Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Walton, Paul H.' 'Archibald, Stephen J.' 'Foxon, Simon P.' 'Freeman, Jonathan D.' 'Hobson, James E.' 'Perutz, Robin' _publ_contact_author_name 'Prof Paul H Walton' _publ_contact_author_address ; Chemistry University of York Heslington YORK N. Yorks YO10 5DD UNITED KINGDOM ; _publ_contact_author_email 'PHW2@YORK.AC.UK' _publ_contact_author_fax '+44 (1904) 43 25 16' _publ_contact_author_phone '+44 (1904) 43 25 80' _publ_section_title ; Preparation of cationic cobalt phenoxide and ethoxide complexes and their reversible reaction with carbon dioxide ; data_sja60_01 _database_code_CSD 185609 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H61 B Co N3 O1.50' _chemical_formula_weight 917.86 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.053(2) _cell_length_b 15.812(3) _cell_length_c 16.503(3) _cell_angle_alpha 65.866(12) _cell_angle_beta 86.349(14) _cell_angle_gamma 72.640(14) _cell_volume 2506.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lathe _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.946 _exptl_absorpt_correction_T_max 0.973 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDSII image plate' _diffrn_measurement_method '180 frames at 2^o intervals, exposure time 4 minutes' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47525 _diffrn_reflns_av_R_equivalents 0.1698 _diffrn_reflns_av_sigmaI/netI 0.2413 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.00 _reflns_number_total 14596 _reflns_number_gt 5081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA' _computing_cell_refinement 'X-AREA' _computing_data_reduction 'X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL 97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0146(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14596 _refine_ls_number_parameters 600 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2087 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2510 _refine_ls_wR_factor_gt 0.2216 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1967(5) -0.0084(4) 0.2654(4) 0.0344(12) Uani 1 1 d . . . H1 H -0.1837 0.0553 0.2322 0.041 Uiso 1 1 calc R . . C2 C -0.1481(5) -0.0461(4) 0.3618(4) 0.0380(13) Uani 1 1 d . . . H2A H -0.1838 0.0045 0.3831 0.046 Uiso 1 1 calc R . . H2B H -0.0566 -0.0596 0.3642 0.046 Uiso 1 1 calc R . . C3 C -0.1809(5) -0.1379(4) 0.4243(4) 0.0355(12) Uani 1 1 d . . . H3 H -0.1584 -0.1509 0.4856 0.043 Uiso 1 1 calc R . . C4 C -0.3241(5) -0.1243(4) 0.4154(4) 0.0383(13) Uani 1 1 d . . . H4A H -0.3393 -0.1863 0.4491 0.046 Uiso 1 1 calc R . . H4B H -0.3696 -0.0801 0.4418 0.046 Uiso 1 1 calc R . . C5 C -0.3776(5) -0.0853(4) 0.3209(4) 0.0357(12) Uani 1 1 d . . . H5 H -0.4705 -0.0648 0.3210 0.043 Uiso 1 1 calc R . . C6 C -0.3375(5) 0.0028(4) 0.2577(4) 0.0360(12) Uani 1 1 d . . . H6A H -0.3605 0.0159 0.1970 0.043 Uiso 1 1 calc R . . H6B H -0.3853 0.0588 0.2689 0.043 Uiso 1 1 calc R . . C7 C -0.0371(5) -0.0496(4) 0.1712(4) 0.0361(12) Uani 1 1 d . . . H7 H -0.0261 0.0105 0.1583 0.043 Uiso 1 1 calc R . . C8 C 0.0400(5) -0.1100(4) 0.1295(4) 0.0383(13) Uani 1 1 d . . . H8 H 0.0240 -0.1677 0.1388 0.046 Uiso 1 1 calc R . . C9 C 0.1342(5) -0.0857(4) 0.0777(4) 0.0393(13) Uani 1 1 d . . . H9 H 0.1536 -0.0305 0.0725 0.047 Uiso 1 1 calc R . . C10 C 0.2077(5) -0.1417(4) 0.0293(4) 0.0375(12) Uani 1 1 d . . . C11 C 0.1628(6) -0.2045(5) 0.0105(4) 0.0504(16) Uani 1 1 d . . . H11 H 0.0842 -0.2127 0.0290 0.061 Uiso 1 1 calc R . . C12 C 0.2352(7) -0.2559(5) -0.0361(5) 0.0545(17) Uani 1 1 d . . . H12 H 0.2025 -0.2957 -0.0512 0.065 Uiso 1 1 calc R . . C13 C 0.3512(6) -0.2489(5) -0.0597(4) 0.0480(15) Uani 1 1 d . . . H13 H 0.3986 -0.2849 -0.0897 0.058 Uiso 1 1 calc R . . C14 C 0.4006(5) -0.1893(4) -0.0400(4) 0.0441(14) Uani 1 1 d . . . H14 H 0.4818 -0.1856 -0.0557 0.053 Uiso 1 1 calc R . . C15 C 0.3284(5) -0.1345(4) 0.0037(4) 0.0386(13) Uani 1 1 d . . . H15 H 0.3607 -0.0927 0.0160 0.046 Uiso 1 1 calc R . . C16 C -0.0217(5) -0.2900(4) 0.4661(4) 0.0396(13) Uani 1 1 d . . . H16 H -0.0151 -0.2857 0.5201 0.048 Uiso 1 1 calc R . . C17 C 0.0642(5) -0.3717(4) 0.4535(4) 0.0387(13) Uani 1 1 d . . . H17 H 0.0518 -0.3810 0.4030 0.046 Uiso 1 1 calc R . . C18 C 0.1605(5) -0.4342(4) 0.5120(4) 0.0416(13) Uani 1 1 d . . . H18 H 0.1659 -0.4258 0.5641 0.050 Uiso 1 1 calc R . . C19 C 0.2597(5) -0.5152(4) 0.5028(4) 0.0413(13) Uani 1 1 d . . . C20 C 0.2474(6) -0.5509(5) 0.4413(5) 0.0555(17) Uani 1 1 d . . . H20 H 0.1712 -0.5270 0.4074 0.067 Uiso 1 1 calc R . . C21 C 0.3467(7) -0.6220(5) 0.4291(6) 0.065(2) Uani 1 1 d . . . H21 H 0.3371 -0.6445 0.3867 0.078 Uiso 1 1 calc R . . C22 C 0.4604(6) -0.6593(5) 0.4804(5) 0.0562(18) Uani 1 1 d . . . H22 H 0.5281 -0.7058 0.4718 0.067 Uiso 1 1 calc R . . C23 C 0.4713(6) -0.6259(5) 0.5445(5) 0.0589(18) Uani 1 1 d . . . H23 H 0.5462 -0.6519 0.5804 0.071 Uiso 1 1 calc R . . C24 C 0.3729(6) -0.5547(5) 0.5558(5) 0.0503(16) Uani 1 1 d . . . H24 H 0.3819 -0.5330 0.5990 0.060 Uiso 1 1 calc R . . C25 C -0.4268(5) -0.1891(4) 0.2649(4) 0.0386(13) Uani 1 1 d . . . H25 H -0.5104 -0.1614 0.2742 0.046 Uiso 1 1 calc R . . C26 C -0.4034(5) -0.2605(4) 0.2278(4) 0.0422(13) Uani 1 1 d . . . H26 H -0.3209 -0.2881 0.2164 0.051 Uiso 1 1 calc R . . C27 C -0.4967(6) -0.2871(4) 0.2100(4) 0.0474(15) Uani 1 1 d . . . H27 H -0.5783 -0.2580 0.2218 0.057 Uiso 1 1 calc R . . C28 C -0.4818(7) -0.3604(5) 0.1723(5) 0.0539(17) Uani 