(5) . . . . ? C5 C6 C19 C20 -170.9(5) . . . . ? C7 C6 C19 C20 65.0(7) . . . . ? C18 C6 C19 C20 -44.0(7) . . . . ? N3 C19 C20 C21 1.3(6) . . . . ? C6 C19 C20 C21 -173.9(5) . . . . ? C19 C20 C21 C22 -2.1(6) . . . . ? C19 N3 C22 C21 -1.3(6) . . . . ? Co1 N3 C22 C21 179.6(3) . . . . ? C19 N3 C22 C23 -174.2(4) . . . . ? Co1 N3 C22 C23 6.7(5) . . . . ? C20 C21 C22 N3 2.1(5) . . . . ? C20 C21 C22 C23 172.1(6) . . . . ? C24 N4 C23 C22 174.3(4) . . . . ? Co1 N4 C23 C22 -4.1(5) . . . . ? N3 C22 C23 N4 -1.4(6) . . . . ? C21 C22 C23 N4 -171.1(6) . . . . ? C23 N4 C24 C31 73.6(6) . . . . ? Co1 N4 C24 C31 -108.3(5) . . . . ? C23 N4 C24 C25 -106.5(6) . . . . ? Co1 N4 C24 C25 71.6(6) . . . . ? C31 C24 C25 C26 -2.6(9) . . . . ? N4 C24 C25 C26 177.5(5) . . . . ? C24 C25 C26 C29 0.6(9) . . . . ? C24 C25 C26 C27 -178.6(6) . . . . ? C25 C26 C29 C30 1.2(9) . . . . ? C27 C26 C29 C30 -179.6(6) . . . . ? C25 C26 C29 C28 -178.4(6) . . . . ? C27 C26 C29 C28 0.8(10) . . . . ? C26 C29 C30 C31 -0.9(8) . . . . ? C28 C29 C30 C31 178.7(5) . . . . ? C25 C24 C31 C30 2.9(7) . . . . ? N4 C24 C31 C30 -177.2(5) . . . . ? C25 C24 C31 N5 -176.1(5) . . . . ? N4 C24 C31 N5 3.8(7) . . . . ? C29 C30 C31 C24 -1.2(8) . . . . ? C29 C30 C31 N5 177.7(5) . . . . ? C32 N5 C31 C24 -99.0(5) . . . . ? Co2 N5 C31 C24 75.9(6) . . . . ? C32 N5 C31 C30 82.0(6) . . . . ? Co2 N5 C31 C30 -103.1(5) . . . . ? C31 N5 C32 C33 179.0(4) . . . . ? Co2 N5 C32 C33 3.4(5) . . . . ? C36 N6 C33 C34 0.1(6) . . . . ? Co2 N6 C33 C34 177.0(3) . . . . ? C36 N6 C33 C32 -177.9(4) . . . . ? Co2 N6 C33 C32 -1.1(5) . . . . ? N5 C32 C33 N6 -1.6(6) . . . . ? N5 C32 C33 C34 -178.9(6) . . . . ? N6 C33 C34 C35 0.1(6) . . . . ? C32 C33 C34 C35 177.4(6) . . . . ? C33 C34 C35 C36 -0.3(6) . . . . ? C33 N6 C36 C35 -0.3(5) . . . . ? Co2 N6 C36 C35 -176.4(4) . . . . ? C33 N6 C36 C37 -178.4(4) . . . . ? Co2 N6 C36 C37 5.5(8) . . . . ? C34 C35 C36 N6 0.4(6) . . . . ? C34 C35 C36 C37 178.3(5) . . . . ? N6 C36 C37 C50 -16.4(7) . . . . ? C35 C36 C37 C50 166.0(5) . . . . ? N6 C36 C37 C38 -142.2(5) . . . . ? C35 C36 C37 C38 40.1(7) . . . . ? N6 C36 C37 C49 108.1(5) . . . . ? C35 C36 C37 C49 -69.6(6) . . . . ? C36 C37 C38 C39 65.9(6) . . . . ? C50 C37 C38 C39 -61.2(7) . . . . ? C49 C37 C38 C39 -178.6(5) . . . . ? C36 C37 C38 C43 -111.2(4) . . . . ? C50 C37 C38 C43 121.7(4) . . . . ? C49 C37 C38 C43 4.3(5) . . . . ? C43 C38 C39 C40 4.1(8) . . . . ? C37 C38 C39 C40 -172.7(5) . . . . ? C38 C39 C40 C41 -0.3(8) . . . . ? C39 C40 C41 C42 -2.8(9) . . . . ? C40 C41 C42 C43 2.0(9) . . . . ? C39 C38 C43 C42 -4.8(7) . . . . ? C37 C38 C43 C42 172.5(4) . . . . ? C39 C38 C43 C44 177.0(5) . . . . ? C37 C38 C43 C44 -5.6(5) . . . . ? C41 C42 C43 C38 1.7(8) . . . . ? C41 C42 C43 C44 179.4(5) . . . . ? C38 C43 C44 C45 -174.6(5) . . . . ? C42 C43 C44 C45 7.5(9) . . . . ? C38 C43 C44 C49 4.6(6) . . . . ? C42 C43 C44 C49 -173.3(5) . . . . ? C49 C44 C45 C46 2.2(7) . . . . ? C43 C44 C45 C46 -178.7(5) . . . . ? C44 C45 C46 C47 0.4(8) . . . . ? C45 C46 C47 C48 -1.5(8) . . . . ? C46 C47 C48 C49 0.1(8) . . . . ? C47 C48 C49 C44 2.5(7) . . . . ? C47 C48 C49 C37 -179.0(5) . . . . ? C45 C44 C49 C48 -3.7(7) . . . . ? C43 C44 C49 C48 177.0(4) . . . . ? C45 C44 C49 C37 177.6(4) . . . . ? C43 C44 C49 C37 -1.7(5) . . . . ? C36 C37 C49 C48 -64.8(6) . . . . ? C50 C37 C49 C48 61.7(6) . . . . ? C38 C37 C49 C48 180.0(5) . . . . ? C36 C37 C49 C44 113.8(4) . . . . ? C50 C37 C49 C44 -119.7(4) . . . . ? C38 C37 C49 C44 -1.4(5) . . . . ? C53 N7 C50 C51 1.7(5) . . . . ? Co2 N7 C50 C51 166.6(4) . . . . ? C53 N7 C50 C37 178.7(4) . . . . ? Co2 N7 C50 C37 -16.3(8) . . . . ? C36 C37 C50 N7 21.0(7) . . . . ? C38 C37 C50 N7 145.6(5) . . . . ? C49 C37 C50 N7 -103.0(5) . . . . ? C36 C37 C50 C51 -162.6(5) . . . . ? C38 C37 C50 C51 -38.0(7) . . . . ? C49 C37 C50 C51 73.4(6) . . . . ? N7 C50 C51 C52 -0.7(6) . . . . ? C37 C50 C51 C52 -177.5(5) . . . . ? C50 C51 C52 C53 -0.6(6) . . . . ? C50 N7 C53 C52 -2.0(6) . . . . ? Co2 N7 C53 C52 -170.5(3) . . . . ? C50 N7 C53 C54 178.0(4) . . . . ? Co2 N7 C53 C54 9.6(5) . . . . ? C51 C52 C53 N7 1.6(6) . . . . ? C51 C52 C53 C54 -178.5(6) . . . . ? C55 N8 C54 C53 175.7(4) . . . . ? Co2 N8 C54 C53 -6.8(6) . . . . ? N7 C53 C54 N8 -1.4(6) . . . . ? C52 C53 C54 N8 178.7(6) . . . . ? C54 N8 C55 C56 -111.4(5) . . . . ? Co2 N8 C55 C56 