# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a data_1 #TrackingRef '15833_web_deposit_cif_file_0_AndrewBond_1354442523.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H42 Co2 N6 O5 2+, 2(B F4 -), H2 O' _chemical_formula_sum 'C38 H44 B2 Co2 F8 N6 O6' _chemical_formula_weight 972.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0799(2) _cell_length_b 21.2024(4) _cell_length_c 15.9892(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.633(1) _cell_angle_gamma 90.00 _cell_volume 4093.54(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5675 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 25.99 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.828517 ; _exptl_special_details ; H atoms of water molecule located in difference Fourier and refined with O---H distances restrained to a common refined value with s.u. of 0.02 \%A. Max residual density in the region of one BF4^-^ anion. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 23478 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 26.67 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.67 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 8586 _reflns_number_gt 6563 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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^)+(0.0504P)^2^+1.9158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8586 _refine_ls_number_parameters 567 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.708 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.067 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 0.55061(3) 0.698993(15) 0.38630(2) 0.01943(9) Uani 1 1 d . . . Co2 Co 0.45523(2) 0.771174(15) 0.227388(19) 0.01792(9) Uani 1 1 d . . . O1 O 0.44479(13) 0.75752(8) 0.34369(9) 0.0190(3) Uani 1 1 d . . . O2 O 0.63409(13) 0.70902(8) 0.29094(10) 0.0226(4) Uani 1 1 d . . . O3 O 0.60727(13) 0.76605(8) 0.24802(11) 0.0234(4) Uani 1 1 d . . . O4 O 0.47229(13) 0.63356(8) 0.32714(10) 0.0219(4) Uani 1 1 d . . . O5 O 0.43520(13) 0.68322(8) 0.20397(10) 0.0215(4) Uani 1 1 d . . . N1 N 0.46146(17) 0.68500(9) 0.48859(12) 0.0217(4) Uani 1 1 d . . . N2 N 0.62593(16) 0.76335(10) 0.45138(13) 0.0224(4) Uani 1 1 d . . . N3 N 0.64010(17) 0.63191(10) 0.43209(13) 0.0247(5) Uani 1 1 d . . . N4 N 0.46372(15) 0.86345(9) 0.23373(12) 0.0190(4) Uani 1 1 d . . . N5 N 0.29172(16) 0.78603(9) 0.22523(12) 0.0191(4) Uani 1 1 d . . . N6 N 0.48047(17) 0.78668(10) 0.11147(13) 0.0233(5) Uani 1 1 d . . . C1 C 0.39927(19) 0.79997(11) 0.39641(15) 0.0195(5) Uani 1 1 d . . . C2 C 0.34175(19) 0.77670(12) 0.46376(15) 0.0219(5) Uani 1 1 d . . . C3 C 0.2956(2) 0.81889(12) 0.51929(16) 0.0248(5) Uani 1 1 d . . . H3A H 0.2565 0.8031 0.5656 0.030 Uiso 1 1 calc R . . C4 C 0.3054(2) 0.88391(12) 0.50868(16) 0.0255(6) Uani 1 1 d . . . C5 C 0.3646(2) 0.90531(12) 0.44023(16) 0.0244(5) Uani 1 1 d . . . H5A H 0.3715 0.9494 0.4316 0.029 Uiso 1 1 calc R . . C6 C 0.41347(19) 0.86453(12) 0.38461(15) 0.0209(5) Uani 1 1 d . . . C7 C 0.2552(2) 0.93146(13) 0.56923(18) 0.0323(6) Uani 1 1 d . . . C8 C 0.1615(3) 0.96698(16) 0.5246(2) 0.0504(9) Uani 1 1 d . . . H8A H 0.1897 0.9879 0.4749 0.076 Uiso 1 1 calc R . . H8B H 0.1316 0.9987 0.5624 0.076 Uiso 1 1 calc R . . H8C H 0.1028 0.9373 0.5079 0.076 Uiso 1 1 calc R . . C9 C 0.3454(3) 0.97811(14) 0.59926(19) 0.0398(7) Uani 1 1 d . . . H9A H 0.3755 1.0000 0.5509 0.060 Uiso 1 1 calc R . . H9B H 0.4050 0.9551 0.6288 0.060 Uiso 1 1 calc R . . H9C H 0.3133 1.0090 0.6372 0.060 Uiso 1 1 calc R . . C10 C 0.2108(3) 0.89905(15) 0.6474(2) 0.0495(9) Uani 1 1 d . . . H10A H 0.1530 0.8688 0.6307 0.074 Uiso 1 1 calc R . . H10B H 0.1798 0.9309 0.6845 0.074 Uiso 1 1 calc R . . H10C H 0.2714 0.8768 0.6769 0.074 Uiso 1 1 calc R . . C11 C 0.3434(2) 0.70633(12) 0.47710(16) 0.0237(5) Uani 1 1 d . . . H11A H 0.3011 0.6954 0.5272 0.028 Uiso 1 1 calc R . . H11B H 0.3084 0.6848 0.4282 0.028 Uiso 1 1 calc R . . C12 C 0.5154(2) 0.72004(12) 0.56002(15) 0.0255(6) Uani 1 1 d . . . H12A H 0.4579 0.7370 0.5967 0.031 Uiso 1 1 calc R . . H12B H 0.5628 0.6908 0.5935 0.031 Uiso 1 1 calc R . . C13 C 0.5842(2) 0.77301(12) 0.52829(15) 0.0235(5) Uani 1 1 d . . . C14 C 0.6098(2) 0.82681(13) 0.57396(17) 0.0310(6) Uani 1 1 d . . . H14A H 0.5761 0.8344 0.6260 0.037 Uiso 1 1 calc R . . C15 C 0.6849(2) 0.86927(13) 0.54268(18) 0.0351(7) Uani 1 1 d . . . H15A H 0.7037 0.9064 0.5731 0.042 Uiso 1 1 calc R . . C16 C 0.7324(2) 0.85724(13) 0.46692(17) 0.0325(6) Uani 1 1 d . . . H16A H 0.7866 0.8850 0.4457 0.039 Uiso 1 1 calc R . . C17 C 0.7003(2) 0.80443(12) 0.42237(17) 0.0266(6) Uani 1 1 d . . . H17A H 0.7317 0.7968 0.3695 0.032 Uiso 1 1 calc R . . C18 C 0.4693(2) 0.61602(12) 0.50351(16) 0.0267(6) Uani 1 1 d . . . H18A H 0.4184 0.5932 0.4646 0.032 Uiso 1 1 calc R . . H18B H 0.4489 0.6060 0.5616 0.032 Uiso 1 1 calc R . . C19 C 0.5873(2) 0.59674(12) 0.48921(16) 0.0272(6) Uani 1 1 d . . . C20 C 0.6394(3) 0.54696(13) 0.52913(17) 0.0350(7) Uani 1 1 d . . . H20A H 0.6026 0.5234 0.5706 0.042 Uiso 1 1 calc R . . C21 C 0.7467(3) 0.53175(14) 0.50771(19) 0.0392(7) Uani 1 1 d . . . H21A H 0.7845 0.4978 0.5349 0.047 Uiso 1 1 calc R . . C22 C 0.7981(2) 0.56617(14) 0.44674(19) 0.0377(7) Uani 1 1 d . . . H22A H 0.8703 0.5552 0.4297 0.045 Uiso 1 1 calc R . . C23 C 0.7431(2) 0.61668(13) 0.41096(18) 0.0314(6) Uani 1 1 d . . . H23A H 0.7792 0.6413 0.3703 0.038 Uiso 1 1 calc R . . C24 C 0.4916(2) 0.88773(12) 0.31913(15) 0.0215(5) Uani 1 1 d . . . H24A H 0.4898 0.9344 0.3180 0.026 Uiso 1 1 calc R . . H24B H 0.5679 0.8746 0.3351 0.026 Uiso 1 1 calc R . . C25 C 0.35553(19) 0.89061(12) 0.20315(15) 0.0221(5) Uani 1 1 d . . . H25A H 0.3444 0.9326 0.2286 0.026 Uiso 1 1 calc R . . H25B H 0.3557 0.8957 0.1416 0.026 Uiso 1 1 calc R . . C26 C 0.26398(19) 0.84730(11) 0.22661(14) 0.0201(5) Uani 1 1 d . . . C27 C 0.1599(2) 0.86817(13) 0.24715(16) 0.0251(5) Uani 1 1 d . . . H27A H 0.1430 0.9119 0.2479 0.030 Uiso 1 1 calc R . . C28 C 0.0806(2) 0.82363(13) 0.26669(16) 0.0270(6) Uani 1 1 d . . . H28A H 0.0084 0.8364 0.2816 0.032 Uiso 1 1 calc R . . C29 C 0.1079(2) 0.76049(13) 0.26423(15) 0.0251(6) Uani 1 1 d . . . H29A H 0.0541 0.7293 0.2759 0.030 Uiso 1 1 calc R . . C30 C 0.21453(19) 0.74307(12) 0.24454(14) 0.0213(5) Uani 1 1 d . . . H30A H 0.2337 0.6996 0.2447 0.026 Uiso 1 1 calc R . . C31 C 0.5520(2) 0.88096(12) 0.17426(15) 0.0240(5) Uani 1 1 d . . . H31A H 0.6262 0.8720 0.1994 0.029 Uiso 1 1 calc R . . H31B H 0.5477 0.9264 0.1605 0.029 Uiso 1 1 calc R . . C32 C 0.5324(2) 0.84203(12) 0.09720(16) 0.0240(5) Uani 1 1 d . . . C33 C 0.5620(2) 0.85918(14) 0.01796(17) 0.0364(7) Uani 1 1 d . . . H33A H 0.5981 0.8982 0.0086 0.044 Uiso 1 1 calc R . . C34 C 0.5385(3) 0.81893(16) -0.04756(19) 0.0462(8) Uani 1 1 d . . . H34A H 0.5592 0.8297 -0.1026 0.055 Uiso 1 1 calc R . . C35 C 0.4844(3) 0.76278(15) -0.03271(18) 0.0421(8) Uani 1 1 d . . . H35A H 0.4667 0.7348 -0.0775 0.050 Uiso 1 1 calc R . . C36 C 0.4567(2) 0.74801(14) 0.04772(16) 0.0302(6) Uani 1 1 d . . . H36A H 0.4196 0.7094 0.0581 0.036 Uiso 1 1 calc R . . C37 C 0.44367(18) 0.63479(12) 0.25032(15) 0.0213(5) Uani 1 1 d . . . C38 C 0.4143(2) 0.57278(12) 0.21063(17) 0.0294(6) Uani 1 1 d . . . H38A H 0.4238 0.5390 0.2520 0.044 Uiso 1 1 calc R . . H38B H 0.4628 0.5650 0.1636 0.044 Uiso 1 1 calc R . . H38C H 0.3370 0.5738 0.1902 0.044 Uiso 1 1 calc R . . F1D F 0.55260(15) 0.97183(9) 0.84694(12) 0.0507(5) Uani 1 1 d . . . F1C F 0.63501(17) 0.96635(9) 0.72121(11) 0.0525(5) Uani 1 1 d . . . F1B F 0.69360(16) 0.90501(11) 0.83093(13) 0.0674(6) Uani 1 1 d . . . F1A F 0.5303(2) 0.88518(9) 0.76609(13) 0.0718(7) Uani 1 1 d . . . B1 B 0.6026(3) 0.93256(16) 0.7912(2) 0.0373(8) Uani 1 1 d . . . F2D F 0.76148(16) 0.97147(10) 0.20283(14) 0.0643(6) Uani 1 1 d . . . F2C F 0.82194(16) 0.87366(10) 0.16819(13) 0.0606(6) Uani 1 1 d . . . F2B F 0.94421(15) 0.95167(10) 0.19146(13) 0.0612(6) Uani 1 1 d . . . F2A F 0.8494(2) 0.91137(12) 0.29775(13) 0.0870(8) Uani 1 1 d . . . B2 B 0.8433(3) 0.92857(18) 0.2151(2) 0.0389(8) Uani 1 1 d . . . O1W O 0.35096(18) 0.75044(13) 0.7373(2) 0.0622(7) Uani 1 1 d D . . H1W H 0.337(2) 0.7151(9) 0.7137(19) 0.043(10) Uiso 1 1 d D . . H2W H 0.2884(15) 0.7675(14) 0.746(2) 0.077(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02138(17) 0.01749(18) 0.01940(17) -0.00027(14) 0.00019(12) 0.00104(13) Co2 0.01810(16) 0.01688(18) 0.01875(17) 0.00079(13) 0.00009(12) -0.00075(13) O1 0.0231(8) 0.0168(9) 0.0171(8) 0.0011(7) -0.0004(6) 0.0030(7) O2 0.0226(8) 0.0208(9) 0.0245(9) 0.0021(7) 0.0015(7) 0.0040(7) O3 0.0209(8) 0.0215(9) 0.0278(9) 0.0062(8) -0.0002(7) -0.0007(7) O4 0.0252(9) 0.0173(9) 0.0232(9) -0.0001(7) -0.0002(7) -0.0005(7) O5 0.0225(8) 0.0189(9) 0.0232(9) -0.0018(7) -0.0002(7) -0.0008(7) N1 0.0273(11) 0.0175(11) 0.0202(10) 0.0019(9) 0.0007(8) 0.0020(8) N2 0.0228(10) 0.0214(11) 0.0228(11) -0.0011(9) -0.0033(8) 0.0026(8) N3 0.0280(11) 0.0198(11) 0.0261(11) -0.0022(9) -0.0034(9) 0.0033(9) N4 0.0189(10) 0.0176(10) 0.0205(10) 0.0028(8) -0.0004(8) -0.0005(8) N5 0.0198(10) 0.0213(11) 0.0160(10) 0.0004(8) -0.0030(8) -0.0010(8) N6 0.0229(10) 0.0246(12) 0.0224(11) 0.0022(9) 0.0005(8) -0.0004(9) C1 0.0190(11) 0.0196(13) 0.0198(12) -0.0021(10) -0.0019(9) 0.0027(10) C2 0.0211(12) 0.0214(13) 0.0232(12) 0.0007(10) -0.0008(9) -0.0003(10) C3 0.0227(12) 0.0254(14) 0.0266(13) -0.0005(11) 0.0043(10) 0.0008(10) C4 0.0243(12) 0.0241(14) 0.0284(13) -0.0031(11) 0.0028(10) 0.0027(10) C5 0.0263(13) 0.0165(13) 0.0301(14) -0.0021(11) -0.0029(10) 0.0009(10) C6 0.0205(12) 0.0213(13) 0.0207(12) -0.0001(10) -0.0033(9) -0.0006(10) C7 0.0364(15) 0.0230(14) 0.0381(16) -0.0055(12) 0.0130(12) 0.0019(12) C8 0.0423(18) 0.0393(19) 0.070(2) -0.0156(17) 0.0047(16) 0.0125(15) C9 0.0482(18) 0.0321(16) 0.0398(17) -0.0128(14) 0.0104(14) -0.0016(14) C10 0.068(2) 0.0321(18) 0.050(2) -0.0108(16) 0.0327(17) -0.0002(16) C11 0.0234(12) 0.0207(13) 0.0273(13) 0.0023(11) 0.0049(10) -0.0004(10) C12 0.0333(14) 0.0249(14) 0.0183(12) 0.0009(11) -0.0009(10) 0.0050(11) C13 0.0292(13) 0.0217(13) 0.0191(12) 0.0002(10) -0.0059(10) 0.0068(11) C14 0.0425(16) 0.0285(15) 0.0215(13) -0.0024(12) -0.0079(11) 0.0061(12) C15 0.0479(17) 0.0241(15) 0.0325(15) -0.0032(12) -0.0144(13) -0.0027(13) C16 0.0330(14) 0.0289(15) 0.0348(15) 0.0025(13) -0.0096(12) -0.0036(12) C17 0.0237(13) 0.0271(15) 0.0288(14) 0.0022(12) -0.0044(10) 0.0013(11) C18 0.0349(14) 0.0200(13) 0.0254(13) 0.0047(11) 0.0050(11) 0.0027(11) C19 0.0378(15) 0.0196(14) 0.0240(13) -0.0019(11) -0.0039(11) 0.0040(11) C20 0.0532(18) 0.0208(15) 0.0306(15) 0.0000(12) -0.0051(13) 0.0036(13) C21 0.0495(18) 0.0266(16) 0.0406(17) -0.0043(14) -0.0147(14) 0.0159(14) C22 0.0327(15) 0.0341(17) 0.0457(18) -0.0076(14) -0.0087(13) 0.0128(13) C23 0.0275(14) 0.0316(16) 0.0349(15) -0.0055(12) -0.0047(11) 0.0029(12) C24 0.0261(12) 0.0161(13) 0.0224(12) -0.0022(10) -0.0011(10) -0.0024(10) C25 0.0224(12) 0.0199(13) 0.0239(12) 0.0053(10) -0.0001(10) 0.0009(10) C26 0.0240(12) 0.0200(13) 0.0162(11) 0.0029(10) -0.0047(9) -0.0012(10) C27 0.0246(13) 0.0231(14) 0.0275(13) 0.0007(11) 0.0000(10) 0.0028(10) C28 0.0223(12) 0.0325(15) 0.0262(13) 0.0010(12) 0.0024(10) 0.0029(11) C29 0.0255(13) 0.0279(15) 0.0220(13) 0.0046(11) 0.0008(10) -0.0038(11) C30 0.0245(12) 0.0199(13) 0.0192(12) 0.0014(10) -0.0024(10) -0.0036(10) C31 0.0233(12) 0.0232(13) 0.0257(13) 0.0059(11) 0.0034(10) -0.0045(10) C32 0.0219(12) 0.0231(13) 0.0274(13) 0.0030(11) 0.0046(10) -0.0001(10) C33 0.0449(17) 0.0335(17) 0.0316(15) 0.0033(13) 0.0132(13) -0.0070(13) C34 0.066(2) 0.047(2) 0.0273(15) 0.0020(14) 0.0177(15) -0.0086(17) C35 0.058(2) 0.0427(19) 0.0256(15) -0.0058(14) 0.0098(14) -0.0082(15) C36 0.0349(15) 0.0303(15) 0.0255(14) -0.0035(12) 0.0020(11) -0.0053(12) C37 0.0162(11) 0.0206(13) 0.0271(13) -0.0027(11) 0.0018(10) 0.0017(9) C38 0.0351(14) 0.0211(14) 0.0317(15) -0.0032(11) -0.0029(11) -0.0001(11) F1D 0.0577(12) 0.0356(10) 0.0599(12) -0.0075(9) 0.0233(9) 0.0030(9) F1C 0.0805(14) 0.0346(10) 0.0431(10) 0.0086(9) 0.0151(9) 0.0081(9) F1B 0.0522(12) 0.0801(16) 0.0705(14) 0.0311(12) 0.0121(10) 0.0196(11) F1A 0.120(2) 0.0321(11) 0.0618(13) -0.0006(10) -0.0181(13) -0.0213(12) B1 0.049(2) 0.0225(17) 0.0403(19) 0.0007(15) 0.0029(16) 0.0050(15) F2D 0.0491(12) 0.0560(13) 0.0876(16) 0.0016(12) -0.0046(11) 0.0132(10) F2C 0.0537(12) 0.0566(13) 0.0729(14) -0.0248(11) 0.0264(10) -0.0193(10) F2B 0.0393(10) 0.0704(15) 0.0743(14) -0.0288(12) 0.0104(9) -0.0194(10) F2A 0.125(2) 0.0903(19) 0.0468(13) 0.0084(13) 0.0259(13) 0.0435(16) B2 0.0357(18) 0.042(2) 0.0398(19) -0.0091(16) 0.0057(15) 0.0055(15) O1W 0.0272(12) 0.0503(16) 0.110(2) 0.0036(17) 0.0174(13) 0.0039(11) _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 O2 1.8640(17) . ? Co1 O1 1.8943(16) . ? Co1 O4 1.9141(17) . ? Co1 N3 1.919(2) . ? Co1 N2 1.928(2) . ? Co1 N1 2.006(2) . ? Co2 O3 1.8600(16) . ? Co2 O1 1.8898(15) . ? Co2 N6 1.915(2) . ? Co2 O5 1.9160(17) . ? Co2 N4 1.962(2) . ? Co2 N5 1.9994(19) . ? O1 C1 1.360(3) . ? O2 O3 1.423(2) . ? O4 C37 1.267(3) . ? O5 C37 1.269(3) . ? N1 C18 1.484(3) . ? N1 C12 1.496(3) . ? N1 C11 1.503(3) . ? N2 C17 1.343(3) . ? N2 C13 1.358(3) . ? N3 C23 1.339(3) . ? N3 C19 1.353(3) . ? N4 C24 1.489(3) . ? N4 C31 1.496(3) . ? N4 C25 1.497(3) . ? N5 C26 1.342(3) . ? N5 C30 1.346(3) . ? N6 C36 1.333(3) . ? N6 C32 1.353(3) . ? C1 C2 1.389(3) . ? C1 C6 1.393(3) . ? C2 C3 1.388(3) . ? C2 C11 1.507(3) . ? C3 C4 1.394(4) . ? C3 H3A 0.9500 . ? C4 C5 1.400(4) . ? C4 C7 1.534(3) . ? C5 C6 1.384(3) . ? C5 H5A 0.9500 . ? C6 C24 1.511(3) . ? C7 C8 1.520(4) . ? C7 C10 1.537(4) . ? C7 C9 1.538(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.494(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.385(4) . ? C14 C15 1.382(4) . ? C14 H14A 0.9500 . ? C15 C16 1.379(4) . ? C15 H15A 0.9500 . ? C16 C17 1.377(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.506(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.376(4) . ? C20 C21 1.388(4) . ? C20 H20A 0.9500 . ? C21 C22 1.379(4) . ? C21 H21A 0.9500 . ? C22 C23 1.376(4) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.494(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.382(3) . ? C27 C28 1.387(4) . ? C27 H27A 0.9500 . ? C28 C29 1.380(4) . ? C28 H28A 0.9500 . ? C29 C30 1.385(3) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.496(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.375(4) . ? C33 C34 1.375(4) . ? C33 H33A 0.9500 . ? C34 C35 1.382(4) . ? C34 H34A 0.9500 . ? C35 C36 1.374(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.498(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? F1D B1 1.373(4) . ? F1C B1 1.393(4) . ? F1B B1 1.383(4) . ? F1A B1 1.383(4) . ? F2D B2 1.353(4) . ? F2C B2 1.405(4) . ? F2B B2 1.377(4) . ? F2A B2 1.370(4) . ? O1W H1W 0.854(10) . ? O1W H2W 0.854(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 O2 Co1 O1 90.37(7) . . ? O2 Co1 O4 87.12(7) . . ? O1 Co1 O4 88.75(7) . . ? O2 Co1 N3 94.85(8) . . ? O1 Co1 N3 171.80(8) . . ? O4 Co1 N3 85.21(8) . . ? O2 Co1 N2 95.90(8) . . ? O1 Co1 N2 91.93(8) . . ? O4 Co1 N2 176.90(8) . . ? N3 Co1 N2 93.82(9) . . ? O2 Co1 N1 178.04(8) . . ? O1 Co1 N1 91.01(7) . . ? O4 Co1 N1 91.52(8) . . ? N3 Co1 N1 83.63(9) . . ? N2 Co1 N1 85.45(8) . . ? O3 Co2 O1 84.82(7) . . ? O3 Co2 N6 89.88(8) . . ? O1 Co2 N6 174.54(8) . . ? O3 Co2 O5 95.53(7) . . ? O1 Co2 O5 91.81(7) . . ? N6 Co2 O5 90.04(8) . . ? O3 Co2 N4 89.95(8) . . ? O1 Co2 N4 96.13(8) . . ? N6 Co2 N4 82.49(9) . . ? O5 Co2 N4 170.73(8) . . ? O3 Co2 N5 169.19(8) . . ? O1 Co2 N5 86.99(7) . . ? N6 Co2 N5 98.09(8) . . ? O5 Co2 N5 91.77(8) . . ? N4 Co2 N5 83.91(8) . . ? C1 O1 Co2 123.23(14) . . ? C1 O1 Co1 119.43(14) . . ? Co2 O1 Co1 113.02(8) . . ? O3 O2 Co1 111.74(12) . . ? O2 O3 Co2 110.19(12) . . ? C37 O4 Co1 125.57(16) . . ? C37 O5 Co2 131.75(16) . . ? C18 N1 C12 110.00(19) . . ? C18 N1 C11 111.86(19) . . ? C12 N1 C11 109.59(19) . . ? C18 N1 Co1 104.08(15) . . ? C12 N1 Co1 108.46(15) . . ? C11 N1 Co1 112.68(15) . . ? C17 N2 C13 119.0(2) . . ? C17 N2 Co1 125.61(18) . . ? C13 N2 Co1 114.44(17) . . ? C23 N3 C19 119.8(2) . . ? C23 N3 Co1 126.89(19) . . ? C19 N3 Co1 113.24(17) . . ? C24 N4 C31 110.53(18) . . ? C24 N4 C25 109.81(18) . . ? C31 N4 C25 109.18(18) . . ? C24 N4 Co2 113.73(15) . . ? C31 N4 Co2 104.58(15) . . ? C25 N4 Co2 108.83(14) . . ? C26 N5 C30 118.5(2) . . ? C26 N5 Co2 113.53(15) . . ? C30 N5 Co2 125.45(17) . . ? C36 N6 C32 119.7(2) . . ? C36 N6 Co2 126.69(18) . . ? C32 N6 Co2 113.54(17) . . ? O1 C1 C2 117.7(2) . . ? O1 C1 C6 120.9(2) . . ? C2 C1 C6 121.4(2) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 C11 123.5(2) . . ? C1 C2 C11 117.2(2) . . ? C2 C3 C4 121.5(2) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C3 C4 C5 117.5(2) . . ? C3 C4 C7 122.4(2) . . ? C5 C4 C7 120.0(2) . . ? C6 C5 C4 122.4(2) . . ? C6 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C5 C6 C1 118.1(2) . . ? C5 C6 C24 121.8(2) . . ? C1 C6 C24 119.7(2) . . ? C8 C7 C4 109.4(2) . . ? C8 C7 C10 109.3(3) . . ? C4 C7 C10 111.9(2) . . ? C8 C7 C9 109.8(2) . . ? C4 C7 C9 109.3(2) . . ? C10 C7 C9 107.1(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 108.89(19) . . ? N1 C11 H11A 109.9 . . ? C2 C11 H11A 109.9 . . ? N1 C11 H11B 109.9 . . ? C2 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C13 C12 N1 110.4(2) . . ? C13 C12 H12A 109.6 . . ? N1 C12 H12A 109.6 . . ? C13 C12 H12B 109.6 . . ? N1 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N2 C13 C14 121.3(2) . . ? N2 C13 C12 114.7(2) . . ? C14 C13 C12 123.9(2) . . ? C15 C14 C13 119.0(3) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C16 C15 C14 119.4(3) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C17 C16 C15 119.1(3) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? N2 C17 C16 122.0(3) . . ? N2 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? N1 C18 C19 107.4(2) . . ? N1 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? N1 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? N3 C19 C20 121.2(3) . . ? N3 C19 C18 114.8(2) . . ? C20 C19 C18 124.0(3) . . ? C19 C20 C21 118.8(3) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C23 C22 C21 119.0(3) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? N3 C23 C22 121.6(3) . . ? N3 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? N4 C24 C6 113.18(19) . . ? N4 C24 H24A 108.9 . . ? C6 C24 H24A 108.9 . . ? N4 C24 H24B 108.9 . . ? C6 C24 H24B 108.9 . . ? H24A C24 H24B 107.8 . . ? C26 C25 N4 109.10(19) . . ? C26 C25 H25A 109.9 . . ? N4 C25 H25A 109.9 . . ? C26 C25 H25B 109.9 . . ? N4 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? N5 C26 C27 122.9(2) . . ? N5 C26 C25 113.8(2) . . ? C27 C26 C25 123.3(2) . . ? C26 C27 C28 118.3(2) . . ? C26 C27 H27A 120.8 . . ? C28 C27 H27A 120.8 . . ? C29 C28 C27 119.1(2) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 119.3(2) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? N5 C30 C29 121.8(2) . . ? N5 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? N4 C31 C32 106.72(19) . . ? N4 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? N4 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? N6 C32 C33 121.2(2) . . ? N6 C32 C31 113.7(2) . . ? C33 C32 C31 125.0(2) . . ? C34 C33 C32 119.0(3) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 C35 119.5(3) . . ? C33 C34 H34A 120.2 . . ? C35 C34 H34A 120.2 . . ? C36 C35 C34 119.1(3) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? N6 C36 C35 121.5(3) . . ? N6 C36 H36A 119.3 . . ? C35 C36 H36A 119.3 . . ? O4 C37 O5 126.7(2) . . ? O4 C37 C38 116.6(2) . . ? O5 C37 C38 116.7(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F1D B1 F1A 110.0(3) . . ? F1D B1 F1B 108.4(3) . . ? F1A B1 F1B 108.3(3) . . ? F1D B1 F1C 110.4(3) . . ? F1A B1 F1C 109.3(3) . . ? F1B B1 F1C 110.4(3) . . ? F2D B2 F2A 109.8(3) . . ? F2D B2 F2B 111.7(3) . . ? F2A B2 F2B 109.6(3) . . ? F2D B2 F2C 110.9(3) . . ? F2A B2 F2C 107.4(3) . . ? F2B B2 F2C 107.3(2) . . ? H1W O1W H2W 106.5(16) . . ? 