1 1 d . . . C29 C -0.3751(8) -0.3876(5) 0.1299(5) 0.066(2) Uani 1 1 d . . . H29 H -0.3095 -0.3601 0.1234 0.079 Uiso 1 1 calc R . . C30 C -0.3679(11) -0.4575(7) 0.0968(7) 0.097(3) Uani 1 1 d . . . H30 H -0.2967 -0.4769 0.0680 0.117 Uiso 1 1 calc R . . C31 C -0.4634(12) -0.4969(6) 0.1063(7) 0.091(3) Uani 1 1 d . . . H31 H -0.4559 -0.5442 0.0850 0.109 Uiso 1 1 calc R . . C32 C -0.5688(11) -0.4698(7) 0.1457(7) 0.089(3) Uani 1 1 d . . . H32 H -0.6337 -0.4975 0.1504 0.107 Uiso 1 1 calc R . . C33 C -0.5815(9) -0.4001(6) 0.1797(6) 0.074(2) Uani 1 1 d . . . H33 H -0.6546 -0.3805 0.2067 0.089 Uiso 1 1 calc R . . C34 C -0.0498(6) -0.3806(7) 0.2490(5) 0.066(2) Uani 1 1 d . . . H34A H -0.1205 -0.3870 0.2224 0.079 Uiso 1 1 calc R . . H34B H -0.0498 -0.4150 0.3130 0.079 Uiso 1 1 calc R . . C35 C 0.0724(10) -0.4303(6) 0.2184(7) 0.103(3) Uani 1 1 d . . . H35A H 0.0784 -0.4973 0.2355 0.154 Uiso 1 1 calc R . . H35B H 0.1437 -0.4262 0.2455 0.154 Uiso 1 1 calc R . . H35C H 0.0726 -0.3988 0.1548 0.154 Uiso 1 1 calc R . . C36 C 0.2287(5) 0.1265(4) 0.1616(4) 0.0325(11) Uani 1 1 d . . . C37 C 0.1483(5) 0.1891(5) 0.0849(4) 0.0446(14) Uani 1 1 d . . . H37 H 0.0729 0.2322 0.0900 0.054 Uiso 1 1 calc R . . C38 C 0.1767(6) 0.1897(5) 0.0016(4) 0.0543(17) Uani 1 1 d . . . H38 H 0.1206 0.2328 -0.0475 0.065 Uiso 1 1 calc R . . C39 C 0.2873(6) 0.1267(5) -0.0092(4) 0.0479(15) Uani 1 1 d . . . H39 H 0.3051 0.1253 -0.0645 0.058 Uiso 1 1 calc R . . C40 C 0.3708(5) 0.0660(5) 0.0642(4) 0.0431(14) Uani 1 1 d . . . H40 H 0.4474 0.0249 0.0581 0.052 Uiso 1 1 calc R . . C41 C 0.3415(5) 0.0660(4) 0.1458(4) 0.0385(13) Uani 1 1 d . . . H41 H 0.3995 0.0235 0.1939 0.046 Uiso 1 1 calc R . . C42 C 0.1997(5) 0.0137(4) 0.3322(4) 0.0334(11) Uani 1 1 d . . . C43 C 0.2212(5) -0.0679(4) 0.3129(4) 0.0376(13) Uani 1 1 d . . . H43 H 0.2376 -0.0611 0.2549 0.045 Uiso 1 1 calc R . . C44 C 0.2193(5) -0.1577(4) 0.3752(4) 0.0429(14) Uani 1 1 d . . . H44 H 0.2340 -0.2091 0.3584 0.051 Uiso 1 1 calc R . . C45 C 0.1956(5) -0.1725(4) 0.4628(4) 0.0427(14) Uani 1 1 d . . . H45 H 0.1981 -0.2338 0.5056 0.051 Uiso 1 1 calc R . . C46 C 0.1684(6) -0.0937(5) 0.4845(4) 0.0445(14) Uani 1 1 d . . . H46 H 0.1500 -0.1014 0.5425 0.053 Uiso 1 1 calc R . . C47 C 0.1680(5) -0.0033(4) 0.4213(4) 0.0396(13) Uani 1 1 d . . . H47 H 0.1460 0.0488 0.4377 0.048 Uiso 1 1 calc R . . C48 C 0.0709(5) 0.2013(4) 0.2659(4) 0.0360(12) Uani 1 1 d . . . C49 C 0.0599(6) 0.2787(5) 0.2867(4) 0.0475(15) Uani 1 1 d . . . H49 H 0.1331 0.2901 0.2989 0.057 Uiso 1 1 calc R . . C50 C -0.0608(6) 0.3419(5) 0.2900(5) 0.0559(18) Uani 1 1 d . . . H50 H -0.0652 0.3944 0.3034 0.067 Uiso 1 1 calc R . . C51 C -0.1699(6) 0.3267(5) 0.2740(4) 0.0552(18) Uani 1 1 d . . . H51 H -0.2486 0.3682 0.2765 0.066 Uiso 1 1 calc R . . C52 C -0.1620(6) 0.2494(6) 0.2542(5) 0.0602(19) Uani 1 1 d . . . H52 H -0.2356 0.2380 0.2428 0.072 Uiso 1 1 calc R . . C53 C -0.0433(5) 0.1878(5) 0.2510(4) 0.0474(15) Uani 1 1 d . . . H53 H -0.0402 0.1351 0.2383 0.057 Uiso 1 1 calc R . . C54 C 0.3248(4) 0.1493(4) 0.2901(4) 0.0312(11) Uani 1 1 d . . . C55 C 0.3602(5) 0.2308(4) 0.2291(4) 0.0407(13) Uani 1 1 d . . . H55 H 0.3187 0.2649 0.1727 0.049 Uiso 1 1 calc R . . C56 C 0.4537(6) 0.2614(4) 0.2502(4) 0.0449(15) Uani 1 1 d . . . H56 H 0.4717 0.3166 0.2088 0.054 Uiso 1 1 calc R . . C57 C 0.5219(5) 0.2102(5) 0.3334(4) 0.0435(14) Uani 1 1 d . . . H57 H 0.5864 0.2297 0.3473 0.052 Uiso 1 1 calc R . . C58 C 0.4909(5) 0.1306(4) 0.3936(4) 0.0398(13) Uani 1 1 d . . . H58 H 0.5344 0.0958 0.4493 0.048 Uiso 1 1 calc R . . C59 C 0.3942(5) 0.1013(4) 0.3719(4) 0.0346(12) Uani 1 1 d . . . H59 H 0.3756 0.0470 0.4144 0.042 Uiso 1 1 calc R . . B1 B 0.2063(5) 0.1211(4) 0.2630(4) 0.0337(13) Uani 1 1 d . . . Co1 Co -0.14969(7) -0.20831(5) 0.28274(5) 0.0311(2) Uani 1 1 d . . . N1 N -0.1210(4) -0.0769(3) 0.2259(3) 0.0326(10) Uani 1 1 d . . . N2 N -0.1073(4) -0.2224(3) 0.4062(3) 0.0329(10) Uani 1 1 d . . . N3 N -0.3403(4) -0.1613(3) 0.2858(3) 0.0323(10) Uani 1 1 d . . . O1 O -0.0688(4) -0.2945(4) 0.2316(3) 0.0499(11) Uani 1 1 d . . . O1S O 0.0889(15) -0.4732(10) 0.0393(11) 0.093(5) Uiso 0.50 1 d PD . . H1S H 0.1577 -0.5019 0.0680 0.139 Uiso 0.50 1 calc PR . . C1S C 0.027(2) -0.5450(15) 0.0407(13) 0.112(7) Uiso 0.50 1 d PD . . H1S1 H -0.0386 -0.5446 0.0828 0.134 Uiso 0.50 1 calc PR . . H1S2 H 0.0901 -0.6080 0.0672 0.134 Uiso 0.50 1 calc PR . . C2S C -0.0350(18) -0.5434(13) -0.0402(11) 0.064(4) Uiso 0.50 1 d PD . . H2S1 H -0.0701 -0.5966 -0.0217 0.096 Uiso 0.50 1 calc PR . . H2S2 H 0.0278 -0.5494 -0.0821 0.096 Uiso 0.50 1 calc PR . . H2S3 H -0.1014 -0.4833 -0.0676 0.096 Uiso 0.50 1 calc 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 C1 0.031(3) 0.031(3) 0.038(3) -0.013(2) 0.004(2) -0.006(2) C2 0.031(3) 0.043(3) 0.044(3) -0.025(3) 0.004(2) -0.006(2) C3 0.034(3) 0.035(3) 0.033(3) -0.017(2) -0.002(2) 0.003(2) C4 0.038(3) 0.037(3) 0.036(3) -0.020(3) 0.007(2) -0.001(2) C5 0.025(2) 0.039(3) 0.040(3) -0.020(3) 0.006(2) -0.003(2) C6 0.032(3) 0.034(3) 0.036(3) -0.015(3) -0.002(2) 0.001(2) C7 0.036(3) 0.036(3) 0.035(3) -0.015(3) 0.004(2) -0.010(2) C8 0.041(3) 0.038(3) 0.037(3) -0.018(3) 0.006(2) -0.008(2) C9 0.034(3) 0.046(3) 0.040(3) -0.020(3) 0.008(2) -0.013(2) C10 0.038(3) 0.037(3) 0.031(3) -0.011(3) 0.005(2) -0.006(2) C11 0.041(3) 0.073(4) 0.052(4) -0.035(4) 0.015(3) -0.025(3) C12 0.068(4) 0.053(4) 0.056(4) -0.034(4) 0.019(3) -0.023(3) C13 