71.7(6) . . . . ? C54 N8 C55 C62 68.3(6) . . . . ? Co2 N8 C55 C62 -108.6(5) . . . . ? C62 C55 C56 C57 -4.4(8) . . . . ? N8 C55 C56 C57 175.2(5) . . . . ? C55 C56 C57 C60 0.8(8) . . . . ? C55 C56 C57 C58 177.1(5) . . . . ? C56 C57 C60 C61 2.4(9) . . . . ? C58 C57 C60 C61 -174.0(6) . . . . ? C56 C57 C60 C59 -178.1(6) . . . . ? C58 C57 C60 C59 5.6(9) . . . . ? C57 C60 C61 C62 -2.0(9) . . . . ? C59 C60 C61 C62 178.5(6) . . . . ? C60 C61 C62 C55 -1.6(9) . . . . ? C60 C61 C62 N1 176.0(5) . . . . ? C56 C55 C62 C61 4.7(7) . . . . ? N8 C55 C62 C61 -174.9(5) . . . . ? C56 C55 C62 N1 -172.9(5) . . . . ? N8 C55 C62 N1 7.4(7) . . . . ? C1 N1 C62 C61 75.2(7) . . . . ? Co1 N1 C62 C61 -106.5(5) . . . . ? C1 N1 C62 C55 -107.2(5) . . . . ? Co1 N1 C62 C55 71.1(6) . . . . ? C67 N9 C63 C64 2.5(8) . . . . ? Co1 N9 C63 C64 -175.4(5) . . . . ? N9 C63 C64 C65 -1.4(9) . . . . ? C63 C64 C65 C66 0.3(9) . . . . ? C64 C65 C66 C67 -0.5(9) . . . . ? C63 N9 C67 C66 -2.7(8) . . . . ? Co1 N9 C67 C66 175.3(5) . . . . ? C65 C66 C67 N9 1.7(9) . . . . ? C72 N10 C68 C69 0.8(7) . . . . ? Co2 N10 C68 C69 -178.5(4) . . . . ? N10 C68 C69 C70 -0.9(9) . . . . ? C68 C69 C70 C71 0.0(9) . . . . ? C69 C70 C71 C72 0.9(8) . . . . ? C68 N10 C72 C71 0.2(7) . . . . ? Co2 N10 C72 C71 179.6(4) . . . . ? C70 C71 C72 N10 -1.1(8) . . . . ? C5S N1S C1S C2S -1.4(10) . . . . ? N1S C1S C2S C3S 2.4(11) . . . . ? C1S C2S C3S C4S -2.1(10) . . . . ? C2S C3S C4S C5S 1.2(10) . . . . ? C1S N1S C5S C4S 0.4(10) . . . . ? C3S C4S C5S N1S -0.3(11) . . . . ? C16S C11S C12S C13S 1.3(10) . . . . ? C10S C11S C12S C13S 179.6(7) . . . . ? C11S C12S C13S C14S -1.1(11) . . . . ? C12S C13S C14S C15S 0.1(12) . . . . ? C13S C14S C15S C16S 0.7(13) . . . . ? C14S C15S C16S C11S -0.5(13) . . . . ? C12S C11S C16S C15S -0.5(11) . . . . ? C10S C11S C16S C15S -178.8(7) . . . . ? C26S C21S C22S C23S 0 . . . . ? C20S C21S C22S C23S 160.3(18) . . . . ? C21S C22S C23S C24S 0 . . . . ? C22S C23S C24S C25S 0 . . . . ? C23S C24S C25S C26S 0 . . . . ? C24S C25S C26S C21S 0 . . . . ? C22S C21S C26S C25S 0 . . . . ? C20S C21S C26S C25S -163.0(15) . . . . ? C36S C31S C32S C33S 0 . . . . ? C30S C31S C32S C33S 179(2) . . . . ? C31S C32S C33S C34S 0 . . . . ? C32S C33S C34S C35S 0 . . . . ? C33S C34S C35S C36S 0 . . . . ? C34S C35S C36S C31S 0 . . . . ? C32S C31S C36S C35S 0 . . . . ? C30S C31S C36S C35S -178.5(19) . . . . ? # END of CIF # Attachment 'Co2OH_L_.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-11-25 at 14:00:20 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : mer data _LOVE2 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_mer _database_code_depnum_ccdc_archive 'CCDC 749305' #TrackingRef 'Co2OH_L_.cif' _audit_creation_date 2008-11-25T14:00:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_analytical ? _chemical_formula_sum 'C71 H54 Cl12 Co2 N9 O' _chemical_formula_weight 1592.49 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.627(2) _cell_length_b 22.087(3) _cell_length_c 30.628(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13953(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20612 _cell_measurement_theta_min 1.6561 _cell_measurement_theta_max 28.4967 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6472 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8533 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 14.7059 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_ub_11 0.0484 _diffrn_orient_matrix_ub_12 -0.0014 _diffrn_orient_matrix_ub_13 -0.0022 _diffrn_orient_matrix_ub_21 0.0021 _diffrn_orient_matrix_ub_22 0.0396 _diffrn_orient_matrix_ub_23 0.0219 _diffrn_orient_matrix_ub_31 0.0008 _diffrn_orient_matrix_ub_32 -0.0159 _diffrn_orient_matrix_ub_33 0.0285 _diffrn_measurement_device ; Mercury (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_av_R_equivalents 0.2903 _diffrn_reflns_av_unetI/netI 0.2266 _diffrn_reflns_number 85490 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 12745 _reflns_number_gt 5685 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process 'Lp corrections applied' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Two partially-occupied and overlapping CHCl3 groups (C4s, Cl10, Cl11, Cl12; C5s, Cl13, Cl14, Cl15) isotropic model with 60:40 occupancy. The bridging hydroxyl hydrogen atom H1A was located using a 2-site free-variable refinement procedure and refined with fixed thermal parameters. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 12745 _refine_ls_number_parameters 859 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.2146 _refine_ls_R_factor_gt 0.0981 _refine_ls_wR_factor_ref 0.2514 _refine_ls_wR_factor_gt 0.2 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.985 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3619(4) 0.1582(4) 0.5004(3) 0.031(2) Uani 1 1 d . . . H1 H 0.3841 0.1389 0.5229 0.037 Uiso 1 1 calc R . . C1S C 0.1051(4) 0.5175(4) 0.3926(3) 0.048(3) Uani 1 1 d . . . H1S H 0.0758 0.5439 0.4091 0.058 Uiso 1 1 calc R . . C2 C 0.3904(4) 0.1651(4) 0.4597(3) 0.0286(19) Uani 1 1 d . . . C2S C 0.6253(4) 0.0365(5) 0.4328(4) 0.062(3) Uani 1 1 d . . . H2S H 0.6534 0.0723 0.4338 0.074 Uiso 1 1 calc R . . C3 C 0.4516(4) 0.1527(4) 0.4407(3) 0.034(2) Uani 1 1 d . . . H3 H 0.4864 0.1337 0.4543 0.041 Uiso 1 1 calc R . . C3S C 0.6713(4) 0.3173(4) 0.1931(3) 0.047(3) Uani 1 1 d . . . H3S H 0.7129 0.3238 0.1784 0.056 Uiso 1 1 calc R . . C4 C 0.4501(4) 0.1740(4) 0.3981(3) 0.035(2) Uani 1 1 d . . . H4 H 0.4832 0.1715 0.3776 0.042 Uiso 1 1 calc R . . C5 C 0.3881(3) 0.2003(4) 0.3923(3) 0.0278(19) Uani 1 1 d . . . C6 C 0.3598(3) 0.2310(4) 0.3520(3) 0.0275(19) Uani 1 1 d . . . C7 C 0.3177(4) 0.1853(4) 0.3261(3) 0.032(2) Uani 1 1 d . . . C8 C 0.2647(4) 0.1520(4) 0.3406(3) 0.040(2) Uani 1 1 d . . . H8 H 0.2492 0.1565 0.3689 0.048 Uiso 1 1 calc R . . C9 C 0.2351(4) 0.1116(4) 0.3118(3) 0.046(3) Uani 1 1 d . . . H9 H 0.2007 0.0879 0.3212 0.056 Uiso 1 1 calc R . . C10 C 0.2571(5) 0.1067(5) 0.2685(3) 0.053(3) Uani 1 1 d . . . H10 H 0.2356 0.0812 0.2491 0.064 Uiso 1 1 calc R . . C11 C 0.3107(4) 0.1396(5) 0.2542(3) 0.049(3) Uani 1 1 d . . . H11 H 0.3268 0.1349 0.2261 0.058 Uiso 1 1 calc R . . C12 C 0.3388(4) 0.1792(4) 0.2830(3) 0.037(2) Uani 1 1 d . . . C13 C 0.3972(4) 0.2192(4) 0.2776(3) 0.040(2) Uani 1 1 d . . . C14 C 0.4358(4) 0.2301(5) 0.2418(3) 0.053(3) Uani 1 1 d . . . H14 H 0.4263 0.2117 0.2152 0.064 Uiso 1 1 calc R . . C15 C 0.4871(5) 0.2672(6) 0.2451(4) 0.063(3) Uani 1 1 d . . . H15 H 0.5122 0.275 0.2206 0.075 Uiso 1 1 calc R . . C16 C 0.5032(4) 0.2940(5) 0.2844(4) 0.065(3) Uani 1 1 d . . . H16 H 0.54 0.3181 0.2865 0.078 Uiso 1 1 calc R . . C17 C 0.4638(4) 0.2847(4) 0.3211(3) 0.045(3) Uani 1 1 d . . . H17 H 0.4733 0.3035 0.3475 0.054 Uiso 1 1 calc R . . C18 C 0.4099(4) 0.2467(4) 0.3171(3) 0.039(2) Uani 1 1 d . . . C19 C 0.3223(4) 0.2873(4) 0.3648(3) 0.029(2) Uani 1 1 d . . . C20 C 0.3216(4) 0.3456(4) 0.3469(3) 0.034(2) Uani 1 1 d . . . H20 H 0.3433 0.3578 0.3218 0.04 Uiso 1 1 calc R . . C21 C 0.2832(4) 0.3821(4) 0.3729(3) 0.033(2) Uani 1 1 d . . . H21 H 0.2744 0.423 0.3689 0.04 Uiso 1 1 calc R . . C22 C 0.2602(4) 0.3445(4) 0.4065(3) 0.030(2) Uani 1 1 d . . . C23 C 0.2330(3) 0.3542(4) 0.4486(3) 0.0289(19) Uani 1 1 d . . . H23 H 0.2147 0.3914 0.4557 0.035 Uiso 1 1 calc R . . C24 C 0.2075(4) 0.3149(4) 0.5194(3) 0.030(2) Uani 1 1 d . . . C25 C 0.2458(4) 0.3356(4) 0.5538(3) 0.032(2) Uani 1 1 d . . . H25 H 0.2865 0.3515 0.5475 0.038 Uiso 1 1 calc R . . C26 C 0.2259(4) 0.3336(4) 0.5970(3) 0.036(2) Uani 1 1 d . . . C27 C 0.2698(4) 0.3530(4) 0.6343(3) 0.046(3) Uani 1 1 d . . . H27A H 0.2475 0.382 0.6522 0.069 Uiso 1 1 calc R . . H27B H 0.3085 0.3711 0.6226 0.069 Uiso 1 1 calc R . . H27C H 0.2811 0.3183 0.6515 0.069 Uiso 1 1 calc R . . C28 C 0.1640(4) 0.3097(4) 0.6065(3) 0.034(2) Uani 1 1 d . . . C29 C 0.1392(4) 0.3076(5) 0.6531(3) 0.052(3) Uani 1 1 d . . . H29A H 0.172 0.2908 0.6718 0.078 Uiso 1 1 calc R . . H29B H 0.101 0.2827 0.6544 0.078 Uiso 1 1 calc R . . H29C H 0.1288 0.3478 0.6627 0.078 Uiso 1 1 calc R . . C30 C 0.1259(3) 0.2889(4) 0.5721(3) 0.029(2) Uani 1 1 d . . . H30 H 0.0851 0.2731 0.5781 0.035 Uiso 1 1 calc R . . C31 C 0.1466(3) 0.2911(4) 0.5290(3) 0.0262(19) Uani 1 1 d . . . C32 C 0.0722(4) 0.2998(4) 0.4714(2) 0.030(2) Uani 1 1 d . . . H32 H 0.07 0.3414 0.4757 0.036 Uiso 1 1 calc R . . C33 C 0.0357(3) 0.2696(4) 0.4380(3) 0.0276(19) Uani 1 1 d . . . C34 C -0.0118(3) 0.2861(4) 0.4066(3) 0.030(2) Uani 1 1 d . . . H34 H -0.0302 0.3242 0.4025 0.036 Uiso 1 1 calc R . . C35 C -0.0249(4) 0.2336(4) 0.3833(3) 0.034(2) Uani 1 1 d . . . H35 H -0.0539 0.23 0.3602 0.041 Uiso 1 1 calc R . . C36 C 0.0138(3) 0.1863(3) 0.4010(3) 0.0240(18) Uani 