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 O3 Co2 O1 C1 118.13(17) . . . . ? O5 Co2 O1 C1 -146.47(17) . . . . ? N4 Co2 O1 C1 28.74(17) . . . . ? N5 Co2 O1 C1 -54.80(17) . . . . ? O3 Co2 O1 Co1 -38.28(9) . . . . ? O5 Co2 O1 Co1 57.12(9) . . . . ? N4 Co2 O1 Co1 -127.67(9) . . . . ? N5 Co2 O1 Co1 148.79(10) . . . . ? O2 Co1 O1 C1 -139.89(17) . . . . ? O4 Co1 O1 C1 133.00(16) . . . . ? N2 Co1 O1 C1 -43.97(17) . . . . ? N1 Co1 O1 C1 41.51(17) . . . . ? O2 Co1 O1 Co2 17.51(9) . . . . ? O4 Co1 O1 Co2 -69.60(9) . . . . ? N2 Co1 O1 Co2 113.43(10) . . . . ? N1 Co1 O1 Co2 -161.09(9) . . . . ? O1 Co1 O2 O3 19.73(13) . . . . ? O4 Co1 O2 O3 108.45(13) . . . . ? N3 Co1 O2 O3 -166.61(13) . . . . ? N2 Co1 O2 O3 -72.25(13) . . . . ? Co1 O2 O3 Co2 -52.51(14) . . . . ? O1 Co2 O3 O2 53.73(13) . . . . ? N6 Co2 O3 O2 -127.62(14) . . . . ? O5 Co2 O3 O2 -37.59(13) . . . . ? N4 Co2 O3 O2 149.89(13) . . . . ? N5 Co2 O3 O2 94.7(4) . . . . ? O2 Co1 O4 C37 -39.46(18) . . . . ? O1 Co1 O4 C37 50.97(18) . . . . ? N3 Co1 O4 C37 -134.58(19) . . . . ? N1 Co1 O4 C37 141.94(19) . . . . ? O3 Co2 O5 C37 68.0(2) . . . . ? O1 Co2 O5 C37 -16.9(2) . . . . ? N6 Co2 O5 C37 157.9(2) . . . . ? N5 Co2 O5 C37 -104.0(2) . . . . ? O1 Co1 N1 C18 139.58(15) . . . . ? O4 Co1 N1 C18 50.81(15) . . . . ? N3 Co1 N1 C18 -34.19(16) . . . . ? N2 Co1 N1 C18 -128.56(16) . . . . ? O1 Co1 N1 C12 -103.32(15) . . . . ? O4 Co1 N1 C12 167.91(15) . . . . ? N3 Co1 N1 C12 82.90(16) . . . . ? N2 Co1 N1 C12 -11.46(15) . . . . ? O1 Co1 N1 C11 18.19(16) . . . . ? O4 Co1 N1 C11 -70.58(16) . . . . ? N3 Co1 N1 C11 -155.59(17) . . . . ? N2 Co1 N1 C11 110.05(16) . . . . ? O2 Co1 N2 C17 8.9(2) . . . . ? O1 Co1 N2 C17 -81.7(2) . . . . ? N3 Co1 N2 C17 104.2(2) . . . . ? N1 Co1 N2 C17 -172.5(2) . . . . ? O2 Co1 N2 C13 177.34(17) . . . . ? O1 Co1 N2 C13 86.77(17) . . . . ? N3 Co1 N2 C13 -87.38(18) . . . . ? N1 Co1 N2 C13 -4.09(17) . . . . ? O2 Co1 N3 C23 17.9(2) . . . . ? O4 Co1 N3 C23 104.6(2) . . . . ? N2 Co1 N3 C23 -78.4(2) . . . . ? N1 Co1 N3 C23 -163.3(2) . . . . ? O2 Co1 N3 C19 -159.62(17) . . . . ? O4 Co1 N3 C19 -72.93(17) . . . . ? N2 Co1 N3 C19 104.13(18) . . . . ? N1 Co1 N3 C19 19.14(17) . . . . ? O3 Co2 N4 C24 -68.32(15) . . . . ? O1 Co2 N4 C24 16.47(16) . . . . ? N6 Co2 N4 C24 -158.21(16) . . . . ? N5 Co2 N4 C24 102.77(16) . . . . ? O3 Co2 N4 C31 52.36(14) . . . . ? O1 Co2 N4 C31 137.15(14) . . . . ? N6 Co2 N4 C31 -37.53(14) . . . . ? N5 Co2 N4 C31 -136.55(15) . . . . ? O3 Co2 N4 C25 168.94(15) . . . . ? O1 Co2 N4 C25 -106.27(14) . . . . ? N6 Co2 N4 C25 79.05(15) . . . . ? N5 Co2 N4 C25 -19.98(15) . . . . ? O3 Co2 N5 C26 57.3(5) . . . . ? O1 Co2 N5 C26 98.12(16) . . . . ? N6 Co2 N5 C26 -79.86(17) . . . . ? O5 Co2 N5 C26 -170.15(16) . . . . ? N4 Co2 N5 C26 1.63(16) . . . . ? O3 Co2 N5 C30 -104.1(4) . . . . ? O1 Co2 N5 C30 -63.34(19) . . . . ? N6 Co2 N5 C30 118.7(2) . . . . ? O5 Co2 N5 C30 28.4(2) . . . . ? N4 Co2 N5 C30 -159.8(2) . . . . ? O3 Co2 N6 C36 111.3(2) . . . . ? O5 Co2 N6 C36 15.8(2) . . . . ? N4 Co2 N6 C36 -158.7(2) . . . . ? N5 Co2 N6 C36 -76.0(2) . . . . ? O3 Co2 N6 C32 -65.57(17) . . . . ? O5 Co2 N6 C32 -161.10(17) . . . . ? N4 Co2 N6 C32 24.40(17) . . . . ? N5 Co2 N6 C32 107.11(18) . . . . ? Co2 O1 C1 C2 145.66(18) . . . . ? Co1 O1 C1 C2 -59.4(3) . . . . ? Co2 O1 C1 C6 -36.6(3) . . . . ? Co1 O1 C1 C6 118.4(2) . . . . ? O1 C1 C2 C3 179.2(2) . . . . ? C6 C1 C2 C3 1.4(4) . . . . ? O1 C1 C2 C11 5.3(3) . . . . ? C6 C1 C2 C11 -172.4(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C11 C2 C3 C4 173.7(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C2 C3 C4 C7 -179.9(2) . . . . ? C3 C4 C5 C6 -0.7(4) . . . . ? C7 C4 C5 C6 178.7(2) . . . . ? C4 C5 C6 C1 2.2(4) . . . . ? C4 C5 C6 C24 -170.4(2) . . . . ? O1 C1 C6 C5 179.7(2) . . . . ? C2 C1 C6 C5 -2.6(3) . . . . ? O1 C1 C6 C24 -7.5(3) . . . . ? C2 C1 C6 C24 170.2(2) . . . . ? C3 C4 C7 C8 -112.5(3) . . . . ? C5 C4 C7 C8 68.2(3) . . . . ? C3 C4 C7 C10 8.8(4) . . . . ? C5 C4 C7 C10 -170.5(3) . . . . ? C3 C4 C7 C9 127.3(3) . . . . ? C5 C4 C7 C9 -52.0(3) . . . . ? C18 N1 C11 C2 179.1(2) . . . . ? C12 N1 C11 C2 56.8(2) . . . . ? Co1 N1 C11 C2 -64.1(2) . . . . ? C3 C2 C11 N1 -115.1(3) . . . . ? C1 C2 C11 N1 58.5(3) . . . . ? C18 N1 C12 C13 136.8(2) . . . . ? C11 N1 C12 C13 -99.8(2) . . . . ? Co1 N1 C12 C13 23.6(2) . . . . ? C17 N2 C13 C14 5.4(4) . . . . ? Co1 N2 C13 C14 -163.87(19) . . . . ? C17 N2 C13 C12 -171.4(2) . . . . ? Co1 N2 C13 C12 19.4(3) . . . . ? N1 C12 C13 N2 -28.7(3) . . . . ? N1 C12 C13 C14 154.7(2) . . . . ? N2 C13 C14 C15 -4.3(4) . . . . ? C12 C13 C14 C15 172.2(2) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? C14 C15 C16 C17 2.7(4) . . . . ? C13 N2 C17 C16 -2.4(4) . . . . ? Co1 N2 C17 C16 165.56(19) . . . . ? C15 C16 C17 N2 -1.6(4) . . . . ? C12 N1 C18 C19 -74.1(2) . . . . ? C11 N1 C18 C19 163.8(2) . . . . ? Co1 N1 C18 C19 41.9(2) . . . . ? C23 N3 C19 C20 3.0(4) . . . . ? Co1 N3 C19 C20 -179.3(2) . . . . ? C23 N3 C19 C18 -176.2(2) . . . . ? Co1 N3 C19 C18 1.5(3) . . . . ? N1 C18 C19 N3 -30.3(3) . . . . ? N1 C18 C19 C20 150.6(2) . . . . ? N3 C19 C20 C21 -2.2(4) . . . . ? C18 C19 C20 C21 176.8(3) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C20 C21 C22 C23 2.7(4) . . . . ? C19 N3 C23 C22 -0.8(4) . . . . ? Co1 N3 C23 C22 -178.1(2) . . . . ? C21 C22 C23 N3 -2.1(4) . . . . ? C31 N4 C24 C6 -172.5(2) . . . . ? C25 N4 C24 C6 67.0(2) . . . . ? Co2 N4 C24 C6 -55.2(2) . . . . ? C5 C6 C24 N4 -130.6(2) . . . . ? C1 C6 C24 N4 56.9(3) . . . . ? C24 N4 C25 C26 -91.3(2) . . . . ? C31 N4 C25 C26 147.3(2) . . . . ? Co2 N4 C25 C26 33.7(2) . . . . ? C30 N5 C26 C27 0.2(3) . . . . ? Co2 N5 C26 C27 -162.71(19) . . . . ? C30 N5 C26 C25 -179.3(2) . . . . ? Co2 N5 C26 C25 17.9(2) . . . . ? N4 C25 C26 N5 -34.2(3) . . . . ? N4 C25 C26 C27 146.4(2) . . . . ? N5 C26 C27 C28 -0.4(4) . . . . ? C25 C26 C27 C28 179.0(2) . . . . ? C26 C27 C28 C29 -0.6(4) . . . . ? C27 C28 C29 C30 1.7(4) . . . . ? C26 N5 C30 C29 1.0(3) . . . . ? Co2 N5 C30 C29 161.68(18) . . . . ? C28 C29 C30 N5 -2.0(4) . . . . ? C24 N4 C31 C32 166.31(19) . . . . ? C25 N4 C31 C32 -72.8(2) . . . . ? Co2 N4 C31 C32 43.5(2) . . . . ? C36 N6 C32 C33 -0.4(4) . . . . ? Co2 N6 C32 C33 176.7(2) . . . . ? C36 N6 C32 C31 179.0(2) . . . . ? Co2 N6 C32 C31 -3.9(3) . . . . ? N4 C31 C32 N6 -27.0(3) . . . . ? N4 C31 C32 C33 152.4(3) . . . . ? N6 C32 C33 C34 -0.3(4) . . . . ? C31 C32 C33 C34 -179.7(3) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C33 C34 C35 C36 -0.8(5) . . . . ? C32 N6 C36 C35 0.5(4) . . . . ? Co2 N6 C36 C35 -176.2(2) . . . . ? C34 C35 C36 N6 0.1(5) . . . . ? Co1 O4 C37 O5 -19.2(3) . . . . ? Co1 O4 C37 C38 162.29(16) . . . . ? Co2 O5 C37 O4 -2.3(4) . . . . ? Co2 O5 C37 C38 176.15(16) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 913563' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a data_2 #TrackingRef '15833_web_deposit_cif_file_0_AndrewBond_1354442523.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C38 H41 Cl Co2 N6 O5 2+, 2(B F4 -), 2.25(H2 O) ; _chemical_formula_sum 'C38 H45.50 B2 Cl Co2 F8 N6 O7.25' _chemical_formula_weight 1029.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6177(4) _cell_length_b 11.6326(4) _cell_length_c 18.3035(6) _cell_angle_alpha 82.523(1) _cell_angle_beta 84.474(1) _cell_angle_gamma 74.401(1) _cell_volume 2154.46(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8513 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.09 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1053 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.908358 ; _exptl_special_details ? _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 48901 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 28.40 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.977 _reflns_number_total 10577 _reflns_number_gt 8437 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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^)+(0.0682P)^2^+1.6951P] 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 10577 _refine_ls_number_parameters 623 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.096 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.077 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 0.54014(3) 0.28031(3) 0.165686(17) 0.01896(9) Uani 1 1 d . . . Co2 Co 0.23940(3) 0.38030(3) 0.212390(18) 0.01993(9) Uani 1 1 d . . . Cl1 Cl 0.14014(9) 0.15966(9) 0.04295(6) 0.0551(2) Uani 1 1 d . . . O1 O 0.40620(16) 0.28816(15) 0.24280(9) 0.0209(3) Uani 1 1 d . . . O2 O 0.43462(17) 0.41183(15) 0.11123(9) 0.0224(4) Uani 1 1 d . . . O3 O 0.33105(16) 0.47990(15) 0.15577(10) 0.0224(4) Uani 1 1 d . . . O4 O 0.46073(18) 0.17951(16) 0.11951(10) 0.0246(4) Uani 1 1 d . . . O5 O 0.24778(18) 0.27948(16) 0.13651(10) 0.0259(4) Uani 1 1 d . . . N1 N 0.6600(2) 0.13659(18) 0.21827(12) 0.0224(4) Uani 1 1 d . . . N2 N 0.6287(2) 0.37233(18) 0.21163(11) 0.0202(4) Uani 1 1 d . . . N3 N 0.6723(2) 0.25112(19) 0.08791(12) 0.0227(4) Uani 1 1 d . . . N4 N 0.2020(2) 0.48647(19) 0.29119(12) 0.0223(4) Uani 1 1 d . . . N5 N 0.1564(2) 0.2737(2) 0.28476(12) 0.0257(5) Uani 1 1 d . . . N6 N 0.0784(2) 0.4837(2) 0.17724(12) 0.0253(5) Uani 1 1 d . . . C1 C 0.4431(2) 0.2747(2) 0.31340(13) 0.0209(5) Uani 1 1 d . . . C2 C 0.5328(2) 0.1676(2) 0.33688(14) 0.0226(5) Uani 1 1 d . . . C3 C 0.5744(3) 0.1526(2) 0.40816(14) 0.0249(5) Uani 1 1 d . . . H3A H 0.6368 0.0806 0.4243 0.030 Uiso 1 1 calc R . . C4 C 0.5272(3) 0.2399(2) 0.45652(14) 0.0245(5) Uani 1 1 d . . . C5 C 0.4391(2) 0.3467(2) 0.43038(14) 0.0231(5) Uani 1 1 d . . . H5A H 0.4059 0.4075 0.4625 0.028 Uiso 1 1 calc R . . C6 C 0.3985(2) 0.3667(2) 0.35841(13) 0.0218(5) Uani 1 1 d . . . C7 C 0.5781(3) 0.2198(3) 0.53409(15) 0.0311(6) Uani 1 1 d . . . C8 C 0.5648(4) 0.0981(3) 0.57228(17) 0.0452(8) Uani 1 1 d . . . H8A H 0.5980 0.0851 0.6216 0.068 Uiso 1 1 calc R . . H8B H 0.6155 0.0342 0.5431 0.068 Uiso 1 1 calc R . . H8C H 0.4724 0.0972 0.5765 0.068 Uiso 1 1 calc R . . C9 C 0.5015(4) 0.3153(3) 0.58289(17) 0.0456(8) Uani 1 1 d . . . H9A H 0.5374 0.2987 0.6317 0.068 Uiso 1 1 calc R . . H9B H 0.4091 0.3139 0.5882 0.068 Uiso 1 1 calc R . . H9C H 0.5086 0.3945 0.5602 0.068 Uiso 1 1 calc R . . C10 C 0.7220(4) 0.2209(4) 0.5269(2) 0.0551(10) Uani 1 1 d . . . H10A H 0.7559 0.2074 0.5761 0.083 Uiso 1 1 calc R . . H10B H 0.7305 0.2988 0.5025 0.083 Uiso 1 1 calc R . . H10C H 0.7721 0.1571 0.4975 0.083 Uiso 1 1 calc R . . C11 C 0.5879(3) 0.0787(2) 0.28127(14) 0.0242(5) Uani 1 1 d . . . H11A H 0.6485 0.0062 0.3050 0.029 Uiso 1 1 calc R . . H11B H 0.5159 0.0539 0.2625 0.029 Uiso 1 1 calc R . . C12 C 0.7677(2) 0.1759(2) 0.24674(15) 0.0253(5) Uani 1 1 d . . . H12A H 0.8465 0.1589 0.2122 0.030 Uiso 1 1 calc R . . H12B H 0.7911 0.1304 0.2953 0.030 Uiso 1 1 calc R . . C13 C 0.7246(2) 0.3078(2) 0.25461(14) 0.0239(5) Uani 1 1 d . . . C14 C 0.7824(3) 0.3615(3) 0.30039(16) 0.0311(6) Uani 1 1 d . . . H14A H 0.8482 0.3145 0.3316 0.037 Uiso 1 1 calc R . . C15 C 0.7422(3) 0.4859(3) 0.29992(17) 0.0336(6) Uani 1 1 d . . . H15A H 0.7789 0.5248 0.3317 0.040 Uiso 1 1 calc R . . C16 C 0.6487(3) 0.5518(2) 0.25294(16) 0.0290(6) Uani 1 1 d . . . H16A H 0.6229 0.6369 0.2505 0.035 Uiso 1 1 calc R . . C17 C 0.5929(2) 0.4929(2) 0.20940(14) 0.0233(5) Uani 1 1 d . . . H17A H 0.5280 0.5383 0.1772 0.028 Uiso 1 1 calc R . . C18 C 0.7154(3) 0.0568(2) 0.15924(14) 0.0260(5) Uani 1 1 d . . . H18A H 0.6512 0.0140 0.1488 0.031 Uiso 1 1 calc R . . H18B H 0.7962 -0.0035 0.1749 0.031 Uiso 1 1 calc R . . C19 C 0.7457(2) 0.1357(2) 0.09145(14) 0.0242(5) Uani 1 1 d . . . C20 C 0.8387(3) 0.0990(3) 0.03579(16) 0.0322(6) Uani 1 1 d . . . H20A H 0.8924 0.0189 0.0391 0.039 Uiso 1 1 calc R . . C21 C 0.8538(3) 0.1795(3) -0.02523(16) 0.0373(7) Uani 1 1 d . . . H21A H 0.9151 0.1540 -0.0650 0.045 Uiso 1 1 calc R . . C22 C 0.7790(3) 0.2969(3) -0.02789(16) 0.0328(6) Uani 1 1 d . . . H22A H 0.7891 0.3534 -0.0690 0.039 Uiso 1 1 calc R . . C23 C 0.6894(3) 0.3306(2) 0.03027(14) 0.0264(5) Uani 1 1 d . . . H23A H 0.6388 0.4116 0.0295 0.032 Uiso 1 1 calc R . . C24 C 0.3229(2) 0.4886(2) 0.32657(14) 0.0231(5) Uani 1 1 d . . . H24A H 0.2974 0.5420 0.3664 0.028 Uiso 1 1 calc R . . H24B H 0.3806 0.5229 0.2893 0.028 Uiso 1 1 calc R . . C25 C 0.1063(2) 0.4487(2) 0.34857(14) 0.0269(5) Uani 1 1 d . . . H25A H 0.0163 0.4962 0.3379 0.032 Uiso 1 1 calc R . . H25B H 0.1247 0.4648 0.3977 0.032 Uiso 1 1 calc R . . C26 C 0.1154(2) 0.3176(2) 0.34954(15) 0.0265(5) Uani 1 1 d . . . C27 C 0.0778(3) 0.2486(3) 0.41113(17) 0.0368(7) Uani 1 1 d . . . H27A H 0.0501 0.2814 0.4567 0.044 Uiso 1 1 calc R . . C28 C 0.0816(3) 0.1313(3) 0.40450(19) 0.0453(8) Uani 1 1 d . . . H28A H 0.0571 0.0816 0.4458 0.054 Uiso 1 1 calc R . . C29 C 0.1206(3) 0.0864(3) 0.3381(2) 0.0431(8) Uani 1 1 d . . . H29A H 0.1214 0.0061 0.3327 0.052 Uiso 1 1 calc R . . C30 C 0.1591(3) 0.1590(3) 0.27873(17) 0.0346(6) Uani 1 1 d . . . H30A H 0.1878 0.1272 0.2330 0.042 Uiso 1 1 calc R . . C31 C 0.1398(2) 0.6084(2) 0.25379(14) 0.0253(5) Uani 1 1 d . . . H31A H 0.2073 0.6437 0.2257 0.030 Uiso 1 1 calc R . . H31B H 0.0932 0.6626 0.2908 0.030 Uiso 1 1 calc R . . C32 C 0.0450(2) 0.5921(2) 0.20254(14) 0.0256(5) Uani 1 1 d . . . C33 C -0.0668(3) 0.6793(3) 0.18146(16) 0.0335(6) Uani 1 1 d . . . H33A H -0.0904 0.7548 0.2006 0.040 Uiso 1 1 calc R . . C34 C -0.1429(3) 0.6533(3) 0.13181(17) 0.0379(7) Uani 1 1 d . . . H34A H -0.2199 0.7114 0.1163 0.046 Uiso 1 1 calc R . . C35 C -0.1073(3) 0.5434(3) 0.10492(17) 0.0381(7) Uani 1 1 d . . . H35A H -0.1586 0.5254 0.0704 0.046 Uiso 1 1 calc R . . C36 C 0.0040(3) 0.4593(3) 0.12871(16) 0.0315(6) Uani 1 1 d . . . H36A H 0.0285 0.3830 0.1105 0.038 Uiso 1 1 calc R . . C37 C 0.3407(3) 0.2041(2) 0.10822(14) 0.0247(5) Uani 1 1 d . . . C38 C 0.3105(3) 0.1323(3) 0.05163(16) 0.0327(6) Uani 1 1 d . . . H38A H 0.3476 0.0456 0.0663 0.039 Uiso 1 1 calc R . . H38B H 0.3531 0.1533 0.0031 0.039 Uiso 1 1 calc R . . B1 B 0.4129(4) 0.8386(3) 0.1789(2) 0.0412(8) Uani 1 1 d D . . F1A F 0.3810(3) 0.7422(2) 0.2167(2) 0.0944(10) Uani 1 1 d DU . . F1B F 0.5250(3) 0.8510(2) 0.20362(19) 0.0883(9) Uani 1 1 d DU . . F1C F 0.3129(2) 0.93976(18) 0.18500(14) 0.0674(7) Uani 1 1 d DU . . F1D F 0.4375(4) 0.8230(3) 0.10569(17) 0.1209(13) Uani 1 1 d DU . . B2 B 0.8946(4) 0.8194(4) 0.3809(2) 0.0566(12) Uani 1 1 d D . . F2A F 0.9122(6) 0.8772(4) 0.3131(2) 0.0795(17) Uani 0.60 1 d PDU A 1 F2B F 0.8457(10) 0.9036(7) 0.4247(4) 0.164(4) Uani 0.60 1 d PDU A 1 F2C F 1.0041(4) 0.7465(6) 0.4073(2) 0.0818(16) Uani 0.60 1 d PDU A 1 F2D F 0.8204(9) 0.7464(9) 0.3695(6) 0.202(4) Uani 0.60 1 d PDU A 1 F2E F 0.7948(7) 0.8666(8) 0.4271(5) 0.079(3) Uani 0.40 1 d PDU A 2 F2F F 0.9277(12) 0.6999(6) 0.4042(5) 0.125(4) Uani 0.40 1 d PDU A 2 F2G F 1.0033(9) 0.8528(12) 0.3748(9) 0.193(6) Uani 0.40 1 d PDU A 2 F2H F 0.8460(11) 0.8377(11) 0.3134(4) 0.134(4) Uani 0.40 1 d PDU A 2 O1W O 0.0385(3) 0.9428(3) 0.18718(17) 0.0685(8) Uani 1 1 d . . . H1W H 0.1179 0.9419 0.1864 0.103 Uiso 1 1 d R . . H2W H 0.0155 0.9173 0.2301 0.103 Uiso 1 1 d R . . O2W O 0.1410(9) 0.4610(12) 0.5317(5) 0.058(3) Uani 0.25 1 d P . . H3W H 0.0868 0.5091 0.5043 0.087 Uiso 0.25 1 d PR . . H4W H 0.1097 0.4046 0.5517 0.087 Uiso 0.25 1 d PR . . O3W O 0.6168(2) 0.62683(18) 0.03169(11) 0.0355(5) Uani 1 1 d . . . H5W H 0.5998 0.6069 -0.0080 0.053 Uiso 1 1 d R . . H6W H 0.5463 0.6686 0.0498 0.053 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 0.01963(17) 0.01687(16) 0.01966(17) -0.00184(12) -0.00230(12) -0.00321(12) Co2 0.01753(17) 0.02173(17) 0.02039(17) -0.00052(12) -0.00406(12) -0.00471(13) Cl1 0.0490(5) 0.0560(5) 0.0715(6) -0.0193(4) -0.0266(4) -0.0190(4) O1 0.0194(8) 0.0241(9) 0.0176(8) -0.0004(6) -0.0034(6) -0.0031(7) O2 0.0212(8) 0.0225(9) 0.0202(8) -0.0015(7) -0.0010(7) -0.0007(7) O3 0.0198(8) 0.0207(8) 0.0250(9) -0.0027(7) 0.0005(7) -0.0028(7) O4 0.0278(9) 0.0218(9) 0.0248(9) -0.0036(7) -0.0044(7) -0.0060(7) O5 0.0260(9) 0.0271(9) 0.0267(9) -0.0031(7) -0.0073(7) -0.0084(7) N1 0.0231(10) 0.0189(10) 0.0249(11) -0.0020(8) -0.0034(8) -0.0043(8) N2 0.0204(10) 0.0199(10) 0.0200(10) -0.0020(8) -0.0010(8) -0.0049(8) N3 0.0217(10) 0.0206(10) 0.0252(11) -0.0040(8) -0.0026(8) -0.0037(8) N4 0.0183(10) 0.0232(10) 0.0239(10) 0.0007(8) -0.0028(8) -0.0039(8) N5 0.0205(10) 0.0281(11) 0.0288(11) 0.0027(9) -0.0054(8) -0.0080(9) N6 0.0185(10) 0.0307(12) 0.0253(11) 0.0017(9) -0.0045(8) -0.0052(9) C1 0.0187(11) 0.0246(12) 0.0205(11) 0.0020(9) -0.0037(9) -0.0088(9) C2 0.0224(12) 0.0211(12) 0.0248(12) 0.0021(9) -0.0027(9) -0.0083(10) C3 0.0248(12) 0.0230(12) 0.0262(13) 0.0064(10) -0.0076(10) -0.0073(10) C4 0.0265(13) 0.0275(13) 0.0219(12) 0.0029(10) -0.0070(10) -0.0118(10) C5 0.0244(12) 0.0256(12) 0.0206(12) -0.0022(9) -0.0029(9) -0.0082(10) C6 0.0184(11) 0.0251(12) 0.0224(12) -0.0002(9) -0.0038(9) -0.0068(9) C7 0.0377(15) 0.0346(15) 0.0233(13) 0.0010(11) -0.0112(11) -0.0119(12) C8 0.071(2) 0.0386(17) 0.0279(15) 0.0074(13) -0.0152(15) -0.0189(16) C9 0.064(2) 0.0463(19) 0.0253(15) -0.0049(13) -0.0148(14) -0.0088(16) C10 0.046(2) 0.083(3) 0.044(2) 0.0038(18) -0.0209(16) -0.0271(19) C11 0.0272(13) 0.0196(12) 0.0246(12) 0.0026(9) -0.0044(10) -0.0054(10) C12 0.0222(12) 0.0234(12) 0.0289(13) -0.0011(10) -0.0068(10) -0.0027(10) C13 0.0199(12) 0.0255(13) 0.0271(13) -0.0034(10) -0.0005(9) -0.0075(10) C14 0.0227(13) 0.0371(15) 0.0346(15) -0.0078(12) -0.0094(11) -0.0056(11) C15 0.0304(14) 0.0365(15) 0.0401(16) -0.0150(13) -0.0038(12) -0.0140(12) C16 0.0239(13) 0.0263(13) 0.0388(15) -0.0086(11) 0.0005(11) -0.0086(10) C17 0.0220(12) 0.0219(12) 0.0258(12) -0.0021(10) -0.0002(9) -0.0058(10) C18 0.0266(13) 0.0200(12) 0.0290(13) -0.0048(10) -0.0011(10) -0.0010(10) C19 0.0221(12) 0.0229(12) 0.0270(13) -0.0060(10) -0.0033(10) -0.0029(10) C20 0.0263(14) 0.0322(14) 0.0333(15) -0.0083(12) -0.0023(11) 0.0028(11) C21 0.0284(14) 0.0491(18) 0.0281(15) -0.0067(13) 0.0029(11) 0.0002(13) C22 0.0298(14) 0.0388(16) 0.0267(14) 0.0026(11) -0.0015(11) -0.0065(12) C23 0.0257(13) 0.0255(13) 0.0268(13) -0.0008(10) -0.0026(10) -0.0051(10) C24 0.0210(12) 0.0248(12) 0.0237(12) -0.0031(10) -0.0047(9) -0.0049(10) C25 0.0205(12) 0.0338(14) 0.0243(13) 0.0000(10) 0.0010(10) -0.0055(10) C26 0.0174(12) 0.0339(14) 0.0275(13) 0.0041(11) -0.0052(10) -0.0075(10) C27 0.0335(15) 0.0445(17) 0.0295(15) 0.0083(12) -0.0029(12) -0.0105(13) C28 0.0450(18) 0.0461(19) 0.0437(19) 0.0173(15) -0.0061(14) -0.0193(15) C29 0.0462(19) 0.0337(16) 0.052(2) 0.0096(14) -0.0112(15) -0.0188(14) C30 0.0341(15) 0.0335(15) 0.0386(16) 0.0022(12) -0.0075(12) -0.0139(12) C31 0.0221(12) 0.0239(12) 0.0266(13) -0.0007(10) -0.0044(10) -0.0004(10) C32 0.0202(12) 0.0294(13) 0.0248(13) 0.0029(10) -0.0027(10) -0.0047(10) C33 0.0270(14) 0.0331(15) 0.0345(15) 0.0043(12) -0.0042(11) -0.0010(11) C34 0.0246(14) 0.0460(18) 0.0366(16) 0.0089(13) -0.0085(12) -0.0020(13) C35 0.0284(14) 0.0522(19) 0.0332(15) 0.0023(13) -0.0123(12) -0.0095(13) C36 0.0242(13) 0.0407(16) 0.0312(14) -0.0023(12) -0.0075(11) -0.0100(12) C37 0.0312(14) 0.0219(12) 0.0224(12) -0.0007(9) -0.0061(10) -0.0086(10) C38 0.0392(16) 0.0287(14) 0.0346(15) -0.0053(11) -0.0122(12) -0.0120(12) B1 0.043(2) 0.0270(17) 0.052(2) -0.0066(15) -0.0088(17) -0.0030(15) F1A 0.0624(15) 0.0402(13) 0.178(3) 0.0262(16) -0.0215(17) -0.0216(11) F1B 0.0719(17) 0.0566(15) 0.149(3) -0.0042(16) -0.0376(17) -0.0301(13) F1C 0.0639(14) 0.0366(11) 0.0830(17) 0.0046(11) 0.0162(12) 0.0064(10) F1D 0.127(3) 0.130(3) 0.083(2) -0.051(2) -0.0041(19) 0.024(2) B2 0.041(2) 0.076(3) 0.041(2) 0.003(2) -0.0024(17) 0.001(2) F2A 0.123(5) 0.065(3) 0.048(3) -0.001(2) 0.026(3) -0.034(3) F2B 0.217(8) 0.141(6) 0.055(4) -0.041(4) -0.011(5) 0.104(6) F2C 0.048(2) 0.123(4) 0.055(2) -0.020(3) -0.0108(19) 0.018(3) F2D 0.145(6) 0.244(8) 0.250(9) 0.049(7) -0.040(6) -0.134(6) F2E 0.042(3) 0.103(6) 0.059(4) 0.012(4) 0.017(3) 0.021(3) F2F 0.150(8) 0.058(4) 0.139(7) -0.017(4) 0.074(6) -0.004(5) F2G 0.150(8) 0.182(9) 0.276(11) 0.030(8) -0.055(8) -0.102(8) F2H 0.143(8) 0.159(8) 0.067(5) -0.035(6) -0.032(5) 0.038(6) O1W 0.0532(16) 0.091(2) 0.0639(18) -0.0183(16) -0.0007(13) -0.0196(16) O2W 0.030(5) 0.117(10) 0.028(5) -0.022(5) 0.001(4) -0.015(5) O3W 0.0372(11) 0.0375(11) 0.0310(10) 0.0006(8) -0.0129(8) -0.0066(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.8670(17) . ? Co1 N3 1.896(2) . ? Co1 O1 1.8975(17) . ? Co1 N2 1.915(2) . ? Co1 O4 1.9306(18) . ? Co1 N1 2.004(2) . ? Co2 O3 1.8610(17) . ? Co2 O1 1.8997(17) . ? Co2 O5 1.9121(18) . ? Co2 N6 1.920(2) . ? Co2 N4 1.963(2) . ? Co2 N5 2.001(2) . ? Cl1 C38 1.769(3) . ? O1 C1 1.364(3) . ? O2 O3 1.424(2) . ? O4 C37 1.260(3) . ? O5 C37 1.251(3) . ? N1 C18 1.490(3) . ? N1 C12 1.499(3) . ? N1 C11 1.509(3) . ? N2 C13 1.344(3) . ? N2 C17 1.347(3) . ? N3 C23 1.342(3) . ? N3 C19 1.356(3) . ? N4 C25 1.498(3) . ? N4 C31 1.499(3) . ? N4 C24 1.499(3) . ? N5 C26 1.340(4) . ? N5 C30 1.346(4) . ? N6 C32 1.346(4) . ? N6 C36 1.347(3) . ? C1 C6 1.389(4) . ? C1 C2 1.395(3) . ? C2 C3 1.392(4) . ? C2 C11 1.511(4) . ? C3 C4 1.393(4) . ? C3 H3A 0.9500 . ? C4 C5 1.398(4) . ? C4 C7 1.535(4) . ? C5 C6 1.397(3) . ? C5 H5A 0.9500 . ? C6 C24 1.503(3) . ? C7 C10 1.523(5) . ? C7 C9 1.525(4) . ? C7 C8 1.531(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.501(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.382(4) . ? C14 C15 1.393(4) . ? C14 H14A 0.9500 . ? C15 C16 1.376(4) . ? C15 H15A 0.9500 . ? C16 C17 1.381(4) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.507(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.374(4) . ? C20 C21 1.387(4) . ? C20 H20A 0.9500 . ? C21 C22 1.380(4) . ? C21 H21A 0.9500 . ? C22 C23 1.380(4) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.500(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.388(4) . ? C27 C28 1.374(5) . ? C27 H27A 0.9500 . ? C28 C29 1.369(5) . ? C28 H28A 0.9500 . ? C29 C30 1.386(4) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.503(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.388(4) . ? C33 C34 1.385(4) . ? C33 H33A 0.9500 . ? C34 C35 1.374(5) . ? C34 H34A 0.9500 . ? C35 C36 1.382(4) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.519(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? B1 F1A 1.345(4) . ? B1 F1B 1.362(4) . ? B1 F1C 1.365(4) . ? B1 F1D 1.366(4) . ? B2 F2G 1.304(7) . ? B2 F2B 1.312(6) . ? B2 F2C 1.332(5) . ? B2 F2E 1.332(6) . ? B2 F2D 1.351(7) . ? B2 F2H 1.354(7) . ? B2 F2A 1.354(5) . ? B2 F2F 1.359(7) . ? O1W H1W 0.8400 . ? O1W H2W 0.8400 . ? O2W H3W 0.8400 . ? O2W H4W 0.8401 . ? O3W H5W 0.8400 . ? O3W H6W 0.8400 . ? 