0.060(4) 0.046(3) 0.043(4) -0.025(3) 0.014(3) -0.014(3) C14 0.037(3) 0.047(3) 0.046(4) -0.018(3) 0.013(3) -0.012(3) C15 0.037(3) 0.041(3) 0.038(3) -0.017(3) 0.009(2) -0.011(2) C16 0.036(3) 0.048(3) 0.036(3) -0.020(3) 0.005(2) -0.012(3) C17 0.040(3) 0.030(3) 0.040(3) -0.009(3) -0.003(2) -0.007(2) C18 0.040(3) 0.038(3) 0.043(4) -0.018(3) -0.002(3) -0.003(2) C19 0.041(3) 0.030(3) 0.043(3) -0.008(3) 0.000(3) -0.005(2) C20 0.048(4) 0.046(4) 0.065(5) -0.028(4) -0.010(3) 0.007(3) C21 0.057(4) 0.054(4) 0.082(6) -0.040(4) -0.007(4) 0.005(3) C22 0.049(4) 0.041(3) 0.063(5) -0.018(3) 0.007(3) 0.002(3) C23 0.034(3) 0.059(4) 0.067(5) -0.022(4) -0.005(3) 0.005(3) C24 0.046(3) 0.045(3) 0.052(4) -0.019(3) -0.002(3) -0.003(3) C25 0.034(3) 0.036(3) 0.041(3) -0.013(3) 0.004(2) -0.009(2) C26 0.040(3) 0.040(3) 0.044(4) -0.017(3) -0.001(3) -0.007(2) C27 0.051(4) 0.037(3) 0.050(4) -0.014(3) -0.004(3) -0.012(3) C28 0.072(4) 0.040(3) 0.046(4) -0.012(3) -0.015(3) -0.017(3) C29 0.076(5) 0.047(4) 0.075(5) -0.035(4) -0.008(4) -0.004(3) C30 0.128(8) 0.079(6) 0.099(8) -0.065(6) -0.016(6) -0.005(6) C31 0.148(9) 0.040(4) 0.086(7) -0.025(5) -0.024(6) -0.023(5) C32 0.114(8) 0.066(6) 0.096(7) -0.042(6) -0.011(6) -0.023(5) C33 0.100(6) 0.061(5) 0.073(6) -0.021(4) 0.000(5) -0.047(5) C34 0.040(3) 0.125(8) 0.039(4) -0.037(5) 0.004(3) -0.028(4) C35 0.114(8) 0.053(5) 0.114(8) -0.031(5) 0.038(6) 0.002(5) C36 0.031(3) 0.032(3) 0.033(3) -0.013(2) 0.002(2) -0.009(2) C37 0.027(3) 0.061(4) 0.033(3) -0.010(3) 0.000(2) -0.009(3) C38 0.037(3) 0.082(5) 0.033(3) -0.011(3) -0.003(3) -0.019(3) C39 0.050(4) 0.070(4) 0.034(3) -0.027(3) 0.012(3) -0.026(3) C40 0.037(3) 0.058(4) 0.044(4) -0.030(3) 0.016(3) -0.016(3) C41 0.034(3) 0.049(3) 0.035(3) -0.021(3) 0.003(2) -0.010(2) C42 0.026(2) 0.045(3) 0.033(3) -0.019(3) 0.003(2) -0.011(2) C43 0.026(2) 0.044(3) 0.041(3) -0.022(3) 0.003(2) -0.001(2) C44 0.033(3) 0.042(3) 0.049(4) -0.016(3) 0.000(3) -0.006(2) C45 0.033(3) 0.038(3) 0.047(4) -0.009(3) -0.003(3) -0.008(2) C46 0.047(3) 0.051(4) 0.034(3) -0.011(3) 0.003(3) -0.020(3) C47 0.044(3) 0.042(3) 0.040(3) -0.020(3) 0.005(3) -0.017(3) C48 0.031(3) 0.041(3) 0.031(3) -0.015(3) 0.007(2) -0.005(2) C49 0.039(3) 0.050(4) 0.043(4) -0.018(3) 0.003(3) 0.000(3) C50 0.052(4) 0.047(4) 0.049(4) -0.020(3) 0.007(3) 0.011(3) C51 0.034(3) 0.067(4) 0.048(4) -0.024(4) 0.007(3) 0.008(3) C52 0.032(3) 0.086(5) 0.062(5) -0.038(4) 0.011(3) -0.008(3) C53 0.029(3) 0.062(4) 0.058(4) -0.034(3) 0.012(3) -0.010(3) C54 0.027(2) 0.035(3) 0.032(3) -0.018(2) 0.008(2) -0.004(2) C55 0.047(3) 0.036(3) 0.039(3) -0.017(3) 0.009(3) -0.013(3) C56 0.049(3) 0.043(3) 0.050(4) -0.026(3) 0.023(3) -0.019(3) C57 0.036(3) 0.058(4) 0.051(4) -0.034(3) 0.013(3) -0.019(3) C58 0.034(3) 0.051(3) 0.041(3) -0.026(3) 0.007(2) -0.011(2) C59 0.031(3) 0.037(3) 0.034(3) -0.017(3) 0.009(2) -0.007(2) B1 0.027(3) 0.038(3) 0.035(3) -0.018(3) 0.001(2) -0.003(2) Co1 0.0292(4) 0.0315(4) 0.0320(4) -0.0157(3) 0.0033(3) -0.0046(3) N1 0.025(2) 0.034(2) 0.036(3) -0.014(2) 0.0017(18) -0.0050(17) N2 0.029(2) 0.032(2) 0.033(3) -0.015(2) -0.0001(19) -0.0014(18) N3 0.029(2) 0.028(2) 0.037(3) -0.015(2) 0.0024(19) -0.0033(17) O1 0.052(3) 0.065(3) 0.042(3) -0.032(2) 0.008(2) -0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.506(6) . ? C1 C6 1.521(7) . ? C1 C2 1.522(8) . ? C2 C3 1.531(8) . ? C3 N2 1.477(6) . ? C3 C4 1.541(7) . ? C4 C5 1.509(8) . ? C5 N3 1.482(6) . ? C5 C6 1.531(8) . ? C7 N1 1.295(7) . ? C7 C8 1.444(7) . ? C8 C9 1.349(8) . ? C9 C10 1.465(7) . ? C10 C11 1.377(8) . ? C10 C15 1.397(8) . ? C11 C12 1.391(8) . ? C12 C13 1.338(9) . ? C13 C14 1.368(9) . ? C14 C15 1.392(7) . ? C16 N2 1.291(7) . ? C16 C17 1.440(7) . ? C17 C18 1.328(8) . ? C18 C19 1.472(7) . ? C19 C20 1.378(9) . ? C19 C24 1.395(9) . ? C20 C21 1.388(8) . ? C21 C22 1.388(10) . ? C22 C23 1.388(10) . ? C23 C24 1.378(8) . ? C25 N3 1.281(7) . ? C25 C26 1.444(8) . ? C26 C27 1.314(8) . ? C27 C28 1.489(9) . ? C28 C29 1.380(10) . ? C28 C33 1.399(10) . ? C29 C30 1.402(10) . ? C30 C31 1.348(14) . ? C31 C32 1.341(14) . ? C32 C33 1.398(11) . ? C34 O1 1.224(10) . ? C34 C35 1.518(11) . ? C36 C37 1.402(8) . ? C36 C41 1.410(7) . ? C36 B1 1.646(8) . ? C37 C38 1.387(9) . ? C38 C39 1.382(9) . ? C39 C40 1.379(9) . ? C40 C41 1.365(8) . ? C42 C43 1.403(7) . ? C42 C47 1.423(8) . ? C42 B1 1.634(9) . ? C43 C44 1.376(8) . ? C44 C45 1.387(9) . ? C45 C46 1.378(8) . ? C46 C47 1.382(8) . ? C48 C49 1.372(8) . ? C48 C53 1.393(8) . ? C48 B1 1.661(7) . ? C49 C50 1.422(8) . ? C50 C51 1.359(10) . ? C51 C52 1.367(10) . ? C52 C53 1.394(8) . ? C54 C59 1.391(8) . ? C54 C55 1.420(8) . ? C54 B1 1.644(8) . ? C55 C56 1.381(8) . ? C56 C57 1.402(9) . ? C57 C58 1.371(8) . ? C58 C59 1.401(8) . ? Co1 O1 1.867(4) . ? Co1 N1 2.014(4) . ? Co1 N3 2.019(4) . ? Co1 N2 2.027(4) . ? O1S C1S 1.484(16) . ? C1S C2S 1.526(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C6 110.3(4) . . ? N1 C1 C2 109.0(4) . . ? C6 C1 C2 111.7(4) . . ? C1 C2 C3 114.0(4) . . ? N2 C3 C2 110.8(4) . . ? N2 C3 C4 109.8(4) . . ? C2 C3 C4 111.1(4) . . ? C5 C4 C3 114.3(4) . . ? N3 C5 C4 111.2(4) . . ? N3 C5 C6 109.0(4) . . ? C4 C5 C6 113.0(5) . . ? C1 C6 C5 114.9(4) . . ? N1 C7 C8 121.8(5) . . ? C9 C8 C7 122.4(5) . . ? C8 C9 C10 123.6(5) . . ? C11 C10 C15 118.3(5) . . ? C11 C10 C9 121.7(5) . . ? C15 C10 C9 120.0(5) . . ? C10 C11 C12 119.9(6) . . ? C13 C12 C11 121.2(6) . . ? C12 C13 C14 120.6(5) . . ? C13 