1 1 d . . . C37 C 0.0195(4) 0.1211(4) 0.3852(3) 0.032(2) Uani 1 1 d . . . C38 C 0.0225(4) 0.1160(4) 0.3361(3) 0.033(2) Uani 1 1 d . . . C39 C 0.0691(4) 0.1403(4) 0.3077(3) 0.039(2) Uani 1 1 d . . . H39 H 0.1027 0.1642 0.3184 0.047 Uiso 1 1 calc R . . C40 C 0.0644(4) 0.1282(4) 0.2640(3) 0.047(3) Uani 1 1 d . . . H40 H 0.0949 0.1443 0.2449 0.056 Uiso 1 1 calc R . . C41 C 0.0140(5) 0.0919(5) 0.2477(3) 0.060(3) Uani 1 1 d . . . H41 H 0.0114 0.0841 0.2179 0.072 Uiso 1 1 calc R . . C42 C -0.0309(5) 0.0681(5) 0.2751(4) 0.058(3) Uani 1 1 d . . . H42 H -0.0642 0.0444 0.2639 0.069 Uiso 1 1 calc R . . C43 C -0.0277(4) 0.0788(4) 0.3201(3) 0.040(2) Uani 1 1 d . . . C44 C -0.0676(4) 0.0603(4) 0.3572(3) 0.042(2) Uani 1 1 d . . . C45 C -0.1224(4) 0.0217(4) 0.3582(4) 0.057(3) Uani 1 1 d . . . H45 H -0.1387 0.0039 0.333 0.068 Uiso 1 1 calc R . . C46 C -0.1503(5) 0.0122(5) 0.3983(5) 0.065(3) Uani 1 1 d . . . H46 H -0.1865 -0.0129 0.3999 0.078 Uiso 1 1 calc R . . C47 C -0.1272(5) 0.0379(5) 0.4363(4) 0.057(3) Uani 1 1 d . . . H47 H -0.148 0.0307 0.4627 0.068 Uiso 1 1 calc R . . C48 C -0.0722(4) 0.0748(4) 0.4346(3) 0.042(2) Uani 1 1 d . . . H48 H -0.056 0.0926 0.4599 0.051 Uiso 1 1 calc R . . C49 C -0.0426(4) 0.0846(4) 0.3956(3) 0.032(2) Uani 1 1 d . . . C50 C 0.0766(3) 0.0889(4) 0.4065(3) 0.0238(18) Uani 1 1 d . . . C51 C 0.1071(4) 0.0341(4) 0.3920(3) 0.033(2) Uani 1 1 d . . . H51 H 0.0965 0.0121 0.3672 0.039 Uiso 1 1 calc R . . C52 C 0.1555(4) 0.0200(4) 0.4222(3) 0.032(2) Uani 1 1 d . . . H52 H 0.183 -0.0134 0.4215 0.038 Uiso 1 1 calc R . . C53 C 0.1546(3) 0.0657(4) 0.4534(3) 0.0266(19) Uani 1 1 d . . . C54 C 0.1910(3) 0.0847(4) 0.4896(3) 0.032(2) Uani 1 1 d . . . H54 H 0.2257 0.0615 0.4995 0.038 Uiso 1 1 calc R . . C55 C 0.2082(3) 0.1513(4) 0.5484(3) 0.0251(19) Uani 1 1 d . . . C56 C 0.1775(4) 0.1434(4) 0.5880(3) 0.030(2) Uani 1 1 d . . . H56 H 0.134 0.1322 0.5882 0.035 Uiso 1 1 calc R . . C57 C 0.2093(4) 0.1517(4) 0.6282(3) 0.032(2) Uani 1 1 d . . . C58 C 0.1750(4) 0.1378(4) 0.6702(3) 0.046(2) Uani 1 1 d . . . H58A H 0.1692 0.1745 0.6866 0.068 Uiso 1 1 calc R . . H58B H 0.2004 0.1098 0.687 0.068 Uiso 1 1 calc R . . H58C H 0.1334 0.1203 0.664 0.068 Uiso 1 1 calc R . . C59 C 0.2730(4) 0.1731(4) 0.6270(3) 0.034(2) Uani 1 1 d . . . C60 C 0.3096(4) 0.1839(5) 0.6704(3) 0.051(3) Uani 1 1 d . . . H60A H 0.2857 0.2119 0.6881 0.076 Uiso 1 1 calc R . . H60B H 0.3518 0.2003 0.6644 0.076 Uiso 1 1 calc R . . H60C H 0.3142 0.1462 0.6857 0.076 Uiso 1 1 calc R . . C61 C 0.3036(4) 0.1833(4) 0.5878(3) 0.032(2) Uani 1 1 d . . . H61 H 0.3458 0.1981 0.5876 0.039 Uiso 1 1 calc R . . C62 C 0.2719(4) 0.1716(4) 0.5479(3) 0.030(2) Uani 1 1 d . . . C63 C 0.0374(4) 0.0976(4) 0.5297(3) 0.031(2) Uani 1 1 d . . . H63 H 0.0715 0.0715 0.5232 0.037 Uiso 1 1 calc R . . C64 C -0.0113(4) 0.0766(4) 0.5558(3) 0.040(2) Uani 1 1 d . . . H64 H -0.0104 0.0371 0.5664 0.048 Uiso 1 1 calc R . . C65 C -0.0617(4) 0.1145(4) 0.5662(3) 0.039(2) Uani 1 1 d . . . H65 H -0.0949 0.1017 0.5846 0.047 Uiso 1 1 calc R . . C66 C -0.0620(4) 0.1728(4) 0.5485(3) 0.038(2) Uani 1 1 d . . . H66 H -0.0961 0.1992 0.5543 0.045 Uiso 1 1 calc R . . C67 C -0.0117(4) 0.1908(4) 0.5226(3) 0.036(2) Uani 1 1 d . . . H67 H -0.0121 0.2298 0.5111 0.043 Uiso 1 1 calc R . . Co1 Co 0.26884(5) 0.22811(5) 0.45053(4) 0.0296(3) Uani 1 1 d . . . Co2 Co 0.10952(5) 0.17912(5) 0.47348(4) 0.0262(3) Uani 1 1 d . . . N1 N 0.3029(3) 0.1794(3) 0.5068(2) 0.0285(16) Uani 1 1 d . . . N2 N 0.3530(3) 0.1941(3) 0.4284(2) 0.0305(17) Uani 1 1 d . . . N3 N 0.2834(3) 0.2866(3) 0.4000(2) 0.0285(16) Uani 1 1 d . . . N4 N 0.2341(3) 0.3104(3) 0.4771(2) 0.0297(16) Uani 1 1 d . . . N5 N 0.1089(3) 0.2646(3) 0.4952(2) 0.0247(15) Uani 1 1 d . . . N6 N 0.0495(3) 0.2100(3) 0.4332(2) 0.0261(16) Uani 1 1 d . . . N7 N 0.1055(3) 0.1063(3) 0.4435(2) 0.0243(15) Uani 1 1 d . . . N8 N 0.1756(3) 0.1355(3) 0.5095(2) 0.0267(16) Uani 1 1 d . . . N9 N 0.0390(3) 0.1539(3) 0.5129(2) 0.0296(16) Uani 1 1 d . . . O1 O 0.1799(3) 0.2003(2) 0.43564(18) 0.0294(13) Uani 1 1 d D . . Cl1 Cl 0.09951(13) 0.53732(13) 0.33695(9) 0.0668(8) Uani 1 1 d . . . Cl2 Cl 0.07911(13) 0.44234(13) 0.39978(10) 0.0696(8) Uani 1 1 d . . . Cl3 Cl 0.18303(12) 0.52835(12) 0.41219(10) 0.0616(8) Uani 1 1 d . . . Cl4 Cl 0.67388(15) -0.02606(17) 0.42269(14) 0.1118(15) Uani 1 1 d . . . Cl5 