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 O2 Co1 N3 93.46(8) . . ? O2 Co1 O1 90.54(7) . . ? N3 Co1 O1 172.26(8) . . ? O2 Co1 N2 95.50(8) . . ? N3 Co1 N2 92.73(9) . . ? O1 Co1 N2 93.47(8) . . ? O2 Co1 O4 87.53(8) . . ? N3 Co1 O4 85.17(8) . . ? O1 Co1 O4 88.40(8) . . ? N2 Co1 O4 176.42(8) . . ? O2 Co1 N1 176.43(8) . . ? N3 Co1 N1 83.05(9) . . ? O1 Co1 N1 92.83(8) . . ? N2 Co1 N1 85.48(9) . . ? O4 Co1 N1 91.38(8) . . ? O3 Co2 O1 85.46(7) . . ? O3 Co2 O5 94.87(8) . . ? O1 Co2 O5 91.04(8) . . ? O3 Co2 N6 89.52(8) . . ? O1 Co2 N6 174.95(8) . . ? O5 Co2 N6 89.95(9) . . ? O3 Co2 N4 90.38(8) . . ? O1 Co2 N4 96.28(8) . . ? O5 Co2 N4 171.31(8) . . ? N6 Co2 N4 83.16(9) . . ? O3 Co2 N5 171.93(8) . . ? O1 Co2 N5 88.89(8) . . ? O5 Co2 N5 90.97(9) . . ? N6 Co2 N5 96.05(9) . . ? N4 Co2 N5 84.51(9) . . ? C1 O1 Co1 117.25(14) . . ? C1 O1 Co2 123.85(15) . . ? Co1 O1 Co2 112.91(8) . . ? O3 O2 Co1 112.49(12) . . ? O2 O3 Co2 110.56(12) . . ? C37 O4 Co1 124.30(16) . . ? C37 O5 Co2 132.11(17) . . ? C18 N1 C12 109.5(2) . . ? C18 N1 C11 113.19(19) . . ? C12 N1 C11 110.01(19) . . ? C18 N1 Co1 103.94(15) . . ? C12 N1 Co1 108.42(15) . . ? C11 N1 Co1 111.55(15) . . ? C13 N2 C17 119.7(2) . . ? C13 N2 Co1 115.29(17) . . ? C17 N2 Co1 124.69(17) . . ? C23 N3 C19 120.6(2) . . ? C23 N3 Co1 125.63(18) . . ? C19 N3 Co1 113.54(17) . . ? C25 N4 C31 109.42(19) . . ? C25 N4 C24 109.80(19) . . ? C31 N4 C24 110.31(19) . . ? C25 N4 Co2 109.67(16) . . ? C31 N4 Co2 104.69(15) . . ? C24 N4 Co2 112.81(15) . . ? C26 N5 C30 118.8(2) . . ? C26 N5 Co2 113.90(18) . . ? C30 N5 Co2 126.2(2) . . ? C32 N6 C36 119.7(2) . . ? C32 N6 Co2 113.80(17) . . ? C36 N6 Co2 126.4(2) . . ? O1 C1 C6 121.2(2) . . ? O1 C1 C2 117.1(2) . . ? C6 C1 C2 121.6(2) . . ? C3 C2 C1 118.4(2) . . ? C3 C2 C11 123.5(2) . . ? C1 C2 C11 117.9(2) . . ? C2 C3 C4 122.0(2) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C3 C4 C5 117.8(2) . . ? C3 C4 C7 119.9(2) . . ? C5 C4 C7 122.2(2) . . ? C6 C5 C4 121.9(2) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C1 C6 C5 118.3(2) . . ? C1 C6 C24 119.9(2) . . ? C5 C6 C24 121.4(2) . . ? C10 C7 C9 109.4(3) . . ? C10 C7 C8 109.5(3) . . ? C9 C7 C8 107.3(3) . . ? C10 C7 C4 108.7(2) . . ? C9 C7 C4 112.5(2) . . ? C8 C7 C4 109.5(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 109.03(19) . . ? N1 C11 H11A 109.9 . . ? C2 C11 H11A 109.9 . . ? N1 C11 H11B 109.9 . . ? C2 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N1 C12 C13 110.1(2) . . ? N1 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? N1 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.2 . . ? N2 C13 C14 121.6(2) . . ? N2 C13 C12 115.5(2) . . ? C14 C13 C12 122.8(2) . . ? C13 C14 C15 118.7(3) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? N2 C17 C16 121.3(2) . . ? N2 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? N1 C18 C19 107.1(2) . . ? N1 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? N1 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? N3 C19 C20 120.1(2) . . ? N3 C19 C18 114.7(2) . . ? C20 C19 C18 125.2(2) . . ? C19 C20 C21 119.6(3) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 118.7(3) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? N3 C23 C22 121.2(2) . . ? N3 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? N4 C24 C6 113.4(2) . . ? N4 C24 H24A 108.9 . . ? C6 C24 H24A 108.9 . . ? N4 C24 H24B 108.9 . . ? C6 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? N4 C25 C26 110.7(2) . . ? N4 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? N4 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? N5 C26 C27 122.4(3) . . ? N5 C26 C25 114.5(2) . . ? C27 C26 C25 123.0(3) . . ? C28 C27 C26 118.2(3) . . ? C28 C27 H27A 120.9 . . ? C26 C27 H27A 120.9 . . ? C29 C28 C27 119.7(3) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 119.5(3) . . ? C28 C29 H29A 120.2 . . ? C30 C29 H29A 120.2 . . ? N5 C30 C29 121.2(3) . . ? N5 C30 H30A 119.4 . . ? C29 C30 H30A 119.4 . . ? N4 C31 C32 107.0(2) . . ? N4 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? N4 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? N6 C32 C33 121.7(3) . . ? N6 C32 C31 113.9(2) . . ? C33 C32 C31 124.5(3) . . ? C34 C33 C32 118.2(3) . . ? C34 C33 H33A 120.9 . . ? C32 C33 H33A 120.9 . . ? C35 C34 C33 120.0(3) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 119.3(3) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? N6 C36 C35 121.1(3) . . ? N6 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? O5 C37 O4 128.3(2) . . ? O5 C37 C38 118.2(2) . . ? O4 C37 C38 113.5(2) . . ? C37 C38 Cl1 112.2(2) . . ? C37 C38 H38A 109.2 . . ? Cl1 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? Cl1 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? F1A B1 F1B 109.5(3) . . ? F1A B1 F1C 110.9(3) . . ? F1B B1 F1C 111.1(3) . . ? F1A B1 F1D 110.2(3) . . ? F1B B1 F1D 107.1(3) . . ? F1C B1 F1D 107.9(3) . . ? F2B B2 F2A 105.9(5) . . ? F2C B2 F2A 114.1(4) . . ? F2D B2 F2A 103.7(5) . . ? F2B B2 F2C 109.5(5) . . ? F2B B2 F2D 118.5(6) . . ? F2C B2 F2D 105.2(5) . . ? F2G B2 F2E 121.4(7) . . ? F2G B2 F2H 108.4(7) . . ? F2E B2 F2H 106.0(6) . . ? F2G B2 F2F 106.1(6) . . ? F2E B2 F2F 104.9(5) . . ? F2H B2 F2F 109.7(7) . . ? H1W O1W H2W 107.9 . . ? H3W O2W H4W 110.2 . . ? H5W O3W H6W 106.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 -136.66(17) . . . . ? N2 Co1 O1 C1 -41.12(17) . . . . ? O4 Co1 O1 C1 135.83(17) . . . . ? N1 Co1 O1 C1 44.53(17) . . . . ? O2 Co1 O1 Co2 17.22(10) . . . . ? N2 Co1 O1 Co2 112.76(10) . . . . ? O4 Co1 O1 Co2 -70.29(10) . . . . ? N1 Co1 O1 Co2 -161.60(10) . . . . ? O3 Co2 O1 C1 114.51(18) . . . . ? O5 Co2 O1 C1 -150.68(18) . . . . ? N4 Co2 O1 C1 24.62(19) . . . . ? N5 Co2 O1 C1 -59.73(18) . . . . ? O3 Co2 O1 Co1 -37.37(9) . . . . ? O5 Co2 O1 Co1 57.43(10) . . . . ? N4 Co2 O1 Co1 -127.26(10) . . . . ? N5 Co2 O1 Co1 148.39(10) . . . . ? N3 Co1 O2 O3 -167.65(14) . . . . ? O1 Co1 O2 O3 18.98(14) . . . . ? N2 Co1 O2 O3 -74.56(14) . . . . ? O4 Co1 O2 O3 107.35(14) . . . . ? Co1 O2 O3 Co2 -50.91(15) . . . . ? O1 Co2 O3 O2 52.15(13) . . . . ? O5 Co2 O3 O2 -38.51(14) . . . . ? N6 Co2 O3 O2 -128.42(14) . . . . ? N4 Co2 O3 O2 148.42(14) . . . . ? O2 Co1 O4 C37 -40.8(2) . . . . ? N3 Co1 O4 C37 -134.5(2) . . . . ? O1 Co1 O4 C37 49.8(2) . . . . ? N1 Co1 O4 C37 142.6(2) . . . . ? O3 Co2 O5 C37 70.1(2) . . . . ? O1 Co2 O5 C37 -15.4(2) . . . . ? N6 Co2 O5 C37 159.6(2) . . . . ? N5 Co2 O5 C37 -104.3(2) . . . . ? N3 Co1 N1 C18 -36.61(16) . . . . ? O1 Co1 N1 C18 136.82(16) . . . . ? N2 Co1 N1 C18 -129.92(16) . . . . ? O4 Co1 N1 C18 48.35(16) . . . . ? N3 Co1 N1 C12 79.81(16) . . . . ? O1 Co1 N1 C12 -106.77(16) . . . . ? N2 Co1 N1 C12 -13.51(16) . . . . ? O4 Co1 N1 C12 164.77(16) . . . . ? N3 Co1 N1 C11 -158.91(17) . . . . ? O1 Co1 N1 C11 14.52(16) . . . . ? N2 Co1 N1 C11 107.78(16) . . . . ? O4 Co1 N1 C11 -73.95(16) . . . . ? O2 Co1 N2 C13 -176.01(17) . . . . ? N3 Co1 N2 C13 -82.27(18) . . . . ? O1 Co1 N2 C13 93.11(18) . . . . ? N1 Co1 N2 C13 0.54(18) . . . . ? O2 Co1 N2 C17 10.9(2) . . . . ? N3 Co1 N2 C17 104.6(2) . . . . ? O1 Co1 N2 C17 -80.0(2) . . . . ? N1 Co1 N2 C17 -172.6(2) . . . . ? O2 Co1 N3 C23 19.7(2) . . . . ? N2 Co1 N3 C23 -76.0(2) . . . . ? O4 Co1 N3 C23 106.9(2) . . . . ? N1 Co1 N3 C23 -161.1(2) . . . . ? O2 Co1 N3 C19 -155.04(18) . . . . ? N2 Co1 N3 C19 109.28(18) . . . . ? O4 Co1 N3 C19 -67.82(18) . . . . ? N1 Co1 N3 C19 24.17(18) . . . . ? O3 Co2 N4 C25 171.28(16) . . . . ? O1 Co2 N4 C25 -103.25(16) . . . . ? N6 Co2 N4 C25 81.81(16) . . . . ? N5 Co2 N4 C25 -14.98(16) . . . . ? O3 Co2 N4 C31 53.97(15) . . . . ? O1 Co2 N4 C31 139.45(15) . . . . ? N6 Co2 N4 C31 -35.50(15) . . . . ? N5 Co2 N4 C31 -132.28(16) . . . . ? O3 Co2 N4 C24 -65.99(16) . . . . ? O1 Co2 N4 C24 19.48(17) . . . . ? N6 Co2 N4 C24 -155.46(17) . . . . ? N5 Co2 N4 C24 107.75(17) . . . . ? O1 Co2 N5 C26 96.40(18) . . . . ? O5 Co2 N5 C26 -172.58(18) . . . . ? N6 Co2 N5 C26 -82.52(18) . . . . ? N4 Co2 N5 C26 -0.02(18) . . . . ? O1 Co2 N5 C30 -71.7(2) . . . . ? O5 Co2 N5 C30 19.3(2) . . . . ? N6 Co2 N5 C30 109.4(2) . . . . ? N4 Co2 N5 C30 -168.1(2) . . . . ? O3 Co2 N6 C32 -68.86(18) . . . . ? O5 Co2 N6 C32 -163.73(18) . . . . ? N4 Co2 N6 C32 21.58(18) . . . . ? N5 Co2 N6 C32 105.29(19) . . . . ? O3 Co2 N6 C36 107.6(2) . . . . ? O5 Co2 N6 C36 12.7(2) . . . . ? N4 Co2 N6 C36 -162.0(2) . . . . ? N5 Co2 N6 C36 -78.3(2) . . . . ? Co1 O1 C1 C6 117.2(2) . . . . ? Co2 O1 C1 C6 -33.5(3) . . . . ? Co1 O1 C1 C2 -59.3(2) . . . . ? Co2 O1 C1 C2 149.88(17) . . . . ? O1 C1 C2 C3 178.6(2) . . . . ? C6 C1 C2 C3 2.0(4) . . . . ? O1 C1 C2 C11 3.6(3) . . . . ? C6 C1 C2 C11 -173.0(2) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C11 C2 C3 C4 176.0(2) . . . . ? C2 C3 C4 C5 -2.3(4) . . . . ? C2 C3 C4 C7 -178.9(2) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C7 C4 C5 C6 176.6(2) . . . . ? O1 C1 C6 C5 179.4(2) . . . . ? C2 C1 C6 C5 -4.1(4) . . . . ? O1 C1 C6 C24 -8.1(3) . . . . ? C2 C1 C6 C24 168.3(2) . . . . ? C4 C5 C6 C1 3.0(4) . . . . ? C4 C5 C6 C24 -169.3(2) . . . . ? C3 C4 C7 C10 67.3(3) . . . . ? C5 C4 C7 C10 -109.1(3) . . . . ? C3 C4 C7 C9 -171.4(3) . . . . ? C5 C4 C7 C9 12.1(4) . . . . ? C3 C4 C7 C8 -52.2(3) . . . . ? C5 C4 C7 C8 131.3(3) . . . . ? C18 N1 C11 C2 -178.5(2) . . . . ? C12 N1 C11 C2 58.6(2) . . . . ? Co1 N1 C11 C2 -61.7(2) . . . . ? C3 C2 C11 N1 -114.0(3) . . . . ? C1 C2 C11 N1 60.7(3) . . . . ? C18 N1 C12 C13 135.6(2) . . . . ? C11 N1 C12 C13 -99.4(2) . . . . ? Co1 N1 C12 C13 22.8(2) . . . . ? C17 N2 C13 C14 4.1(4) . . . . ? Co1 N2 C13 C14 -169.4(2) . . . . ? C17 N2 C13 C12 -173.3(2) . . . . ? Co1 N2 C13 C12 13.2(3) . . . . ? N1 C12 C13 N2 -24.2(3) . . . . ? N1 C12 C13 C14 158.5(2) . . . . ? N2 C13 C14 C15 -1.9(4) . . . . ? C12 C13 C14 C15 175.3(3) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C14 C15 C16 C17 2.6(4) . . . . ? C13 N2 C17 C16 -2.9(4) . . . . ? Co1 N2 C17 C16 169.94(19) . . . . ? C15 C16 C17 N2 -0.4(4) . . . . ? C12 N1 C18 C19 -74.3(2) . . . . ? C11 N1 C18 C19 162.6(2) . . . . ? Co1 N1 C18 C19 41.4(2) . . . . ? C23 N3 C19 C20 0.1(4) . . . . ? Co1 N3 C19 C20 175.1(2) . . . . ? C23 N3 C19 C18 -179.9(2) . . . . ? Co1 N3 C19 C18 -4.9(3) . . . . ? N1 C18 C19 N3 -25.9(3) . . . . ? N1 C18 C19 C20 154.2(3) . . . . ? N3 C19 C20 C21 -2.3(4) . . . . ? C18 C19 C20 C21 177.6(3) . . . . ? C19 C20 C21 C22 2.8(5) . . . . ? C20 C21 C22 C23 -0.9(5) . . . . ? C19 N3 C23 C22 1.8(4) . . . . ? Co1 N3 C23 C22 -172.5(2) . . . . ? C21 C22 C23 N3 -1.4(4) . . . . ? C25 N4 C24 C6 65.3(3) . . . . ? C31 N4 C24 C6 -174.0(2) . . . . ? Co2 N4 C24 C6 -57.3(2) . . . . ? C1 C6 C24 N4 57.3(3) . . . . ? C5 C6 C24 N4 -130.5(2) . . . . ? C31 N4 C25 C26 140.7(2) . . . . ? C24 N4 C25 C26 -98.1(2) . . . . ? Co2 N4 C25 C26 26.4(2) . . . . ? C30 N5 C26 C27 1.2(4) . . . . ? Co2 N5 C26 C27 -167.9(2) . . . . ? C30 N5 C26 C25 -175.4(2) . . . . ? Co2 N5 C26 C25 15.5(3) . . . . ? N4 C25 C26 N5 -27.9(3) . . . . ? N4 C25 C26 C27 155.6(2) . . . . ? N5 C26 C27 C28 -0.8(4) . . . . ? C25 C26 C27 C28 175.5(3) . . . . ? C26 C27 C28 C29 -0.6(5) . . . . ? C27 C28 C29 C30 1.6(5) . . . . ? C26 N5 C30 C29 -0.2(4) . . . . ? Co2 N5 C30 C29 167.4(2) . . . . ? C28 C29 C30 N5 -1.2(5) . . . . ? C25 N4 C31 C32 -74.9(2) . . . . ? C24 N4 C31 C32 164.2(2) . . . . ? Co2 N4 C31 C32 42.6(2) . . . . ? C36 N6 C32 C33 1.8(4) . . . . ? Co2 N6 C32 C33 178.5(2) . . . . ? C36 N6 C32 C31 -177.6(2) . . . . ? Co2 N6 C32 C31 -0.9(3) . . . . ? N4 C31 C32 N6 -28.4(3) . . . . ? N4 C31 C32 C33 152.3(2) . . . . ? N6 C32 C33 C34 -1.5(4) . . . . ? C31 C32 C33 C34 177.8(3) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C33 C34 C35 C36 0.8(5) . . . . ? C32 N6 C36 C35 -0.8(4) . . . . ? Co2 N6 C36 C35 -177.0(2) . . . . ? C34 C35 C36 N6 -0.5(5) . . . . ? Co2 O5 C37 O4 -5.5(4) . . . . ? Co2 O5 C37 C38 175.75(18) . . . . ? Co1 O4 C37 O5 -16.4(4) . . . . ? Co1 O4 C37 C38 162.41(17) . . . . ? O5 C37 C38 Cl1 -6.1(3) . . . . ? O4 C37 C38 Cl1 174.95(19) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 913565' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a data_3 #TrackingRef '15833_web_deposit_cif_file_0_AndrewBond_1354442523.submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C38 H40 Cl2 Co2 N6 O5 2+, 2(B F4 -), 1.25(H2 O) ; _chemical_formula_sum 'C38 H42.50 B2 Cl2 Co2 F8 N6 O6.25' _chemical_formula_weight 1045.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6153(12) _cell_length_b 11.3123(15) _cell_length_c 18.840(2) _cell_angle_alpha 81.346(5) _cell_angle_beta 83.427(5) _cell_angle_gamma 75.393(4) _cell_volume 2157.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1996 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 20.30 _exptl_crystal_description lath _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1065 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.608652 ; _exptl_special_details ? _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 19324 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 25.29 _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.948 _reflns_number_total 7445 _reflns_number_gt 4197 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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^)+(0.0469P)^2^] 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 7445 _refine_ls_number_parameters 623 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.761 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.091 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 0.54018(6) 0.28994(6) 0.16880(3) 0.0219(2) Uani 1 1 d . . . Co2 Co 0.23958(6) 0.38525(6) 0.21688(3) 0.0226(2) Uani 1 1 d . . . Cl1 Cl 0.15103(14) 0.16824(13) 0.04219(8) 0.0487(4) Uani 1 1 d . . . Cl2 Cl 0.40870(16) 0.18399(17) -0.02571(8) 0.0656(5) Uani 1 1 d . . . O1 O 0.4074(3) 0.2944(3) 0.24564(16) 0.0212(8) Uani 1 1 d . . . O2 O 0.4331(3) 0.4218(3) 0.11558(17) 0.0252(8) Uani 1 1 d . . . O3 O 0.3333(3) 0.4896(3) 0.16034(17) 0.0267(8) Uani 1 1 d . . . O4 O 0.4613(3) 0.1818(3) 0.12735(17) 0.0268(8) Uani 1 1 d . . . O5 O 0.2477(3) 0.2836(3) 0.14206(17) 0.0264(8) Uani 1 1 d . . . N1 N 0.6613(4) 0.1438(3) 0.22086(19) 0.0201(10) Uani 1 1 d . . . N2 N 0.6283(4) 0.3872(3) 0.2110(2) 0.0215(10) Uani 1 1 d . . . N3 N 0.6697(4) 0.2594(4) 0.0904(2) 0.0261(10) Uani 1 1 d . . . N4 N 0.2022(4) 0.4941(3) 0.2922(2) 0.0227(10) Uani 1 1 d . . . N6 N 0.0803(4) 0.4900(4) 0.1822(2) 0.0276(11) Uani 1 1 d . . . N5 N 0.1562(4) 0.2740(4) 0.2893(2) 0.0262(10) Uani 1 1 d . . . C1 C 0.4432(4) 0.2801(4) 0.3145(2) 0.0188(11) Uani 1 1 d . . . C2 C 0.5342(4) 0.1724(4) 0.3377(2) 0.0191(11) Uani 1 1 d . . . C3 C 0.5757(5) 0.1583(4) 0.4064(3) 0.0236(12) Uani 1 1 d . . . H3A H 0.6402 0.0868 0.4218 0.028 Uiso 1 1 calc R . . C4 C 0.5260(5) 0.2454(4) 0.4534(3) 0.0222(12) Uani 1 1 d . . . C5 C 0.4365(4) 0.3521(4) 0.4282(3) 0.0221(12) Uani 1 1 d . . . H5A H 0.4009 0.4126 0.4597 0.026 Uiso 1 1 calc R . . C6 C 0.3974(4) 0.3730(4) 0.3583(3) 0.0202(12) Uani 1 1 d . . . C7 C 0.5747(5) 0.2257(4) 0.5293(3) 0.0254(12) Uani 1 1 d . . . C8 C 0.5654(5) 0.0969(4) 0.5675(3) 0.0408(15) Uani 1 1 d . . . H8A H 0.5965 0.0847 0.6157 0.061 Uiso 1 1 calc R . . H8B H 0.6195 0.0336 0.5393 0.061 Uiso 1 1 calc R . . H8C H 0.4744 0.0907 0.5716 0.061 Uiso 1 1 calc R . . C9 C 0.4926(5) 0.3186(5) 0.5771(3) 0.0417(15) Uani 1 1 d . . . H9A H 0.4955 0.4021 0.5550 0.063 Uiso 1 1 calc R . . H9B H 0.5273 0.3028 0.6245 0.063 Uiso 1 1 calc R . . H9C H 0.4020 0.3107 0.5826 0.063 Uiso 1 1 calc R . . C10 C 0.7161(5) 0.2360(5) 0.5221(3) 0.0512(17) Uani 1 1 d . . . H10A H 0.7212 0.3179 0.4980 0.077 Uiso 1 1 calc R . . H10B H 0.7698 0.1731 0.4937 0.077 Uiso 1 1 calc R . . H10C H 0.7481 0.2237 0.5701 0.077 Uiso 1 1 calc R . . C11 C 0.5909(5) 0.0824(4) 0.2843(2) 0.0253(13) Uani 1 1 d . . . H11A H 0.5200 0.0535 0.2676 0.030 Uiso 1 1 calc R . . H11B H 0.6525 0.0100 0.3077 0.030 Uiso 1 1 calc R . . C12 C 0.7680(5) 0.1896(4) 0.2457(3) 0.0247(12) Uani 1 1 d . . . H12A H 0.7940 0.1425 0.2926 0.030 Uiso 1 1 calc R . . H12B H 0.8453 0.1756 0.2105 0.030 Uiso 1 1 calc R . . C13 C 0.7248(4) 0.3227(4) 0.2534(3) 0.0209(12) Uani 1 1 d . . . C14 C 0.7789(5) 0.3795(5) 0.2975(3) 0.0274(13) Uani 1 1 d . . . H14A H 0.8441 0.3328 0.3279 0.033 Uiso 1 1 calc R . . C15 C 0.7368(5) 0.5062(5) 0.2968(3) 0.0352(14) Uani 1 1 d . . . H15A H 0.7715 0.5470 0.3277 0.042 Uiso 1 1 calc R . . C16 C 0.6438(5) 0.5728(5) 0.2508(3) 0.0307(13) Uani 1 1 d . . . H16A H 0.6171 0.6599 0.2481 0.037 Uiso 1 1 calc R . . C17 C 0.5909(5) 0.5111(4) 0.2094(3) 0.0250(12) Uani 1 1 d . . . H17A H 0.5258 0.5567 0.1786 0.030 Uiso 1 1 calc R . . C18 C 0.7165(5) 0.0622(4) 0.1641(2) 0.0240(12) Uani 1 1 d . . . H18A H 0.6535 0.0148 0.1566 0.029 Uiso 1 1 calc R . . H18B H 0.7982 0.0034 0.1787 0.029 Uiso 1 1 calc R . . C19 C 0.7434(5) 0.1429(4) 0.0958(3) 0.0255(12) Uani 1 1 d . . . C20 C 0.8317(5) 0.1041(5) 0.0399(3) 0.0342(14) Uani 1 1 d . . . H20A H 0.8857 0.0229 0.0446 0.041 Uiso 1 1 calc R . . C21 C 0.8429(5) 0.1825(5) -0.0236(3) 0.0396(15) Uani 1 1 d . . . H21A H 0.9016 0.1549 -0.0630 0.047 Uiso 1 1 calc R . . C22 C 0.7658(5) 0.3028(5) -0.0280(3) 0.0350(14) Uani 1 1 d . . . H22A H 0.7722 0.3593 -0.0703 0.042 Uiso 1 1 calc R . . C23 C 0.6808(5) 0.3381(5) 0.0294(3) 0.0292(13) Uani 1 1 d . . . H23A H 0.6281 0.4198 0.0266 0.035 Uiso 1 1 calc R . . C24 C 0.3211(4) 0.4984(4) 0.3266(3) 0.0223(12) Uani 1 1 d . . . H24A H 0.2940 0.5522 0.3652 0.027 Uiso 1 1 calc R . . H24B H 0.3791 0.5360 0.2901 0.027 Uiso 1 1 calc R . . C25 C 0.1048(5) 0.4537(4) 0.3490(3) 0.0286(13) Uani 1 1 d . . . H25A H 0.1220 0.4709 0.3965 0.034 Uiso 1 1 calc R . . H25B H 0.0156 0.5012 0.3384 0.034 Uiso 1 1 calc R . . C26 C 0.1130(5) 0.3197(4) 0.3518(3) 0.0255(13) Uani 1 1 d . . . C27 C 0.0743(5) 0.2481(5) 0.4126(3) 0.0383(15) Uani 1 1 d . . . H27A H 0.0452 0.2819 0.4565 0.046 Uiso 1 1 calc R . . C28 C 0.0790(6) 0.1266(5) 0.4079(3) 0.0459(17) Uani 1 1 d . . . H28A H 0.0526 0.0756 0.4488 0.055 Uiso 1 1 calc R . . C29 C 0.1214(5) 0.0798(5) 0.3447(3) 0.0405(15) Uani 1 1 d . . . H29A H 0.1238 -0.0035 0.3408 0.049 Uiso 1 1 calc R . . C30 C 0.1610(5) 0.1551(5) 0.2860(3) 0.0356(14) Uani 1 1 d . . . H30A H 0.1924 0.1218 0.2421 0.043 Uiso 1 1 calc R . . C31 C 0.1424(5) 0.6190(4) 0.2546(3) 0.0291(13) Uani 1 1 d . . . H31A H 0.0957 0.6744 0.2901 0.035 Uiso 1 1 calc R . . H31B H 0.2108 0.6558 0.2265 0.035 Uiso 1 1 calc R . . C32 C 0.0491(5) 0.6010(5) 0.2056(3) 0.0255(12) Uani 1 1 d . . . C33 C -0.0597(5) 0.6896(5) 0.1837(3) 0.0332(14) Uani 1 1 d . . . H33A H -0.0826 0.7671 0.2015 0.040 Uiso 1 1 calc R . . C34 C -0.1344(5) 0.6636(6) 0.1355(3) 0.0425(16) Uani 1 1 d . . . H34A H -0.2084 0.7243 0.1193 0.051 Uiso 1 1 calc R . . C35 C -0.1030(5) 0.5514(5) 0.1111(3) 0.0397(15) Uani 1 1 d . . . H35A H -0.1543 0.5330 0.0780 0.048 Uiso 1 1 calc R . . C36 C 0.0057(5) 0.4647(5) 0.1358(3) 0.0327(14) Uani 1 1 d . . . H36A H 0.0281 0.3859 0.1197 0.039 Uiso 1 1 calc R . . C37 C 0.3427(5) 0.2097(4) 0.1141(3) 0.0241(12) Uani 1 1 d . . . C38 C 0.3194(5) 0.1416(5) 0.0552(3) 0.0372(14) Uani 1 1 d . . . H38A H 0.3533 0.0514 0.0699 0.045 Uiso 1 1 calc R . . B1 B 0.6213(6) 0.1508(5) 0.7959(3) 0.0407(18) Uani 1 1 d D . . F1A F 0.6713(4) 0.1941(4) 0.73004(19) 0.0901(14) Uani 1 1 d DU . . F1B F 0.5006(3) 0.1307(3) 0.7933(2) 0.0884(14) Uani 1 1 d DU . . F1C F 0.7041(3) 0.0436(3) 0.8223(2) 0.0825(13) Uani 1 1 d DU . . F1D F 0.6118(4) 0.2364(3) 0.8404(2) 0.0799(12) Uani 1 1 d DU . . B2 B 0.1074(6) 0.1828(5) 0.6198(3) 0.050(2) Uani 1 1 d D . . F2A F 0.1020(9) 0.1131(9) 0.6857(4) 0.072(3) Uani 0.60 1 d PDU A 1 F2B F 0.1447(9) 0.2856(7) 0.6318(6) 0.108(4) Uani 0.60 1 d PDU A 1 F2C F -0.0122(7) 0.2195(9) 0.5963(5) 0.091(3) Uani 0.60 1 d PDU A 1 F2D F 0.1996(9) 0.1236(10) 0.5744(5) 0.083(4) Uani 0.60 1 d PDU A 1 F2E F 0.1580(16) 0.0985(14) 0.5740(8) 0.128(9) Uani 0.40 1 d PDU A 2 F2H F 0.0187(13) 0.2791(11) 0.5880(8) 0.104(6) Uani 0.40 1 d PDU A 2 F2G F 0.0438(16) 0.1266(15) 0.6777(8) 0.141(9) Uani 0.40 1 d PDU A 2 F2F F 0.1993(13) 0.2241(14) 0.6442(10) 0.167(9) Uani 0.40 1 d PDU A 2 O1W O 0.9687(4) 0.0412(4) 0.8140(2) 0.0737(14) Uani 1 1 d . . . H1W H 0.8890 0.0418 0.8171 0.111 Uiso 1 1 d R . . H2W H 1.0061 0.0635 0.7744 0.111 Uiso 1 1 d R . . O2W O 0.1367(18) 0.4718(19) 0.5301(10) 0.095(7) Uani 0.25 1 d P . . H3W H 0.0881 0.5047 0.4968 0.143 Uiso 0.25 1 d PR . . H4W H 0.1109 0.4096 0.5501 0.143 Uiso 0.25 1 d PR . . 