C14 C15 119.4(5) . . ? C14 C15 C10 120.5(5) . . ? N2 C16 C17 123.4(5) . . ? C18 C17 C16 122.1(6) . . ? C17 C18 C19 126.8(6) . . ? C20 C19 C24 118.6(5) . . ? C20 C19 C18 122.6(5) . . ? C24 C19 C18 118.7(5) . . ? C19 C20 C21 121.3(6) . . ? C22 C21 C20 119.9(7) . . ? C21 C22 C23 118.9(6) . . ? C24 C23 C22 121.0(6) . . ? C23 C24 C19 120.3(6) . . ? N3 C25 C26 124.5(5) . . ? C27 C26 C25 121.1(5) . . ? C26 C27 C28 124.9(6) . . ? C29 C28 C33 120.4(7) . . ? C29 C28 C27 121.9(6) . . ? C33 C28 C27 117.6(7) . . ? C28 C29 C30 118.4(8) . . ? C31 C30 C29 120.5(10) . . ? C32 C31 C30 121.9(9) . . ? C31 C32 C33 120.2(9) . . ? C32 C33 C28 118.6(9) . . ? O1 C34 C35 116.1(7) . . ? C37 C36 C41 113.8(5) . . ? C37 C36 B1 126.9(5) . . ? C41 C36 B1 119.2(5) . . ? C38 C37 C36 122.8(5) . . ? C39 C38 C37 120.7(6) . . ? C40 C39 C38 118.3(5) . . ? C41 C40 C39 120.4(5) . . ? C40 C41 C36 124.0(6) . . ? C43 C42 C47 113.7(5) . . ? C43 C42 B1 126.2(5) . . ? C47 C42 B1 120.1(5) . . ? C44 C43 C42 123.5(5) . . ? C43 C44 C45 120.9(6) . . ? C46 C45 C44 117.9(6) . . ? C45 C46 C47 120.9(6) . . ? C46 C47 C42 122.9(5) . . ? C49 C48 C53 115.5(5) . . ? C49 C48 B1 125.6(5) . . ? C53 C48 B1 118.7(5) . . ? C48 C49 C50 121.5(6) . . ? C51 C50 C49 121.0(6) . . ? C50 C51 C52 118.8(5) . . ? C51 C52 C53 119.8(6) . . ? C48 C53 C52 123.3(6) . . ? C59 C54 C55 114.6(5) . . ? C59 C54 B1 125.2(5) . . ? C55 C54 B1 120.1(5) . . ? C56 C55 C54 122.7(6) . . ? C55 C56 C57 120.6(6) . . ? C58 C57 C56 118.1(5) . . ? C57 C58 C59 120.7(6) . . ? C54 C59 C58 123.2(5) . . ? C42 B1 C54 112.4(4) . . ? C42 B1 C36 111.2(4) . . ? C54 B1 C36 105.9(4) . . ? C42 B1 C48 107.4(4) . . ? C54 B1 C48 108.6(4) . . ? C36 B1 C48 111.3(4) . . ? O1 Co1 N1 115.11(19) . . ? O1 Co1 N3 122.96(18) . . ? N1 Co1 N3 97.41(17) . . ? O1 Co1 N2 125.82(19) . . ? N1 Co1 N2 91.76(18) . . ? N3 Co1 N2 96.51(17) . . ? C7 N1 C1 117.6(4) . . ? C7 N1 Co1 129.2(4) . . ? C1 N1 Co1 112.5(3) . . ? C16 N2 C3 117.8(4) . . ? C16 N2 Co1 129.2(4) . . ? C3 N2 Co1 112.8(3) . . ? C25 N3 C5 119.1(4) . . ? C25 N3 Co1 130.1(3) . . ? C5 N3 Co1 110.9(3) . . ? C34 O1 Co1 136.8(5) . . ? O1S C1S C2S 125.4(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 N1 C1 C2 C3 -70.7(5) . . . . ? C6 C1 C2 C3 51.5(6) . . . . ? C1 C2 C3 N2 70.2(5) . . . . ? C1 C2 C3 C4 -52.2(5) . . . . ? N2 C3 C4 C5 -72.8(6) . . . . ? C2 C3 C4 C5 50.2(6) . . . . ? C3 C4 C5 N3 75.1(6) . . . . ? C3 C4 C5 C6 -47.7(6) . . . . ? N1 C1 C6 C5 72.9(6) . . . . ? C2 C1 C6 C5 -48.5(6) . . . . ? N3 C5 C6 C1 -77.0(6) . . . . ? C4 C5 C6 C1 47.1(6) . . . . ? N1 C7 C8 C9 -174.8(6) . . . . ? C7 C8 C9 C10 -175.3(5) . . . . ? C8 C9 C10 C11 20.4(9) . . . . ? C8 C9 C10 C15 -157.4(6) . . . . ? C15 C10 C11 C12 -2.6(10) . . . . ? C9 C10 C11 C12 179.6(6) . . . . ? C10 C11 C12 C13 3.2(11) . . . . ? C11 C12 C13 C14 -1.3(11) . . . . ? C12 C13 C14 C15 -1.0(10) . . . . ? C13 C14 C15 C10 1.6(9) . . . . ? C11 C10 C15 C14 0.2(9) . . . . ? C9 C10 C15 C14 178.1(6) . . . . ? N2 C16 C17 C18 172.2(6) . . . . ? C16 C17 C18 C19 -174.7(6) . . . . ? C17 C18 C19 C20 -16.4(10) . . . . ? C17 C18 C19 C24 160.8(6) . . . . ? C24 C19 C20 C21 -2.6(11) . . . . ? C18 C19 C20 C21 174.6(7) . . . . ? C19 C20 C21 C22 0.9(12) . . . . ? C20 C21 C22 C23 1.4(11) . . . . ? C21 C22 C23 C24 -2.0(11) . . . . ? C22 C23 C24 C19 0.3(11) . . . . ? C20 C19 C24 C23 2.0(10) . . . . ? C18 C19 C24 C23 -175.3(6) . . . . ? N3 C25 C26 C27 178.4(6) . . . . ? C25 C26 C27 C28 -179.6(6) . . . . ? C26 C27 C28 C29 -18.4(11) . . . . ? C26 C27 C28 C33 162.8(7) . . . . ? C33 C28 C29 C30 -1.7(12) . . . . ? C27 C28 C29 C30 179.6(7) . . . . ? C28 C29 C30 C31 0.1(14) . . . . ? C29 C30 C31 C32 1.3(16) . . . . ? C30 C31 C32 C33 -1.1(16) . . . . ? C31 C32 C33 C28 -0.5(14) . . . . ? C29 C28 C33 C32 1.9(12) . . . . ? C27 C28 C33 C32 -179.3(7) . . . . ? C41 C36 C37 C38 1.3(9) . . . . ? B1 C36 C37 C38 178.6(6) . . . . ? C36 C37 C38 C39 0.3(10) . . . . ? C37 C38 C39 C40 -2.4(10) . . . . ? C38 C39 C40 C41 2.6(9) . . . . ? C39 C40 C41 C36 -0.9(9) . . . . ? C37 C36 C41 C40 -1.1(8) . . . . ? B1 C36 C41 C40 -178.6(5) . . . . ? C47 C42 C43 C44 -3.6(8) . . . . ? B1 C42 C43 C44 177.3(5) . . . . ? C42 C43 C44 C45 -0.2(8) . . . . ? C43 C44 C45 C46 3.0(8) . . . . ? C44 C45 C46 C47 -1.7(9) . . . . ? C45 C46 C47 C42 -2.4(9) . . . . ? C43 C42 C47 C46 4.9(8) . . . . ? B1 C42 C47 C46 -175.9(5) . . . . ? C53 C48 C49 C50 -1.8(9) . . . . ? B1 C48 C49 C50 -178.0(6) . . . . ? C48 C49 C50 C51 1.1(10) . . . . ? C49 C50 C51 C52 -0.2(10) . . . . ? C50 C51 C52 C53 0.2(11) . . . . ? C49 C48 C53 C52 1.8(10) . . . . ? B1 C48 C53 C52 178.3(6) . . . . ? C51 C52 C53 C48 -1.0(11) . . . . ? C59 C54 C55 C56 -1.7(7) . . . . ? B1 C54 C55 C56 176.0(5) . . . . ? C54 C55 C56 C57 2.3(8) . . . . ? C55 C56 C57 C58 -1.6(8) . . . . ? C56 C57 C58 C59 0.4(7) . . . . ? C55 C54 C59 C58 0.5(7) . . . . ? B1 C54 C59 C58 -177.0(4) . . . . ? C57 C58 C59 C54 0.1(7) . . . . ? C43 C42 B1 C54 -113.2(5) . . . . ? C47 C42 B1 C54 67.8(6) . . . . ? C43 C42 B1 C36 5.5(7) . . . . ? C47 C42 B1 C36 -173.6(5) . . . . ? C43 C42 B1 C48 127.4(5) . . . . ? C47 C42 B1 C48 -51.6(6) . . . . ? C59 C54 B1 C42 -14.7(6) . . . . ? C55 C54 B1 C42 167.9(4) . . . . ? C59 C54 B1 C36 -136.3(5) . . . . ? C55 C54 B1 C36 46.2(6) . . . . ? C59 C54 B1 C48 104.0(5) . . . . ? C55 C54 B1 C48 -73.4(6) . . . . ? C37 C36 B1 C42 120.0(6) . . . . ? C41 C36 B1 C42 -62.8(6) . . . . ? C37 C36 B1 C54 -117.5(6) . . . . ? C41 C36 B1 C54 59.6(6) . . . . ? C37 C36 B1 C48 0.4(8) . . . . ? C41 C36 B1 C48 177.5(5) . . . . ? C49 C48 B1 C42 122.3(6) . . . . ? C53 C48 B1 C42 -53.9(7) . . . . ? C49 C48 B1 C54 0.5(8) . . . . ? C53 C48 B1 C54 -175.7(5) . . . . ? C49 C48 B1 C36 -115.8(6) . . . . ? C53 C48 B1 C36 68.1(7) . . . . ? C8 C7 N1 C1 -179.8(5) . . . . ? C8 C7 N1 Co1 10.7(8) . . . . ? C6 C1 N1 C7 131.8(5) . . . . ? C2 C1 N1 C7 -105.1(5) . . . . ? C6 C1 N1 Co1 -56.9(5) . . . . ? C2 C1 N1 Co1 66.1(5) . . . . ? O1 Co1 N1 C7 -14.5(5) . . . . ? N3 Co1 N1 C7 -146.3(5) . . . . ? N2 Co1 N1 C7 116.9(5) . . . . ? O1 Co1 N1 C1 175.5(3) . . . . ? N3 Co1 N1 C1 43.7(4) . . . . ? N2 Co1 N1 C1 -53.1(3) . . . . ? C17 C16 N2 C3 -174.2(5) . . . . ? C17 C16 N2 Co1 0.5(8) . . . . ? C2 C3 N2 C16 111.8(5) . . . . ? C4 C3 N2 C16 -125.1(5) . . . . ? C2 C3 N2 Co1 -63.7(5) . . . . ? C4 C3 N2 Co1 59.4(5) . . . . ? O1 Co1 N2 C16 0.1(6) . . . . ? N1 Co1 N2 C16 -123.0(5) . . . . ? N3 Co1 N2 C16 139.3(5) . . . . ? O1 Co1 N2 C3 175.0(3) . . . . ? N1 Co1 N2 C3 51.9(4) . . . . ? N3 Co1 N2 C3 -45.8(4) . . . . ? C26 C25 N3 C5 178.2(5) . . . . ? C26 C25 N3 Co1 -3.9(9) . . . . ? C4 C5 N3 C25 116.2(5) . . . . ? C6 C5 N3 C25 -118.6(5) . . . . ? C4 C5 N3 Co1 -62.0(5) . . . . ? C6 C5 N3 Co1 63.2(5) . . . . ? O1 Co1 N3 C25 8.6(6) . . . . ? N1 Co1 N3 C25 135.1(5) . . . . ? N2 Co1 N3 C25 -132.3(5) . . . . ? O1 Co1 N3 C5 -173.4(3) . . . . ? N1 Co1 N3 C5 -47.0(4) . . . . ? N2 Co1 N3 C5 45.7(4) . . . . ? C35 C34 O1 Co1 -148.8(7) . . . . ? N1 Co1 O1 C34 170.9(6) . . . . ? N3 Co1 O1 C34 -70.8(7) . . . . ? N2 Co1 O1 C34 58.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.676 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.094 data_shelxl _database_code_CSD 185610 #------------------------------------------------------------------------------ _audit_creation_date '2000-03-08' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #------------------------------------------------------------------------------ _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C39 H38 Co N3 O1)1+, 2(C24 H20 B)1-, 3(C H2 CL2), 2(C6 H12) ; _chemical_formula_sum 'C141 H146 B2 Cl6 Co2 N6 O2' _chemical_formula_weight 2308.82 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.31(3) _cell_length_b 22.022(11) _cell_length_c 17.219(6) _cell_angle_alpha 98.97(4) _cell_angle_beta 92.61(7) _cell_angle_gamma 67.78(5) _cell_volume 6348(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.6 _cell_measurement_theta_max 5.4 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; The scan width was (1.47+0.34tan\q)\% with an \w scan speed of 4\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku AFC6s' _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_interval_count 3 _diffrn_standards_number 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.024 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -4 3 -2 -5 0 -2 -5 2 _diffrn_reflns_number 12510 _diffrn_reflns_av_R_equivalents 0.10152 _diffrn_reflns_av_sigmaI/netI 0.130 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 22.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00406 _diffrn_orient_matrix_UB_12 -0.04424 _diffrn_orient_matrix_UB_13 -0.01606 _diffrn_orient_matrix_UB_21 -0.02123 _diffrn_orient_matrix_UB_22 0.00263 _diffrn_orient_matrix_UB_23 0.05344 _diffrn_orient_matrix_UB_31 -0.05491 _diffrn_orient_matrix_UB_32 0.02231 _diffrn_orient_matrix_UB_33 -0.01855 _reflns_number_total 11978 _reflns_number_gt 5773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'DIRDIF92 (Beurskens, P.T., et al, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan (MSC, 1992-1997)' _computing_publication_material 'ORTEPII (Johnson, 1976)' _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^)+(0.1213P)^2^+22.9267P] 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 11971 _refine_ls_number_parameters 1432 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.2534 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.41882(9) 0.25284(8) -0.23323(9) 0.0344(5) Uani 1 1 d . . . Co2 Co 0.05810(9) 0.29716(7) 0.23074(8) 0.0289(4) Uani 1 1 d . . . Cl1 Cl 0.4052(3) 0.2392(3) 0.0978(4) 0.149(2) Uani 1 1 d . . . Cl2 Cl 0.2830(2) 0.3211(2) 0.2089(2) 0.0877(13) Uani 1 1 d . . . Cl3 Cl 0.2999(2) 0.16392(19) 0.7305(2) 0.0808(12) Uani 1 1 d . . . Cl4 Cl 0.4517(2) 0.15289(19) 0.6693(2) 0.0738(12) Uani 1 1 d . . . Cl5 Cl 0.6889(2) 0.31419(19) 0.5498(2) 0.0665(11) Uani 1 1 d . . . Cl6 Cl 0.8011(3) 0.3016(2) 0.6755(2) 0.0894(14) Uani 1 1 d . . . O1 O -0.3633(5) 0.1600(4) -0.2474(4) 0.037(2) Uani 1 1 d . . . O2 O 0.0834(4) 0.2063(4) 0.2139(4) 0.0326(19) Uani 1 1 d . . . N1 N -0.3718(5) 0.3192(5) -0.1850(5) 0.036(3) Uani 1 1 d . . . N2 N -0.5096(6) 0.2870(5) -0.1584(5) 0.037(3) Uani 1 1 d . . . N3 N -0.4762(5) 0.3015(5) -0.3211(5) 0.036(3) Uani 1 1 d . . . N4 N 0.1113(5) 0.3454(4) 0.3069(5) 0.029(2) Uani 1 1 d . . . N5 N -0.0498(6) 0.3503(4) 0.2787(5) 0.033(2) Uani 1 1 d . . . N6 N 0.0438(5) 0.3497(4) 0.1418(6) 0.034(2) Uani 1 1 d . . . C1 C -0.4299(6) 0.3875(6) -0.1768(7) 0.042(3) Uani 1 1 d . . . H1 H -0.4035 0.4175 -0.1550 0.051 Uiso 1 1 calc R . . C2 C -0.4952(7) 0.3952(6) -0.1191(7) 0.043(3) Uani 1 1 d . . . H2A H -0.5261 0.4422 -0.1044 0.052 Uiso 1 1 calc R . . H2B H -0.4708 0.3781 -0.0718 0.052 Uiso 1 1 calc R . . C3 C -0.5515(6) 0.3601(6) -0.1503(7) 0.040(3) Uani 1 1 d . . . H3 H -0.5958 0.3737 -0.1132 0.048 Uiso 1 1 calc R . . C4 C -0.5834(6) 0.3802(6) -0.2303(6) 0.039(3) Uani 1 1 d . . . H4A H -0.6204 0.4259 -0.2217 0.047 Uiso 1 1 calc R . . H4B H -0.6125 0.3530 -0.2525 0.047 Uiso 1 1 calc R . . C5 C -0.5208(7) 0.3739(5) -0.2911(7) 0.039(3) Uani 1 1 d . . . H5 H -0.5478 0.3960 -0.3354 0.047 Uiso 1 1 calc R . . C6 C -0.4646(7) 0.4064(6) -0.2563(7) 0.041(3) Uani 1 1 d . . . H6A H -0.4923 0.4542 -0.2502 0.049 Uiso 1 1 calc R . . H6B H -0.4214 0.3948 -0.2935 0.049 Uiso 1 1 calc R . . C7 C -0.3037(7) 0.3079(6) -0.1537(7) 0.040(3) Uani 1 1 d . . . H7 H -0.2924 0.3446 -0.1315 0.048 Uiso 1 1 calc R . . C8 C -0.2447(7) 0.2448(6) -0.1503(7) 0.041(3) Uani 1 1 d . . . H8 H -0.2528 0.2077 -0.1765 0.049 Uiso 1 1 calc R . . C9 C -0.1787(7) 0.2359(6) -0.1117(6) 0.039(3) Uani 1 1 d . . . H9 H -0.1698 0.2738 -0.0895 0.046 Uiso 1 1 calc R . . C10 C -0.1172(7) 0.1711(6) -0.1003(7) 0.038(3) Uani 1 1 d . . . C11 C -0.1136(8) 0.1115(7) -0.1459(8) 0.054(4) Uani 1 1 d . . . H11 H -0.1495 0.1128 -0.1863 0.065 Uiso 1 1 calc R . . C12 C -0.0601(9) 0.0526(7) -0.1333(9) 0.063(4) Uani 1 1 d . . . H12 H -0.0601 0.0136 -0.1633 0.075 Uiso 1 1 calc R . . C13 C -0.0044(9) 0.0503(8) -0.0748(9) 0.065(4) Uani 1 1 d . . . H13 H 0.0338 0.0096 -0.0669 0.077 Uiso 1 1 calc R . . C14 C -0.0051(8) 0.1076(9) -0.0283(8) 0.061(4) Uani 1 1 d . . . H14 H 0.0316 0.1060 0.0113 0.074 Uiso 1 1 calc R . . C15 C -0.0614(7) 0.1673(6) -0.0419(7) 0.044(3) Uani 1 1 d . . . H15 H -0.0621 0.2062 -0.0112 0.053 Uiso 1 1 calc R . . C16 C -0.5446(7) 0.2572(7) -0.1217(7) 0.047(3) Uani 1 1 d . . . H16 H -0.5876 0.2827 -0.0887 0.057 Uiso 1 1 calc R . . C17 C -0.5172(8) 0.1845(7) -0.1318(7) 0.058(4) Uani 1 1 d . . . H17 H -0.4694 0.1591 -0.1577 0.069 Uiso 1 1 calc R . . C18 C -0.5609(8) 0.1528(9) -0.1035(8) 0.069(5) Uani 1 1 d . . . H18 H -0.6056 0.1802 -0.0736 0.083 Uiso 1 1 calc R . . C19 C -0.5457(9) 0.0827(8) -0.1146(9) 0.065(4) Uani 1 1 d . . . C20 C -0.5888(9) 0.0599(10) -0.0719(10) 0.082(5) Uani 1 1 d . . . H20 H -0.6268 0.0896 -0.0359 0.099 Uiso 1 1 calc R . . C21 C -0.5761(11) -0.0076(11) -0.0821(12) 0.097(6) Uani 1 1 d . . . H21 H -0.6031 -0.0232 -0.0506 0.116 Uiso 1 1 calc R . . C22 C -0.5227(11) -0.0515(10) -0.1398(13) 0.095(6) Uani 1 1 d . . . H22 H -0.5158 -0.0961 -0.1476 0.114 Uiso 1 1 calc R . . C23 C -0.4800(10) -0.0300(8) -0.1853(9) 0.071(4) Uani 1 1 d . . . H23 H -0.4446 -0.0595 -0.2236 0.085 Uiso 1 1 calc R . . C24 C -0.4911(8) 0.0361(9) -0.1727(9) 0.065(4) Uani 1 1 d . . . H24 H -0.4622 0.0511 -0.2028 0.078 Uiso 1 1 calc R . . C25 C -0.4741(6) 0.2808(6) -0.3958(7) 0.031(3) Uani 1 1 d . . . H25 H -0.5011 0.3113 -0.4290 0.037 Uiso 1 1 calc R . . C26 C -0.4328(6) 0.2143(6) -0.4294(7) 0.032(3) Uani 1 1 d . . . H26 H -0.4083 0.1828 -0.3967 0.038 Uiso 1 1 calc R . . C27 C -0.4282(7) 0.1955(6) -0.5082(7) 0.044(3) Uani 1 1 d . . . H27 H -0.4555 0.2281 -0.5387 0.052 Uiso 1 1 calc R . . C28 C -0.3832(7) 0.1271(6) -0.5515(8) 0.041(3) Uani 1 1 d . . . C29 C -0.3854(7) 0.1160(7) -0.6333(7) 0.051(4) Uani 1 1 d . . . H29 H -0.4133 0.1505 -0.6611 0.061 Uiso 1 1 calc R . . C30 C -0.3452(11) 0.0528(10) -0.6724(8) 0.084(5) Uani 1 1 d . . . H30 H -0.3470 0.0448 -0.7270 0.101 Uiso 1 1 calc R . . C31 C -0.3034(10) 0.0025(8) -0.6330(10) 0.067(4) Uani 1 1 d . . . H31 H -0.2760 -0.0394 -0.6607 0.080 Uiso 1 1 calc R . . C32 C -0.3007(8) 0.0125(6) -0.5520(9) 0.061(4) Uani 1 1 d . . . H32 H -0.2729 -0.0227 -0.5252 0.073 Uiso 1 1 calc R . . C33 C -0.3396(8) 0.0751(6) -0.5107(7) 0.047(3) Uani 1 1 d . . . H33 H -0.3369 0.0825 -0.4562 0.056 Uiso 1 1 calc R . . C34 C -0.2969(7) 0.1275(6) -0.2866(7) 0.034(3) Uani 1 1 d . . . C35 C -0.2570(8) 0.0587(6) -0.2822(7) 0.044(3) Uani 1 1 d . . . H35 H -0.2782 0.0382 -0.2512 0.052 Uiso 1 1 calc R . . C36 C -0.1877(9) 0.0223(7) -0.3230(9) 0.059(4) Uani 1 1 d . . . H36 H -0.1638 -0.0228 -0.3205 0.071 Uiso 1 1 calc R . . C37 C -0.1523(9) 0.0505(8) -0.3675(8) 0.064(4) Uani 1 1 d . . . H37 H -0.1050 0.0252 -0.3943 0.077 Uiso 1 1 calc R . . C38 C -0.1896(8) 0.1182(8) -0.3713(7) 0.052(4) Uani 1 1 d . . . H38 H -0.1668 0.1386 -0.4008 0.062 Uiso 1 1 calc R . . C39 C -0.2583(8) 0.1542(6) -0.3326(7) 0.043(3) Uani 1 1 d . . . H39 H -0.2815 0.1992 -0.3364 0.052 Uiso 1 1 calc R . . C40 C 0.0713(7) 0.4181(5) 0.3116(6) 0.037(3) Uani 1 1 d . . . H40 H 0.1012 0.4387 0.3477 0.044 Uiso 1 1 calc R . . C41 C -0.0114(6) 0.4414(6) 0.3453(6) 0.033(3) Uani 1 1 d . . . H41A H -0.0312 0.4893 0.3598 0.039 Uiso 1 1 calc R . . H41B H -0.0092 0.4223 0.3929 0.039 Uiso 1 1 calc R . . C42 C -0.0697(6) 0.4230(5) 0.2883(6) 0.032(3) Uani 1 1 d . . . H42 H -0.1230 0.4456 0.3111 0.038 Uiso 1 1 calc R . . C43 C -0.0683(7) 0.4456(6) 0.2101(7) 0.038(3) Uani 1 1 d . . . H43A H -0.0912 0.4937 0.2174 0.046 Uiso 1 1 calc R . . H43B H -0.1015 0.4296 0.1740 0.046 Uiso 1 1 calc R . . C44 C 0.0142(7) 0.4223(6) 0.1720(6) 0.035(3) Uani 1 1 d . . . H44 H 0.0097 0.4460 0.1272 0.042 Uiso 1 1 calc R . . C45 C 0.0712(7) 0.4399(6) 0.2311(6) 0.040(3) Uani 1 1 d . . . H45A H 0.1242 0.4193 0.2089 0.048 Uiso 1 1 calc R . . H45B H 0.0572 0.4876 0.2387 0.048 Uiso 1 1 calc R . . C46 C 0.1660(7) 0.3225(6) 0.3567(6) 0.033(3) Uani 1 1 d . . . H46 H 0.1787 0.3530 0.3927 0.040 Uiso 1 1 calc R . . C47 C 0.2083(6) 0.2539(6) 0.3603(6) 0.029(3) Uani 1 1 d . . . H47 H 0.1927 0.2229 0.3283 0.035 Uiso 1 1 calc R . . C48 C 0.2693(7) 0.2322(6) 0.4079(7) 0.034(3) Uani 