Cl 0.5865(2) 0.03011(18) 0.48362(14) 0.1192(14) Uani 1 1 d . . . Cl6 Cl 0.56994(13) 0.04698(15) 0.39078(12) 0.0856(10) Uani 1 1 d . . . Cl7 Cl 0.68250(11) 0.26018(12) 0.23156(8) 0.0546(7) Uani 1 1 d . . . Cl8 Cl 0.61436(11) 0.29523(12) 0.15300(8) 0.0512(7) Uani 1 1 d . . . Cl9 Cl 0.64832(16) 0.38515(14) 0.21624(10) 0.0800(9) Uani 1 1 d . . . C4S C 0.4286(10) 0.432(2) 0.2525(5) 0.28(4) Uiso 0.6 1 d PD A 1 H4S H 0.4154 0.3897 0.2548 0.34 Uiso 0.6 1 calc PR A 1 Cl10 Cl 0.4668(3) 0.4289(3) 0.2037(2) 0.118(2) Uiso 0.6 1 d PD A 1 Cl11 Cl 0.4715(4) 0.4375(4) 0.2987(3) 0.133(3) Uiso 0.6 1 d PD A 1 Cl12 Cl 0.3559(4) 0.4643(4) 0.2558(3) 0.137(3) Uiso 0.6 1 d PD A 1 C5S C 0.3459(7) 0.4513(12) 0.2346(7) 0.052(7) Uiso 0.4 1 d PD B 2 H5S H 0.3315 0.4156 0.2183 0.062 Uiso 0.4 1 calc PR B 2 Cl13 Cl 0.2830(4) 0.4548(4) 0.2663(3) 0.088(2) Uiso 0.4 1 d PD B 2 Cl14 Cl 0.3498(5) 0.4972(5) 0.1914(4) 0.126(4) Uiso 0.4 1 d PD B 2 Cl15 Cl 0.4175(4) 0.4203(4) 0.2523(3) 0.073(3) Uiso 0.4 1 d PD B 2 H1A H 0.169(5) 0.224(4) 0.416(3) 0.087 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(5) 0.033(5) 0.023(5) 0.007(4) -0.002(4) -0.011(4) C1S 0.052(6) 0.044(6) 0.048(7) -0.017(5) -0.002(5) 0.003(4) C2 0.027(5) 0.035(5) 0.024(5) 0.004(4) 0.000(4) 0.001(4) C2S 0.048(6) 0.041(7) 0.097(10) 0.014(6) -0.006(5) -0.006(5) C3 0.021(5) 0.038(6) 0.042(6) -0.012(4) 0.000(4) 0.010(4) C3S 0.042(6) 0.061(7) 0.037(6) -0.002(5) -0.005(4) -0.010(5) C4 0.035(5) 0.045(6) 0.024(5) 0.003(4) 0.006(4) 0.002(4) C5 0.019(5) 0.032(5) 0.032(5) -0.001(4) -0.004(4) 0.000(3) C6 0.017(4) 0.034(5) 0.032(5) 0.003(4) 0.001(3) 0.003(3) C7 0.038(5) 0.038(6) 0.020(5) -0.005(4) -0.004(4) 0.006(4) C8 0.026(5) 0.054(7) 0.039(6) -0.007(5) -0.001(4) 0.011(4) C9 0.030(5) 0.061(7) 0.048(7) -0.002(5) -0.016(4) 0.000(4) C10 0.049(7) 0.067(8) 0.044(7) -0.018(6) -0.010(5) 0.012(5) C11 0.046(6) 0.071(8) 0.029(6) -0.022(5) -0.010(5) 0.023(5) C12 0.034(5) 0.048(6) 0.027(6) -0.007(5) -0.002(4) 0.016(4) C13 0.049(6) 0.046(6) 0.025(6) 0.004(4) -0.002(4) 0.014(4) C14 0.031(6) 0.073(8) 0.055(7) 0.010(6) 0.018(5) 0.016(5) C15 0.032(6) 0.110(10) 0.046(8) 0.026(7) 0.018(5) 0.014(6) C16 0.025(6) 0.091(9) 0.079(10) 0.017(7) 0.008(6) 0.005(5) C17 0.026(5) 0.069(7) 0.041(6) 0.011(5) 0.009(4) -0.006(5) C18 0.026(5) 0.057(7) 0.034(6) 0.006(5) 0.005(4) 0.014(4) C19 0.032(5) 0.036(6) 0.019(5) 0.007(4) -0.006(4) -0.008(4) C20 0.032(5) 0.041(6) 0.028(5) 0.001(4) 0.000(4) -0.002(4) C21 0.039(5) 0.028(5) 0.033(5) 0.004(4) -0.002(4) -0.010(4) C22 0.035(5) 0.036(6) 0.018(5) 0.008(4) -0.001(3) 0.002(4) C23 0.032(5) 0.030(5) 0.025(5) -0.008(4) -0.002(4) -0.003(4) C24 0.033(5) 0.030(5) 0.027(5) -0.005(4) -0.006(4) 0.006(4) C25 0.020(5) 0.034(5) 0.042(6) -0.002(4) 0.006(4) -0.001(3) C26 0.044(6) 0.030(5) 0.035(6) -0.008(4) 0.003(4) -0.009(4) C27 0.063(6) 0.060(7) 0.015(5) -0.011(5) -0.006(4) -0.021(5) C28 0.047(6) 0.026(5) 0.030(6) -0.003(4) 0.000(4) 0.005(4) C29 0.054(6) 0.066(8) 0.036(7) 0.000(5) -0.004(5) -0.011(5) C30 0.021(5) 0.032(5) 0.034(6) -0.010(4) 0.002(4) -0.008(3) C31 0.021(4) 0.030(5) 0.028(5) -0.009(4) 0.002(4) 0.007(3) C32 0.036(5) 0.042(6) 0.011(5) 0.002(4) 0.011(4) -0.008(4) C33 0.020(4) 0.034(6) 0.028(5) -0.002(4) 0.002(3) 0.007(3) C34 0.030(5) 0.037(6) 0.023(5) 0.001(4) -0.003(4) 0.008(4) C35 0.035(5) 0.051(6) 0.017(5) 0.003(4) -0.005(3) 0.005(4) C36 0.025(4) 0.026(5) 0.022(5) 0.000(4) 0.001(3) -0.004(3) C37 0.033(5) 0.035(6) 0.028(5) 0.007(4) 0.005(4) -0.005(4) C38 0.036(5) 0.039(6) 0.024(5) -0.001(4) -0.003(4) 0.010(4) C39 0.043(6) 0.041(6) 0.032(6) -0.004(5) -0.003(4) 0.004(4) C40 0.059(7) 0.055(7) 0.027(6) -0.004(5) -0.008(4) 0.012(5) C41 0.064(7) 0.089(9) 0.026(6) -0.027(6) -0.011(5) 0.017(6) C42 0.041(6) 0.078(8) 0.054(8) -0.035(6) -0.028(5) 0.002(5) C43 0.032(5) 0.035(6) 0.052(7) -0.010(5) -0.013(4) 0.007(4) C44 0.028(5) 0.047(6) 0.051(7) -0.012(5) -0.009(4) 0.013(4) C45 0.043(6) 0.029(6) 0.099(10) -0.007(6) -0.010(6) -0.002(4) C46 0.031(6) 0.045(7) 0.119(12) 0.002(7) 0.000(7) 0.000(5) C47 0.047(7) 0.039(7) 0.083(9) 0.012(6) 0.008(6) 0.004(5) C48 0.030(5) 0.039(6) 0.057(7) 0.004(5) 0.000(4) 0.004(4) C49 0.031(5) 0.034(6) 0.030(6) -0.002(4) 0.001(4) 0.002(4) C50 0.020(4) 0.031(5) 0.020(5) 0.004(4) 0.003(3) 0.001(3) C51 0.038(5) 0.034(6) 0.026(5) -0.007(4) -0.001(4) 0.000(4) C52 0.036(5) 