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 0.0218(4) 0.0215(4) 0.0215(4) -0.0001(3) -0.0034(3) -0.0039(3) Co2 0.0208(4) 0.0251(4) 0.0217(4) -0.0004(3) -0.0037(3) -0.0059(3) Cl1 0.0438(10) 0.0590(10) 0.0517(10) -0.0169(8) -0.0202(8) -0.0146(8) Cl2 0.0467(11) 0.1151(15) 0.0306(9) -0.0152(10) -0.0077(8) -0.0056(10) O1 0.023(2) 0.0216(18) 0.0182(19) 0.0002(15) -0.0043(15) -0.0044(15) O2 0.023(2) 0.0254(19) 0.022(2) -0.0009(16) -0.0017(16) 0.0020(16) O3 0.025(2) 0.0224(19) 0.031(2) 0.0017(16) -0.0030(17) -0.0040(16) O4 0.030(2) 0.027(2) 0.025(2) -0.0037(16) -0.0061(17) -0.0074(16) O5 0.026(2) 0.031(2) 0.023(2) -0.0053(17) -0.0040(17) -0.0062(17) N1 0.025(2) 0.020(2) 0.017(2) -0.0039(19) -0.0039(19) -0.0064(19) N2 0.018(2) 0.021(2) 0.024(2) -0.0014(19) 0.0023(19) -0.0036(18) N3 0.026(3) 0.029(3) 0.024(3) -0.001(2) -0.007(2) -0.007(2) N4 0.017(2) 0.023(2) 0.026(3) -0.0011(19) -0.0022(19) -0.0038(19) N6 0.023(3) 0.035(3) 0.024(3) 0.001(2) -0.001(2) -0.008(2) N5 0.026(3) 0.026(3) 0.028(3) -0.001(2) -0.007(2) -0.007(2) C1 0.018(3) 0.024(3) 0.017(3) 0.001(2) -0.004(2) -0.012(2) C2 0.017(3) 0.020(3) 0.020(3) -0.002(2) 0.000(2) -0.006(2) C3 0.023(3) 0.022(3) 0.024(3) 0.003(2) -0.005(2) -0.004(2) C4 0.022(3) 0.027(3) 0.020(3) 0.000(2) -0.004(2) -0.012(2) C5 0.021(3) 0.024(3) 0.024(3) -0.010(2) 0.001(2) -0.006(2) C6 0.013(3) 0.024(3) 0.024(3) -0.005(2) -0.003(2) -0.004(2) C7 0.032(3) 0.028(3) 0.019(3) -0.005(2) -0.006(2) -0.008(2) C8 0.059(4) 0.035(3) 0.029(3) 0.004(3) -0.013(3) -0.011(3) C9 0.055(4) 0.043(4) 0.029(3) -0.001(3) -0.013(3) -0.013(3) C10 0.045(4) 0.073(5) 0.041(4) -0.002(3) -0.015(3) -0.023(3) C11 0.030(3) 0.019(3) 0.026(3) 0.007(2) -0.007(2) -0.009(2) C12 0.023(3) 0.025(3) 0.026(3) -0.005(2) -0.005(2) -0.002(2) C13 0.014(3) 0.025(3) 0.022(3) -0.002(2) 0.000(2) -0.003(2) C14 0.021(3) 0.034(3) 0.030(3) -0.005(3) -0.008(2) -0.008(2) C15 0.028(3) 0.041(4) 0.044(4) -0.021(3) 0.003(3) -0.014(3) C16 0.027(3) 0.023(3) 0.045(4) -0.009(3) -0.001(3) -0.008(2) C17 0.021(3) 0.024(3) 0.027(3) 0.001(2) 0.001(2) -0.002(2) C18 0.026(3) 0.018(3) 0.026(3) -0.007(2) -0.002(2) 0.001(2) C19 0.028(3) 0.027(3) 0.022(3) -0.007(3) -0.001(3) -0.006(3) C20 0.030(3) 0.037(3) 0.032(3) -0.003(3) -0.006(3) -0.001(3) C21 0.029(3) 0.061(4) 0.023(3) -0.010(3) 0.002(3) 0.001(3) C22 0.030(3) 0.044(4) 0.026(3) 0.001(3) -0.001(3) -0.004(3) C23 0.026(3) 0.031(3) 0.029(3) 0.000(3) -0.007(3) -0.003(2) C24 0.019(3) 0.023(3) 0.025(3) -0.005(2) -0.006(2) -0.003(2) C25 0.021(3) 0.037(3) 0.026(3) -0.003(3) 0.004(2) -0.007(2) C26 0.020(3) 0.030(3) 0.025(3) 0.006(3) -0.004(2) -0.008(2) C27 0.034(4) 0.047(4) 0.031(3) 0.004(3) -0.002(3) -0.009(3) C28 0.049(4) 0.040(4) 0.043(4) 0.017(3) 0.001(3) -0.016(3) C29 0.049(4) 0.031(3) 0.044(4) 0.007(3) -0.007(3) -0.019(3) C30 0.040(4) 0.031(3) 0.038(4) -0.004(3) -0.005(3) -0.013(3) C31 0.031(3) 0.022(3) 0.029(3) -0.003(2) -0.001(3) 0.003(2) C32 0.019(3) 0.031(3) 0.023(3) 0.004(3) -0.005(2) -0.002(2) C33 0.024(3) 0.033(3) 0.036(4) 0.002(3) -0.005(3) 0.001(3) C34 0.027(4) 0.053(4) 0.037(4) 0.009(3) -0.010(3) 0.004(3) C35 0.030(4) 0.056(4) 0.032(4) 0.001(3) -0.018(3) -0.006(3) C36 0.027(3) 0.040(3) 0.034(3) -0.004(3) -0.007(3) -0.012(3) C37 0.035(4) 0.025(3) 0.015(3) 0.000(2) -0.007(3) -0.012(3) C38 0.040(4) 0.040(3) 0.033(3) -0.003(3) -0.018(3) -0.008(3) B1 0.040(5) 0.031(4) 0.046(5) 0.003(4) -0.015(4) 0.002(3) F1A 0.115(4) 0.111(3) 0.055(3) 0.024(2) -0.020(2) -0.060(3) F1B 0.064(3) 0.065(3) 0.143(4) 0.009(3) -0.031(3) -0.029(2) F1C 0.068(3) 0.050(2) 0.110(3) 0.012(2) 0.002(2) 0.005(2) F1D 0.089(3) 0.068(3) 0.093(3) -0.034(2) -0.007(2) -0.023(2) B2 0.037(5) 0.068(6) 0.038(5) -0.011(5) 0.000(4) 0.006(4) F2A 0.067(6) 0.082(6) 0.042(4) 0.016(4) 0.009(4) 0.009(4) F2B 0.090(7) 0.070(6) 0.178(9) -0.045(6) 0.026(7) -0.044(6) F2C 0.036(4) 0.155(9) 0.081(6) -0.018(7) -0.020(4) -0.016(5) F2D 0.057(5) 0.122(8) 0.053(6) -0.015(5) -0.002(4) 0.012(5) F2E 0.147(14) 0.115(12) 0.065(11) -0.041(9) -0.021(10) 0.097(10) F2H 0.130(13) 0.085(9) 0.070(9) -0.038(7) -0.031(9) 0.047(8) F2G 0.139(15) 0.120(14) 0.176(16) -0.040(11) 0.065(11) -0.077(12) F2F 0.104(12) 0.156(15) 0.271(18) -0.045(13) -0.059(12) -0.056(11) O1W 0.048(3) 0.089(3) 0.086(4) -0.015(3) -0.007(3) -0.018(3) O2W 0.070(15) 0.16(2) 0.057(13) -0.023(13) 0.022(11) -0.035(14) _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 O2 1.865(3) . ? Co1 O1 1.898(3) . ? Co1 N3 1.907(4) . ? Co1 N2 1.916(4) . ? Co1 O4 1.939(3) . ? Co1 N1 2.019(4) . ? Co2 O3 1.867(3) . ? Co2 O1 1.912(3) . ? Co2 N6 1.923(4) . ? Co2 O5 1.931(3) . ? Co2 N4 1.958(4) . ? Co2 N5 2.000(4) . ? Cl1 C38 1.775(5) . ? Cl2 C38 1.770(5) . ? O1 C1 1.368(5) . ? O2 O3 1.415(4) . ? O4 C37 1.263(6) . ? O5 C37 1.257(6) . ? N1 C18 1.491(6) . ? N1 C12 1.504(5) . ? N1 C11 1.509(5) . ? N2 C17 1.354(5) . ? N2 C13 1.363(5) . ? N3 C19 1.349(6) . ? N3 C23 1.357(6) . ? N4 C24 1.498(5) . ? N4 C31 1.500(5) . ? N4 C25 1.504(5) . ? N6 C32 1.344(6) . ? N6 C36 1.349(6) . ? N5 C26 1.343(6) . ? N5 C30 1.343(6) . ? C1 C6 1.392(6) . ? C1 C2 1.397(6) . ? C2 C3 1.389(6) . ? C2 C11 1.508(6) . ? C3 C4 1.387(7) . ? C3 H3A 0.9500 . ? C4 C5 1.392(6) . ? C4 C7 1.543(6) . ? C5 C6 1.394(6) . ? C5 H5A 0.9500 . ? C6 C24 1.518(6) . ? C7 C9 1.522(7) . ? C7 C10 1.523(7) . ? C7 C8 1.546(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.483(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.374(6) . ? C14 C15 1.389(6) . ? C14 H14A 0.9500 . ? C15 C16 1.385(7) . ? C15 H15A 0.9500 . ? C16 C17 1.368(6) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.504(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.373(7) . ? C20 C21 1.390(7) . ? C20 H20A 0.9500 . ? C21 C22 1.396(7) . ? C21 H21A 0.9500 . ? C22 C23 1.367(7) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.489(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.386(6) . ? C27 C28 1.379(7) . ? C27 H27A 0.9500 . ? C28 C29 1.360(8) . ? C28 H28A 0.9500 . ? C29 C30 1.384(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.496(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.382(6) . ? C33 C34 1.380(7) . ? C33 H33A 0.9500 . ? C34 C35 1.365(7) . ? C34 H34A 0.9500 . ? C35 C36 1.387(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.517(7) . ? C38 H38A 1.0000 . ? B1 F1D 1.351(6) . ? B1 F1A 1.364(6) . ? B1 F1B 1.364(6) . ? B1 F1C 1.368(6) . ? B2 F2F 1.333(8) . ? B2 F2C 1.337(7) . ? B2 F2D 1.338(7) . ? B2 F2E 1.351(8) . ? B2 F2H 1.360(8) . ? B2 F2A 1.370(7) . ? B2 F2G 1.373(8) . ? B2 F2B 1.375(7) . ? O1W H1W 0.8400 . ? O1W H2W 0.8400 . ? O2W H3W 0.8401 . ? O2W H4W 0.8400 . ? 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 O2 Co1 O1 90.47(13) . . ? O2 Co1 N3 93.64(15) . . ? O1 Co1 N3 170.61(15) . . ? O2 Co1 N2 96.11(15) . . ? O1 Co1 N2 93.45(14) . . ? N3 Co1 N2 94.50(16) . . ? O2 Co1 O4 87.58(13) . . ? O1 Co1 O4 88.04(13) . . ? N3 Co1 O4 83.72(15) . . ? N2 Co1 O4 176.00(16) . . ? O2 Co1 N1 176.61(15) . . ? O1 Co1 N1 92.52(14) . . ? N3 Co1 N1 83.17(16) . . ? N2 Co1 N1 85.30(15) . . ? O4 Co1 N1 90.93(14) . . ? O3 Co2 O1 84.22(13) . . ? O3 Co2 N6 89.48(14) . . ? O1 Co2 N6 173.67(14) . . ? O3 Co2 O5 94.29(14) . . ? O1 Co2 O5 91.94(14) . . ? N6 Co2 O5 89.10(17) . . ? O3 Co2 N4 89.98(14) . . ? O1 Co2 N4 96.17(15) . . ? N6 Co2 N4 83.22(17) . . ? O5 Co2 N4 171.19(15) . . ? O3 Co2 N5 171.30(15) . . ? O1 Co2 N5 89.57(14) . . ? N6 Co2 N5 96.63(16) . . ? O5 Co2 N5 92.00(15) . . ? N4 Co2 N5 84.63(16) . . ? C1 O1 Co1 118.1(3) . . ? C1 O1 Co2 123.7(3) . . ? Co1 O1 Co2 112.73(15) . . ? O3 O2 Co1 111.6(2) . . ? O2 O3 Co2 110.4(2) . . ? C37 O4 Co1 122.9(3) . . ? C37 O5 Co2 130.7(3) . . ? C18 N1 C12 109.8(4) . . ? C18 N1 C11 113.2(3) . . ? C12 N1 C11 110.2(3) . . ? C18 N1 Co1 103.9(3) . . ? C12 N1 Co1 107.5(2) . . ? C11 N1 Co1 111.9(3) . . ? C17 N2 C13 118.7(4) . . ? C17 N2 Co1 125.1(3) . . ? C13 N2 Co1 115.6(3) . . ? C19 N3 C23 120.2(5) . . ? C19 N3 Co1 113.6(3) . . ? C23 N3 Co1 125.7(4) . . ? C24 N4 C31 109.9(3) . . ? C24 N4 C25 109.4(4) . . ? C31 N4 C25 109.7(4) . . ? C24 N4 Co2 113.6(3) . . ? C31 N4 Co2 104.7(3) . . ? C25 N4 Co2 109.4(3) . . ? C32 N6 C36 119.8(4) . . ? C32 N6 Co2 113.2(3) . . ? C36 N6 Co2 126.9(4) . . ? C26 N5 C30 118.6(4) . . ? C26 N5 Co2 113.8(3) . . ? C30 N5 Co2 126.5(4) . . ? O1 C1 C6 121.2(4) . . ? O1 C1 C2 117.8(4) . . ? C6 C1 C2 120.9(4) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 C11 123.3(4) . . ? C1 C2 C11 117.8(4) . . ? C4 C3 C2 122.1(5) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C7 120.3(4) . . ? C5 C4 C7 121.9(5) . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C1 C6 C5 118.4(4) . . ? C1 C6 C24 119.5(4) . . ? C5 C6 C24 121.7(4) . . ? C9 C7 C10 109.5(4) . . ? C9 C7 C4 112.4(4) . . ? C10 C7 C4 108.7(4) . . ? C9 C7 C8 106.5(4) . . ? C10 C7 C8 109.9(4) . . ? C4 C7 C8 109.7(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 N1 109.8(3) . . ? C2 C11 H11A 109.7 . . ? N1 C11 H11A 109.7 . . ? C2 C11 H11B 109.7 . . ? N1 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C13 C12 N1 111.3(4) . . ? C13 C12 H12A 109.4 . . ? N1 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? N1 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N2 C13 C14 121.5(4) . . ? N2 C13 C12 114.5(4) . . ? C14 C13 C12 123.9(4) . . ? C13 C14 C15 119.0(5) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C17 C16 C15 119.0(5) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? N2 C17 C16 122.1(5) . . ? N2 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? N1 C18 C19 107.7(4) . . ? N1 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? N1 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? N3 C19 C20 120.0(4) . . ? N3 C19 C18 115.3(4) . . ? C20 C19 C18 124.7(5) . . ? C19 C20 C21 120.7(5) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C22 118.4(5) . . ? C20 C21 H21A 120.8 . . ? C22 C21 H21A 120.8 . . ? C23 C22 C21 118.9(5) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? N3 C23 C22 121.8(5) . . ? N3 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? N4 C24 C6 113.6(3) . . ? N4 C24 H24A 108.8 . . ? C6 C24 H24A 108.8 . . ? N4 C24 H24B 108.8 . . ? C6 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 N4 110.9(4) . . ? C26 C25 H25A 109.5 . . ? N4 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? N4 C25 H25B 109.5 . . ? H25A C25 H25B 108.0 . . ? N5 C26 C27 122.1(5) . . ? N5 C26 C25 114.6(4) . . ? C27 C26 C25 123.3(5) . . ? C28 C27 C26 118.4(5) . . ? C28 C27 H27A 120.8 . . ? C26 C27 H27A 120.8 . . ? C29 C28 C27 119.9(5) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 119.2(5) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? N5 C30 C29 121.8(5) . . ? N5 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? C32 C31 N4 106.7(4) . . ? C32 C31 H31A 110.4 . . ? N4 C31 H31A 110.4 . . ? C32 C31 H31B 110.4 . . ? N4 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? N6 C32 C33 120.9(5) . . ? N6 C32 C31 114.6(4) . . ? C33 C32 C31 124.5(5) . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 120.6(5) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 118.3(5) . . ? C34 C35 H35A 120.8 . . ? C36 C35 H35A 120.8 . . ? N6 C36 C35 121.5(5) . . ? N6 C36 H36A 119.3 . . ? C35 C36 H36A 119.3 . . ? O5 C37 O4 129.1(5) . . ? O5 C37 C38 118.9(5) . . ? O4 C37 C38 111.9(5) . . ? C37 C38 Cl2 109.4(3) . . ? C37 C38 Cl1 112.3(4) . . ? Cl2 C38 Cl1 110.9(3) . . ? C37 C38 H38A 108.0 . . ? Cl2 C38 H38A 108.0 . . ? Cl1 C38 H38A 108.0 . . ? F1D B1 F1A 107.5(5) . . ? F1D B1 F1B 108.9(5) . . ? F1A B1 F1B 112.1(5) . . ? F1D B1 F1C 109.1(5) . . ? F1A B1 F1C 109.8(5) . . ? F1B B1 F1C 109.4(4) . . ? F2A B2 F2B 105.7(6) . . ? F2C B2 F2A 109.3(6) . . ? F2D B2 F2A 110.9(7) . . ? F2C B2 F2B 107.9(6) . . ? F2D B2 F2B 107.4(6) . . ? F2C B2 F2D 115.1(7) . . ? F2F B2 F2E 112.3(8) . . ? F2F B2 F2H 109.7(7) . . ? F2E B2 F2H 110.8(8) . . ? F2F B2 F2G 108.3(8) . . ? F2E B2 F2G 107.6(8) . . ? F2H B2 F2G 108.1(8) . . ? H1W O1W H2W 120.1 . . ? H3W O2W H4W 107.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 -138.0(3) . . . . ? N2 Co1 O1 C1 -41.8(3) . . . . ? O4 Co1 O1 C1 134.5(3) . . . . ? N1 Co1 O1 C1 43.6(3) . . . . ? O2 Co1 O1 Co2 16.90(17) . . . . ? N2 Co1 O1 Co2 113.05(17) . . . . ? O4 Co1 O1 Co2 -70.67(16) . . . . ? N1 Co1 O1 Co2 -161.51(17) . . . . ? O3 Co2 O1 C1 115.4(3) . . . . ? O5 Co2 O1 C1 -150.5(3) . . . . ? N4 Co2 O1 C1 26.0(3) . . . . ? N5 Co2 O1 C1 -58.5(3) . . . . ? O3 Co2 O1 Co1 -37.88(16) . . . . ? O5 Co2 O1 Co1 56.23(16) . . . . ? N4 Co2 O1 Co1 -127.23(16) . . . . ? N5 Co2 O1 Co1 148.22(18) . . . . ? O1 Co1 O2 O3 20.7(2) . . . . ? N3 Co1 O2 O3 -167.8(2) . . . . ? N2 Co1 O2 O3 -72.8(2) . . . . ? O4 Co1 O2 O3 108.7(2) . . . . ? Co1 O2 O3 Co2 -54.0(3) . . . . ? O1 Co2 O3 O2 54.4(2) . . . . ? N6 Co2 O3 O2 -126.1(3) . . . . ? O5 Co2 O3 O2 -37.1(2) . . . . ? N4 Co2 O3 O2 150.6(2) . . . . ? O2 Co1 O4 C37 -35.6(4) . . . . ? O1 Co1 O4 C37 55.0(4) . . . . ? N3 Co1 O4 C37 -129.5(4) . . . . ? N1 Co1 O4 C37 147.5(4) . . . . ? O3 Co2 O5 C37 68.9(4) . . . . ? O1 Co2 O5 C37 -15.5(4) . . . . ? N6 Co2 O5 C37 158.3(4) . . . . ? N5 Co2 O5 C37 -105.1(4) . . . . ? O1 Co1 N1 C18 136.7(3) . . . . ? N3 Co1 N1 C18 -35.0(3) . . . . ? N2 Co1 N1 C18 -130.1(3) . . . . ? O4 Co1 N1 C18 48.6(3) . . . . ? O1 Co1 N1 C12 -107.0(3) . . . . ? N3 Co1 N1 C12 81.3(3) . . . . ? N2 Co1 N1 C12 -13.8(3) . . . . ? O4 Co1 N1 C12 164.9(3) . . . . ? O1 Co1 N1 C11 14.1(3) . . . . ? N3 Co1 N1 C11 -157.5(3) . . . . ? N2 Co1 N1 C11 107.4(3) . . . . ? O4 Co1 N1 C11 -73.9(3) . . . . ? O2 Co1 N2 C17 12.3(4) . . . . ? O1 Co1 N2 C17 -78.5(4) . . . . ? N3 Co1 N2 C17 106.5(4) . . . . ? N1 Co1 N2 C17 -170.8(4) . . . . ? O2 Co1 N2 C13 -176.8(3) . . . . ? O1 Co1 N2 C13 92.4(3) . . . . ? N3 Co1 N2 C13 -82.6(3) . . . . ? N1 Co1 N2 C13 0.1(3) . . . . ? O2 Co1 N3 C19 -156.1(3) . . . . ? N2 Co1 N3 C19 107.5(3) . . . . ? O4 Co1 N3 C19 -68.9(3) . . . . ? N1 Co1 N3 C19 22.8(3) . . . . ? O2 Co1 N3 C23 15.8(4) . . . . ? N2 Co1 N3 C23 -80.7(4) . . . . ? O4 Co1 N3 C23 102.9(4) . . . . ? N1 Co1 N3 C23 -165.4(4) . . . . ? O3 Co2 N4 C24 -66.1(3) . . . . ? O1 Co2 N4 C24 18.0(3) . . . . ? N6 Co2 N4 C24 -155.6(3) . . . . ? N5 Co2 N4 C24 107.0(3) . . . . ? O3 Co2 N4 C31 53.8(3) . . . . ? O1 Co2 N4 C31 138.0(3) . . . . ? N6 Co2 N4 C31 -35.7(3) . . . . ? N5 Co2 N4 C31 -133.0(3) . . . . ? O3 Co2 N4 C25 171.3(3) . . . . ? O1 Co2 N4 C25 -104.5(3) . . . . ? N6 Co2 N4 C25 81.8(3) . . . . ? N5 Co2 N4 C25 -15.5(3) . . . . ? O3 Co2 N6 C32 -68.2(3) . . . . ? O5 Co2 N6 C32 -162.5(3) . . . . ? N4 Co2 N6 C32 21.8(3) . . . . ? N5 Co2 N6 C32 105.6(3) . . . . ? O3 Co2 N6 C36 108.1(4) . . . . ? O5 Co2 N6 C36 13.8(4) . . . . ? N4 Co2 N6 C36 -161.8(4) . . . . ? N5 Co2 N6 C36 -78.1(4) . . . . ? O1 Co2 N5 C26 97.2(3) . . . . ? N6 Co2 N5 C26 -81.5(4) . . . . ? O5 Co2 N5 C26 -170.9(3) . . . . ? N4 Co2 N5 C26 1.0(3) . . . . ? O1 Co2 N5 C30 -70.2(4) . . . . ? N6 Co2 N5 C30 111.1(4) . . . . ? O5 Co2 N5 C30 21.8(4) . . . . ? N4 Co2 N5 C30 -166.4(4) . . . . ? Co1 O1 C1 C6 117.9(4) . . . . ? Co2 O1 C1 C6 -34.1(5) . . . . ? Co1 O1 C1 C2 -58.0(4) . . . . ? Co2 O1 C1 C2 150.1(3) . . . . ? O1 C1 C2 C3 177.5(4) . . . . ? C6 C1 C2 C3 1.6(6) . . . . ? O1 C1 C2 C11 2.7(6) . . . . ? C6 C1 C2 C11 -173.1(4) . . . . ? C1 C2 C3 C4 2.6(6) . . . . ? C11 C2 C3 C4 177.0(4) . . . . ? C2 C3 C4 C5 -3.2(7) . . . . ? C2 C3 C4 C7 179.8(4) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? C7 C4 C5 C6 176.6(4) . . . . ? O1 C1 C6 C5 179.3(4) . . . . ? C2 C1 C6 C5 -4.9(6) . . . . ? O1 C1 C6 C24 -8.2(6) . . . . ? C2 C1 C6 C24 167.6(4) . . . . ? C4 C5 C6 C1 4.4(6) . . . . ? C4 C5 C6 C24 -168.0(4) . . . . ? C3 C4 C7 C9 -169.9(4) . . . . ? C5 C4 C7 C9 13.2(6) . . . . ? C3 C4 C7 C10 68.7(5) . . . . ? C5 C4 C7 C10 -108.2(5) . . . . ? C3 C4 C7 C8 -51.5(6) . . . . ? C5 C4 C7 C8 131.6(5) . . . . ? C3 C2 C11 N1 -114.3(4) . . . . ? C1 C2 C11 N1 60.2(5) . . . . ? C18 N1 C11 C2 -178.0(4) . . . . ? C12 N1 C11 C2 58.6(5) . . . . ? Co1 N1 C11 C2 -60.9(4) . . . . ? C18 N1 C12 C13 136.7(4) . . . . ? C11 N1 C12 C13 -98.0(4) . . . . ? Co1 N1 C12 C13 24.3(4) . . . . ? C17 N2 C13 C14 3.9(6) . . . . ? Co1 N2 C13 C14 -167.6(3) . . . . ? C17 N2 C13 C12 -174.0(4) . . . . ? Co1 N2 C13 C12 14.5(5) . . . . ? N1 C12 C13 N2 -26.0(5) . . . . ? N1 C12 C13 C14 156.1(4) . . . . ? N2 C13 C14 C15 -2.1(7) . . . . ? C12 C13 C14 C15 175.7(4) . . . . ? C13 C14 C15 C16 -1.4(7) . . . . ? C14 C15 C16 C17 3.1(7) . . . . ? C13 N2 C17 C16 -2.2(7) . . . . ? Co1 N2 C17 C16 168.4(4) . . . . ? C15 C16 C17 N2 -1.3(7) . . . . ? C12 N1 C18 C19 -74.6(4) . . . . ? C11 N1 C18 C19 161.7(4) . . . . ? Co1 N1 C18 C19 40.0(4) . . . . ? C23 N3 C19 C20 1.1(7) . . . . ? Co1 N3 C19 C20 173.5(4) . . . . ? C23 N3 C19 C18 -176.4(4) . . . . ? Co1 N3 C19 C18 -4.0(5) . . . . ? N1 C18 C19 N3 -25.7(6) . . . . ? N1 C18 C19 C20 157.0(5) . . . . ? N3 C19 C20 C21 -2.3(8) . . . . ? C18 C19 C20 C21 174.9(5) . . . . ? C19 C20 C21 C22 2.3(8) . . . . ? C20 C21 C22 C23 -1.2(8) . . . . ? C19 N3 C23 C22 0.0(7) . . . . ? Co1 N3 C23 C22 -171.3(4) . . . . ? C21 C22 C23 N3 0.0(8) . . . . ? C31 N4 C24 C6 -173.1(4) . . . . ? C25 N4 C24 C6 66.3(5) . . . . ? Co2 N4 C24 C6 -56.2(4) . . . . ? C1 C6 C24 N4 57.0(6) . . . . ? C5 C6 C24 N4 -130.8(4) . . . . ? C24 N4 C25 C26 -98.2(4) . . . . ? C31 N4 C25 C26 141.1(4) . . . . ? Co2 N4 C25 C26 26.7(5) . . . . ? C30 N5 C26 C27 0.4(7) . . . . ? Co2 N5 C26 C27 -168.1(4) . . . . ? C30 N5 C26 C25 -177.0(4) . . . . ? Co2 N5 C26 C25 14.5(5) . . . . ? N4 C25 C26 N5 -27.4(6) . . . . ? N4 C25 C26 C27 155.2(4) . . . . ? N5 C26 C27 C28 -0.9(8) . . . . ? C25 C26 C27 C28 176.3(5) . . . . ? C26 C27 C28 C29 0.3(8) . . . . ? C27 C28 C29 C30 0.8(9) . . . . ? C26 N5 C30 C29 0.8(7) . . . . ? Co2 N5 C30 C29 167.6(4) . . . . ? C28 C29 C30 N5 -1.4(8) . . . . ? C24 N4 C31 C32 164.8(4) . . . . ? C25 N4 C31 C32 -74.8(5) . . . . ? Co2 N4 C31 C32 42.5(4) . . . . ? C36 N6 C32 C33 0.9(7) . . . . ? Co2 N6 C32 C33 177.5(4) . . . . ? C36 N6 C32 C31 -177.8(4) . . . . ? Co2 N6 C32 C31 -1.1(5) . . . . ? N4 C31 C32 N6 -28.2(5) . . . . ? N4 C31 C32 C33 153.2(4) . . . . ? N6 C32 C33 C34 -1.7(7) . . . . ? C31 C32 C33 C34 176.8(5) . . . . ? C32 C33 C34 C35 1.3(8) . . . . ? C33 C34 C35 C36 -0.1(8) . . . . ? C32 N6 C36 C35 0.4(7) . . . . ? Co2 N6 C36 C35 -175.7(4) . . . . ? C34 C35 C36 N6 -0.8(8) . . . . ? Co2 O5 C37 O4 -0.5(7) . . . . ? Co2 O5 C37 C38 -179.9(3) . . . . ? Co1 O4 C37 O5 -24.1(7) . . . . ? Co1 O4 C37 C38 155.3(3) . . . . ? O5 C37 C38 Cl2 117.4(4) . . . . ? O4 C37 C38 Cl2 -62.1(5) . . . . ? O5 C37 C38 Cl1 -6.3(6) . . . . ? O4 C37 C38 Cl1 174.2(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 913566' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a data_4 #TrackingRef '15833_web_deposit_cif_file_0_AndrewBond_1354442523.submit.cif' ###################################### ## refinement against SQUEEZED data ## ###################################### loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.011 0.000 -0.006 1574.9 691.3 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H39 Cl3 Co2 N6 O5 2+, 2(Cl O4 -)' _chemical_formula_sum 'C38 H39 Cl5 Co2 N6 O13' _chemical_formula_weight 1082.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.340(2) _cell_length_b 16.437(3) _cell_length_c 18.524(3) _cell_angle_alpha 77.664(6) _cell_angle_beta 88.953(6) _cell_angle_gamma 73.611(6) _cell_volume 3517.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5214 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 18.90 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.568 _exptl_absorpt_correction_T_max 0.872 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.651543 ; _exptl_special_details ; Structure contains huge voids occupied by diffuse solvent. Little can be done to model this with discrete atomic sites. Including numerous partially occupied water molecules gives a best wR2 ca 40 %. This CIF is based on refinement against SQUEEZED data (v.d.Sluis & Spek, 1990). SQUEEZE identifies one void of ca 1575 cubic angstrom per unit cell and suggests that it is occupied by ca 700 electrons. This could comprise water, toluene or acetone, or a combination thereof. Comparable results were obtained from two different crystals. The remaining difference density is in the vicinity of the perchlorate anion containing Cl4, suggesting that it is rotationally disordered. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 59425 _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_sigmaI/netI 0.1431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.976 _reflns_number_total 12127 _reflns_number_gt 6429 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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^)+(0.1112P)^2^] 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 12127 _refine_ls_number_parameters 581 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2026 _refine_ls_wR_factor_gt 0.1897 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.281 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.103 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 0.35054(6) 0.29325(4) 0.76303(4) 0.0291(2) Uani 1 1 d . . . Co2 Co 0.32084(6) 0.48667(4) 0.67605(4) 0.0262(2) Uani 1 1 d . . . Cl1 Cl 0.17558(14) 0.41056(10) 0.47628(8) 0.0539(4) Uani 1 1 d . . . Cl2 Cl 0.02285(13) 0.36291(13) 0.58438(9) 0.0671(5) Uani 1 1 d . . . Cl3 Cl 0.22468(19) 0.23429(11) 0.55838(10) 0.0818(6) Uani 1 1 d . . . O1 O 0.2880(3) 0.41321(19) 0.76308(17) 0.0277(8) Uani 1 1 d . . . O2 O 0.4449(3) 0.3213(2) 0.68744(18) 0.0293(8) Uani 1 1 d . . . O3 O 0.4614(3) 0.4039(2) 0.68400(18) 0.0311(8) Uani 1 1 d . . . O4 O 0.2382(3) 0.3086(2) 0.68572(18) 0.0315(8) Uani 1 1 d . . . O5 O 0.2527(3) 0.4334(2) 0.61211(18) 0.0310(8) Uani 1 1 d . . . N1 N 0.2520(4) 0.2563(3) 0.8424(2) 0.0350(11) Uani 1 1 d . . . N2 N 0.4584(3) 0.2758(2) 0.8411(2) 0.0280(10) Uani 1 1 d . . . N3 N 0.3903(4) 0.1730(3) 0.7578(2) 0.0390(12) Uani 1 1 d . . . N4 N 0.3838(3) 0.5563(3) 0.7275(2) 0.0299(10) Uani 1 1 d . . . N5 N 0.1724(3) 0.5728(2) 0.6846(2) 0.0302(10) Uani 1 1 d . . . N6 N 0.3698(3) 0.5541(2) 0.5908(2) 0.0266(10) Uani 1 1 d . . . C1 C 0.2704(4) 0.4353(3) 0.8316(3) 0.0263(12) Uani 1 1 d . . . C2 C 0.1988(4) 0.3966(3) 0.8781(3) 0.0264(12) Uani 1 1 d . . . C3 C 0.1816(4) 0.4175(3) 0.9473(3) 0.0309(13) Uani 1 1 d . . . H3A H 0.1339 0.3923 0.9799 0.037 Uiso 1 1 calc R . . C4 C 0.2313(4) 0.4729(3) 0.9697(3) 0.0357(13) Uani 1 1 d . . . C5 C 0.3016(4) 0.5098(3) 0.9209(3) 0.0351(13) Uani 1 1 d . . . H5A H 0.3348 0.5496 0.9356 0.042 Uiso 1 1 calc R . . C6 C 0.3243(4) 0.4901(3) 0.8521(3) 0.0259(12) Uani 1 1 d . . . C7 C 0.2177(5) 0.4936(4) 1.0481(3) 0.0401(14) Uani 1 1 d . . . C8 C 0.1419(5) 0.4447(4) 1.0960(3) 0.0585(18) Uani 1 1 d . . . H8A H 0.0650 0.4651 1.0736 0.088 Uiso 1 1 calc R . . H8B H 0.1404 0.4559 1.1459 0.088 Uiso 1 1 calc R . . H8C H 0.1724 0.3822 1.0986 0.088 Uiso 1 1 calc R . . C9 C 0.3347(5) 0.4688(5) 1.0888(3) 0.0615(19) Uani 1 1 d . . . H9A H 0.3823 0.5015 1.0601 0.092 Uiso 1 1 calc R . . H9B H 0.3709 0.4064 1.0943 0.092 Uiso 1 1 calc R . . H9C H 0.3250 0.4827 1.1378 0.092 Uiso 1 1 calc R . . C10 C 0.1600(5) 0.5923(4) 1.0404(4) 0.0613(19) Uani 1 1 d . . . H10A H 0.0851 0.6079 1.0157 0.092 Uiso 1 1 calc R . . H10B H 0.2064 0.6255 1.0109 0.092 Uiso 1 1 calc R . . H10C H 0.1521 0.6058 1.0896 0.092 Uiso 1 1 calc R . . C11 C 0.1527(4) 0.3328(3) 0.8532(3) 0.0321(13) Uani 1 1 d . . . H11A H 0.1077 0.3601 0.8061 0.039 Uiso 1 1 calc R . . H11B H 0.1027 0.3121 0.8907 0.039 Uiso 1 1 calc R . . C12 C 0.3226(4) 0.2186(3) 0.9135(3) 0.0320(13) Uani 1 1 d . . . H12A H 0.2772 0.2356 0.9554 0.038 Uiso 1 1 calc R . . H12B H 0.3464 0.1544 0.9222 0.038 Uiso 1 1 calc R . . C13 C 0.4227(4) 0.2504(3) 0.9096(3) 0.0313(13) Uani 1 1 d . . . C14 C 0.4857(5) 0.2515(3) 0.9728(3) 0.0436(15) Uani 1 1 d . . . H14A H 0.4599 0.2365 1.0211 0.052 Uiso 1 1 calc R . . C15 C 0.5840(5) 0.2744(4) 0.9628(3) 0.0503(17) Uani 1 1 d . . . H15A H 0.6269 0.2752 1.0046 0.060 Uiso 1 1 calc R . . C16 C 0.6213(5) 0.2961(4) 0.8934(3) 0.0426(15) Uani 1 1 d . . . H16A H 0.6902 0.3112 0.8869 0.051 Uiso 1 1 calc R . . C17 C 0.5575(4) 0.2960(3) 0.8329(3) 0.0345(13) Uani 1 1 d . . . H17A H 0.5837 0.3104 0.7846 0.041 Uiso 1 1 calc R . . C18 C 0.2120(5) 0.1894(3) 0.8170(3) 0.0385(14) Uani 1 1 d . . . H18A H 0.1487 0.2175 0.7796 0.046 Uiso 1 1 calc R . . H18B H 0.1852 0.1530 0.8592 0.046 Uiso 1 1 calc R . . C19 C 0.3101(5) 0.1348(4) 0.7838(3) 0.0473(16) Uani 1 1 d . . . C20 C 0.3235(7) 0.0477(4) 0.7777(3) 0.0581(19) Uani 1 1 d . . . H20A H 0.2694 0.0186 0.7972 0.070 Uiso 1 1 calc R . . C21 C 0.4134(7) 0.0071(4) 0.7441(4) 0.068(2) Uani 1 1 d . . . H21A H 0.4217 -0.0499 0.7372 0.082 Uiso 1 1 calc R . . C22 C 0.4938(6) 0.0492(4) 0.7197(4) 0.0604(19) Uani 1 1 d . . . H22A H 0.5597 0.0195 0.6983 0.072 Uiso 1 1 calc R . . C23 C 0.4808(5) 0.1303(4) 0.7255(3) 0.0524(17) Uani 1 1 d . . . H23A H 0.5359 0.1586 0.7067 0.063 Uiso 1 1 calc R . . C24 C 0.4167(4) 0.5153(3) 0.8070(3) 0.0313(13) Uani 1 1 d . . . H24A H 0.4428 0.5563 0.8295 0.038 Uiso 1 1 calc R . . H24B H 0.4813 0.4627 0.8097 0.038 Uiso 1 1 calc R . . C25 C 0.3011(4) 0.6432(3) 0.7191(3) 0.0319(13) Uani 1 1 d . . . H25A H 0.3152 0.6820 0.6734 0.038 Uiso 1 1 calc R . . H25B H 0.3109 0.6685 0.7616 0.038 Uiso 1 1 calc R . . C26 C 0.1827(4) 0.6374(3) 0.7151(3) 0.0303(12) Uani 1 1 d . . . C27 C 0.0901(5) 0.6946(4) 0.7374(4) 0.0549(17) Uani 1 1 d . . . H27A H 0.0988 0.7405 0.7582 0.066 Uiso 1 1 calc R . . C28 C -0.0150(6) 0.6837(5) 0.7290(4) 0.073(2) Uani 1 1 d . . . H28A H -0.0799 0.7227 0.7437 0.088 Uiso 1 1 calc R . . C29 C -0.0263(5) 0.6152(4) 0.6988(4) 0.0612(19) Uani 1 1 d . . . H29A H -0.0980 0.6053 0.6950 0.073 Uiso 1 1 calc R . . C30 C 0.0688(4) 0.5623(3) 0.6746(3) 0.0416(15) Uani 1 1 d . . . H30A H 0.0618 0.5182 0.6506 0.050 Uiso 1 1 calc R . . C31 C 0.4875(4) 0.5642(3) 0.6874(2) 0.0257(12) Uani 1 1 d . . . H31A H 0.5495 0.5096 0.7020 0.031 Uiso 1 1 calc R . . H31B H 0.5125 0.6122 0.6994 0.031 Uiso 1 1 calc R . . C32 C 0.4581(4) 0.5825(3) 0.6060(3) 0.0283(12) Uani 1 1 d . . . C33 C 0.5154(5) 0.6221(3) 0.5524(3) 0.0370(14) Uani 1 1 d . . . H33A H 0.5773 0.6408 0.5650 0.044 Uiso 1 1 calc R . . C34 C 0.4804(5) 0.6343(3) 0.4785(3) 0.0419(15) Uani 1 1 d . . . H34A H 0.5181 0.6620 0.4399 0.050 Uiso 1 1 calc R . . C35 C 0.3915(5) 0.6060(3) 0.4624(3) 0.0362(14) Uani 1 1 d . . . H35A H 0.3668 0.6137 0.4125 0.043 Uiso 1 1 calc R . . C36 C 0.3373(4) 0.5656(3) 0.5201(3) 0.0337(13) Uani 1 1 d . . . H36A H 0.2757 0.5458 0.5087 0.040 Uiso 1 1 calc R . . C37 C 0.2273(4) 0.3637(3) 0.6279(3) 0.0312(13) Uani 1 1 d . . . C38 C 0.1653(4) 0.3443(3) 0.5633(3) 0.0316(13) Uani 1 1 d . . . Cl4 Cl 0.31931(18) 0.80638(11) 0.83599(9) 0.0653(5) Uani 1 1 d D . . O4A O 0.2766(8) 0.8355(4) 0.7638(3) 0.196(5) Uani 1 1 d D . . O4B O 0.2949(6) 0.7292(3) 0.8708(2) 0.123(2) Uani 1 1 d D . . O4C O 0.4355(5) 0.7932(6) 0.8412(5) 0.246(6) Uani 1 1 d D . . O4D O 0.2719(8) 0.8695(4) 0.8787(3) 0.210(5) Uani 1 1 d D . . Cl5 Cl 0.20151(12) 0.55926(12) 0.28676(8) 0.0533(4) Uani 1 1 d D . . O5A O 0.2739(3) 0.5937(3) 0.2360(2) 0.0660(13) Uani 1 1 d D . . O5B O 0.2002(4) 0.5887(4) 0.3524(2) 0.104(2) Uani 1 1 d D . . O5C O 0.2457(4) 0.4666(3) 0.3023(3) 0.104(2) Uani 1 1 d D . . O5D O 0.0903(3) 0.5829(3) 0.2550(2) 0.0745(14) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0319(4) 0.0367(4) 0.0205(4) -0.0046(3) -0.0015(3) -0.0139(3) Co2 0.0275(4) 0.0361(4) 0.0185(4) -0.0059(3) -0.0013(3) -0.0149(3) Cl1 0.0668(11) 0.0815(11) 0.0241(8) -0.0047(7) -0.0068(8) -0.0427(9) Cl2 0.0398(9) 0.1250(15) 0.0504(11) -0.0227(10) 0.0027(8) -0.0427(10) Cl3 0.1225(17) 0.0580(10) 0.0610(12) -0.0323(9) -0.0252(12) -0.0035(10) O1 0.035(2) 0.0329(19) 0.0180(19) -0.0066(15) 0.0026(17) -0.0144(16) O2 0.032(2) 0.037(2) 0.025(2) -0.0144(15) 0.0075(17) -0.0143(16) O3 0.031(2) 0.0338(19) 0.030(2) -0.0027(15) -0.0019(17) -0.0149(16) O4 0.046(2) 0.0316(19) 0.0178(19) -0.0001(16) -0.0064(17) -0.0168(17) O5 0.037(2) 0.036(2) 0.024(2) -0.0067(15) -0.0031(17) -0.0160(17) N1 0.040(3) 0.036(2) 0.033(3) -0.004(2) -0.005(2) -0.020(2) N2 0.024(2) 0.034(2) 0.023(3) -0.0028(19) -0.003(2) -0.0066(19) N3 0.049(3) 0.042(3) 0.030(3) -0.008(2) 0.002(3) -0.019(2) N4 0.026(2) 0.047(3) 0.024(2) -0.009(2) -0.001(2) -0.022(2) N5 0.028(3) 0.038(2) 0.026(2) -0.004(2) -0.002(2) -0.012(2) N6 0.031(2) 0.037(2) 0.015(2) -0.0062(18) -0.006(2) -0.014(2) C1 0.024(3) 0.034(3) 0.025(3) -0.012(2) 0.008(2) -0.011(2) C2 0.027(3) 0.037(3) 0.016(3) -0.006(2) 0.009(2) -0.010(2) C3 0.026(3) 0.048(3) 0.020(3) -0.003(2) 0.009(3) -0.017(2) C4 0.028(3) 0.046(3) 0.027(3) 0.001(3) -0.007(3) -0.008(3) C5 0.036(3) 0.032(3) 0.039(4) -0.007(3) 0.000(3) -0.015(3) C6 0.030(3) 0.034(3) 0.017(3) -0.004(2) -0.002(2) -0.014(2) C7 0.044(4) 0.062(4) 0.021(3) -0.018(3) 0.007(3) -0.018(3) C8 0.060(4) 0.097(5) 0.031(4) -0.024(3) 0.024(3) -0.037(4) C9 0.044(4) 0.117(6) 0.028(4) -0.026(4) -0.006(3) -0.023(4) C10 0.051(4) 0.091(5) 0.056(5) -0.043(4) 0.016(4) -0.024(4) C11 0.028(3) 0.043(3) 0.027(3) -0.006(2) 0.006(3) -0.014(3) C12 0.036(3) 0.037(3) 0.026(3) -0.001(2) -0.009(3) -0.018(2) C13 0.033(3) 0.034(3) 0.024(3) 0.000(2) -0.002(3) -0.008(2) C14 0.048(4) 0.052(4) 0.034(3) 0.000(3) -0.005(3) -0.026(3) C15 0.045(4) 0.065(4) 0.037(4) 0.006(3) -0.014(3) -0.021(3) C16 0.034(3) 0.062(4) 0.032(4) 0.003(3) -0.003(3) -0.024(3) C17 0.029(3) 0.046(3) 0.025(3) -0.002(2) -0.001(3) -0.010(3) C18 0.044(4) 0.043(3) 0.032(3) -0.007(3) -0.001(3) -0.018(3) C19 0.066(4) 0.056(4) 0.030(3) -0.007(3) -0.007(3) -0.034(3) C20 0.098(6) 0.040(4) 0.042(4) -0.004(3) -0.014(4) -0.031(4) C21 0.104(6) 0.040(4) 0.059(5) -0.018(3) 0.006(5) -0.012(4) C22 0.076(5) 0.049(4) 0.051(4) -0.011(3) 0.013(4) -0.011(4) C23 0.054(4) 0.061(4) 0.045(4) -0.022(3) 0.020(4) -0.014(3) C24 0.038(3) 0.043(3) 0.020(3) -0.009(2) -0.001(3) -0.021(3) C25 0.041(3) 0.034(3) 0.028(3) -0.012(2) -0.003(3) -0.018(3) C26 0.032(3) 0.037(3) 0.026(3) -0.012(2) 0.002(3) -0.013(3) C27 0.049(4) 0.062(4) 0.066(5) -0.034(3) 0.006(4) -0.020(3) C28 0.037(4) 0.085(5) 0.112(7) -0.060(5) 0.012(4) -0.012(4) C29 0.028(4) 0.081(5) 0.084(5) -0.039(4) -0.003(4) -0.014(3) C30 0.024(3) 0.040(3) 0.066(4) -0.017(3) -0.011(3) -0.013(3) C31 0.025(3) 0.040(3) 0.016(3) -0.006(2) -0.003(2) -0.015(2) C32 0.032(3) 0.033(3) 0.024(3) -0.009(2) 0.003(3) -0.014(2) C33 0.050(4) 0.045(3) 0.023(3) -0.006(3) 0.001(3) -0.027(3) C34 0.048(4) 0.050(3) 0.033(4) -0.010(3) 0.017(3) -0.022(3) C35 0.059(4) 0.037(3) 0.021(3) -0.008(2) -0.003(3) -0.026(3) C36 0.038(3) 0.039(3) 0.026(3) -0.006(2) -0.001(3) -0.014(3) C37 0.027(3) 0.043(3) 0.031(3) -0.021(3) -0.002(3) -0.011(3) C38 0.028(3) 0.045(3) 0.022(3) -0.011(2) 0.001(3) -0.010(2) Cl4 0.0999(15) 0.0633(11) 0.0443(10) -0.0068(8) -0.0096(10) -0.0445(10) O4A 0.423(14) 0.087(4) 0.082(5) 0.029(3) -0.122(7) -0.106(6) O4B 0.247(8) 0.115(4) 0.047(3) -0.013(3) -0.018(4) -0.118(5) O4C 0.101(6) 0.332(13) 0.220(10) 0.120(9) -0.002(7) -0.062(7) O4D 0.417(15) 0.098(5) 0.122(6) -0.047(5) -0.073(8) -0.059(7) Cl5 0.0329(9) 0.0973(13) 0.0360(9) -0.0131(8) 0.0025(8) -0.0295(9) O5A 0.051(3) 0.102(3) 0.043(3) 0.008(2) 0.013(2) -0.038(3) O5B 0.057(3) 0.237(7) 0.046(3) -0.070(4) 0.012(3) -0.058(4) O5C 0.057(3) 0.075(4) 0.168(6) 0.015(3) 0.001(4) -0.031(3) O5D 0.039(3) 0.129(4) 0.061(3) -0.027(3) -0.014(2) -0.026(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 O2 1.870(3) . ? Co1 N2 1.903(4) . ? Co1 O1 1.904(3) . ? Co1 N3 1.921(4) . ? Co1 O4 1.939(3) . ? Co1 N1 1.995(4) . ? Co1 Co2 3.1642(10) . ? Co2 O3 1.863(3) . ? Co2 O1 1.908(3) . ? Co2 N6 1.920(4) . ? Co2 O5 1.942(3) . ? Co2 N4 1.953(4) . ? Co2 N5 2.002(4) . ? Cl1 C38 1.766(5) . ? Cl2 C38 1.749(5) . ? Cl3 C38 1.771(5) . ? O1 C1 1.390(6) . ? O2 O3 1.417(4) . ? O4 C37 1.229(6) . ? O5 C37 1.246(6) . ? N1 C18 1.488(6) . ? N1 C12 1.505(6) . ? N1 C11 1.534(6) . ? N2 C17 1.352(6) . ? N2 C13 1.356(6) . ? N3 C23 1.345(7) . ? N3 C19 1.346(7) . ? N4 C25 1.481(6) . ? N4 C31 1.491(6) . ? N4 C24 1.494(6) . ? N6 C36 1.335(6) . ? N6 C32 1.356(6) . ? N5 C26 1.340(6) . ? N5 C30 1.358(6) . ? C1 C6 1.375(6) . ? C1 C2 1.408(6) . ? C2 C3 1.394(7) . ? C2 C11 1.480(7) . ? C3 C4 1.365(7) . ? C3 H3A 0.9500 . ? C4 C5 1.404(7) . ? C4 C7 1.557(7) . ? C5 C6 1.385(7) . ? C5 H5A 0.9500 . ? C6 C24 1.500(6) . ? C7 C9 1.548(7) . ? C7 C8 1.548(7) . ? C7 C10 1.553(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.465(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.423(7) . ? C14 C15 1.367(7) . ? C14 H14A 0.9500 . ? C15 C16 1.366(7) . ? C15 H15A 0.9500 . ? C16 C17 1.383(7) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.498(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.423(8) . ? C20 C21 1.340(9) . ? C20 H20A 0.9500 . ? C21 C22 1.381(9) . ? C21 H21A 0.9500 . ? C22 C23 1.324(8) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.495(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.380(8) . ? C27 C28 1.373(8) . ? C27 H27A 0.9500 . ? C28 C29 1.402(8) . ? C28 H28A 0.9500 . ? C29 C30 1.381(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.503(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.367(7) . ? C33 C34 1.399(7) . ? C33 H33A 0.9500 . ? C34 C35 1.368(7) . ? C34 H34A 0.9500 . ? C35 C36 1.397(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.566(7) . ? Cl4 O4A 1.380(5) . ? Cl4 O4C 1.391(6) . ? Cl4 O4B 1.406(4) . ? Cl4 O4D 1.427(6) . ? Cl5 O5B 1.400(4) . ? Cl5 O5D 1.418(4) . ? Cl5 O5A 1.424(3) . ? Cl5 O5C 1.431(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 N2 94.88(16) . . ? O2 Co1 O1 90.22(13) . . ? N2 Co1 O1 93.19(15) . . ? O2 Co1 N3 93.55(17) . . ? N2 Co1 N3 94.61(18) . . ? O1 Co1 N3 171.02(17) . . ? O2 Co1 O4 86.87(14) . . ? N2 Co1 O4 178.08(15) . . ? O1 Co1 O4 87.58(14) . . ? N3 Co1 O4 84.49(16) . . ? O2 Co1 N1 176.59(15) . . ? N2 Co1 N1 85.80(17) . . ? O1 Co1 N1 93.08(15) . . ? N3 Co1 N1 83.06(18) . . ? O4 Co1 N1 92.41(16) . . ? O2 Co1 Co2 57.76(10) . . ? N2 Co1 Co2 104.18(12) . . ? O1 Co1 Co2 33.95(9) . . ? N3 Co1 Co2 146.40(13) . . ? O4 Co1 Co2 77.41(9) . . ? N1 Co1 Co2 125.32(12) . . ? O3 Co2 O1 85.39(14) . . ? O3 Co2 N6 89.00(15) . . ? O1 Co2 N6 174.16(16) . . ? O3 Co2 O5 94.27(14) . . ? O1 Co2 O5 92.12(14) . . ? N6 Co2 O5 89.91(15) . . ? O3 Co2 N4 90.26(16) . . ? O1 Co2 N4 96.03(15) . . ? N6 Co2 N4 82.35(16) . . ? O5 Co2 N4 170.97(15) . . ? O3 Co2 N5 171.06(16) . . ? O1 Co2 N5 87.86(15) . . ? N6 Co2 N5 97.55(16) . . ? O5 Co2 N5 91.82(16) . . ? N4 Co2 N5 84.63(17) . . ? O3 Co2 Co1 59.57(9) . . ? O1 Co2 Co1 33.86(10) . . ? N6 Co2 Co1 142.44(12) . . ? O5 Co2 Co1 73.93(10) . . ? N4 Co2 Co1 115.09(12) . . ? N5 Co2 Co1 116.24(11) . . ? C1 O1 Co1 117.0(3) . . ? C1 O1 Co2 124.7(3) . . ? Co1 O1 Co2 112.20(16) . . ? O3 O2 Co1 112.3(2) . . ? O2 O3 Co2 109.0(2) . . ? C37 O4 Co1 122.5(3) . . ? C37 O5 Co2 128.6(3) . . ? C18 N1 C12 111.5(4) . . ? C18 N1 C11 111.3(4) . . ? C12 N1 C11 109.2(4) . . ? C18 N1 Co1 104.6(3) . . ? C12 N1 Co1 108.4(3) . . ? C11 N1 Co1 111.7(3) . . ? C17 N2 C13 120.2(4) . . ? C17 N2 Co1 125.1(3) . . ? C13 N2 Co1 114.2(3) . . ? C23 N3 C19 120.7(5) . . ? C23 N3 Co1 126.4(4) . . ? C19 N3 Co1 112.5(4) . . ? C25 N4 C31 109.7(4) . . ? C25 N4 C24 111.3(4) . . ? C31 N4 C24 108.7(4) . . ? C25 N4 Co2 108.3(3) . . ? C31 N4 Co2 104.6(3) . . ? C24 N4 Co2 113.9(3) . . ? C36 N6 C32 118.4(4) . . ? C36 N6 Co2 127.6(3) . . ? C32 N6 Co2 113.3(3) . . ? C26 N5 C30 120.3(5) . . ? C26 N5 Co2 113.1(3) . . ? C30 N5 Co2 125.6(4) . . ? C6 C1 O1 120.3(4) . . ? C6 C1 C2 123.2(5) . . ? O1 C1 C2 116.5(4) . . ? C3 C2 C1 117.0(5) . . ? C3 C2 C11 124.0(4) . . ? C1 C2 C11 118.9(4) . . ? C4 C3 C2 122.1(4) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 118.4(5) . . ? C3 C4 C7 122.9(5) . . ? C5 C4 C7 118.7(5) . . ? C6 C5 C4 122.3(5) . . ? C6 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C1 C6 C5 117.0(4) . . ? C1 C6 C24 120.6(4) . . ? C5 C6 C24 121.7(4) . . ? C9 C7 C8 108.7(5) . . ? C9 C7 C10 109.4(5) . . ? C8 C7 C10 107.1(5) . . ? C9 C7 C4 110.3(4) . . ? C8 C7 C4 112.1(5) . . ? C10 C7 C4 109.1(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 N1 108.3(4) . . ? C2 C11 H11A 110.0 . . ? N1 C11 H11A 110.0 . . ? C2 C11 H11B 110.0 . . ? N1 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C13 C12 N1 110.0(4) . . ? C13 C12 H12A 109.7 . . ? N1 C12 H12A 109.7 . . ? C13 C12 H12B 109.7 . . ? N1 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N2 C13 C14 119.5(5) . . ? N2 C13 C12 116.5(5) . . ? C14 C13 C12 123.9(5) . . ? C15 C14 C13 118.9(5) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C16 C15 C14 120.8(6) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 119.2(5) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? N2 C17 C16 121.3(5) . . ? N2 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? N1 C18 C19 107.1(4) . . ? N1 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? N1 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? N3 C19 C20 118.8(6) . . ? N3 C19 C18 116.0(5) . . ? C20 C19 C18 125.2(6) . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 119.2(6) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C23 C22 C21 121.1(7) . . ? C23 C22 H22A 119.4 . . ? C21 C22 H22A 119.4 . . ? C22 C23 N3 120.8(6) . . ? C22 C23 H23A 119.6 . . ? N3 C23 H23A 119.6 . . ? N4 C24 C6 114.8(4) . . ? N4 C24 H24A 108.6 . . ? C6 C24 H24A 108.6 . . ? N4 C24 H24B 108.6 . . ? C6 C24 H24B 108.6 . . ? H24A C24 H24B 107.5 . . ? N4 C25 C26 111.0(4) . . ? N4 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? N4 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N5 C26 C27 121.8(5) . . ? N5 C26 C25 113.9(4) . . ? C27 C26 C25 124.3(5) . . ? C28 C27 C26 118.7(6) . . ? C28 C27 H27A 120.7 . . ? C26 C27 H27A 120.7 . . ? C27 C28 C29 120.0(6) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 118.7(6) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.7 . . ? N5 C30 C29 120.5(5) . . ? N5 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? N4 C31 C32 107.4(4) . . ? N4 C31 H31A 110.2 . . ? C32 C31 H31A 110.2 . . ? N4 C31 H31B 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? N6 C32 C33 123.0(5) . . ? N6 C32 C31 113.1(4) . . ? C33 C32 C31 123.8(4) . . ? C32 C33 C34 118.2(5) . . ? C32 C33 H33A 120.9 . . ? C34 C33 H33A 120.9 . . ? C35 C34 C33 119.3(5) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 119.4(5) . . ? C34 C35 H35A 120.3 . . ? C36 C35 H35A 120.3 . . ? N6 C36 C35 121.7(5) . . ? N6 C36 H36A 119.2 . . ? C35 C36 H36A 119.2 . . ? O4 C37 O5 131.9(5) . . ? O4 C37 C38 113.6(4) . . ? O5 C37 C38 114.5(4) . . ? C37 C38 Cl2 107.0(3) . . ? C37 C38 Cl1 113.2(3) . . ? Cl2 C38 Cl1 109.1(3) . . ? C37 C38 Cl3 109.0(3) . . ? Cl2 C38 Cl3 110.1(3) . . ? Cl1 C38 Cl3 108.5(3) . . ? O4A Cl4 O4C 112.2(5) . . ? O4A Cl4 O4B 112.2(3) . . ? O4C Cl4 O4B 108.8(4) . . ? O4A Cl4 O4D 110.7(4) . . ? O4C Cl4 O4D 105.4(5) . . ? O4B Cl4 O4D 107.2(4) . . ? O5B Cl5 O5D 110.2(3) . . ? O5B Cl5 O5A 110.5(3) . . ? O5D Cl5 O5A 110.5(3) . . ? O5B Cl5 O5C 109.4(3) . . ? O5D Cl5 O5C 108.9(3) . . ? O5A Cl5 O5C 107.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 Co2 O3 -25.90(16) . . . . ? N2 Co1 Co2 O3 60.90(17) . . . . ? O1 Co1 Co2 O3 135.1(2) . . . . ? N3 Co1 Co2 O3 -61.1(3) . . . . ? O4 Co1 Co2 O3 -120.19(16) . . . . ? N1 Co1 Co2 O3 155.86(19) . . . . ? O2 Co1 Co2 O1 -161.0(2) . . . . ? N2 Co1 Co2 O1 -74.2(2) . . . . ? N3 Co1 Co2 O1 163.8(3) . . . . ? O4 Co1 Co2 O1 104.7(2) . . . . ? N1 Co1 Co2 O1 20.8(2) . . . . ? O2 Co1 Co2 N6 11.3(2) . . . . ? N2 Co1 Co2 N6 98.1(2) . . . . ? O1 Co1 Co2 N6 172.3(3) . . . . ? N3 Co1 Co2 N6 -23.9(3) . . . . ? O4 Co1 Co2 N6 -83.0(2) . . . . ? N1 Co1 Co2 N6 -167.0(2) . . . . ? O2 Co1 Co2 O5 79.11(16) . . . . ? N2 Co1 Co2 O5 165.92(16) . . . . ? O1 Co1 Co2 O5 -119.9(2) . . . . ? N3 Co1 Co2 O5 43.9(3) . . . . ? O4 Co1 Co2 O5 -15.18(15) . . . . ? N1 Co1 Co2 O5 -99.13(18) . . . . ? O2 Co1 Co2 N4 -100.29(18) . . . . ? N2 Co1 Co2 N4 -13.49(19) . . . . ? O1 Co1 Co2 N4 60.7(2) . . . . ? N3 Co1 Co2 N4 -135.5(3) . . . . ? O4 Co1 Co2 N4 165.42(17) . . . . ? N1 Co1 Co2 N4 81.5(2) . . . . ? O2 Co1 Co2 N5 163.07(18) . . . . ? N2 Co1 Co2 N5 -110.12(19) . . . . ? O1 Co1 Co2 N5 -35.9(2) . . . . ? N3 Co1 Co2 N5 127.9(3) . . . . ? O4 Co1 Co2 N5 68.78(17) . . . . ? N1 Co1 Co2 N5 -15.2(2) . . . . ? O2 Co1 O1 C1 -137.9(3) . . . . ? N2 Co1 O1 C1 -43.0(3) . . . . ? O4 Co1 O1 C1 135.3(3) . . . . ? N1 Co1 O1 C1 43.0(3) . . . . ? Co2 Co1 O1 C1 -153.9(4) . . . . ? O2 Co1 O1 Co2 16.00(18) . . . . ? N2 Co1 O1 Co2 110.89(19) . . . . ? O4 Co1 O1 Co2 -70.86(18) . . . . ? N1 Co1 O1 Co2 -163.15(18) . . . . ? O3 Co2 O1 C1 113.9(4) . . . . ? O5 Co2 O1 C1 -152.0(3) . . . . ? N4 Co2 O1 C1 24.1(4) . . . . ? N5 Co2 O1 C1 -60.3(4) . . . . ? Co1 Co2 O1 C1 151.5(4) . . . . ? O3 Co2 O1 Co1 -37.65(18) . . . . ? O5 Co2 O1 Co1 56.47(18) . . . . ? N4 Co2 O1 Co1 -127.43(18) . . . . ? N5 Co2 O1 Co1 148.21(19) . . . . ? N2 Co1 O2 O3 -71.3(3) . . . . ? O1 Co1 O2 O3 21.9(2) . . . . ? N3 Co1 O2 O3 -166.3(3) . . . . ? O4 Co1 O2 O3 109.5(2) . . . . ? Co2 Co1 O2 O3 32.38(19) . . . . ? Co1 O2 O3 Co2 -54.4(3) . . . . ? O1 Co2 O3 O2 54.3(2) . . . . ? N6 Co2 O3 O2 -127.3(2) . . . . ? O5 Co2 O3 O2 -37.5(2) . . . . ? N4 Co2 O3 O2 150.3(2) . . . . ? Co1 Co2 O3 O2 31.04(18) . . . . ? O2 Co1 O4 C37 -35.3(4) . . . . ? O1 Co1 O4 C37 55.1(4) . . . . ? N3 Co1 O4 C37 -129.2(4) . . . . ? N1 Co1 O4 C37 148.1(4) . . . . ? Co2 Co1 O4 C37 22.4(4) . . . . ? O3 Co2 O5 C37 70.2(4) . . . . ? O1 Co2 O5 C37 -15.3(4) . . . . ? N6 Co2 O5 C37 159.2(4) . . . . ? N5 Co2 O5 C37 -103.2(4) . . . . ? Co1 Co2 O5 C37 13.6(4) . . . . ? N2 Co1 N1 C18 -130.8(3) . . . . ? O1 Co1 N1 C18 136.2(3) . . . . ? N3 Co1 N1 C18 -35.6(3) . . . . ? O4 Co1 N1 C18 48.5(3) . . . . ? Co2 Co1 N1 C18 124.8(3) . . . . ? N2 Co1 N1 C12 -11.7(3) . . . . ? O1 Co1 N1 C12 -104.7(3) . . . . ? N3 Co1 N1 C12 83.5(3) . . . . ? O4 Co1 N1 C12 167.6(3) . . . . ? Co2 Co1 N1 C12 -116.1(3) . . . . ? N2 Co1 N1 C11 108.6(3) . . . . ? O1 Co1 N1 C11 15.7(3) . . . . ? N3 Co1 N1 C11 -156.2(3) . . . . ? O4 Co1 N1 C11 -72.0(3) . . . . ? Co2 Co1 N1 C11 4.2(4) . . . . ? O2 Co1 N2 C17 9.8(4) . . . . ? O1 Co1 N2 C17 -80.7(4) . . . . ? N3 Co1 N2 C17 103.8(4) . . . . ? N1 Co1 N2 C17 -173.5(4) . . . . ? Co2 Co1 N2 C17 -48.1(4) . . . . ? O2 Co1 N2 C13 -178.1(3) . . . . ? O1 Co1 N2 C13 91.4(3) . . . . ? N3 Co1 N2 C13 -84.1(3) . . . . ? N1 Co1 N2 C13 -1.4(3) . . . . ? Co2 Co1 N2 C13 124.0(3) . . . . ? O2 Co1 N3 C23 17.2(5) . . . . ? N2 Co1 N3 C23 -78.0(5) . . . . ? O4 Co1 N3 C23 103.7(5) . . . . ? N1 Co1 N3 C23 -163.2(5) . . . . ? Co2 Co1 N3 C23 46.4(6) . . . . ? O2 Co1 N3 C19 -156.1(4) . . . . ? N2 Co1 N3 C19 108.7(4) . . . . ? O4 Co1 N3 C19 -69.6(4) . . . . ? N1 Co1 N3 C19 23.5(4) . . . . ? Co2 Co1 N3 C19 -126.9(3) . . . . ? O3 Co2 N4 C25 167.6(3) . . . . ? O1 Co2 N4 C25 -107.0(3) . . . . ? N6 Co2 N4 C25 78.6(3) . . . . ? N5 Co2 N4 C25 -19.8(3) . . . . ? Co1 Co2 N4 C25 -136.3(3) . . . . ? O3 Co2 N4 C31 50.6(3) . . . . ? O1 Co2 N4 C31 136.0(3) . . . . ? N6 Co2 N4 C31 -38.4(3) . . . . ? N5 Co2 N4 C31 -136.8(3) . . . . ? Co1 Co2 N4 C31 106.7(3) . . . . ? O3 Co2 N4 C24 -67.9(3) . . . . ? O1 Co2 N4 C24 17.4(3) . . . . ? N6 Co2 N4 C24 -156.9(4) . . . . ? N5 Co2 N4 C24 104.7(3) . . . . ? Co1 Co2 N4 C24 -11.8(4) . . . . ? O3 Co2 N6 C36 107.2(4) . . . . ? O5 Co2 N6 C36 12.9(4) . . . . ? N4 Co2 N6 C36 -162.4(4) . . . . ? N5 Co2 N6 C36 -78.9(4) . . . . ? Co1 Co2 N6 C36 75.8(5) . . . . ? O3 Co2 N6 C32 -63.5(3) . . . . ? O5 Co2 N6 C32 -157.8(3) . . . . ? N4 Co2 N6 C32 26.9(3) . . . . ? N5 Co2 N6 C32 110.4(3) . . . . ? Co1 Co2 N6 C32 -94.9(3) . . . . ? O1 Co2 N5 C26 99.9(3) . . . . ? N6 Co2 N5 C26 -77.8(3) . . . . ? O5 Co2 N5 C26 -168.0(3) . . . . ? N4 Co2 N5 C26 3.7(3) . . . . ? Co1 Co2 N5 C26 119.0(3) . . . . ? O1 Co2 N5 C30 -68.4(4) . . . . ? N6 Co2 N5 C30 113.9(4) . . . . ? O5 Co2 N5 C30 23.7(4) . . . . ? N4 Co2 N5 C30 -164.6(5) . . . . ? Co1 Co2 N5 C30 -49.3(5) . . . . ? Co1 O1 C1 C6 119.5(4) . . . . ? Co2 O1 C1 C6 -30.8(6) . . . . ? Co1 O1 C1 C2 -58.5(5) . . . . ? Co2 O1 C1 C2 151.2(3) . . . . ? C6 C1 C2 C3 1.3(7) . . . . ? O1 C1 C2 C3 179.2(4) . . . . ? C6 C1 C2 C11 -174.8(5) . . . . ? O1 C1 C2 C11 3.1(6) . . . . ? C1 C2 C3 C4 0.1(7) . . . . ? C11 C2 C3 C4 176.0(5) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C2 C3 C4 C7 -177.0(5) . . . . ? C3 C4 C5 C6 -1.6(7) . . . . ? C7 C4 C5 C6 175.6(5) . . . . ? O1 C1 C6 C5 179.4(4) . . . . ? C2 C1 C6 C5 -2.7(7) . . . . ? O1 C1 C6 C24 -10.1(7) . . . . ? C2 C1 C6 C24 167.8(4) . . . . ? C4 C5 C6 C1 2.9(7) . . . . ? C4 C5 C6 C24 -167.5(5) . . . . ? C3 C4 C7 C9 121.0(6) . . . . ? C5 C4 C7 C9 -56.1(6) . . . . ? C3 C4 C7 C8 -0.3(7) . . . . ? C5 C4 C7 C8 -177.4(5) . . . . ? C3 C4 C7 C10 -118.8(5) . . . . ? C5 C4 C7 C10 64.1(6) . . . . ? C3 C2 C11 N1 -114.9(5) . . . . ? C1 C2 C11 N1 60.9(6) . . . . ? C18 N1 C11 C2 -179.7(4) . . . . ? C12 N1 C11 C2 56.7(5) . . . . ? Co1 N1 C11 C2 -63.1(4) . . . . ? C18 N1 C12 C13 136.3(4) . . . . ? C11 N1 C12 C13 -100.2(5) . . . . ? Co1 N1 C12 C13 21.7(5) . . . . ? C17 N2 C13 C14 4.7(7) . . . . ? Co1 N2 C13 C14 -167.9(4) . . . . ? C17 N2 C13 C12 -172.1(4) . . . . ? Co1 N2 C13 C12 15.4(5) . . . . ? N1 C12 C13 N2 -24.8(6) . . . . ? N1 C12 C13 C14 158.6(5) . . . . ? N2 C13 C14 C15 -3.0(8) . . . . ? C12 C13 C14 C15 173.6(5) . . . . ? C13 C14 C15 C16 0.2(9) . . . . ? C14 C15 C16 C17 0.9(9) . . . . ? C13 N2 C17 C16 -3.6(7) . . . . ? Co1 N2 C17 C16 168.0(4) . . . . ? C15 C16 C17 N2 0.8(8) . . . . ? C12 N1 C18 C19 -76.7(5) . . . . ? C11 N1 C18 C19 161.1(4) . . . . ? Co1 N1 C18 C19 40.3(4) . . . . ? C23 N3 C19 C20 1.0(8) . . . . ? Co1 N3 C19 C20 174.8(4) . . . . ? C23 N3 C19 C18 -178.5(5) . . . . ? Co1 N3 C19 C18 -4.8(6) . . . . ? N1 C18 C19 N3 -24.9(6) . . . . ? N1 C18 C19 C20 155.6(5) . . . . ? N3 C19 C20 C21 -2.2(9) . . . . ? C18 C19 C20 C21 177.4(6) . . . . ? C19 C20 C21 C22 3.3(10) . . . . ? C20 C21 C22 C23 -3.4(11) . . . . ? C21 C22 C23 N3 2.3(10) . . . . ? C19 N3 C23 C22 -1.1(9) . . . . ? Co1 N3 C23 C22 -173.9(5) . . . . ? C25 N4 C24 C6 68.2(5) . . . . ? C31 N4 C24 C6 -170.8(4) . . . . ? Co2 N4 C24 C6 -54.6(5) . . . . ? C1 C6 C24 N4 56.4(6) . . . . ? C5 C6 C24 N4 -133.5(5) . . . . ? C31 N4 C25 C26 145.6(4) . . . . ? C24 N4 C25 C26 -94.1(5) . . . . ? Co2 N4 C25 C26 31.9(5) . . . . ? C30 N5 C26 C27 0.4(8) . . . . ? Co2 N5 C26 C27 -168.6(4) . . . . ? C30 N5 C26 C25 -177.1(5) . . . . ? Co2 N5 C26 C25 13.9(5) . . . . ? N4 C25 C26 N5 -30.6(6) . . . . ? N4 C25 C26 C27 151.9(5) . . . . ? N5 C26 C27 C28 1.0(9) . . . . ? C25 C26 C27 C28 178.2(6) . . . . ? C26 C27 C28 C29 0.5(11) . . . . ? C27 C28 C29 C30 -3.2(11) . . . . ? C26 N5 C30 C29 -3.2(8) . . . . ? Co2 N5 C30 C29 164.3(4) . . . . ? C28 C29 C30 N5 4.6(10) . . . . ? C25 N4 C31 C32 -73.0(5) . . . . ? C24 N4 C31 C32 165.0(4) . . . . ? Co2 N4 C31 C32 43.0(4) . . . . ? C36 N6 C32 C33 -0.1(7) . . . . ? Co2 N6 C32 C33 171.5(4) . . . . ? C36 N6 C32 C31 -179.0(4) . . . . ? Co2 N6 C32 C31 -7.3(5) . . . . ? N4 C31 C32 N6 -24.3(5) . . . . ? N4 C31 C32 C33 156.8(5) . . . . ? N6 C32 C33 C34 0.4(8) . . . . ? C31 C32 C33 C34 179.2(5) . . . . ? C32 C33 C34 C35 -0.5(8) . . . . ? C33 C34 C35 C36 0.1(8) . . . . ? C32 N6 C36 C35 -0.2(7) . . . . ? Co2 N6 C36 C35 -170.5(4) . . . . ? C34 C35 C36 N6 0.2(8) . . . . ? Co1 O4 C37 O5 -23.8(8) . . . . ? Co1 O4 C37 C38 159.3(3) . . . . ? Co2 O5 C37 O4 -1.2(9) . . . . ? Co2 O5 C37 C38 175.8(3) . . . . ? O4 C37 C38 Cl2 72.1(5) . . . . ? O5 C37 C38 Cl2 -105.4(4) . . . . ? O4 C37 C38 Cl1 -167.7(4) . . . . ? O5 C37 C38 Cl1 14.7(6) . . . . ? O4 C37 C38 Cl3 -47.0(5) . . . . ? O5 C37 C38 Cl3 135.5(4) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 913567' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a data_5 #TrackingRef '15833_web_deposit_cif_file_0_AndrewBond_1354442523.submit.cif' ###################################### ## refinement against SQUEEZED data ## ###################################### loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.280 -0.232 0.507 287 132 ' ' 2 0.720 0.232 0.493 287 131 ' ' 3 0.720 0.268 -0.007 287 132 ' ' 4 0.280 0.732 1.007 287 132 ' ' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H46 Co2 N6 O5 2+, 2(Cl O4 -)' _chemical_formula_sum 'C47 H46 Cl2 Co2 N6 O13' _chemical_formula_weight 1091.