1 1 d . . . H48 H 0.2784 0.2646 0.4439 0.041 Uiso 1 1 calc R . . C49 C 0.3232(7) 0.1645(6) 0.4104(6) 0.038(3) Uani 1 1 d . . . C50 C 0.3108(8) 0.1082(7) 0.3702(7) 0.055(4) Uani 1 1 d . . . H50 H 0.2646 0.1146 0.3419 0.066 Uiso 1 1 calc R . . C51 C 0.3630(8) 0.0453(7) 0.3710(8) 0.060(4) Uani 1 1 d . . . H51 H 0.3540 0.0091 0.3431 0.071 Uiso 1 1 calc R . . C52 C 0.4312(8) 0.0368(7) 0.4154(8) 0.061(4) Uani 1 1 d . . . H52 H 0.4676 -0.0059 0.4182 0.073 Uiso 1 1 calc R . . C53 C 0.4455(8) 0.0909(8) 0.4552(9) 0.059(4) Uani 1 1 d . . . H53 H 0.4921 0.0848 0.4827 0.071 Uiso 1 1 calc R . . C54 C 0.3922(8) 0.1513(7) 0.4538(8) 0.059(4) Uani 1 1 d . . . H54 H 0.4013 0.1869 0.4834 0.071 Uiso 1 1 calc R . . C55 C -0.1014(7) 0.3296(6) 0.2993(6) 0.035(3) Uani 1 1 d . . . H55 H -0.1497 0.3613 0.3181 0.042 Uiso 1 1 calc R . . C56 C -0.0903(7) 0.2599(6) 0.2957(7) 0.036(3) Uani 1 1 d . . . H56 H -0.0459 0.2276 0.2696 0.043 Uiso 1 1 calc R . . C57 C -0.1400(7) 0.2410(6) 0.3275(7) 0.038(3) Uani 1 1 d . . . H57 H -0.1860 0.2752 0.3481 0.046 Uiso 1 1 calc R . . C58 C -0.1344(8) 0.1735(6) 0.3357(7) 0.043(3) Uani 1 1 d . . . C59 C -0.1847(8) 0.1653(7) 0.3862(8) 0.055(4) Uani 1 1 d . . . H59 H -0.2250 0.2025 0.4114 0.065 Uiso 1 1 calc R . . C60 C -0.1767(9) 0.1029(9) 0.4004(8) 0.067(4) Uani 1 1 d . . . H60 H -0.2090 0.0978 0.4370 0.080 Uiso 1 1 calc R . . C61 C -0.1195(10) 0.0484(8) 0.3584(9) 0.066(4) Uani 1 1 d . . . H61 H -0.1143 0.0060 0.3658 0.079 Uiso 1 1 calc R . . C62 C -0.0700(10) 0.0556(8) 0.3060(9) 0.076(5) Uani 1 1 d . . . H62 H -0.0311 0.0185 0.2788 0.092 Uiso 1 1 calc R . . C63 C -0.0789(9) 0.1179(8) 0.2945(8) 0.066(4) Uani 1 1 d . . . H63 H -0.0467 0.1228 0.2577 0.079 Uiso 1 1 calc R . . C64 C 0.0552(6) 0.3302(6) 0.0671(6) 0.033(3) Uani 1 1 d . . . H64 H 0.0430 0.3627 0.0348 0.039 Uiso 1 1 calc R . . C65 C 0.0852(6) 0.2626(5) 0.0304(7) 0.034(3) Uani 1 1 d . . . H65 H 0.1005 0.2294 0.0620 0.040 Uiso 1 1 calc R . . C66 C 0.0923(7) 0.2452(6) -0.0481(6) 0.034(3) Uani 1 1 d . . . H66 H 0.0752 0.2797 -0.0779 0.041 Uiso 1 1 calc R . . C67 C 0.1233(7) 0.1790(7) -0.0912(7) 0.043(3) Uani 1 1 d . . . C68 C 0.1017(9) 0.1674(7) -0.1696(8) 0.064(4) Uani 1 1 d . . . H68 H 0.0689 0.2029 -0.1934 0.076 Uiso 1 1 calc R . . C69 C 0.1282(10) 0.1041(8) -0.2126(8) 0.079(5) Uani 1 1 d . . . H69 H 0.1144 0.0972 -0.2650 0.095 Uiso 1 1 calc R . . C70 C 0.1745(9) 0.0525(7) -0.1766(9) 0.069(4) Uani 1 1 d . . . H70 H 0.1902 0.0095 -0.2036 0.082 Uiso 1 1 calc R . . C71 C 0.1987(8) 0.0630(7) -0.0997(8) 0.060(4) Uani 1 1 d . . . H71 H 0.2333 0.0275 -0.0770 0.072 Uiso 1 1 calc R . . C72 C 0.1715(7) 0.1264(6) -0.0568(7) 0.044(3) Uani 1 1 d . . . H72 H 0.1862 0.1330 -0.0047 0.052 Uiso 1 1 calc R . . C73 C 0.1473(7) 0.1562(6) 0.1819(6) 0.029(3) Uani 1 1 d . . . C74 C 0.1442(7) 0.0937(6) 0.1606(7) 0.044(3) Uani 1 1 d . . . H74 H 0.0977 0.0875 0.1682 0.053 Uiso 1 1 calc R . . C75 C 0.2099(9) 0.0404(6) 0.1280(8) 0.054(4) Uani 1 1 d . . . H75 H 0.2070 -0.0012 0.1157 0.064 Uiso 1 1 calc R . . C76 C 0.2792(9) 0.0474(8) 0.1135(8) 0.063(4) Uani 1 1 d . . . H76 H 0.3227 0.0112 0.0916 0.076 Uiso 1 1 calc R . . C77 C 0.2828(8) 0.1109(8) 0.1325(7) 0.052(4) Uani 1 1 d . . . H77 H 0.3290 0.1170 0.1231 0.063 Uiso 1 1 calc R . . C78 C 0.2174(7) 0.1640(7) 0.1653(6) 0.040(3) Uani 1 1 d . . . H78 H 0.2199 0.2058 0.1767 0.048 Uiso 1 1 calc R . . C79 C 0.2458(6) 0.4098(6) 0.5547(6) 0.028(3) Uani 1 1 d . . . C80 C 0.1685(7) 0.4141(6) 0.5540(6) 0.034(3) Uani 1 1 d . . . H80 H 0.1316 0.4473 0.5295 0.041 Uiso 1 1 calc R . . C81 C 0.1421(7) 0.3727(7) 0.5869(7) 0.045(3) Uani 1 1 d . . . H81 H 0.0891 0.3786 0.5849 0.054 Uiso 1 1 calc R . . C82 C 0.1967(9) 0.3214(6) 0.6235(7) 0.052(4) Uani 1 1 d . . . H82 H 0.1804 0.2930 0.6464 0.063 Uiso 1 1 calc R . . C83 C 0.2741(8) 0.3143(7) 0.6248(7) 0.048(3) Uani 1 1 d . . . H83 H 0.3108 0.2811 0.6493 0.057 Uiso 1 1 calc R . . C84 C 0.2989(7) 0.3568(6) 0.5893(6) 0.038(3) Uani 1 1 d . . . H84 H 0.3524 0.3494 0.5887 0.046 Uiso 1 1 calc R . . C85 C 0.3609(6) 0.4194(6) 0.4728(6) 0.030(3) Uani 1 1 d . . . C86 C 0.3663(7) 0.3658(6) 0.4148(7) 0.036(3) Uani 1 1 d . . . H86 H 0.3221 0.3546 0.4057 0.043 Uiso 1 1 calc R . . C87 C 0.4342(8) 0.3281(6) 0.3700(7) 0.045(3) Uani 1 1 d . . . H87 H 0.4357 0.2916 0.3339 0.054 Uiso 1 1 calc R . . C88 C 0.4982(7) 0.3451(7) 0.3793(7) 0.048(4) Uani 1 1 d . . . H88 H 0.5429 0.3219 0.3476 0.057 Uiso 1 1 calc R . . C89 C 0.4963(7) 0.3977(6) 0.4367(8) 0.049(4) Uani 1 1 d . . . H89 H 0.5406 0.4087 0.4452 0.058 Uiso 1 1 calc R . . C90 C 0.4292(7) 0.4329(6) 0.4805(7) 0.042(3) Uani 1 1 d . . . H90 H 0.4292 0.4683 0.5179 0.051 Uiso 1 1 calc R . . C91 C 0.2924(6) 0.5125(6) 0.5977(7) 0.032(3) Uani 1 1 d . . . C92 C 0.2865(6) 0.5068(5) 0.6767(7) 0.032(3) Uani 1 1 d . . . H92 H 0.2732 0.4725 0.6889 0.039 Uiso 1 1 calc R . . C93 C 0.3004(6) 0.5522(6) 0.7398(7) 0.040(3) Uani 1 1 d . . . H93 H 0.2954 0.5479 0.7920 0.048 Uiso 1 1 calc R . . C94 C 0.3209(7) 0.6015(6) 0.7213(7) 0.041(3) Uani 1 1 d . . . H94 H 0.3320 0.6301 0.7616 0.049 Uiso 1 1 calc R . . C95 C 0.3256(6) 0.6101(6) 0.6450(7) 0.036(3) Uani 1 1 d . . . H95 H 0.3393 0.6444 0.6336 0.043 Uiso 1 1 calc R . . C96 C 0.3095(6) 0.5670(6) 0.5843(7) 0.038(3) Uani 1 1 d . . . H96 H 0.3103 0.5748 0.5329 0.046 Uiso 1 1 calc R . . C97 C 0.2114(6) 0.5089(5) 0.4661(6) 0.029(3) Uani 1 1 d . . . C98 C 0.2119(7) 0.5024(6) 0.3838(6) 0.034(3) Uani 