0.031(5) 0.029(5) -0.001(4) 0.004(4) 0.007(4) C53 0.026(5) 0.027(5) 0.027(5) 0.003(4) 0.001(4) -0.001(3) C54 0.016(4) 0.037(6) 0.042(6) 0.004(4) 0.005(4) 0.001(4) C55 0.019(5) 0.032(5) 0.024(5) -0.007(4) -0.004(3) 0.007(3) C56 0.028(5) 0.039(6) 0.021(5) -0.002(4) 0.000(4) 0.006(4) C57 0.033(5) 0.028(5) 0.036(6) 0.000(4) 0.004(4) 0.001(4) C58 0.051(6) 0.053(7) 0.032(6) -0.010(5) 0.001(4) -0.008(4) C59 0.053(6) 0.036(6) 0.014(5) 0.003(4) -0.007(4) 0.013(4) C60 0.048(6) 0.072(8) 0.032(6) 0.005(5) -0.011(4) -0.018(5) C61 0.028(5) 0.048(6) 0.021(5) 0.010(4) -0.002(4) 0.004(4) C62 0.037(5) 0.030(5) 0.023(5) 0.004(4) 0.005(4) 0.009(4) C63 0.027(5) 0.038(6) 0.028(5) 0.005(4) 0.003(4) 0.000(4) C64 0.045(6) 0.037(6) 0.037(6) 0.015(5) 0.006(4) -0.002(4) C65 0.027(5) 0.051(7) 0.041(6) -0.007(5) 0.018(4) -0.002(4) C66 0.030(5) 0.033(6) 0.049(6) -0.001(5) 0.009(4) 0.008(4) C67 0.036(5) 0.035(6) 0.038(6) 0.002(4) 0.001(4) 0.006(4) Co1 0.0273(6) 0.0346(7) 0.0269(7) 0.0002(5) 0.0034(5) 0.0013(5) Co2 0.0243(6) 0.0314(7) 0.0229(6) -0.0007(5) 0.0017(5) 0.0007(5) N1 0.024(4) 0.037(4) 0.024(4) 0.008(3) 0.000(3) 0.001(3) N2 0.023(4) 0.037(5) 0.031(5) 0.001(3) 0.006(3) -0.002(3) N3 0.029(4) 0.025(4) 0.031(5) 0.002(3) 0.005(3) -0.001(3) N4 0.026(4) 0.032(4) 0.032(5) 0.001(3) 0.000(3) -0.007(3) N5 0.028(4) 0.029(4) 0.017(4) -0.004(3) 0.007(3) -0.001(3) N6 0.023(4) 0.030(4) 0.025(4) 0.002(3) 0.009(3) -0.001(3) N7 0.027(4) 0.028(4) 0.018(4) 0.002(3) 0.000(3) 0.004(3) N8 0.025(4) 0.030(4) 0.025(4) -0.002(3) 0.004(3) 0.004(3) N9 0.032(4) 0.032(4) 0.025(4) 0.006(3) 0.002(3) -0.008(3) O1 0.033(3) 0.031(4) 0.024(4) 0.002(3) 0.006(2) -0.001(2) Cl1 0.085(2) 0.061(2) 0.0541(19) 0.0068(15) -0.0155(14) -0.0037(14) Cl2 0.0780(19) 0.0514(19) 0.079(2) 0.0096(16) -0.0101(15) -0.0110(14) Cl3 0.0499(16) 0.0576(19) 0.077(2) 0.0018(15) -0.0125(13) 0.0023(12) Cl4 0.075(2) 0.102(3) 0.158(4) 0.057(3) 0.036(2) 0.0446(19) Cl5 0.174(4) 0.079(3) 0.104(3) 0.016(2) 0.022(3) 0.033(2) Cl6 0.0608(19) 0.089(3) 0.107(3) 0.000(2) -0.0174(17) 0.0056(15) Cl7 0.0593(16) 0.0595(18) 0.0450(17) -0.0053(13) -0.0068(11) 0.0119(12) Cl8 0.0483(15) 0.0693(19) 0.0362(15) -0.0008(13) -0.0064(11) -0.0102(12) Cl9 0.136(3) 0.053(2) 0.050(2) -0.0040(15) -0.0259(18) 0.0086(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.318(10) . ? C1 C2 1.387(11) . ? C1 H1 0.93 . ? C1S Cl3 1.733(9) . ? C1S Cl2 1.758(10) . ? C1S Cl1 1.763(10) . ? C1S H1S 0.98 . ? C2 N2 1.387(10) . ? C2 C3 1.417(10) . ? C2S Cl4 1.735(11) . ? C2S Cl6 1.735(11) . ? C2S Cl5 1.756(12) . ? C2S H2S 0.98 . ? C3 C4 1.387(11) . ? C3 H3 0.93 . ? C3S Cl9 1.724(10) . ? C3S Cl7 1.740(10) . ? C3S Cl8 1.769(9) . ? C3S H3S 0.98 . ? C4 C5 1.416(11) . ? C4 H4 0.93 . ? C5 N2 1.328(10) . ? C5 C6 1.524(11) . ? C6 C19 1.516(11) . ? C6 C18 1.529(11) . ? C6 C7 1.549(11) . ? C7 C8 1.391(12) . ? C7 C12 1.397(11) . ? C8 C9 1.395(12) . ? C8 H8 0.93 . ? C9 C10 1.405(13) . ? C9 H9 0.93 . ? C10 C11 1.393(13) . ? C10 H10 0.93 . ? C11 C12 1.369(12) . ? C11 H11 0.93 . ? C12 C13 1.505(12) . ? C13 C14 1.375(12) . ? C13 C18 1.377(12) . ? C14 C15 1.342(14) . ? C14 H14 0.93 . ? C15 C16 1.381(15) . ? C15 H15 0.93 . ? C16 C17 1.401(13) . ? C16 H16 0.93 . ? C17 C18 1.399(12) . ? C17 H17 0.93 . ? C19 N3 1.346(10) . ? C19 C20 1.399(11) . ? C20 C21 1.380(11) . ? C20 H20 0.93 . ? C21 C22 1.406(11) . ? C21 H21 0.93 . ? C22 N3 1.379(10) . ? C22 C23 1.423(11) . ? C23 N4 1.303(10) . ? C23 H23 0.93 . ? C24 C31 1.394(11) . ? C24 C25 1.394(11) . ? C24 N4 1.411(10) . ? C25 C26 1.385(12) . ? C25 H25 0.93 . ? C26 C28 1.412(11) . ? C26 C27 1.519(11) . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 C30 1.394(11) . ? C28 C29 1.518(12) . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? C30 C31 1.387(11) . ? C30 H30 0.93 . ? C31 N5 1.421(10) . ? C32 N5 1.307(10) . ? C32 C33 1.434(11) . ? C32 H32 0.93 . ? C33 N6 1.355(10) . ? C33 C34 1.420(10) . ? C34 C35 1.390(11) . ? C34 H34 0.93 . ? C35 C36 1.421(11) . ? C35 H35 0.93 . ? C36 N6 1.337(9) . ? C36 C37 1.524(11) . ? C37 C38 1.509(11) . ? C37 C50 1.523(11) . ? C37 C49 1.548(11) . ? C38 C39 1.402(11) . ? C38 C43 1.409(12) . ? C39 C40 1.369(12) . ? C39 H39 0.93 . ? C40 C41 1.405(13) . ? C40 H40 0.93 . ? C41 C42 1.356(14) . ? C41 H41 0.93 . ? C42 C43 1.399(13) . ? C42 H42 0.93 . ? C43 C44 1.460(13) . ? C44 C49 1.392(12) . ? C44 