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.3433(11) _cell_length_b 18.4942(7) _cell_length_c 21.7739(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.509(2) _cell_angle_gamma 90.00 _cell_volume 9999.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6807 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 19.37 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4496 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details ; SADABS v.2.10 (Sheldrick, 2003) Ratio of minimum to maximum apparent transmission: 0.909616 ; _exptl_special_details ; Refinement based on *SQUEEZED* data. The squeezed molecules not included could be acetone or water (or both). Perchlorate anion Cl4 is modelled as disordered over two orientations with equal occupancy. The displacement parameters are distorted but considered to be acceptable. The structure contains clear pseudoinversion centres between the molecules in the asymmetric unit. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 192465 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.74 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 18985 _reflns_number_gt 12708 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a (Bruker, 2003)' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL v.6.10 (Sheldrick, 2000)' _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^)+(0.0659P)^2^+11.5828P] 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 18985 _refine_ls_number_parameters 1289 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.891 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.081 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 0.17095(2) 0.13444(3) 0.30060(3) 0.02144(13) Uani 1 1 d . . . Co2 Co 0.20662(2) -0.00047(3) 0.23571(3) 0.02271(14) Uani 1 1 d . . . O1 O 0.16479(9) 0.03353(13) 0.28621(12) 0.0220(6) Uani 1 1 d . . . O2 O 0.19989(10) 0.14552(13) 0.23393(13) 0.0256(6) Uani 1 1 d . . . O3 O 0.18734(10) 0.08634(13) 0.19026(12) 0.0248(6) Uani 1 1 d . . . O4 O 0.24345(10) 0.11700(14) 0.35901(12) 0.0244(6) Uani 1 1 d . . . O5 O 0.27125(10) 0.03806(14) 0.29751(12) 0.0254(6) Uani 1 1 d . . . N1 N 0.14064(12) 0.12786(16) 0.37411(15) 0.0233(7) Uani 1 1 d . . . N2 N 0.09780(12) 0.15040(17) 0.24662(16) 0.0250(7) Uani 1 1 d . . . N3 N 0.18266(12) 0.23345(17) 0.32768(16) 0.0251(7) Uani 1 1 d . . . N4 N 0.14818(12) -0.05131(17) 0.17014(15) 0.0264(8) Uani 1 1 d . . . N5 N 0.21595(13) -0.09354(17) 0.28388(16) 0.0272(8) Uani 1 1 d . . . N6 N 0.24572(13) -0.02760(17) 0.17943(16) 0.0265(8) Uani 1 1 d . . . C1 C 0.12005(15) -0.0014(2) 0.28943(19) 0.0237(9) Uani 1 1 d . . . C2 C 0.10873(15) 0.0030(2) 0.34677(19) 0.0242(9) Uani 1 1 d . . . C3 C 0.06346(16) -0.0326(2) 0.3511(2) 0.0273(9) Uani 1 1 d . . . H3A H 0.0550 -0.0288 0.3901 0.033 Uiso 1 1 calc R . . C4 C 0.03031(16) -0.0739(2) 0.2996(2) 0.0275(9) Uani 1 1 d . . . C5 C 0.04190(15) -0.0747(2) 0.2419(2) 0.0258(9) Uani 1 1 d . . . H5A H 0.0192 -0.1014 0.2059 0.031 Uiso 1 1 calc R . . C6 C 0.08566(15) -0.0379(2) 0.23541(19) 0.0260(9) Uani 1 1 d . . . C7 C -0.01919(17) -0.1133(2) 0.3063(2) 0.0356(11) Uani 1 1 d . . . C8 C -0.04362(19) -0.1662(2) 0.2500(2) 0.0460(12) Uani 1 1 d . . . H8A H -0.0553 -0.1396 0.2087 0.069 Uiso 1 1 calc R . . H8B H -0.0746 -0.1906 0.2560 0.069 Uiso 1 1 calc R . . H8C H -0.0165 -0.2022 0.2493 0.069 Uiso 1 1 calc R . . C9 C -0.0015(2) -0.1570(3) 0.3703(3) 0.0541(14) Uani 1 1 d . . . H9A H 0.0255 -0.1929 0.3691 0.081 Uiso 1 1 calc R . . H9B H -0.0328 -0.1817 0.3753 0.081 Uiso 1 1 calc R . . H9C H 0.0140 -0.1242 0.4071 0.081 Uiso 1 1 calc R . . C10 C -0.0614(2) -0.0572(3) 0.3074(3) 0.0634(16) Uani 1 1 d . . . H10A H -0.0728 -0.0302 0.2664 0.095 Uiso 1 1 calc R . . H10B H -0.0460 -0.0238 0.3438 0.095 Uiso 1 1 calc R . . H10C H -0.0927 -0.0817 0.3129 0.095 Uiso 1 1 calc R . . C11 C 0.14372(16) 0.0512(2) 0.39975(19) 0.0269(9) Uani 1 1 d . . . H11A H 0.1814 0.0339 0.4137 0.032 Uiso 1 1 calc R . . H11B H 0.1313 0.0499 0.4379 0.032 Uiso 1 1 calc R . . C12 C 0.08321(16) 0.1535(2) 0.34973(19) 0.0287(9) Uani 1 1 d . . . H12A H 0.0613 0.1238 0.3692 0.034 Uiso 1 1 calc R . . H12B H 0.0815 0.2044 0.3630 0.034 Uiso 1 1 calc R . . C13 C 0.06107(15) 0.1478(2) 0.2775(2) 0.0260(9) Uani 1 1 d . . . C14 C 0.00654(16) 0.1428(2) 0.2434(2) 0.0353(11) Uani 1 1 d . . . H14A H -0.0186 0.1379 0.2658 0.042 Uiso 1 1 calc R . . C15 C -0.01071(18) 0.1452(3) 0.1762(2) 0.0413(12) Uani 1 1 d . . . H15A H -0.0480 0.1419 0.1517 0.050 Uiso 1 1 calc R . . C16 C 0.02680(17) 0.1526(2) 0.1449(2) 0.0382(11) Uani 1 1 d . . . H16A H 0.0157 0.1562 0.0988 0.046 Uiso 1 1 calc R . . C17 C 0.08068(16) 0.1544(2) 0.1819(2) 0.0315(10) Uani 1 1 d . . . H17A H 0.1065 0.1587 0.1603 0.038 Uiso 1 1 calc R . . C18 C 0.17450(16) 0.1790(2) 0.42385(19) 0.0289(9) Uani 1 1 d . . . H18A H 0.2096 0.1565 0.4480 0.035 Uiso 1 1 calc R . . H18B H 0.1562 0.1920 0.4553 0.035 Uiso 1 1 calc R . . C19 C 0.18291(15) 0.2454(2) 0.3887(2) 0.0289(10) Uani 1 1 d . . . C20 C 0.19074(17) 0.3141(2) 0.4150(2) 0.0381(11) Uani 1 1 d . . . H20A H 0.1896 0.3225 0.4576 0.046 Uiso 1 1 calc R . . C21 C 0.20029(19) 0.3705(2) 0.3786(3) 0.0467(13) Uani 1 1 d . . . H21A H 0.2060 0.4180 0.3960 0.056 Uiso 1 1 calc R . . C22 C 0.20151(17) 0.3573(2) 0.3172(2) 0.0380(11) Uani 1 1 d . . . H22A H 0.2091 0.3953 0.2922 0.046 Uiso 1 1 calc R . . C23 C 0.19170(15) 0.2883(2) 0.2920(2) 0.0297(10) Uani 1 1 d . . . H23A H 0.1913 0.2794 0.2489 0.036 Uiso 1 1 calc R . . C24 C 0.09336(15) -0.0294(2) 0.1702(2) 0.0304(10) Uani 1 1 d . . . H24A H 0.0659 -0.0589 0.1377 0.036 Uiso 1 1 calc R . . H24B H 0.0871 0.0218 0.1566 0.036 Uiso 1 1 calc R . . C25 C 0.15546(18) -0.1312(2) 0.1812(2) 0.0361(11) Uani 1 1 d . . . H25A H 0.1198 -0.1553 0.1668 0.043 Uiso 1 1 calc R . . H25B H 0.1767 -0.1508 0.1551 0.043 Uiso 1 1 calc R . . C26 C 0.18366(18) -0.1468(2) 0.2513(2) 0.0364(11) Uani 1 1 d . . . C27 C 0.1790(2) -0.2112(3) 0.2810(3) 0.0656(17) Uani 1 1 d . . . H27A H 0.1563 -0.2486 0.2569 0.079 Uiso 1 1 calc R . . C28 C 0.2077(3) -0.2204(3) 0.3454(3) 0.085(2) Uani 1 1 d . . . H28A H 0.2050 -0.2644 0.3666 0.102 Uiso 1 1 calc R . . C29 C 0.2407(2) -0.1654(3) 0.3799(3) 0.0694(18) Uani 1 1 d . . . H29A H 0.2609 -0.1708 0.4248 0.083 Uiso 1 1 calc R . . C30 C 0.24325(18) -0.1027(2) 0.3471(2) 0.0403(11) Uani 1 1 d . . . H30A H 0.2654 -0.0644 0.3705 0.048 Uiso 1 1 calc R . . C31 C 0.15455(16) -0.0320(2) 0.10690(19) 0.0313(10) Uani 1 1 d . . . H31A H 0.1419 0.0180 0.0943 0.038 Uiso 1 1 calc R . . H31B H 0.1335 -0.0654 0.0722 0.038 Uiso 1 1 calc R . . C32 C 0.21342(16) -0.0383(2) 0.1168(2) 0.0300(10) Uani 1 1 d . . . C33 C 0.23458(18) -0.0543(3) 0.0684(2) 0.0411(11) Uani 1 1 d . . . H33A H 0.2117 -0.0609 0.0247 0.049 Uiso 1 1 calc R . . C34 C 0.28998(19) -0.0605(3) 0.0849(2) 0.0430(12) Uani 1 1 d . . . H34A H 0.3055 -0.0716 0.0524 0.052 Uiso 1 1 calc R . . C35 C 0.32244(18) -0.0505(2) 0.1486(2) 0.0353(11) Uani 1 1 d . . . H35A H 0.3604 -0.0547 0.1605 0.042 Uiso 1 1 calc R . . C36 C 0.29912(16) -0.0343(2) 0.1948(2) 0.0302(10) Uani 1 1 d . . . H36A H 0.3215 -0.0277 0.2388 0.036 Uiso 1 1 calc R . . C37 C 0.27880(15) 0.0808(2) 0.34483(19) 0.0238(9) Uani 1 1 d . . . C38 C 0.33597(15) 0.0850(2) 0.39133(19) 0.0237(9) Uani 1 1 d . . . C39 C 0.36575(15) 0.0226(2) 0.4040(2) 0.0295(10) Uani 1 1 d . . . H39A H 0.3510 -0.0201 0.3807 0.035 Uiso 1 1 calc R . . C40 C 0.41735(16) 0.0204(2) 0.4505(2) 0.0358(11) Uani 1 1 d . . . H40A H 0.4369 -0.0237 0.4591 0.043 Uiso 1 1 calc R . . C41 C 0.43953(16) 0.0814(2) 0.4834(2) 0.0347(11) Uani 1 1 d . . . H41A H 0.4743 0.0791 0.5156 0.042 Uiso 1 1 calc R . . C42 C 0.41173(16) 0.1482(2) 0.4704(2) 0.0306(10) Uani 1 1 d . . . C43 C 0.43563(17) 0.2123(2) 0.5023(2) 0.0367(11) Uani 1 1 d . . . H43A H 0.4706 0.2104 0.5341 0.044 Uiso 1 1 calc R . . C44 C 0.40960(18) 0.2762(2) 0.4885(2) 0.0412(12) Uani 1 1 d . . . H44A H 0.4264 0.3186 0.5107 0.049 Uiso 1 1 calc R . . C45 C 0.35773(17) 0.2809(2) 0.4413(2) 0.0362(11) Uani 1 1 d . . . H45A H 0.3400 0.3263 0.4315 0.043 Uiso 1 1 calc R . . C46 C 0.33300(16) 0.2196(2) 0.4098(2) 0.0281(9) Uani 1 1 d . . . H46A H 0.2981 0.2231 0.3781 0.034 Uiso 1 1 calc R . . C47 C 0.35859(14) 0.1507(2) 0.42346(18) 0.0235(9) Uani 1 1 d . . . Co1' Co 0.327334(19) 0.39482(3) 0.19821(2) 0.02131(13) Uani 1 1 d . . . Co2' Co 0.28261(2) 0.53238(3) 0.24950(3) 0.02369(14) Uani 1 1 d . . . O1' O 0.33099(10) 0.49712(14) 0.20833(13) 0.0247(6) Uani 1 1 d . . . O2' O 0.29175(10) 0.38667(14) 0.25862(12) 0.0250(6) Uani 1 1 d . . . O3' O 0.30030(10) 0.44809(13) 0.29934(12) 0.0253(6) Uani 1 1 d . . . O4' O 0.25734(10) 0.40847(13) 0.13185(12) 0.0236(6) Uani 1 1 d . . . O5' O 0.22238(10) 0.49018(13) 0.18441(13) 0.0244(6) Uani 1 1 d . . . N1' N 0.36509(12) 0.39734(16) 0.13127(15) 0.0224(7) Uani 1 1 d . . . N2' N 0.39783(12) 0.38056(17) 0.26008(16) 0.0251(7) Uani 1 1 d . . . N3' N 0.31842(12) 0.29491(16) 0.17437(16) 0.0232(7) Uani 1 1 d . . . N4' N 0.33556(13) 0.58792(18) 0.31804(16) 0.0289(8) Uani 1 1 d . . . N5' N 0.27487(13) 0.62246(17) 0.19767(17) 0.0295(8) Uani 1 1 d . . . N6' N 0.23574(13) 0.56089(17) 0.29646(16) 0.0274(8) Uani 1 1 d . . . C1' C 0.37792(15) 0.5309(2) 0.21198(19) 0.0259(9) Uani 1 1 d . . . C2' C 0.39655(15) 0.5224(2) 0.15918(19) 0.0237(9) Uani 1 1 d . . . C3' C 0.44546(15) 0.5549(2) 0.1626(2) 0.0281(9) Uani 1 1 d . . . H3A' H 0.4589 0.5485 0.1275 0.034 Uiso 1 1 calc R . . C4' C 0.47475(15) 0.5963(2) 0.2159(2) 0.0279(9) Uani 1 1 d . . . C5' C 0.45496(16) 0.6028(2) 0.2674(2) 0.0308(10) Uani 1 1 d . . . H5A' H 0.4745 0.6312 0.3040 0.037 Uiso 1 1 calc R . . C6' C 0.40753(15) 0.5694(2) 0.2674(2) 0.0277(9) Uani 1 1 d . . . C7' C 0.52857(16) 0.6307(2) 0.2185(2) 0.0322(10) Uani 1 1 d . . . C8' C 0.5212(2) 0.6731(3) 0.1549(2) 0.0522(14) Uani 1 1 d . . . H8A' H 0.5076 0.6404 0.1175 0.078 Uiso 1 1 calc R . . H8B' H 0.5559 0.6933 0.1560 0.078 Uiso 1 1 calc R . . H8C' H 0.4954 0.7125 0.1508 0.078 Uiso 1 1 calc R . . C9' C 0.54955(17) 0.6836(2) 0.2751(2) 0.0404(11) Uani 1 1 d . . . H9A' H 0.5549 0.6582 0.3162 0.061 Uiso 1 1 calc R . . H9B' H 0.5233 0.7226 0.2702 0.061 Uiso 1 1 calc R . . H9C' H 0.5839 0.7041 0.2751 0.061 Uiso 1 1 calc R . . C10' C 0.57000(18) 0.5701(3) 0.2272(3) 0.0548(14) Uani 1 1 d . . . H10D H 0.5742 0.5439 0.2677 0.082 Uiso 1 1 calc R . . H10E H 0.6047 0.5909 0.2290 0.082 Uiso 1 1 calc R . . H10F H 0.5576 0.5366 0.1903 0.082 Uiso 1 1 calc R . . C11' C 0.36579(16) 0.4727(2) 0.10529(19) 0.0272(9) Uani 1 1 d . . . H11C H 0.3828 0.4720 0.0710 0.033 Uiso 1 1 calc R . . H11D H 0.3284 0.4905 0.0855 0.033 Uiso 1 1 calc R . . C12' C 0.42160(15) 0.3707(2) 0.1631(2) 0.0276(9) Uani 1 1 d . . . H12C H 0.4237 0.3189 0.1526 0.033 Uiso 1 1 calc R . . H12D H 0.4463 0.3980 0.1460 0.033 Uiso 1 1 calc R . . C13' C 0.43846(15) 0.3801(2) 0.23515(19) 0.0261(9) Uani 1 1 d . . . C14' C 0.49137(16) 0.3842(2) 0.2751(2) 0.0337(10) Uani 1 1 d . . . H14B H 0.5195 0.3853 0.2569 0.040 Uiso 1 1 calc R . . C15' C 0.50344(17) 0.3867(2) 0.3420(2) 0.0388(11) Uani 1 1 d . . . H15B H 0.5398 0.3902 0.3701 0.047 Uiso 1 1 calc R . . C16' C 0.46238(17) 0.3842(2) 0.3673(2) 0.0366(11) Uani 1 1 d . . . H16B H 0.4700 0.3846 0.4131 0.044 Uiso 1 1 calc R . . C17' C 0.40993(17) 0.3810(2) 0.3256(2) 0.0319(10) Uani 1 1 d . . . H17B H 0.3815 0.3790 0.3433 0.038 Uiso 1 1 calc R . . C18' C 0.33418(16) 0.3453(2) 0.08080(19) 0.0251(9) Uani 1 1 d . . . H18C H 0.3556 0.3307 0.0532 0.030 Uiso 1 1 calc R . . H18D H 0.3003 0.3678 0.0526 0.030 Uiso 1 1 calc R . . C19' C 0.32198(14) 0.2807(2) 0.11507(19) 0.0237(9) Uani 1 1 d . . . C20' C 0.31464(16) 0.2111(2) 0.0899(2) 0.0310(10) Uani 1 1 d . . . H20B H 0.3187 0.2012 0.0490 0.037 Uiso 1 1 calc R . . C21' C 0.30130(16) 0.1563(2) 0.1250(2) 0.0348(11) Uani 1 1 d . . . H21B H 0.2958 0.1085 0.1079 0.042 Uiso 1 1 calc R . . C22' C 0.29607(15) 0.1709(2) 0.1843(2) 0.0296(10) Uani 1 1 d . . . H22B H 0.2859 0.1339 0.2082 0.035 Uiso 1 1 calc R . . C23' C 0.30589(15) 0.2408(2) 0.2088(2) 0.0285(10) Uani 1 1 d . . . H23B H 0.3038 0.2509 0.2507 0.034 Uiso 1 1 calc R . . C24' C 0.39196(16) 0.5661(2) 0.3278(2) 0.0316(10) Uani 1 1 d . . . H24C H 0.3973 0.5160 0.3448 0.038 Uiso 1 1 calc R . . H24D H 0.4165 0.5978 0.3613 0.038 Uiso 1 1 calc R . . C25' C 0.32790(18) 0.6672(2) 0.3030(2) 0.0343(10) Uani 1 1 d . . . H25C H 0.3046 0.6882 0.3258 0.041 Uiso 1 1 calc R . . H25D H 0.3632 0.6919 0.3189 0.041 Uiso 1 1 calc R . . C26' C 0.30293(19) 0.6791(2) 0.2319(2) 0.0425(12) Uani 1 1 d . . . C27' C 0.3073(3) 0.7434(3) 0.2013(3) 0.086(2) Uani 1 1 d . . . H27B H 0.3256 0.7835 0.2262 0.104 Uiso 1 1 calc R . . C28' C 0.2849(4) 0.7487(3) 0.1348(3) 0.125(4) Uani 1 1 d . . . H28B H 0.2903 0.7909 0.1129 0.150 Uiso 1 1 calc R . . C29' C 0.2539(3) 0.6913(3) 0.0997(3) 0.093(2) Uani 1 1 d . . . H29B H 0.2352 0.6952 0.0542 0.111 Uiso 1 1 calc R . . C30' C 0.2515(2) 0.6287(2) 0.1335(2) 0.0491(13) Uani 1 1 d . . . H30B H 0.2324 0.5884 0.1099 0.059 Uiso 1 1 calc R . . C31' C 0.32210(16) 0.5723(2) 0.37793(19) 0.0303(10) Uani 1 1 d . . . H31C H 0.3395 0.6082 0.4123 0.036 Uiso 1 1 calc R . . H31D H 0.3349 0.5235 0.3946 0.036 Uiso 1 1 calc R . . C32' C 0.26239(16) 0.5766(2) 0.3598(2) 0.0292(10) Uani 1 1 d . . . C33' C 0.23491(17) 0.5938(2) 0.4018(2) 0.0343(10) Uani 1 1 d . . . H33B H 0.2541 0.6055 0.4460 0.041 Uiso 1 1 calc R . . C34' C 0.17867(18) 0.5939(2) 0.3789(2) 0.0377(11) Uani 1 1 d . . . H34B H 0.1589 0.6047 0.4072 0.045 Uiso 1 1 calc R . . C35' C 0.15267(18) 0.5780(2) 0.3145(2) 0.0365(11) Uani 1 1 d . . . H35B H 0.1144 0.5773 0.2978 0.044 Uiso 1 1 calc R . . C36' C 0.18190(16) 0.5628(2) 0.2736(2) 0.0307(10) Uani 1 1 d . . . H36B H 0.1634 0.5537 0.2287 0.037 Uiso 1 1 calc R . . C37' C 0.21893(15) 0.4430(2) 0.14078(19) 0.0229(9) Uani 1 1 d . . . C38' C 0.16326(14) 0.4300(2) 0.09417(18) 0.0223(9) Uani 1 1 d . . . C39' C 0.13010(15) 0.4888(2) 0.07332(19) 0.0259(9) Uani 1 1 d . . . H39B H 0.1429 0.5355 0.0894 0.031 Uiso 1 1 calc R . . C40' C 0.07733(16) 0.4813(2) 0.0284(2) 0.0306(10) Uani 1 1 d . . . H40B H 0.0550 0.5226 0.0142 0.037 Uiso 1 1 calc R . . C41' C 0.05879(16) 0.4143(2) 0.0059(2) 0.0304(10) Uani 1 1 d . . . H41B H 0.0237 0.4095 -0.0253 0.036 Uiso 1 1 calc R . . C42' C 0.09046(15) 0.3516(2) 0.02776(19) 0.0248(9) Uani 1 1 d . . . C43' C 0.07033(16) 0.2821(2) 0.0067(2) 0.0294(10) Uani 1 1 d . . . H43B H 0.0351 0.2771 -0.0241 0.035 Uiso 1 1 calc R . . C44' C 0.10056(17) 0.2217(2) 0.0298(2) 0.0341(10) Uani 1 1 d . . . H44B H 0.0862 0.1753 0.0152 0.041 Uiso 1 1 calc R . . C45' C 0.15247(16) 0.2281(2) 0.07494(19) 0.0282(9) Uani 1 1 d . . . H45B H 0.1731 0.1859 0.0910 0.034 Uiso 1 1 calc R . . C46' C 0.17381(16) 0.2946(2) 0.09622(19) 0.0270(9) Uani 1 1 d . . . H46B H 0.2091 0.2980 0.1271 0.032 Uiso 1 1 calc R . . C47' C 0.14393(14) 0.3586(2) 0.07284(18) 0.0209(8) Uani 1 1 d . . . Cl1 Cl 0.42061(4) 0.84460(6) 0.34141(6) 0.0418(3) Uani 1 1 d D . . O11 O 0.44190(15) 0.77525(17) 0.3398(2) 0.0763(12) Uani 1 1 d D . . O12 O 0.3776(2) 0.8428(2) 0.3643(3) 0.126(2) Uani 1 1 d D . . O13 O 0.46184(14) 0.8938(2) 0.3734(2) 0.0869(14) Uani 1 1 d D . . O14 O 0.39980(17) 0.8709(3) 0.2754(2) 0.1062(17) Uani 1 1 d D . . Cl2 Cl 0.08145(4) 0.67548(6) 0.12488(6) 0.0441(3) Uani 1 1 d D . . O21 O 0.0636(2) 0.6144(2) 0.1505(3) 0.1040(17) Uani 1 1 d D . . O22 O 0.13792(12) 0.6827(2) 0.1511(2) 0.0745(12) Uani 1 1 d D . . O23 O 0.05620(14) 0.73907(17) 0.1363(2) 0.0716(12) Uani 1 1 d D . . O24 O 0.06734(17) 0.6654(2) 0.05531(17) 0.0915(15) Uani 1 1 d D . . Cl3 Cl 0.39322(6) 0.02862(7) 0.02929(6) 0.0577(4) Uani 1 1 d D . . O31 O 0.39145(13) -0.04771(15) 0.03808(16) 0.0513(9) Uani 1 1 d D . . O32 O 0.4234(3) 0.0620(3) 0.0869(2) 0.157(3) Uani 1 1 d D . . O33 O 0.41227(17) 0.0446(2) -0.02246(19) 0.0790(13) Uani 1 1 d D . . O34 O 0.33875(19) 0.0553(2) 0.0098(3) 0.1132(19) Uani 1 1 d D . . Cl4 Cl 0.08217(6) 0.46263(8) 0.43379(7) 0.0640(4) Uani 0.50 1 d PD A 1 O41 O 0.13575(14) 0.4494(2) 0.47325(17) 0.0721(12) Uani 0.50 1 d PD A 1 O42 O 0.0615(5) 0.3986(5) 0.3973(5) 0.115(6) Uani 0.50 1 d PD A 1 O43 O 0.0708(5) 0.5239(6) 0.4010(7) 0.224(12) Uani 0.50 1 d PD A 1 O44 O 0.0541(3) 0.4608(5) 0.4840(4) 0.079(3) Uani 0.50 1 d PD A 1 Cl4A Cl 0.08217(6) 0.46263(8) 0.43379(7) 0.0640(4) Uani 0.50 1 d P B 2 O45 O 0.13575(14) 0.4494(2) 0.47325(17) 0.0721(12) Uani 0.50 1 d PD B 2 O46 O 0.0842(4) 0.4834(5) 0.3684(3) 0.092(3) Uani 0.50 1 d PD B 2 O47 O 0.0500(4) 0.4015(6) 0.4206(5) 0.106(6) Uani 0.50 1 d PD B 2 O48 O 0.0603(5) 0.5227(6) 0.4546(5) 0.185(9) Uani 0.50 1 d PD 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 0.0200(3) 0.0190(3) 0.0270(3) 0.0004(2) 0.0101(2) -0.0008(2) Co2 0.0225(3) 0.0209(3) 0.0251(3) -0.0033(2) 0.0086(2) -0.0033(2) O1 0.0219(14) 0.0176(14) 0.0282(15) 0.0009(11) 0.0105(12) -0.0028(11) O2 0.0251(14) 0.0217(14) 0.0331(16) -0.0047(12) 0.0140(12) -0.0067(12) O3 0.0273(15) 0.0236(15) 0.0244(15) -0.0069(12) 0.0100(12) -0.0049(12) O4 0.0227(14) 0.0235(15) 0.0269(15) -0.0034(12) 0.0081(12) 0.0004(12) O5 0.0236(14) 0.0264(15) 0.0257(15) -0.0058(12) 0.0075(12) -0.0016(12) N1 0.0238(17) 0.0195(17) 0.0274(19) 0.0028(14) 0.0097(15) 0.0001(14) N2 0.0254(18) 0.0206(18) 0.031(2) 0.0035(14) 0.0114(15) -0.0004(14) N3 0.0213(17) 0.0220(18) 0.037(2) 0.0007(15) 0.0168(15) 0.0019(14) N4 0.0242(18) 0.0292(19) 0.0263(19) -0.0050(15) 0.0090(15) -0.0039(15) N5 0.0287(18) 0.0213(18) 0.030(2) -0.0001(15) 0.0078(16) -0.0007(15) N6 0.0288(19) 0.0222(18) 0.030(2) -0.0030(15) 0.0121(16) 0.0010(15) C1 0.021(2) 0.017(2) 0.033(2) 0.0057(17) 0.0094(18) -0.0015(17) C2 0.028(2) 0.016(2) 0.028(2) 0.0008(17) 0.0090(18) -0.0010(17) C3 0.033(2) 0.020(2) 0.034(2) 0.0044(18) 0.0183(19) 0.0005(18) C4 0.027(2) 0.018(2) 0.039(3) 0.0055(18) 0.0129(19) 0.0007(17) C5 0.024(2) 0.019(2) 0.035(2) 0.0023(17) 0.0095(18) -0.0022(17) C6 0.024(2) 0.025(2) 0.028(2) 0.0028(18) 0.0075(18) -0.0022(18) C7 0.038(3) 0.021(2) 0.055(3) 0.002(2) 0.025(2) -0.0071(19) C8 0.045(3) 0.036(3) 0.061(3) -0.001(2) 0.024(3) -0.018(2) C9 0.065(3) 0.042(3) 0.066(4) 0.003(3) 0.035(3) -0.019(3) C10 0.052(3) 0.042(3) 0.113(5) 0.001(3) 0.050(3) 0.002(3) C11 0.033(2) 0.021(2) 0.030(2) 0.0035(17) 0.0137(19) -0.0004(18) C12 0.031(2) 0.024(2) 0.035(2) 0.0039(18) 0.0159(19) 0.0022(18) C13 0.026(2) 0.019(2) 0.036(2) 0.0057(18) 0.0137(19) 0.0017(17) C14 0.022(2) 0.044(3) 0.042(3) 0.005(2) 0.014(2) -0.002(2) C15 0.028(2) 0.050(3) 0.042(3) 0.008(2) 0.006(2) -0.003(2) C16 0.034(3) 0.043(3) 0.034(3) 0.008(2) 0.006(2) 0.000(2) C17 0.029(2) 0.035(2) 0.032(3) 0.0066(19) 0.013(2) 0.0004(19) C18 0.030(2) 0.030(2) 0.030(2) -0.0035(18) 0.0151(19) -0.0015(19) C19 0.023(2) 0.027(2) 0.043(3) -0.0025(19) 0.0190(19) -0.0003(18) C20 0.041(3) 0.031(3) 0.052(3) -0.012(2) 0.028(2) -0.008(2) C21 0.054(3) 0.024(3) 0.074(4) -0.011(2) 0.037(3) -0.008(2) C22 0.034(2) 0.025(2) 0.064(3) 0.000(2) 0.028(2) -0.004(2) C23 0.027(2) 0.024(2) 0.044(3) 0.003(2) 0.019(2) 0.0013(18) C24 0.023(2) 0.035(2) 0.033(2) -0.0021(19) 0.0085(18) -0.0079(19) C25 0.038(3) 0.029(2) 0.041(3) -0.010(2) 0.012(2) -0.012(2) C26 0.043(3) 0.024(2) 0.039(3) -0.002(2) 0.009(2) -0.006(2) C27 0.079(4) 0.033(3) 0.067(4) 0.001(3) 0.001(3) -0.024(3) C28 0.110(5) 0.046(4) 0.068(4) 0.022(3) -0.012(4) -0.020(4) C29 0.082(4) 0.052(4) 0.050(4) 0.017(3) -0.010(3) -0.008(3) C30 0.044(3) 0.027(2) 0.042(3) 0.004(2) 0.004(2) 0.000(2) C31 0.032(2) 0.037(3) 0.024(2) -0.0040(19) 0.0087(19) -0.006(2) C32 0.032(2) 0.031(2) 0.029(2) -0.0058(19) 0.0127(19) -0.0088(19) C33 0.043(3) 0.050(3) 0.036(3) -0.010(2) 0.020(2) -0.006(2) C34 0.050(3) 0.044(3) 0.045(3) -0.010(2) 0.029(3) 0.000(2) C35 0.033(2) 0.033(3) 0.045(3) -0.010(2) 0.020(2) 0.000(2) C36 0.027(2) 0.026(2) 0.037(3) -0.0020(19) 0.0105(19) -0.0005(18) C37 0.021(2) 0.022(2) 0.029(2) 0.0015(18) 0.0095(18) -0.0004(17) C38 0.023(2) 0.023(2) 0.026(2) -0.0051(17) 0.0092(17) -0.0007(17) C39 0.024(2) 0.027(2) 0.035(2) -0.0095(19) 0.0081(19) 0.0000(18) C40 0.026(2) 0.038(3) 0.041(3) -0.006(2) 0.009(2) 0.009(2) C41 0.020(2) 0.050(3) 0.034(3) -0.003(2) 0.0098(19) 0.005(2) C42 0.025(2) 0.037(3) 0.034(2) -0.009(2) 0.0159(19) -0.0074(19) C43 0.030(2) 0.040(3) 0.041(3) -0.014(2) 0.014(2) -0.012(2) C44 0.042(3) 0.034(3) 0.053(3) -0.015(2) 0.022(2) -0.019(2) C45 0.035(3) 0.026(2) 0.050(3) -0.004(2) 0.017(2) -0.003(2) C46 0.024(2) 0.029(2) 0.032(2) -0.0052(18) 0.0103(18) -0.0035(18) C47 0.019(2) 0.027(2) 0.026(2) -0.0044(17) 0.0108(17) -0.0009(17) Co1' 0.0192(3) 0.0193(3) 0.0270(3) -0.0014(2) 0.0098(2) -0.0028(2) Co2' 0.0240(3) 0.0201(3) 0.0281(3) -0.0060(2) 0.0102(2) -0.0056(2) O1' 0.0193(13) 0.0236(15) 0.0325(16) -0.0054(12) 0.0101(12) -0.0055(12) O2' 0.0256(14) 0.0228(15) 0.0293(16) -0.0054(12) 0.0128(12) -0.0065(12) O3' 0.0300(15) 0.0209(14) 0.0261(15) -0.0016(12) 0.0110(12) -0.0033(12) O4' 0.0221(14) 0.0212(14) 0.0296(15) -0.0043(12) 0.0115(12) -0.0024(12) O5' 0.0215(14) 0.0215(14) 0.0297(15) -0.0091(12) 0.0078(12) -0.0036(11) N1' 0.0217(17) 0.0213(17) 0.0255(18) -0.0027(14) 0.0096(14) -0.0054(14) N2' 0.0208(17) 0.0248(18) 0.031(2) 0.0033(15) 0.0097(15) -0.0015(14) N3' 0.0155(16) 0.0200(17) 0.035(2) 0.0003(15) 0.0098(14) -0.0002(13) N4' 0.0311(19) 0.0286(19) 0.030(2) -0.0064(15) 0.0139(16) -0.0094(15) N5' 0.035(2) 0.0225(19) 0.031(2) -0.0032(15) 0.0119(17) -0.0051(15) N6' 0.032(2) 0.0197(17) 0.032(2) -0.0042(15) 0.0128(16) -0.0038(15) C1' 0.020(2) 0.024(2) 0.034(2) -0.0023(18) 0.0103(18) -0.0054(17) C2' 0.025(2) 0.019(2) 0.027(2) -0.0012(17) 0.0096(18) -0.0057(17) C3' 0.030(2) 0.026(2) 0.033(2) 0.0034(18) 0.0165(19) -0.0010(18) C4' 0.024(2) 0.022(2) 0.037(3) -0.0007(18) 0.0101(19) -0.0049(17) C5' 0.026(2) 0.031(2) 0.033(2) -0.0057(19) 0.0069(19) -0.0065(19) C6' 0.022(2) 0.027(2) 0.035(2) -0.0042(19) 0.0112(18) -0.0064(18) C7' 0.023(2) 0.031(2) 0.045(3) -0.003(2) 0.014(2) -0.0066(18) C8' 0.046(3) 0.052(3) 0.060(3) 0.005(3) 0.021(3) -0.026(3) C9' 0.032(2) 0.034(3) 0.059(3) -0.009(2) 0.020(2) -0.010(2) C10' 0.027(3) 0.046(3) 0.091(4) -0.006(3) 0.019(3) 0.003(2) C11' 0.028(2) 0.028(2) 0.027(2) -0.0012(18) 0.0112(18) -0.0047(18) C12' 0.024(2) 0.023(2) 0.039(3) -0.0003(18) 0.0157(19) -0.0034(17) C13' 0.023(2) 0.026(2) 0.031(2) 0.0025(18) 0.0108(18) -0.0008(17) C14' 0.026(2) 0.033(2) 0.043(3) 0.001(2) 0.014(2) -0.0007(19) C15' 0.025(2) 0.051(3) 0.034(3) -0.001(2) 0.002(2) 0.000(2) C16' 0.031(2) 0.045(3) 0.028(2) 0.000(2) 0.003(2) 0.005(2) C17' 0.033(2) 0.033(2) 0.031(3) 0.0068(19) 0.014(2) 0.0057(19) C18' 0.029(2) 0.020(2) 0.027(2) -0.0052(17) 0.0105(18) -0.0044(17) C19' 0.018(2) 0.024(2) 0.031(2) 0.0002(18) 0.0096(17) -0.0013(16) C20' 0.031(2) 0.025(2) 0.040(3) -0.0051(19) 0.015(2) -0.0020(18) C21' 0.031(2) 0.020(2) 0.056(3) -0.002(2) 0.019(2) -0.0025(18) C22' 0.027(2) 0.022(2) 0.044(3) 0.0033(19) 0.017(2) -0.0004(18) C23' 0.020(2) 0.029(2) 0.039(3) 0.0080(19) 0.0141(19) 0.0034(18) C24' 0.028(2) 0.033(2) 0.033(2) -0.0074(19) 0.0087(19) -0.0088(19) C25' 0.043(3) 0.022(2) 0.043(3) -0.0088(19) 0.020(2) -0.011(2) C26' 0.055(3) 0.028(3) 0.047(3) -0.006(2) 0.020(2) -0.012(2) C27' 0.154(7) 0.028(3) 0.056(4) 0.001(3) 0.007(4) -0.036(4) C28' 0.232(10) 0.044(4) 0.066(5) 0.010(3) 0.006(5) -0.067(5) C29' 0.157(7) 0.051(4) 0.048(4) 0.011(3) 0.005(4) -0.039(4) C30' 0.066(3) 0.028(3) 0.049(3) -0.003(2) 0.013(3) -0.012(2) C31' 0.030(2) 0.037(2) 0.025(2) -0.0088(19) 0.0102(18) -0.0079(19) C32' 0.035(2) 0.021(2) 0.034(3) -0.0014(18) 0.016(2) -0.0061(18) C33' 0.038(3) 0.036(3) 0.033(2) -0.002(2) 0.017(2) -0.006(2) C34' 0.038(3) 0.037(3) 0.045(3) -0.001(2) 0.023(2) -0.003(2) C35' 0.032(2) 0.032(3) 0.049(3) -0.006(2) 0.019(2) 0.001(2) C36' 0.029(2) 0.024(2) 0.040(3) -0.0060(19) 0.014(2) -0.0012(18) C37' 0.025(2) 0.019(2) 0.026(2) 0.0028(17) 0.0110(18) -0.0011(17) C38' 0.020(2) 0.022(2) 0.026(2) -0.0045(17) 0.0105(17) -0.0012(17) C39' 0.026(2) 0.019(2) 0.035(2) -0.0060(17) 0.0125(19) -0.0033(17) C40' 0.029(2) 0.030(2) 0.035(2) 0.0004(19) 0.0134(19) 0.0084(19) C41' 0.022(2) 0.038(3) 0.030(2) -0.0034(19) 0.0065(18) 0.0018(19) C42' 0.021(2) 0.029(2) 0.027(2) -0.0028(18) 0.0107(17) -0.0045(18) C43' 0.025(2) 0.028(2) 0.036(2) -0.0085(19) 0.0098(19) -0.0077(19) C44' 0.041(3) 0.025(2) 0.039(3) -0.0100(19) 0.016(2) -0.013(2) C45' 0.031(2) 0.022(2) 0.033(2) 0.0006(18) 0.0135(19) -0.0033(18) C46' 0.025(2) 0.029(2) 0.029(2) 0.0036(18) 0.0110(18) 0.0019(18) C47' 0.021(2) 0.020(2) 0.025(2) -0.0031(16) 0.0126(17) -0.0005(16) Cl1 0.0350(6) 0.0305(6) 0.0591(8) 0.0010(5) 0.0147(6) 0.0018(5) O11 0.068(3) 0.032(2) 0.126(4) -0.016(2) 0.028(2) 0.0126(18) O12 0.140(5) 0.072(3) 0.233(7) -0.007(4) 0.153(5) 0.002(3) O13 0.057(2) 0.075(3) 0.117(4) -0.048(3) 0.013(2) -0.010(2) O14 0.081(3) 0.130(4) 0.085(3) 0.038(3) -0.003(3) -0.009(3) Cl2 0.0354(6) 0.0337(6) 0.0597(8) -0.0085(6) 0.0110(6) 0.0002(5) O21 0.135(4) 0.055(3) 0.164(5) 0.011(3) 0.106(4) -0.007(3) O22 0.035(2) 0.087(3) 0.090(3) -0.014(2) 0.005(2) 0.003(2) O23 0.063(2) 0.036(2) 0.116(3) -0.026(2) 0.029(2) 0.0044(18) O24 0.088(3) 0.101(4) 0.062(3) -0.025(2) -0.006(2) 0.017(3) Cl3 0.0948(11) 0.0356(7) 0.0485(8) -0.0026(6) 0.0317(8) -0.0030(7) O31 0.058(2) 0.0347(19) 0.061(2) 0.0069(16) 0.0204(18) 0.0081(16) O32 0.288(8) 0.092(4) 0.058(3) -0.030(3) 0.014(4) -0.059(5) O33 0.114(3) 0.070(3) 0.078(3) -0.001(2) 0.066(3) -0.021(2) O34 0.141(4) 0.074(3) 0.159(5) 0.058(3) 0.096(4) 0.064(3) Cl4 0.0758(10) 0.0489(9) 0.0716(10) -0.0024(7) 0.0303(8) 0.0092(8) O41 0.064(3) 0.081(3) 0.066(3) -0.029(2) 0.015(2) 0.002(2) O42 0.183(14) 0.089(9) 0.048(8) -0.021(6) 0.004(7) -0.025(8) O43 0.211(16) 0.121(12) 0.44(3) 0.202(18) 0.24(2) 0.120(12) O44 0.073(6) 0.076(6) 0.111(8) -0.003(6) 0.062(6) -0.003(5) Cl4A 0.0758(10) 0.0489(9) 0.0716(10) -0.0024(7) 0.0303(8) 0.0092(8) O45 0.064(3) 0.081(3) 0.066(3) -0.029(2) 0.015(2) 0.002(2) O46 0.113(8) 0.104(8) 0.041(5) 0.012(5) 0.002(5) -0.051(6) O47 0.105(8) 0.130(12) 0.054(8) 0.059(8) -0.012(6) -0.051(8) O48 0.32(2) 0.116(11) 0.080(8) -0.011(8) 0.010(10) 0.158(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.863(3) . ? Co1 O1 1.890(2) . ? Co1 N2 1.915(3) . ? Co1 N3 1.917(3) . ? Co1 O4 1.936(3) . ? Co1 N1 2.017(3) . ? Co1 Co2 3.1609(7) . ? Co2 O3 1.865(3) . ? Co2 O1 1.905(2) . ? Co2 N6 1.912(3) . ? Co2 O5 1.920(3) . ? Co2 N4 1.956(3) . ? Co2 N5 1.988(3) . ? O1 C1 1.366(4) . ? O2 O3 1.415(3) . ? O4 C37 1.267(4) . ? O5 C37 1.260(4) . ? N1 C18 1.490(5) . ? N1 C12 1.503(5) . ? N1 C11 1.516(5) . ? N2 C17 1.331(5) . ? N2 C13 1.351(5) . ? N3 C19 1.345(5) . ? N3 C23 1.347(5) . ? N4 C31 1.486(5) . ? N4 C25 1.499(5) . ? N4 C24 1.501(5) . ? N5 C30 1.335(5) . ? N5 C26 1.340(5) . ? N6 C36 1.339(5) . ? N6 C32 1.360(5) . ? C1 C2 1.379(5) . ? C1 C6 1.396(5) . ? C2 C3 1.393(5) . ? C2 C11 1.505(5) . ? C3 C4 1.395(6) . ? C3 H3A 0.9500 . ? C4 C5 1.389(5) . ? C4 C7 1.543(5) . ? C5 C6 1.386(5) . ? C5 H5A 0.9500 . ? C6 C24 1.507(5) . ? C7 C10 1.528(6) . ? C7 C8 1.531(6) . ? C7 C9 1.542(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.488(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.382(5) . ? C14 C15 1.380(6) . ? C14 H14A 0.9500 . ? C15 C16 1.381(6) . ? C15 H15A 0.9500 . ? C16 C17 1.379(6) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.500(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.381(6) . ? C20 C21 1.384(6) . ? C20 H20A 0.9500 . ? C21 C22 1.370(6) . ? C21 H21A 0.9500 . ? C22 C23 1.378(6) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.485(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.381(6) . ? C27 C28 1.363(7) . ? C27 H27A 0.9500 . ? C28 C29 1.384(8) . ? C28 H28A 0.9500 . ? C29 C30 1.374(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.497(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.378(6) . ? C33 C34 1.386(6) . ? C33 H33A 0.9500 . ? C34 C35 1.378(6) . ? C34 H34A 0.9500 . ? C35 C36 1.375(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.510(5) . ? C38 C39 1.370(5) . ? C38 C47 1.429(5) . ? C39 C40 1.398(6) . ? C39 H39A 0.9500 . ? C40 C41 1.358(6) . ? C40 H40A 0.9500 . ? C41 C42 1.416(6) . ? C41 H41A 0.9500 . ? C42 C43 1.411(6) . ? C42 C47 1.432(5) . ? C43 C44 1.350(6) . ? C43 H43A 0.9500 . ? C44 C45 1.411(6) . ? C44 H44A 0.9500 . ? C45 C46 1.372(6) . ? C45 H45A 0.9500 . ? C46 C47 1.426(5) . ? C46 H46A 0.9500 . ? Co1' O2' 1.859(2) . ? Co1' O1' 1.903(3) . ? Co1' N3' 1.912(3) . ? Co1' N2' 1.914(3) . ? Co1' O4' 1.942(3) . ? Co1' N1' 2.021(3) . ? Co1' Co2' 3.1601(7) . ? Co2' O3' 1.867(3) . ? Co2' O1' 1.902(2) . ? Co2' O5' 1.906(2) . ? Co2' N6' 1.921(3) . ? Co2' N4' 1.959(3) . ? Co2' N5' 1.984(3) . ? O1' C1' 1.364(4) . ? O2' O3' 1.412(3) . ? O4' C37' 1.265(4) . ? O5' C37' 1.270(4) . ? N1' C18' 1.483(5) . ? N1' C12' 1.500(5) . ? N1' C11' 1.507(5) . ? N2' C13' 1.352(5) . ? N2' C17' 1.355(5) . ? N3' C19' 1.351(5) . ? N3' C23' 1.356(5) . ? N4' C24' 1.485(5) . ? N4' C31' 1.489(5) . ? N4' C25' 1.501(5) . ? N5' C30' 1.330(6) . ? N5' C26' 1.353(5) . ? N6' C36' 1.338(5) . ? N6' C32' 1.353(5) . ? C1' C6' 1.393(5) . ? C1' C2' 1.402(5) . ? C2' C3' 1.401(5) . ? C2' C11' 1.498(5) . ? C3' C4' 1.391(6) . ? C3' H3A' 0.9500 . ? C4' C5' 1.390(6) . ? C4' C7' 1.537(5) . ? C5' C6' 1.395(5) . ? C5' H5A' 0.9500 . ? C6' C24' 1.504(6) . ? C7' C9' 1.525(6) . ? C7' C10' 1.532(6) . ? C7' C8' 1.547(6) . ? C8' H8A' 0.9800 . ? C8' H8B' 0.9800 . ? C8' H8C' 0.9800 . ? C9' H9A' 0.9800 . ? C9' H9B' 0.9800 . ? C9' H9C' 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12' C13' 1.491(5) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? C13' C14' 1.377(5) . ? C14' C15' 1.385(6) . ? C14' H14B 0.9500 . ? C15' C16' 1.368(6) . ? C15' H15B 0.9500 . ? C16' C17' 1.378(6) . ? C16' H16B 0.9500 . ? C17' H17B 0.9500 . ? C18' C19' 1.499(5) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' C20' 1.387(5) . ? C20' C21' 1.384(6) . ? C20' H20B 0.9500 . ? C21' C22' 1.371(6) . ? C21' H21B 0.9500 . ? C22' C23' 1.390(6) . ? C22' H22B 0.9500 . ? C23' H23B 0.9500 . ? C24' H24C 0.9900 . ? C24' H24D 0.9900 . ? C25' C26' 1.482(6) . ? C25' H25C 0.9900 . ? C25' H25D 0.9900 . ? C26' C27' 1.386(7) . ? C27' C28' 1.371(8) . ? C27' H27B 0.9500 . ? C28' C29' 1.400(8) . ? C28' H28B 0.9500 . ? C29' C30' 1.386(7) . ? C29' H29B 0.9500 . ? C30' H30B 0.9500 . ? C31' C32' 1.490(5) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' C33' 1.380(6) . ? C33' C34' 1.397(6) . ? C33' H33B 0.9500 . ? C34' C35' 1.372(6) . ? C34' H34B 0.9500 . ? C35' C36' 1.387(6) . ? C35' H35B 0.9500 . ? C36' H36B 0.9500 . ? C37' C38' 1.498(5) . ? C38' C39' 1.374(5) . ? C38' C47' 1.435(5) . ? C39' C40' 1.414(5) . ? C39' H39B 0.9500 . ? C40' C41' 1.363(6) . ? C40' H40B 0.9500 . ? C41' C42' 1.415(6) . ? C41' H41B 0.9500 . ? C42' C43' 1.406(5) . ? C42' C47' 1.429(5) . ? C43' C44' 1.367(6) . ? C43' H43B 0.9500 . ? C44' C45' 1.397(6) . ? C44' H44B 0.9500 . ? C45' C46' 1.367(5) . ? C45' H45B 0.9500 . ? C46' C47' 1.418(5) . ? C46' H46B 0.9500 . ? Cl1 O12 1.383(4) . ? Cl1 O11 1.405(3) . ? Cl1 O13 1.409(3) . ? Cl1 O14 1.441(4) . ? Cl2 O21 1.410(4) . ? Cl2 O22 1.411(3) . ? Cl2 O23 1.413(3) . ? Cl2 O24 1.446(4) . ? Cl3 O32 1.385(4) . ? Cl3 O33 1.409(3) . ? Cl3 O31 1.428(3) . ? Cl3 O34 1.441(4) . ? Cl4 O43 1.319(6) . ? Cl4 O41 1.407(3) . ? Cl4 O42 1.429(7) . ? Cl4 O44 1.511(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O1 90.82(11) . . ? O2 Co1 N2 95.42(13) . . ? O1 Co1 N2 92.15(12) . . ? O2 Co1 N3 93.95(12) . . ? O1 Co1 N3 171.96(13) . . ? N2 Co1 N3 93.84(13) . . ? O2 Co1 O4 87.69(11) . . ? O1 Co1 O4 87.46(11) . . ? N2 Co1 O4 176.87(12) . . ? N3 Co1 O4 86.27(12) . . ? O2 Co1 N1 177.00(12) . . ? O1 Co1 N1 92.13(11) . . ? N2 Co1 N1 84.98(13) . . ? N3 Co1 N1 83.06(13) . . ? O4 Co1 N1 91.93(12) . . ? O2 Co1 Co2 58.56(8) . . ? O1 Co1 Co2 33.75(7) . . ? N2 Co1 Co2 103.64(10) . . ? N3 Co1 Co2 148.24(9) . . ? O4 Co1 Co2 77.69(8) . . ? N1 Co1 Co2 124.24(9) . . ? O3 Co2 O1 85.10(11) . . ? O3 Co2 N6 89.73(12) . . ? O1 Co2 N6 174.70(12) . . ? O3 Co2 O5 94.18(11) . . ? O1 Co2 O5 91.23(11) . . ? N6 Co2 O5 90.30(12) . . ? O3 Co2 N4 91.03(12) . . ? O1 Co2 N4 96.54(12) . . ? N6 Co2 N4 82.37(13) . . ? O5 Co2 N4 170.99(12) . . ? O3 Co2 N5 171.52(12) . . ? O1 Co2 N5 88.55(12) . . ? N6 Co2 N5 96.48(14) . . ? O5 Co2 N5 91.56(12) . . ? N4 Co2 N5 84.11(13) . . ? O3 Co2 Co1 59.26(8) . . ? O1 Co2 Co1 33.46(7) . . ? N6 Co2 Co1 142.90(10) . . ? O5 Co2 Co1 73.75(8) . . ? N4 Co2 Co1 115.26(10) . . ? N5 Co2 Co1 116.77(10) . . ? C1 O1 Co1 119.1(2) . . ? C1 O1 Co2 123.3(2) . . ? Co1 O1 Co2 112.79(12) . . ? O3 O2 Co1 111.96(18) . . ? O2 O3 Co2 110.38(18) . . ? C37 O4 Co1 124.9(2) . . ? C37 O5 Co2 131.8(2) . . ? C18 N1 C12 110.1(3) . . ? C18 N1 C11 112.4(3) . . ? C12 N1 C11 110.4(3) . . ? C18 N1 Co1 103.8(2) . . ? C12 N1 Co1 108.6(2) . . ? C11 N1 Co1 111.2(2) . . ? C17 N2 C13 118.9(3) . . ? C17 N2 Co1 125.0(3) . . ? C13 N2 Co1 115.5(3) . . ? C19 N3 C23 120.2(3) . . ? C19 N3 Co1 114.0(3) . . ? C23 N3 Co1 125.7(3) . . ? C31 N4 C25 109.8(3) . . ? C31 N4 C24 110.1(3) . . ? C25 N4 C24 109.7(3) . . ? C31 N4 Co2 104.8(2) . . ? C25 N4 Co2 109.2(2) . . ? C24 N4 Co2 113.1(2) . . ? C30 N5 C26 118.8(4) . . ? C30 N5 Co2 125.7(3) . . ? C26 N5 Co2 114.3(3) . . ? C36 N6 C32 119.4(3) . . ? C36 N6 Co2 127.6(3) . . ? C32 N6 Co2 113.0(3) . . ? O1 C1 C2 118.0(3) . . ? O1 C1 C6 120.9(3) . . ? C2 C1 C6 121.0(3) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 C11 117.8(3) . . ? C3 C2 C11 123.2(4) . . ? C2 C3 C4 121.6(4) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C7 121.8(4) . . ? C3 C4 C7 120.3(4) . . ? C6 C5 C4 121.9(4) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C1 118.7(4) . . ? C5 C6 C24 121.7(4) . . ? C1 C6 C24 119.3(3) . . ? C10 C7 C8 109.5(4) . . ? C10 C7 C9 110.0(4) . . ? C8 C7 C9 107.9(4) . . ? C10 C7 C4 108.9(3) . . ? C8 C7 C4 111.7(4) . . ? C9 C7 C4 108.8(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 N1 109.1(3) . . ? C2 C11 H11A 109.9 . . ? N1 C11 H11A 109.9 . . ? C2 C11 H11B 109.9 . . ? N1 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C13 C12 N1 110.1(3) . . ? C13 C12 H12A 109.6 . . ? N1 C12 H12A 109.6 . . ? C13 C12 H12B 109.6 . . ? N1 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N2 C13 C14 121.6(4) . . ? N2 C13 C12 115.5(3) . . ? C14 C13 C12 122.9(4) . . ? C15 C14 C13 118.8(4) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 C16 119.3(4) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 118.8(4) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? N2 C17 C16 122.3(4) . . ? N2 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? N1 C18 C19 107.6(3) . . ? N1 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? N1 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? N3 C19 C20 120.8(4) . . ? N3 C19 C18 114.7(3) . . ? C20 C19 C18 124.6(4) . . ? C19 C20 C21 119.1(4) . . ? C19 C20 H20A 120.4 . . ? C21 C20 H20A 120.4 . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 119.4(4) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? N3 C23 C22 120.9(4) . . ? N3 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? N4 C24 C6 113.9(3) . . ? N4 C24 H24A 108.8 . . ? C6 C24 H24A 108.8 . . ? N4 C24 H24B 108.8 . . ? C6 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 N4 110.5(3) . . ? C26 C25 H25A 109.6 . . ? N4 C25 H25A 109.6 . . ? C26 C25 H25B 109.6 . . ? N4 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N5 C26 C27 121.7(4) . . ? N5 C26 C25 114.4(4) . . ? C27 C26 C25 123.9(4) . . ? C28 C27 C26 119.0(5) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C29 119.9(5) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 118.0(5) . . ? C30 C29 H29A 121.0 . . ? C28 C29 H29A 121.0 . . ? N5 C30 C29 122.7(4) . . ? N5 C30 H30A 118.7 . . ? C29 C30 H30A 118.7 . . ? N4 C31 C32 106.3(3) . . ? N4 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? N4 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? N6 C32 C33 121.4(4) . . ? N6 C32 C31 113.8(3) . . ? C33 C32 C31 124.8(4) . . ? C32 C33 C34 118.7(4) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C36 C35 C34 119.2(4) . . ? C36 C35 H35A 120.4 . . ? C34 C35 H35A 120.4 . . ? N6 C36 C35 121.7(4) . . ? N6 C36 H36A 119.1 . . ? C35 C36 H36A 119.1 . . ? O5 C37 O4 127.1(3) . . ? O5 C37 C38 115.5(3) . . ? O4 C37 C38 117.3(3) . . ? C39 C38 C47 120.0(3) . . ? C39 C38 C37 117.8(3) . . ? C47 C38 C37 122.1(3) . . ? C38 C39 C40 121.6(4) . . ? C38 C39 H39A 119.2 . . ? C40 C39 H39A 119.2 . . ? C41 C40 C39 120.0(4) . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C40 C41 C42 121.1(4) . . ? C40 C41 H41A 119.4 . . ? C42 C41 H41A 119.4 . . ? C43 C42 C41 121.3(4) . . ? C43 C42 C47 119.6(4) . . ? C41 C42 C47 119.1(4) . . ? C44 C43 C42 121.1(4) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C45 120.8(4) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C46 C45 C44 119.8(4) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C45 C46 C47 121.4(4) . . ? C45 C46 H46A 119.3 . . ? C47 C46 H46A 119.3 . . ? C46 C47 C38 124.5(3) . . ? C46 C47 C42 117.3(4) . . ? C38 C47 C42 118.1(3) . . ? O2' Co1' O1' 90.96(11) . . ? O2' Co1' N3' 93.93(12) . . ? O1' Co1' N3' 171.36(13) . . ? O2' Co1' N2' 95.21(12) . . ? O1' Co1' N2' 93.20(12) . . ? N3' Co1' N2' 93.46(13) . . ? O2' Co1' O4' 87.66(11) . . ? O1' Co1' O4' 87.46(11) . . ? N3' Co1' O4' 85.62(12) . . ? N2' Co1' O4' 177.04(12) . . ? O2' Co1' N1' 176.56(12) . . ? O1' Co1' N1' 92.44(12) . . ? N3' Co1' N1' 82.64(13) . . ? N2' Co1' N1' 85.14(13) . . ? O4' Co1' N1' 91.95(11) . . ? O2' Co1' Co2' 58.64(8) . . ? O1' Co1' Co2' 33.83(7) . . ? N3' Co1' Co2' 147.92(9) . . ? N2' Co1' Co2' 104.53(10) . . ? O4' Co1' Co2' 77.58(7) . . ? N1' Co1' Co2' 124.59(9) . . ? O3' Co2' O1' 84.91(11) . . ? O3' Co2' O5' 94.27(11) . . ? O1' Co2' O5' 91.82(11) . . ? O3' Co2' N6' 89.98(13) . . ? O1' Co2' N6' 174.86(13) . . ? O5' Co2' N6' 89.12(12) . . ? O3' Co2' N4' 91.09(13) . . ? O1' Co2' N4' 96.89(12) . . ? O5' Co2' N4' 170.15(13) . . ? N6' Co2' N4' 82.61(13) . . ? O3' Co2' N5' 171.79(13) . . ? O1' Co2' N5' 88.72(13) . . ? O5' Co2' N5' 91.09(13) . . ? N6' Co2' N5' 96.32(14) . . ? N4' Co2' N5' 84.54(14) . . ? O3' Co2' Co1' 58.88(8) . . ? O1' Co2' Co1' 33.87(8) . . ? O5' Co2' Co1' 73.96(8) . . ? N6' Co2' Co1' 142.25(10) . . ? N4' Co2' Co1' 115.89(10) . . ? N5' Co2' Co1' 117.04(10) . . ? C1' O1' Co2' 123.5(2) . . ? C1' O1' Co1' 118.2(2) . . ? Co2' O1' Co1' 112.30(12) . . ? O3' O2' Co1' 111.51(18) . . ? O2' O3' Co2' 110.50(18) . . ? C37' O4' Co1' 124.1(2) . . ? C37' O5' Co2' 132.1(2) . . ? C18' N1' C12' 110.1(3) . . ? C18' N1' C11' 113.2(3) . . ? C12' N1' C11' 110.0(3) . . ? C18' N1' Co1' 103.8(2) . . ? C12' N1' Co1' 108.1(2) . . ? C11' N1' Co1' 111.3(2) . . ? C13' N2' C17' 118.9(3) . . ? C13' N2' Co1' 115.5(3) . . ? C17' N2' Co1' 124.9(3) . . ? C19' N3' C23' 119.5(3) . . ? C19' N3' Co1' 113.9(2) . . ? C23' N3' Co1' 126.4(3) . . ? C24' N4' C31' 110.0(3) . . ? C24' N4' C25' 110.6(3) . . ? C31' N4' C25' 109.1(3) . . ? C24' N4' Co2' 113.0(2) . . ? C31' N4' Co2' 104.4(2) . . ? C25' N4' Co2' 109.6(2) . . ? C30' N5' C26' 119.1(4) . . ? C30' N5' Co2' 126.4(3) . . ? C26' N5' Co2' 113.8(3) . . ? C36' N6' C32' 119.9(3) . . ? C36' N6' Co2' 126.8(3) . . ? C32' N6' Co2' 113.2(3) . . ? O1' C1' C6' 121.3(3) . . ? O1' C1' C2' 117.4(3) . . ? C6' C1' C2' 121.3(3) . . ? C3' C2' C1' 118.4(3) . . ? C3' C2' C11' 123.5(4) . . ? C1' C2' C11' 117.8(3) . . ? C4' C3' C2' 121.6(4) . . ? C4' C3' H3A' 119.2 . . ? C2' C3' H3A' 119.2 . . ? C5' C4' C3' 117.9(4) . . ? C5' C4' C7' 121.6(4) . . ? C3' C4' C7' 120.4(4) . . ? C4' C5' C6' 122.6(4) . . ? C4' C5' H5A' 118.7 . . ? C6' C5' H5A' 118.7 . . ? C1' C6' C5' 118.0(4) . . ? C1' C6' C24' 120.0(3) . . ? C5' C6' C24' 121.6(4) . . ? C9' C7' C10' 108.6(4) . . ? C9' C7' C4' 112.1(3) . . ? C10' C7' C4' 108.2(3) . . ? C9' C7' C8' 107.5(4) . . ? C10' C7' C8' 110.6(4) . . ? C4' C7' C8' 109.8(3) . . ? C7' C8' H8A' 109.5 . . ? C7' C8' H8B' 109.5 . . ? H8A' C8' H8B' 109.5 . . ? C7' C8' H8C' 109.5 . . ? H8A' C8' H8C' 109.5 . . ? H8B' C8' H8C' 109.5 . . ? C7' C9' H9A' 109.5 . . ? C7' C9' H9B' 109.5 . . ? H9A' C9' H9B' 109.5 . . ? C7' C9' H9C' 109.5 . . ? H9A' C9' H9C' 109.5 . . ? H9B' C9' H9C' 109.5 . . ? C7' C10' H10D 109.5 . . ? C7' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C2' C11' N1' 110.2(3) . . ? C2' C11' H11C 109.6 . . ? N1' C11' H11C 109.6 . . ? C2' C11' H11D 109.6 . . ? N1' C11' H11D 109.6 . . ? H11C C11' H11D 108.1 . . ? C13' C12' N1' 110.4(3) . . ? C13' C12' H12C 109.6 . . ? N1' C12' H12C 109.6 . . ? C13' C12' H12D 109.6 . . ? N1' C12' H12D 109.6 . . ? H12C C12' H12D 108.1 . . ? N2' C13' C14' 121.1(4) . . ? N2' C13' C12' 115.2(3) . . ? C14' C13' C12' 123.7(4) . . ? C13' C14' C15' 119.7(4) . . ? C13' C14' H14B 120.2 . . ? C15' C14' H14B 120.2 . . ? C16' C15' C14' 119.2(4) . . ? C16' C15' H15B 120.4 . . ? C14' C15' H15B 120.4 . . ? C15' C16' C17' 119.4(4) . . ? C15' C16' H16B 120.3 . . ? C17' C16' H16B 120.3 . . ? N2' C17' C16' 121.7(4) . . ? N2' C17' H17B 119.2 . . ? C16' C17' H17B 119.2 . . ? N1' C18' C19' 107.7(3) . . ? N1' C18' H18C 110.2 . . ? C19' C18' H18C 110.2 . . ? N1' C18' H18D 110.2 . . ? C19' C18' H18D 110.2 . . ? H18C C18' H18D 108.5 . . ? N3' C19' C20' 120.9(4) . . ? N3' C19' C18' 114.6(3) . . ? C20' C19' C18' 124.6(4) . . ? C21' C20' C19' 119.3(4) . . ? C21' C20' H20B 120.3 . . ? C19' C20' H20B 120.3 . . ? C22' C21' C20' 120.0(4) . . ? C22' C21' H21B 120.0 . . ? C20' C21' H21B 120.0 . . ? C21' C22' C23' 118.7(4) . . ? C21' C22' H22B 120.6 . . ? C23' C22' H22B 120.6 . . ? N3' C23' C22' 121.5(4) . . ? N3' C23' H23B 119.2 . . ? C22' C23' H23B 119.2 . . ? N4' C24' C6' 114.6(3) . . ? N4' C24' H24C 108.6 . . ? C6' C24' H24C 108.6 . . ? N4' C24' H24D 108.6 . . ? C6' C24' H24D 108.6 . . ? H24C C24' H24D 107.6 . . ? C26' C25' N4' 110.8(3) . . ? C26' C25' H25C 109.5 . . ? N4' C25' H25C 109.5 . . ? C26' C25' H25D 109.5 . . ? N4' C25' H25D 109.5 . . ? H25C C25' H25D 108.1 . . ? N5' C26' C27' 121.2(5) . . ? N5' C26' C25' 115.4(4) . . ? C27' C26' C25' 123.4(4) . . ? C28' C27' C26' 119.5(5) . . ? C28' C27' H27B 120.3 . . ? C26' C27' H27B 120.3 . . ? C27' C28' C29' 119.4(5) . . ? C27' C28' H28B 120.3 . . ? C29' C28' H28B 120.3 . . ? C30' C29' C28' 117.6(5) . . ? C30' C29' H29B 121.2 . . ? C28' C29' H29B 121.2 . . ? N5' C30' C29' 