C45 1.416(13) . ? C45 C46 1.373(15) . ? C45 H45 0.93 . ? C46 C47 1.379(15) . ? C46 H46 0.93 . ? C47 C48 1.399(13) . ? C47 H47 0.93 . ? C48 C49 1.357(12) . ? C48 H48 0.93 . ? C50 N7 1.335(9) . ? C50 C51 1.434(11) . ? C51 C52 1.396(11) . ? C51 H51 0.93 . ? C52 C53 1.391(11) . ? C52 H52 0.93 . ? C53 N7 1.387(9) . ? C53 C54 1.404(11) . ? C54 N8 1.317(10) . ? C54 H54 0.93 . ? C55 C56 1.381(11) . ? C55 C62 1.388(10) . ? C55 N8 1.413(10) . ? C56 C57 1.406(11) . ? C56 H56 0.93 . ? C57 C59 1.399(11) . ? C57 C58 1.501(11) . ? C58 H58A 0.96 . ? C58 H58B 0.96 . ? C58 H58C 0.96 . ? C59 C61 1.374(11) . ? C59 C60 1.548(11) . ? C60 H60A 0.96 . ? C60 H60B 0.96 . ? C60 H60C 0.96 . ? C61 C62 1.411(11) . ? C61 H61 0.93 . ? C62 N1 1.423(10) . ? C63 N9 1.347(10) . ? C63 C64 1.366(11) . ? C63 H63 0.93 . ? C64 C65 1.373(11) . ? C64 H64 0.93 . ? C65 C66 1.397(12) . ? C65 H65 0.93 . ? C66 C67 1.367(11) . ? C66 H66 0.93 . ? C67 N9 1.358(10) . ? C67 H67 0.93 . ? Co1 O1 1.987(5) . ? Co1 N2 2.010(6) . ? Co1 N3 2.037(7) . ? Co1 N4 2.115(7) . ? Co1 N1 2.150(6) . ? Co2 N7 1.855(6) . ? Co2 N6 1.878(6) . ? Co2 O1 1.916(5) . ? Co2 N9 1.971(6) . ? Co2 N8 2.000(6) . ? Co2 N5 2.002(6) . ? O1 H1A 0.82(2) . ? C4S Cl12 1.663(15) . ? C4S Cl11 1.672(15) . ? C4S Cl10 1.690(14) . ? C4S H4S 0.98 . ? C5S Cl13 1.622(12) . ? C5S Cl14 1.670(13) . ? C5S Cl15 1.715(12) . ? C5S H5S 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.9(7) . . ? N1 C1 H1 120.5 . . ? C2 C1 H1 120.5 . . ? Cl3 C1S Cl2 111.7(5) . . ? Cl3 C1S Cl1 111.1(5) . . ? Cl2 C1S Cl1 109.6(5) . . ? Cl3 C1S H1S 108.1 . . ? Cl2 C1S H1S 108.1 . . ? Cl1 C1S H1S 108.1 . . ? C1 C2 N2 116.0(7) . . ? C1 C2 C3 136.5(8) . . ? N2 C2 C3 107.4(7) . . ? Cl4 C2S Cl6 110.7(7) . . ? Cl4 C2S Cl5 110.9(6) . . ? Cl6 C2S Cl5 111.6(5) . . ? Cl4 C2S H2S 107.8 . . ? Cl6 C2S H2S 107.8 . . ? Cl5 C2S H2S 107.8 . . ? C4 C3 C2 107.6(7) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Cl9 C3S Cl7 112.9(5) . . ? Cl9 C3S Cl8 110.0(5) . . ? Cl7 C3S Cl8 111.0(5) . . ? Cl9 C3S H3S 107.6 . . ? Cl7 C3S H3S 107.6 . . ? Cl8 C3S H3S 107.6 . . ? C3 C4 C5 106.1(7) . . ? C3 C4 H4 126.9 . . ? C5 C4 H4 126.9 . . ? N2 C5 C4 110.2(7) . . ? N2 C5 C6 120.6(7) . . ? C4 C5 C6 129.2(7) . . ? C19 C6 C5 110.7(7) . . ? C19 C6 C18 109.8(7) . . ? C5 C6 C18 114.1(6) . . ? C19 C6 C7 112.4(6) . . ? C5 C6 C7 109.8(7) . . ? C18 C6 C7 99.7(7) . . ? C8 C7 C12 119.6(8) . . ? C8 C7 C6 128.5(7) . . ? C12 C7 C6 111.9(7) . . ? C7 C8 C9 118.7(9) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C8 C9 C10 120.3(9) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 120.7(9) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 117.9(9) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C7 122.6(9) . . ? C11 C12 C13 130.1(9) . . ? C7 C12 C13 107.2(7) . . ? C14 C13 C18 120.9(9) . . ? C14 C13 C12 130.8(9) . . ? C18 C13 C12 108.3(8) . . ? C15 C14 C13 120.1(10) . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C14 C15 C16 121.2(9) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C17 119.7(10) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 118.6(10) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C13 C18 C17 119.5(8) . . ? C13 C18 C6 112.7(8) . . ? C17 C18 C6 127.8(8) . . ? N3 C19 C20 108.5(7) . . ? N3 C19 C6 120.0(7) . . ? C20 C19 C6 131.4(7) . . ? C21 C20 C19 108.6(8) . . ? C21 C20 H20 125.7 . . ? C19 C20 H20 125.7 . . ? C20 C21 C22 105.7(8) . . ? C20 C21 H21 127.1 . . ? C22 C21 H21 127.1 . . ? N3 C22 C21 109.0(7) . . ? N3 C22 C23 114.0(7) . . ? C21 C22 C23 135.1(8) . . ? N4 C23 C22 119.1(8) . . ? N4 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C31 C24 C25 118.3(8) . . ? C31 C24 N4 121.2(7) . . ? C25 C24 N4 119.9(7) . . ? C26 C25 C24 123.0(8) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C25 C26 C28 118.5(8) . . ? C25 C26 C27 122.2(7) . . ? C28 C26 C27 119.2(8) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C26 118.5(8) . . ? C30 C28 C29 120.7(8) . . ? C26 C28 C29 120.8(8) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C28 122.2(7) . . ? C31 C30 H30 118.9 . . ? C28 C30 H30 118.9 . . ? C30 C31 C24 119.5(7) . . ? C30 C31 N5 120.6(7) . . ? C24 C31 N5 119.7(7) . . ? N5 C32 C33 115.2(8) . . ? N5 C32 H32 122.4 . . ? C33 C32 H32 122.4 . . ? N6 C33 C34 108.7(7) . . ? N6 C33 C32 114.8(7) . . ? C34 C33 C32 136.5(8) . . ? C35 C34 C33 