123.0(5) . . ? N5' C30' H30B 118.5 . . ? C29' C30' H30B 118.5 . . ? N4' C31' C32' 107.2(3) . . ? N4' C31' H31C 110.3 . . ? C32' C31' H31C 110.3 . . ? N4' C31' H31D 110.3 . . ? C32' C31' H31D 110.3 . . ? H31C C31' H31D 108.5 . . ? N6' C32' C33' 121.1(4) . . ? N6' C32' C31' 113.7(3) . . ? C33' C32' C31' 125.3(4) . . ? C32' C33' C34' 119.5(4) . . ? C32' C33' H33B 120.2 . . ? C34' C33' H33B 120.2 . . ? C35' C34' C33' 118.2(4) . . ? C35' C34' H34B 120.9 . . ? C33' C34' H34B 120.9 . . ? C34' C35' C36' 120.4(4) . . ? C34' C35' H35B 119.8 . . ? C36' C35' H35B 119.8 . . ? N6' C36' C35' 120.9(4) . . ? N6' C36' H36B 119.6 . . ? C35' C36' H36B 119.6 . . ? O4' C37' O5' 126.9(3) . . ? O4' C37' C38' 117.8(3) . . ? O5' C37' C38' 115.2(3) . . ? C39' C38' C47' 120.2(3) . . ? C39' C38' C37' 117.8(3) . . ? C47' C38' C37' 121.9(3) . . ? C38' C39' C40' 121.4(4) . . ? C38' C39' H39B 119.3 . . ? C40' C39' H39B 119.3 . . ? C41' C40' C39' 119.3(4) . . ? C41' C40' H40B 120.3 . . ? C39' C40' H40B 120.3 . . ? C40' C41' C42' 121.6(4) . . ? C40' C41' H41B 119.2 . . ? C42' C41' H41B 119.2 . . ? C43' C42' C41' 121.5(4) . . ? C43' C42' C47' 119.1(4) . . ? C41' C42' C47' 119.4(3) . . ? C44' C43' C42' 121.1(4) . . ? C44' C43' H43B 119.5 . . ? C42' C43' H43B 119.5 . . ? C43' C44' C45' 120.2(4) . . ? C43' C44' H44B 119.9 . . ? C45' C44' H44B 119.9 . . ? C46' C45' C44' 120.6(4) . . ? C46' C45' H45B 119.7 . . ? C44' C45' H45B 119.7 . . ? C45' C46' C47' 120.8(4) . . ? C45' C46' H46B 119.6 . . ? C47' C46' H46B 119.6 . . ? C46' C47' C42' 118.2(3) . . ? C46' C47' C38' 123.8(3) . . ? C42' C47' C38' 117.9(3) . . ? O12 Cl1 O11 111.7(3) . . ? O12 Cl1 O13 115.2(3) . . ? O11 Cl1 O13 110.7(2) . . ? O12 Cl1 O14 106.4(3) . . ? O11 Cl1 O14 107.8(3) . . ? O13 Cl1 O14 104.4(3) . . ? O21 Cl2 O22 111.2(3) . . ? O21 Cl2 O23 111.0(2) . . ? O22 Cl2 O23 110.2(2) . . ? O21 Cl2 O24 108.0(3) . . ? O22 Cl2 O24 107.6(2) . . ? O23 Cl2 O24 108.6(2) . . ? O32 Cl3 O33 112.3(3) . . ? O32 Cl3 O31 110.7(3) . . ? O33 Cl3 O31 110.5(2) . . ? O32 Cl3 O34 109.2(3) . . ? O33 Cl3 O34 106.2(3) . . ? O31 Cl3 O34 107.7(2) . . ? O43 Cl4 O41 118.7(6) . . ? O43 Cl4 O42 115.9(7) . . ? O41 Cl4 O42 108.2(5) . . ? O43 Cl4 O44 109.4(5) . . ? O41 Cl4 O44 100.9(4) . . ? O42 Cl4 O44 101.3(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 O2 Co1 Co2 O3 -24.91(13) . . . . ? O1 Co1 Co2 O3 136.04(16) . . . . ? N2 Co1 Co2 O3 63.12(13) . . . . ? N3 Co1 Co2 O3 -58.4(2) . . . . ? O4 Co1 Co2 O3 -119.79(12) . . . . ? N1 Co1 Co2 O3 156.34(14) . . . . ? O2 Co1 Co2 O1 -160.95(17) . . . . ? N2 Co1 Co2 O1 -72.92(17) . . . . ? N3 Co1 Co2 O1 165.6(2) . . . . ? O4 Co1 Co2 O1 104.18(16) . . . . ? N1 Co1 Co2 O1 20.31(17) . . . . ? O2 Co1 Co2 N6 12.38(19) . . . . ? O1 Co1 Co2 N6 173.3(2) . . . . ? N2 Co1 Co2 N6 100.41(19) . . . . ? N3 Co1 Co2 N6 -21.1(3) . . . . ? O4 Co1 Co2 N6 -82.49(18) . . . . ? N1 Co1 Co2 N6 -166.36(19) . . . . ? O2 Co1 Co2 O5 80.26(12) . . . . ? O1 Co1 Co2 O5 -118.79(16) . . . . ? N2 Co1 Co2 O5 168.29(13) . . . . ? N3 Co1 Co2 O5 46.8(2) . . . . ? O4 Co1 Co2 O5 -14.61(11) . . . . ? N1 Co1 Co2 O5 -98.48(14) . . . . ? O2 Co1 Co2 N4 -99.99(14) . . . . ? O1 Co1 Co2 N4 60.96(17) . . . . ? N2 Co1 Co2 N4 -11.96(14) . . . . ? N3 Co1 Co2 N4 -133.5(2) . . . . ? O4 Co1 Co2 N4 165.13(13) . . . . ? N1 Co1 Co2 N4 81.27(15) . . . . ? O2 Co1 Co2 N5 163.64(14) . . . . ? O1 Co1 Co2 N5 -35.41(17) . . . . ? N2 Co1 Co2 N5 -108.33(14) . . . . ? N3 Co1 Co2 N5 130.2(2) . . . . ? O4 Co1 Co2 N5 68.77(13) . . . . ? N1 Co1 Co2 N5 -15.10(15) . . . . ? O2 Co1 O1 C1 -140.0(3) . . . . ? N2 Co1 O1 C1 -44.6(3) . . . . ? O4 Co1 O1 C1 132.3(3) . . . . ? N1 Co1 O1 C1 40.5(3) . . . . ? Co2 Co1 O1 C1 -156.2(3) . . . . ? O2 Co1 O1 Co2 16.17(14) . . . . ? N2 Co1 O1 Co2 111.63(15) . . . . ? O4 Co1 O1 Co2 -71.48(14) . . . . ? N1 Co1 O1 Co2 -163.32(14) . . . . ? O3 Co2 O1 C1 118.2(3) . . . . ? O5 Co2 O1 C1 -147.7(3) . . . . ? N4 Co2 O1 C1 27.8(3) . . . . ? N5 Co2 O1 C1 -56.1(3) . . . . ? Co1 Co2 O1 C1 155.0(3) . . . . ? O3 Co2 O1 Co1 -36.79(13) . . . . ? O5 Co2 O1 Co1 57.31(14) . . . . ? N4 Co2 O1 Co1 -127.26(15) . . . . ? N5 Co2 O1 Co1 148.84(15) . . . . ? O1 Co1 O2 O3 20.5(2) . . . . ? N2 Co1 O2 O3 -71.7(2) . . . . ? N3 Co1 O2 O3 -166.0(2) . . . . ? O4 Co1 O2 O3 108.0(2) . . . . ? Co2 Co1 O2 O3 30.98(16) . . . . ? Co1 O2 O3 Co2 -52.5(2) . . . . ? O1 Co2 O3 O2 52.91(18) . . . . ? N6 Co2 O3 O2 -128.2(2) . . . . ? O5 Co2 O3 O2 -37.97(19) . . . . ? N4 Co2 O3 O2 149.39(19) . . . . ? Co1 Co2 O3 O2 30.32(14) . . . . ? O2 Co1 O4 C37 -39.3(3) . . . . ? O1 Co1 O4 C37 51.7(3) . . . . ? N3 Co1 O4 C37 -133.4(3) . . . . ? N1 Co1 O4 C37 143.7(3) . . . . ? Co2 Co1 O4 C37 19.0(3) . . . . ? O3 Co2 O5 C37 73.3(3) . . . . ? O1 Co2 O5 C37 -11.9(3) . . . . ? N6 Co2 O5 C37 163.1(3) . . . . ? N5 Co2 O5 C37 -100.4(3) . . . . ? Co1 Co2 O5 C37 17.0(3) . . . . ? O1 Co1 N1 C18 139.4(2) . . . . ? N2 Co1 N1 C18 -128.7(2) . . . . ? N3 Co1 N1 C18 -34.2(2) . . . . ? O4 Co1 N1 C18 51.8(2) . . . . ? Co2 Co1 N1 C18 128.2(2) . . . . ? O1 Co1 N1 C12 -103.5(2) . . . . ? N2 Co1 N1 C12 -11.5(2) . . . . ? N3 Co1 N1 C12 83.0(2) . . . . ? O4 Co1 N1 C12 169.0(2) . . . . ? Co2 Co1 N1 C12 -114.6(2) . . . . ? O1 Co1 N1 C11 18.3(2) . . . . ? N2 Co1 N1 C11 110.2(2) . . . . ? N3 Co1 N1 C11 -155.3(3) . . . . ? O4 Co1 N1 C11 -69.3(2) . . . . ? Co2 Co1 N1 C11 7.1(3) . . . . ? O2 Co1 N2 C17 9.6(3) . . . . ? O1 Co1 N2 C17 -81.4(3) . . . . ? N3 Co1 N2 C17 104.0(3) . . . . ? N1 Co1 N2 C17 -173.4(3) . . . . ? Co2 Co1 N2 C17 -49.3(3) . . . . ? O2 Co1 N2 C13 -179.3(3) . . . . ? O1 Co1 N2 C13 89.7(3) . . . . ? N3 Co1 N2 C13 -84.9(3) . . . . ? N1 Co1 N2 C13 -2.2(3) . . . . ? Co2 Co1 N2 C13 121.8(3) . . . . ? O2 Co1 N3 C19 -159.9(3) . . . . ? N2 Co1 N3 C19 104.3(3) . . . . ? O4 Co1 N3 C19 -72.5(3) . . . . ? N1 Co1 N3 C19 19.9(3) . . . . ? Co2 Co1 N3 C19 -131.8(2) . . . . ? O2 Co1 N3 C23 18.1(3) . . . . ? N2 Co1 N3 C23 -77.6(3) . . . . ? O4 Co1 N3 C23 105.5(3) . . . . ? N1 Co1 N3 C23 -162.1(3) . . . . ? Co2 Co1 N3 C23 46.3(4) . . . . ? O3 Co2 N4 C31 51.0(2) . . . . ? O1 Co2 N4 C31 136.2(2) . . . . ? N6 Co2 N4 C31 -38.6(2) . . . . ? N5 Co2 N4 C31 -136.0(3) . . . . ? Co1 Co2 N4 C31 107.1(2) . . . . ? O3 Co2 N4 C25 168.6(3) . . . . ? O1 Co2 N4 C25 -106.3(3) . . . . ? N6 Co2 N4 C25 79.0(3) . . . . ? N5 Co2 N4 C25 -18.4(3) . . . . ? Co1 Co2 N4 C25 -135.3(2) . . . . ? O3 Co2 N4 C24 -68.9(3) . . . . ? O1 Co2 N4 C24 16.3(3) . . . . ? N6 Co2 N4 C24 -158.5(3) . . . . ? N5 Co2 N4 C24 104.1(3) . . . . ? Co1 Co2 N4 C24 -12.8(3) . . . . ? O1 Co2 N5 C30 -66.6(4) . . . . ? N6 Co2 N5 C30 115.1(4) . . . . ? O5 Co2 N5 C30 24.6(4) . . . . ? N4 Co2 N5 C30 -163.3(4) . . . . ? Co1 Co2 N5 C30 -47.9(4) . . . . ? O1 Co2 N5 C26 100.9(3) . . . . ? N6 Co2 N5 C26 -77.4(3) . . . . ? O5 Co2 N5 C26 -167.9(3) . . . . ? N4 Co2 N5 C26 4.2(3) . . . . ? Co1 Co2 N5 C26 119.5(3) . . . . ? O3 Co2 N6 C36 111.6(3) . . . . ? O5 Co2 N6 C36 17.5(3) . . . . ? N4 Co2 N6 C36 -157.3(3) . . . . ? N5 Co2 N6 C36 -74.2(3) . . . . ? Co1 Co2 N6 C36 80.3(4) . . . . ? O3 Co2 N6 C32 -66.0(3) . . . . ? O5 Co2 N6 C32 -160.2(3) . . . . ? N4 Co2 N6 C32 25.0(3) . . . . ? N5 Co2 N6 C32 108.2(3) . . . . ? Co1 Co2 N6 C32 -97.4(3) . . . . ? Co1 O1 C1 C2 -58.5(4) . . . . ? Co2 O1 C1 C2 148.0(3) . . . . ? Co1 O1 C1 C6 119.0(3) . . . . ? Co2 O1 C1 C6 -34.6(5) . . . . ? O1 C1 C2 C3 -179.6(3) . . . . ? C6 C1 C2 C3 3.0(6) . . . . ? O1 C1 C2 C11 5.2(5) . . . . ? C6 C1 C2 C11 -172.2(3) . . . . ? C1 C2 C3 C4 1.6(6) . . . . ? C11 C2 C3 C4 176.5(4) . . . . ? C2 C3 C4 C5 -3.9(6) . . . . ? C2 C3 C4 C7 179.3(4) . . . . ? C3 C4 C5 C6 1.8(6) . . . . ? C7 C4 C5 C6 178.5(4) . . . . ? C4 C5 C6 C1 2.6(6) . . . . ? C4 C5 C6 C24 -170.5(4) . . . . ? O1 C1 C6 C5 177.6(3) . . . . ? C2 C1 C6 C5 -5.0(6) . . . . ? O1 C1 C6 C24 -9.2(5) . . . . ? C2 C1 C6 C24 168.2(4) . . . . ? C5 C4 C7 C10 -106.9(5) . . . . ? C3 C4 C7 C10 69.7(5) . . . . ? C5 C4 C7 C8 14.1(5) . . . . ? C3 C4 C7 C8 -169.3(4) . . . . ? C5 C4 C7 C9 133.1(4) . . . . ? C3 C4 C7 C9 -50.3(5) . . . . ? C1 C2 C11 N1 59.0(4) . . . . ? C3 C2 C11 N1 -116.0(4) . . . . ? C18 N1 C11 C2 -179.8(3) . . . . ? C12 N1 C11 C2 56.8(4) . . . . ? Co1 N1 C11 C2 -63.9(3) . . . . ? C18 N1 C12 C13 135.0(3) . . . . ? C11 N1 C12 C13 -100.3(4) . . . . ? Co1 N1 C12 C13 21.9(4) . . . . ? C17 N2 C13 C14 5.8(6) . . . . ? Co1 N2 C13 C14 -165.9(3) . . . . ? C17 N2 C13 C12 -172.0(3) . . . . ? Co1 N2 C13 C12 16.3(4) . . . . ? N1 C12 C13 N2 -25.4(4) . . . . ? N1 C12 C13 C14 156.8(4) . . . . ? N2 C13 C14 C15 -4.2(6) . . . . ? C12 C13 C14 C15 173.4(4) . . . . ? C13 C14 C15 C16 0.0(7) . . . . ? C14 C15 C16 C17 2.5(7) . . . . ? C13 N2 C17 C16 -3.2(6) . . . . ? Co1 N2 C17 C16 167.7(3) . . . . ? C15 C16 C17 N2 -1.0(7) . . . . ? C12 N1 C18 C19 -74.5(4) . . . . ? C11 N1 C18 C19 162.0(3) . . . . ? Co1 N1 C18 C19 41.7(3) . . . . ? C23 N3 C19 C20 2.0(6) . . . . ? Co1 N3 C19 C20 -179.8(3) . . . . ? C23 N3 C19 C18 -177.6(3) . . . . ? Co1 N3 C19 C18 0.5(4) . . . . ? N1 C18 C19 N3 -29.6(4) . . . . ? N1 C18 C19 C20 150.8(4) . . . . ? N3 C19 C20 C21 -2.3(6) . . . . ? C18 C19 C20 C21 177.3(4) . . . . ? C19 C20 C21 C22 0.4(7) . . . . ? C20 C21 C22 C23 1.8(7) . . . . ? C19 N3 C23 C22 0.2(6) . . . . ? Co1 N3 C23 C22 -177.7(3) . . . . ? C21 C22 C23 N3 -2.1(6) . . . . ? C31 N4 C24 C6 -172.4(3) . . . . ? C25 N4 C24 C6 66.7(4) . . . . ? Co2 N4 C24 C6 -55.6(4) . . . . ? C5 C6 C24 N4 -128.8(4) . . . . ? C1 C6 C24 N4 58.2(5) . . . . ? C31 N4 C25 C26 143.4(4) . . . . ? C24 N4 C25 C26 -95.5(4) . . . . ? Co2 N4 C25 C26 29.0(4) . . . . ? C30 N5 C26 C27 -1.6(7) . . . . ? Co2 N5 C26 C27 -170.0(4) . . . . ? C30 N5 C26 C25 -179.7(4) . . . . ? Co2 N5 C26 C25 11.9(5) . . . . ? N4 C25 C26 N5 -27.1(5) . . . . ? N4 C25 C26 C27 154.9(5) . . . . ? N5 C26 C27 C28 0.7(9) . . . . ? C25 C26 C27 C28 178.6(6) . . . . ? C26 C27 C28 C29 0.1(11) . . . . ? C27 C28 C29 C30 0.0(11) . . . . ? C26 N5 C30 C29 1.7(7) . . . . ? Co2 N5 C30 C29 168.7(4) . . . . ? C28 C29 C30 N5 -0.9(9) . . . . ? C25 N4 C31 C32 -72.9(4) . . . . ? C24 N4 C31 C32 166.2(3) . . . . ? Co2 N4 C31 C32 44.3(3) . . . . ? C36 N6 C32 C33 -1.4(6) . . . . ? Co2 N6 C32 C33 176.4(3) . . . . ? C36 N6 C32 C31 177.7(4) . . . . ? Co2 N6 C32 C31 -4.4(4) . . . . ? N4 C31 C32 N6 -27.1(5) . . . . ? N4 C31 C32 C33 152.1(4) . . . . ? N6 C32 C33 C34 0.9(7) . . . . ? C31 C32 C33 C34 -178.1(4) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C33 C34 C35 C36 -0.1(7) . . . . ? C32 N6 C36 C35 1.2(6) . . . . ? Co2 N6 C36 C35 -176.4(3) . . . . ? C34 C35 C36 N6 -0.4(6) . . . . ? Co2 O5 C37 O4 -9.5(6) . . . . ? Co2 O5 C37 C38 166.6(2) . . . . ? Co1 O4 C37 O5 -15.7(5) . . . . ? Co1 O4 C37 C38 168.3(2) . . . . ? O5 C37 C38 C39 -36.7(5) . . . . ? O4 C37 C38 C39 139.8(4) . . . . ? O5 C37 C38 C47 145.5(4) . . . . ? O4 C37 C38 C47 -38.0(5) . . . . ? C47 C38 C39 C40 3.2(6) . . . . ? C37 C38 C39 C40 -174.6(4) . . . . ? C38 C39 C40 C41 -1.3(7) . . . . ? C39 C40 C41 C42 -1.4(7) . . . . ? C40 C41 C42 C43 -177.1(4) . . . . ? C40 C41 C42 C47 2.2(6) . . . . ? C41 C42 C43 C44 178.0(4) . . . . ? C47 C42 C43 C44 -1.2(6) . . . . ? C42 C43 C44 C45 -0.3(7) . . . . ? C43 C44 C45 C46 0.9(7) . . . . ? C44 C45 C46 C47 0.0(6) . . . . ? C45 C46 C47 C38 -178.2(4) . . . . ? C45 C46 C47 C42 -1.4(6) . . . . ? C39 C38 C47 C46 174.4(4) . . . . ? C37 C38 C47 C46 -7.9(6) . . . . ? C39 C38 C47 C42 -2.4(6) . . . . ? C37 C38 C47 C42 175.3(3) . . . . ? C43 C42 C47 C46 2.0(6) . . . . ? C41 C42 C47 C46 -177.2(4) . . . . ? C43 C42 C47 C38 179.0(4) . . . . ? C41 C42 C47 C38 -0.2(6) . . . . ? O2' Co1' Co2' O3' 25.29(13) . . . . ? O1' Co1' Co2' O3' -135.51(17) . . . . ? N3' Co1' Co2' O3' 60.1(2) . . . . ? N2' Co1' Co2' O3' -61.95(13) . . . . ? O4' Co1' Co2' O3' 120.18(12) . . . . ? N1' Co1' Co2' O3' -156.11(14) . . . . ? O2' Co1' Co2' O1' 160.80(17) . . . . ? N3' Co1' Co2' O1' -164.4(2) . . . . ? N2' Co1' Co2' O1' 73.55(17) . . . . ? O4' Co1' Co2' O1' -104.31(16) . . . . ? N1' Co1' Co2' O1' -20.60(17) . . . . ? O2' Co1' Co2' O5' -80.02(12) . . . . ? O1' Co1' Co2' O5' 119.18(16) . . . . ? N3' Co1' Co2' O5' -45.2(2) . . . . ? N2' Co1' Co2' O5' -167.26(13) . . . . ? O4' Co1' Co2' O5' 14.87(11) . . . . ? N1' Co1' Co2' O5' 98.59(13) . . . . ? O2' Co1' Co2' N6' -13.44(19) . . . . ? O1' Co1' Co2' N6' -174.2(2) . . . . ? N3' Co1' Co2' N6' 21.4(3) . . . . ? N2' Co1' Co2' N6' -100.68(19) . . . . ? O4' Co1' Co2' N6' 81.45(18) . . . . ? N1' Co1' Co2' N6' 165.16(19) . . . . ? O2' Co1' Co2' N4' 99.72(14) . . . . ? O1' Co1' Co2' N4' -61.07(17) . . . . ? N3' Co1' Co2' N4' 134.5(2) . . . . ? N2' Co1' Co2' N4' 12.48(15) . . . . ? O4' Co1' Co2' N4' -165.39(13) . . . . ? N1' Co1' Co2' N4' -81.67(15) . . . . ? O2' Co1' Co2' N5' -162.86(14) . . . . ? O1' Co1' Co2' N5' 36.34(17) . . . . ? N3' Co1' Co2' N5' -128.1(2) . . . . ? N2' Co1' Co2' N5' 109.89(15) . . . . ? O4' Co1' Co2' N5' -67.97(13) . . . . ? N1' Co1' Co2' N5' 15.74(15) . . . . ? O3' Co2' O1' C1' -115.1(3) . . . . ? O5' Co2' O1' C1' 150.8(3) . . . . ? N4' Co2' O1' C1' -24.6(3) . . . . ? N5' Co2' O1' C1' 59.7(3) . . . . ? Co1' Co2' O1' C1' -152.2(4) . . . . ? O3' Co2' O1' Co1' 37.04(14) . . . . ? O5' Co2' O1' Co1' -57.08(14) . . . . ? N4' Co2' O1' Co1' 127.52(15) . . . . ? N5' Co2' O1' Co1' -148.14(15) . . . . ? O2' Co1' O1' C1' 137.5(3) . . . . ? N2' Co1' O1' C1' 42.2(3) . . . . ? O4' Co1' O1' C1' -134.9(3) . . . . ? N1' Co1' O1' C1' -43.1(3) . . . . ? Co2' Co1' O1' C1' 153.8(3) . . . . ? O2' Co1' O1' Co2' -16.31(14) . . . . ? N2' Co1' O1' Co2' -111.59(15) . . . . ? O4' Co1' O1' Co2' 71.30(14) . . . . ? N1' Co1' O1' Co2' 163.15(14) . . . . ? O1' Co1' O2' O3' -20.8(2) . . . . ? N3' Co1' O2' O3' 166.4(2) . . . . ? N2' Co1' O2' O3' 72.5(2) . . . . ? O4' Co1' O2' O3' -108.2(2) . . . . ? Co2' Co1' O2' O3' -31.33(15) . . . . ? Co1' O2' O3' Co2' 53.3(2) . . . . ? O1' Co2' O3' O2' -53.93(19) . . . . ? O5' Co2' O3' O2' 37.52(19) . . . . ? N6' Co2' O3' O2' 126.6(2) . . . . ? N4' Co2' O3' O2' -150.8(2) . . . . ? Co1' Co2' O3' O2' -30.85(15) . . . . ? O2' Co1' O4' C37' 36.7(3) . . . . ? O1' Co1' O4' C37' -54.3(3) . . . . ? N3' Co1' O4' C37' 130.9(3) . . . . ? N1' Co1' O4' C37' -146.7(3) . . . . ? Co2' Co1' O4' C37' -21.6(3) . . . . ? O3' Co2' O5' C37' -70.5(3) . . . . ? O1' Co2' O5' C37' 14.5(3) . . . . ? N6' Co2' O5' C37' -160.4(3) . . . . ? N5' Co2' O5' C37' 103.3(3) . . . . ? Co1' Co2' O5' C37' -14.6(3) . . . . ? O1' Co1' N1' C18' -137.4(2) . . . . ? N3' Co1' N1' C18' 35.4(2) . . . . ? N2' Co1' N1' C18' 129.6(2) . . . . ? O4' Co1' N1' C18' -49.9(2) . . . . ? Co2' Co1' N1' C18' -126.1(2) . . . . ? O1' Co1' N1' C12' 105.6(2) . . . . ? N3' Co1' N1' C12' -81.5(2) . . . . ? N2' Co1' N1' C12' 12.6(2) . . . . ? O4' Co1' N1' C12' -166.8(2) . . . . ? Co2' Co1' N1' C12' 116.9(2) . . . . ? O1' Co1' N1' C11' -15.3(2) . . . . ? N3' Co1' N1' C11' 157.6(2) . . . . ? N2' Co1' N1' C11' -108.3(2) . . . . ? O4' Co1' N1' C11' 72.2(2) . . . . ? Co2' Co1' N1' C11' -4.0(3) . . . . ? O2' Co1' N2' C13' 177.9(3) . . . . ? O1' Co1' N2' C13' -90.8(3) . . . . ? N3' Co1' N2' C13' 83.7(3) . . . . ? N1' Co1' N2' C13' 1.4(3) . . . . ? Co2' Co1' N2' C13' -123.2(3) . . . . ? O2' Co1' N2' C17' -11.4(3) . . . . ? O1' Co1' N2' C17' 79.8(3) . . . . ? N3' Co1' N2' C17' -105.7(3) . . . . ? N1' Co1' N2' C17' 172.0(3) . . . . ? Co2' Co1' N2' C17' 47.5(3) . . . . ? O2' Co1' N3' C19' 157.9(3) . . . . ? N2' Co1' N3' C19' -106.6(3) . . . . ? O4' Co1' N3' C19' 70.6(3) . . . . ? N1' Co1' N3' C19' -22.0(2) . . . . ? Co2' Co1' N3' C19' 128.7(2) . . . . ? O2' Co1' N3' C23' -17.6(3) . . . . ? N2' Co1' N3' C23' 77.9(3) . . . . ? O4' Co1' N3' C23' -104.9(3) . . . . ? N1' Co1' N3' C23' 162.5(3) . . . . ? Co2' Co1' N3' C23' -46.8(4) . . . . ? O3' Co2' N4' C24' 66.9(3) . . . . ? O1' Co2' N4' C24' -18.1(3) . . . . ? N6' Co2' N4' C24' 156.8(3) . . . . ? N5' Co2' N4' C24' -106.1(3) . . . . ? Co1' Co2' N4' C24' 11.3(3) . . . . ? O3' Co2' N4' C31' -52.6(2) . . . . ? O1' Co2' N4' C31' -137.6(2) . . . . ? N6' Co2' N4' C31' 37.3(2) . . . . ? N5' Co2' N4' C31' 134.4(3) . . . . ? Co1' Co2' N4' C31' -108.1(2) . . . . ? O3' Co2' N4' C25' -169.3(3) . . . . ? O1' Co2' N4' C25' 105.7(3) . . . . ? N6' Co2' N4' C25' -79.4(3) . . . . ? N5' Co2' N4' C25' 17.7(3) . . . . ? Co1' Co2' N4' C25' 135.2(2) . . . . ? O1' Co2' N5' C30' 67.8(4) . . . . ? O5' Co2' N5' C30' -24.0(4) . . . . ? N6' Co2' N5' C30' -113.3(4) . . . . ? N4' Co2' N5' C30' 164.8(4) . . . . ? Co1' Co2' N5' C30' 48.5(4) . . . . ? O1' Co2' N5' C26' -102.9(3) . . . . ? O5' Co2' N5' C26' 165.3(3) . . . . ? N6' Co2' N5' C26' 76.0(3) . . . . ? N4' Co2' N5' C26' -5.9(3) . . . . ? Co1' Co2' N5' C26' -122.2(3) . . . . ? O3' Co2' N6' C36' -109.5(3) . . . . ? O5' Co2' N6' C36' -15.2(3) . . . . ? N4' Co2' N6' C36' 159.4(3) . . . . ? N5' Co2' N6' C36' 75.8(3) . . . . ? Co1' Co2' N6' C36' -77.1(4) . . . . ? O3' Co2' N6' C32' 67.2(3) . . . . ? O5' Co2' N6' C32' 161.5(3) . . . . ? N4' Co2' N6' C32' -23.9(3) . . . . ? N5' Co2' N6' C32' -107.5(3) . . . . ? Co1' Co2' N6' C32' 99.6(3) . . . . ? Co2' O1' C1' C6' 32.6(5) . . . . ? Co1' O1' C1' C6' -118.1(3) . . . . ? Co2' O1' C1' C2' -150.6(3) . . . . ? Co1' O1' C1' C2' 58.8(4) . . . . ? O1' C1' C2' C3' -178.2(3) . . . . ? C6' C1' C2' C3' -1.4(6) . . . . ? O1' C1' C2' C11' -4.3(5) . . . . ? C6' C1' C2' C11' 172.5(4) . . . . ? C1' C2' C3' C4' -1.5(6) . . . . ? C11' C2' C3' C4' -175.1(4) . . . . ? C2' C3' C4' C5' 2.1(6) . . . . ? C2' C3' C4' C7' 179.4(4) . . . . ? C3' C4' C5' C6' 0.3(6) . . . . ? C7' C4' C5' C6' -176.9(4) . . . . ? O1' C1' C6' C5' -179.6(4) . . . . ? C2' C1' C6' C5' 3.7(6) . . . . ? O1' C1' C6' C24' 8.1(6) . . . . ? C2' C1' C6' C24' -168.6(4) . . . . ? C4' C5' C6' C1' -3.1(6) . . . . ? C4' C5' C6' C24' 169.0(4) . . . . ? C5' C4' C7' C9' -12.2(6) . . . . ? C3' C4' C7' C9' 170.6(4) . . . . ? C5' C4' C7' C10' 107.6(5) . . . . ? C3' C4' C7' C10' -69.6(5) . . . . ? C5' C4' C7' C8' -131.6(4) . . . . ? C3' C4' C7' C8' 51.2(5) . . . . ? C3' C2' C11' N1' 113.6(4) . . . . ? C1' C2' C11' N1' -60.0(5) . . . . ? C18' N1' C11' C2' 178.7(3) . . . . ? C12' N1' C11' C2' -57.6(4) . . . . ? Co1' N1' C11' C2' 62.2(3) . . . . ? C18' N1' C12' C13' -135.9(3) . . . . ? C11' N1' C12' C13' 98.6(4) . . . . ? Co1' N1' C12' C13' -23.1(3) . . . . ? C17' N2' C13' C14' -3.8(6) . . . . ? Co1' N2' C13' C14' 167.5(3) . . . . ? C17' N2' C13' C12' 173.0(3) . . . . ? Co1' N2' C13' C12' -15.8(4) . . . . ? N1' C12' C13' N2' 26.1(5) . . . . ? N1' C12' C13' C14' -157.3(4) . . . . ? N2' C13' C14' C15' 1.9(6) . . . . ? C12' C13' C14' C15' -174.5(4) . . . . ? C13' C14' C15' C16' 0.8(7) . . . . ? C14' C15' C16' C17' -1.6(7) . . . . ? C13' N2' C17' C16' 2.9(6) . . . . ? Co1' N2' C17' C16' -167.4(3) . . . . ? C15' C16' C17' N2' -0.3(7) . . . . ? C12' N1' C18' C19' 73.7(4) . . . . ? C11' N1' C18' C19' -162.7(3) . . . . ? Co1' N1' C18' C19' -41.9(3) . . . . ? C23' N3' C19' C20' -2.0(5) . . . . ? Co1' N3' C19' C20' -177.9(3) . . . . ? C23' N3' C19' C18' 178.0(3) . . . . ? Co1' N3' C19' C18' 2.1(4) . . . . ? N1' C18' C19' N3' 28.1(4) . . . . ? N1' C18' C19' C20' -151.9(4) . . . . ? N3' C19' C20' C21' 2.7(6) . . . . ? C18' C19' C20' C21' -177.3(4) . . . . ? C19' C20' C21' C22' -0.7(6) . . . . ? C20' C21' C22' C23' -1.8(6) . . . . ? C19' N3' C23' C22' -0.6(5) . . . . ? Co1' N3' C23' C22' 174.7(3) . . . . ? C21' C22' C23' N3' 2.5(6) . . . . ? C31' N4' C24' C6' 171.6(3) . . . . ? C25' N4' C24' C6' -67.8(4) . . . . ? Co2' N4' C24' C6' 55.5(4) . . . . ? C1' C6' C24' N4' -56.3(5) . . . . ? C5' C6' C24' N4' 131.7(4) . . . . ? C24' N4' C25' C26' 99.1(4) . . . . ? C31' N4' C25' C26' -139.8(4) . . . . ? Co2' N4' C25' C26' -26.1(4) . . . . ? C30' N5' C26' C27' 0.6(8) . . . . ? Co2' N5' C26' C27' 172.0(5) . . . . ? C30' N5' C26' C25' -179.6(4) . . . . ? Co2' N5' C26' C25' -8.1(5) . . . . ? N4' C25' C26' N5' 22.7(5) . . . . ? N4' C25' C26' C27' -157.5(5) . . . . ? N5' C26' C27' C28' -3.0(11) . . . . ? C25' C26' C27' C28' 177.1(7) . . . . ? C26' C27' C28' C29' 5.7(13) . . . . ? C27' C28' C29' C30' -5.8(13) . . . . ? C26' N5' C30' C29' -0.9(8) . . . . ? Co2' N5' C30' C29' -171.2(5) . . . . ? C28' C29' C30' N5' 3.5(11) . . . . ? C24' N4' C31' C32' -165.2(3) . . . . ? C25' N4' C31' C32' 73.3(4) . . . . ? Co2' N4' C31' C32' -43.8(3) . . . . ? C36' N6' C32' C33' 0.9(6) . . . . ? Co2' N6' C32' C33' -176.0(3) . . . . ? C36' N6' C32' C31' -179.9(4) . . . . ? Co2' N6' C32' C31' 3.2(4) . . . . ? N4' C31' C32' N6' 27.6(5) . . . . ? N4' C31' C32' C33' -153.2(4) . . . . ? N6' C32' C33' C34' 1.0(6) . . . . ? C31' C32' C33' C34' -178.2(4) . . . . ? C32' C33' C34' C35' -1.1(6) . . . . ? C33' C34' C35' C36' -0.5(6) . . . . ? C32' N6' C36' C35' -2.6(6) . . . . ? Co2' N6' C36' C35' 173.9(3) . . . . ? C34' C35' C36' N6' 2.4(6) . . . . ? Co1' O4' C37' O5' 21.4(5) . . . . ? Co1' O4' C37' C38' -161.1(2) . . . . ? Co2' O5' C37' O4' 3.7(6) . . . . ? Co2' O5' C37' C38' -173.9(2) . . . . ? O4' C37' C38' C39' -138.3(4) . . . . ? O5' C37' C38' C39' 39.5(5) . . . . ? O4' C37' C38' C47' 43.4(5) . . . . ? O5' C37' C38' C47' -138.7(4) . . . . ? C47' C38' C39' C40' -2.9(6) . . . . ? C37' C38' C39' C40' 178.8(3) . . . . ? C38' C39' C40' C41' 0.6(6) . . . . ? C39' C40' C41' C42' 2.0(6) . . . . ? C40' C41' C42' C43' 177.0(4) . . . . ? C40' C41' C42' C47' -2.3(6) . . . . ? C41' C42' C43' C44' -177.7(4) . . . . ? C47' C42' C43' C44' 1.6(6) . . . . ? C42' C43' C44' C45' -0.3(6) . . . . ? C43' C44' C45' C46' -0.4(6) . . . . ? C44' C45' C46' C47' -0.3(6) . . . . ? C45' C46' C47' C42' 1.6(5) . . . . ? C45' C46' C47' C38' 178.5(4) . . . . ? C43' C42' C47' C46' -2.2(5) . . . . ? C41' C42' C47' C46' 177.1(3) . . . . ? C43' C42' C47' C38' -179.3(3) . . . . ? C41' C42' C47' C38' 0.1(5) . . . . ? C39' C38' C47' C46' -174.5(4) . . . . ? C37' C38' C47' C46' 3.8(6) . . . . ? C39' C38' C47' C42' 2.4(5) . . . . ? C37' C38' C47' C42' -179.3(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 913568'