105.5(7) . . ? C35 C34 H34 127.3 . . ? C33 C34 H34 127.3 . . ? C34 C35 C36 108.0(7) . . ? C34 C35 H35 126 . . ? C36 C35 H35 126 . . ? N6 C36 C35 107.6(7) . . ? N6 C36 C37 124.2(7) . . ? C35 C36 C37 128.0(7) . . ? C38 C37 C50 111.2(6) . . ? C38 C37 C36 113.0(7) . . ? C50 C37 C36 111.3(7) . . ? C38 C37 C49 101.6(7) . . ? C50 C37 C49 108.0(6) . . ? C36 C37 C49 111.3(6) . . ? C39 C38 C43 120.8(8) . . ? C39 C38 C37 128.1(8) . . ? C43 C38 C37 111.0(8) . . ? C40 C39 C38 118.8(9) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C39 C40 C41 120.8(9) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 120.4(9) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.8(9) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C42 C43 C38 118.3(9) . . ? C42 C43 C44 133.7(9) . . ? C38 C43 C44 107.9(8) . . ? C49 C44 C45 120.5(10) . . ? C49 C44 C43 110.0(8) . . ? C45 C44 C43 129.4(9) . . ? C46 C45 C44 116.5(10) . . ? C46 C45 H45 121.7 . . ? C44 C45 H45 121.7 . . ? C45 C46 C47 123.1(10) . . ? C45 C46 H46 118.4 . . ? C47 C46 H46 118.4 . . ? C46 C47 C48 119.3(10) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C49 C48 C47 119.3(10) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C48 C49 C44 121.1(8) . . ? C48 C49 C37 129.5(8) . . ? C44 C49 C37 109.4(8) . . ? N7 C50 C51 108.0(6) . . ? N7 C50 C37 125.2(7) . . ? C51 C50 C37 126.8(7) . . ? C52 C51 C50 107.4(7) . . ? C52 C51 H51 126.3 . . ? C50 C51 H51 126.3 . . ? C53 C52 C51 106.4(7) . . ? C53 C52 H52 126.8 . . ? C51 C52 H52 126.8 . . ? N7 C53 C52 109.2(7) . . ? N7 C53 C54 111.8(7) . . ? C52 C53 C54 138.9(8) . . ? N8 C54 C53 119.4(7) . . ? N8 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C56 C55 C62 119.1(7) . . ? C56 C55 N8 119.5(7) . . ? C62 C55 N8 121.3(7) . . ? C55 C56 C57 122.6(7) . . ? C55 C56 H56 118.7 . . ? C57 C56 H56 118.7 . . ? C59 C57 C56 117.4(8) . . ? C59 C57 C58 122.3(8) . . ? C56 C57 C58 120.3(7) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C61 C59 C57 120.6(8) . . ? C61 C59 C60 120.1(8) . . ? C57 C59 C60 119.2(8) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 C62 121.0(8) . . ? C59 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C55 C62 C61 119.2(7) . . ? C55 C62 N1 118.4(7) . . ? C61 C62 N1 122.4(7) . . ? N9 C63 C64 123.7(8) . . ? N9 C63 H63 118.1 . . ? C64 C63 H63 118.1 . . ? C63 C64 C65 119.1(8) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C64 C65 C66 118.5(7) . . ? C64 C65 H65 120.8 . . ? C66 C65 H65 120.8 . . ? C67 C66 C65 119.3(7) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? N9 C67 C66 122.5(8) . . ? N9 C67 H67 118.8 . . ? C66 C67 H67 118.8 . . ? O1 Co1 N2 127.2(3) . . ? O1 Co1 N3 99.1(2) . . ? N2 Co1 N3 81.5(3) . . ? O1 Co1 N4 92.4(2) . . ? N2 Co1 N4 138.0(2) . . ? N3 Co1 N4 78.3(3) . . ? O1 Co1 N1 109.3(2) . . ? N2 Co1 N1 78.5(3) . . ? N3 Co1 N1 151.3(2) . . ? N4 Co1 N1 103.5(3) . . ? N7 Co2 N6 87.7(3) . . ? N7 Co2 O1 86.9(3) . . ? N6 Co2 O1 90.8(2) . . ? N7 Co2 N9 91.5(3) . . ? N6 Co2 N9 91.0(3) . . ? O1 Co2 N9 177.5(3) . . ? N7 Co2 N8 83.4(3) . . ? N6 Co2 N8 170.8(3) . . ? O1 Co2 N8 86.2(2) . . ? N9 Co2 N8 91.7(3) . . ? N7 Co2 N5 169.3(3) . . ? N6 Co2 N5 82.6(3) . . ? O1 Co2 N5 88.6(2) . . ? N9 Co2 N5 93.3(3) . . ? N8 Co2 N5 106.0(3) . . ? C1 N1 C62 120.2(7) . . ? C1 N1 Co1 111.2(5) . . ? C62 N1 Co1 128.5(5) . . ? C5 N2 C2 108.7(6) . . ? C5 N2 Co1 135.5(6) . . ? C2 N2 Co1 114.7(5) . . ? C19 N3 C22 108.1(7) . . ? C19 N3 Co1 134.8(6) . . ? C22 N3 Co1 115.3(5) . . ? C23 N4 C24 123.7(7) . . ? C23 N4 Co1 112.8(6) . . ? C24 N4 Co1 123.1(5) . . ? C32 N5 C31 118.7(7) . . ? C32 N5 Co2 112.2(5) . . ? C31 N5 Co2 128.8(5) . . ? C36 N6 C33 110.2(6) . . ? C36 N6 Co2 134.9(6) . . ? C33 N6 Co2 114.8(5) . . ? C50 N7 C53 109.1(6) . . ? C50 N7 Co2 133.5(5) . . ? C53 N7 Co2 114.8(5) . . ? C54 N8 C55 119.0(7) . . ? C54 N8 Co2 108.8(5) . . ? C55 N8 Co2 132.1(5) . . ? C63 N9 C67 116.9(7) . . ? C63 N9 Co2 120.8(5) . . ? C67 N9 Co2 122.2(6) . . ? Co2 O1 Co1 129.5(3) . . ? Co2 O1 H1A 113(8) . . ? Co1 O1 H1A 102(8) . . ? Cl12 C4S Cl11 113.2(12) . . ? Cl12 C4S Cl10 119.5(14) . . ? Cl11 C4S Cl10 120.4(14) . . ? Cl12 C4S H4S 98.8 . . ? Cl11 C4S H4S 98.8 . . ? Cl10 C4S H4S 98.8 . . ? Cl13 C5S Cl14 119.0(10) . . ? Cl13 C5S Cl15 121.2(10) . . ? Cl14 C5S Cl15 116.9(9) . . ? Cl13 C5S H5S 95.7 . . ? Cl14 C5S H5S 95.7 . . ? Cl15 C5S H5S 95.7 . . ?