1 1 d . . . H98 H 0.2550 0.4697 0.3560 0.041 Uiso 1 1 calc R . . C99 C 0.1508(7) 0.5430(6) 0.3416(7) 0.035(3) Uani 1 1 d . . . H99 H 0.1537 0.5364 0.2870 0.042 Uiso 1 1 calc R . . C100 C 0.0867(7) 0.5921(6) 0.3795(7) 0.035(3) Uani 1 1 d . . . H100 H 0.0463 0.6194 0.3513 0.042 Uiso 1 1 calc R . . C101 C 0.0833(7) 0.6004(6) 0.4608(7) 0.042(3) Uani 1 1 d . . . H101 H 0.0396 0.6330 0.4876 0.051 Uiso 1 1 calc R . . C102 C 0.1436(7) 0.5612(6) 0.5021(7) 0.038(3) Uani 1 1 d . . . H102 H 0.1401 0.5692 0.5567 0.046 Uiso 1 1 calc R . . C103 C 0.6954(6) 0.5080(5) 0.9018(6) 0.028(3) Uani 1 1 d . . . C104 C 0.6968(7) 0.4986(6) 0.8184(7) 0.043(3) Uani 1 1 d . . . H104 H 0.7442 0.4735 0.7917 0.052 Uiso 1 1 calc R . . C105 C 0.6291(8) 0.5257(6) 0.7754(7) 0.043(3) Uani 1 1 d . . . H105 H 0.6328 0.5212 0.7210 0.051 Uiso 1 1 calc R . . C106 C 0.5565(7) 0.5592(6) 0.8126(8) 0.042(3) Uani 1 1 d . . . H106 H 0.5106 0.5745 0.7838 0.051 Uiso 1 1 calc R . . C107 C 0.5544(7) 0.5694(6) 0.8945(8) 0.048(4) Uani 1 1 d . . . H107 H 0.5067 0.5934 0.9213 0.057 Uiso 1 1 calc R . . C108 C 0.6235(7) 0.5436(6) 0.9368(7) 0.038(3) Uani 1 1 d . . . H108 H 0.6202 0.5511 0.9914 0.045 Uiso 1 1 calc R . . C109 C 0.7702(7) 0.4231(6) 1.0068(6) 0.031(3) Uani 1 1 d . . . C110 C 0.7013(7) 0.4124(6) 1.0204(6) 0.032(3) Uani 1 1 d . . . H110 H 0.6539 0.4394 1.0008 0.038 Uiso 1 1 calc R . . C111 C 0.7008(9) 0.3626(7) 1.0623(7) 0.053(4) Uani 1 1 d . . . H111 H 0.6541 0.3566 1.0690 0.064 Uiso 1 1 calc R . . C112 C 0.7715(9) 0.3219(7) 1.0941(7) 0.051(4) Uani 1 1 d . . . H112 H 0.7723 0.2887 1.1219 0.061 Uiso 1 1 calc R . . C113 C 0.8384(8) 0.3326(6) 1.0828(6) 0.038(3) Uani 1 1 d . . . H113 H 0.8855 0.3070 1.1043 0.046 Uiso 1 1 calc R . . C114 C 0.8374(7) 0.3815(6) 1.0394(6) 0.036(3) Uani 1 1 d . . . H114 H 0.8848 0.3863 1.0319 0.043 Uiso 1 1 calc R . . C115 C 0.7752(7) 0.5442(6) 1.0197(7) 0.039(3) Uani 1 1 d . . . C116 C 0.7705(6) 0.5513(6) 1.1021(7) 0.036(3) Uani 1 1 d . . . H116 H 0.7673 0.5166 1.1246 0.044 Uiso 1 1 calc R . . C117 C 0.7703(6) 0.6091(7) 1.1530(7) 0.042(3) Uani 1 1 d . . . H117 H 0.7683 0.6118 1.2073 0.050 Uiso 1 1 calc R . . C118 C 0.7733(7) 0.6604(7) 1.1192(10) 0.059(4) Uani 1 1 d . . . H118 H 0.7732 0.6986 1.1511 0.070 Uiso 1 1 calc R . . C119 C 0.7763(7) 0.6565(7) 1.0390(9) 0.054(4) Uani 1 1 d . . . H119 H 0.7771 0.6925 1.0177 0.064 Uiso 1 1 calc R . . C120 C 0.7783(7) 0.6005(6) 0.9893(7) 0.045(3) Uani 1 1 d . . . H120 H 0.7816 0.5990 0.9352 0.054 Uiso 1 1 calc R . . C121 C 0.8577(7) 0.4452(5) 0.9090(6) 0.031(3) Uani 1 1 d . . . C122 C 0.9245(7) 0.4627(6) 0.9247(6) 0.033(3) Uani 1 1 d . . . H122 H 0.9199 0.4995 0.9620 0.040 Uiso 1 1 calc R . . C123 C 0.9979(7) 0.4261(6) 0.8857(7) 0.032(3) Uani 1 1 d . . . H123 H 1.0412 0.4373 0.9003 0.038 Uiso 1 1 calc R . . C124 C 1.0059(7) 0.3747(6) 0.8272(7) 0.040(3) Uani 1 1 d . . . H124 H 1.0531 0.3533 0.7989 0.048 Uiso 1 1 calc R . . C125 C 0.9424(7) 0.3545(6) 0.8100(7) 0.038(3) Uani 1 1 d . . . H125 H 0.9480 0.3179 0.7722 0.045 Uiso 1 1 calc R . . C126 C 0.8704(6) 0.3897(5) 0.8501(6) 0.026(3) Uani 1 1 d . . . H126 H 0.8287 0.3758 0.8373 0.032 Uiso 1 1 calc R . . C127 C 0.3623(8) 0.3162(7) 0.1552(9) 0.071(4) Uani 1 1 d . . . H12A H 0.4013 0.3245 0.1906 0.086 Uiso 1 1 calc R . . H12B H 0.3451 0.3504 0.1214 0.086 Uiso 1 1 calc R . . C128 C 0.3779(9) 0.1222(8) 0.6636(10) 0.093(6) Uani 1 1 d . . . H12C H 0.4008 0.0761 0.6716 0.112 Uiso 1 1 calc R . . H12D H 0.3568 0.1232 0.6109 0.112 Uiso 1 1 calc R . . C129 C 0.7643(9) 0.3388(8) 0.5932(9) 0.087(5) Uani 1 1 d . . . H12E H 0.8067 0.3269 0.5551 0.105 Uiso 1 1 calc R . . H12F H 0.7437 0.3866 0.6079 0.105 Uiso 1 1 calc R . . C130 C 0.0709(14) 0.2131(11) 0.6073(10) 0.147(9) Uani 1 1 d D . . H13A H 0.0990 0.2107 0.6566 0.177 Uiso 1 1 calc R . . H13B H 0.0405 0.2596 0.6047 0.177 Uiso 1 1 calc R . . C131 C 0.1303(17) 0.1863(18) 0.5410(16) 0.28(2) Uani 1 1 d D . . H13C H 0.1730 0.1474 0.5545 0.340 Uiso 1 1 calc R . . H13D H 0.1523 0.2193 0.5361 0.340 Uiso 1 1 calc R . . C132 C 0.0980(18) 0.1674(17) 0.4600(11) 0.243(19) Uani 1 1 d D . . H13E H 0.0709 0.2075 0.4372 0.291 Uiso 1 1 calc R . . H13F H 0.1423 0.1394 0.4256 0.291 Uiso 1 1 calc R . . C133 C 0.0451(13) 0.1335(12) 0.4615(13) 0.177(12) Uani 1 1 d D . . H13G H 0.0763 0.0870 0.4631 0.213 Uiso 1 1 calc R . . H13H H 0.0165 0.1362 0.4125 0.213 Uiso 1 1 calc R . . C134 C -0.0153(14) 0.1589(19) 0.5297(15) 0.27(2) Uani 1 1 d D . . H13I H -0.0595 0.1970 0.5164 0.325 Uiso 1 1 calc R . . H13J H -0.0351 0.1246 0.5346 0.325 Uiso 1 1 calc R . . C135 C 0.0154(15) 0.1786(18) 0.6083(11) 0.240(19) Uani 1 1 d D . . H13K H -0.0293 0.2072 0.6418 0.288 Uiso 1 1 calc R . . H13L H 0.0417 0.1389 0.6321 0.288 Uiso 1 1 calc R . . C136 C 0.2330(17) -0.1312(11) -0.1256(19) 0.204(18) Uani 1 1 d D . . H13M H 0.1956 -0.1530 -0.1359 0.245 Uiso 1 1 calc R . . H13N H 0.2097 -0.0886 -0.1438 0.245 Uiso 1 1 calc R . . C137 C 0.2432(15) -0.1190(11) -0.037(2) 0.179(12) Uani 1 1 d D . . H13O H 0.2380 -0.0731 -0.0225 0.215 Uiso 1 1 calc R . . H13P H 0.1992 -0.1233 -0.0119 0.215 Uiso 1 1 calc R . . C138 C 0.3132(17) -0.159(2) -0.0020(10) 0.25(2) Uani 1 1 d D . . H13Q H 0.2972 -0.1818 0.0332 0.299 Uiso 1 1 calc R . . H13R H 0.3325 -0.1282 0.0309 0.299 Uiso 1 1 calc R . . C139 C 0.3814(15) -0.2082(12) -0.0467(16) 0.184(13) Uani 1 1 d D . . H13S H 0.3914 -0.2508 -0.0302 0.220 Uiso 1 1 calc R . . H13T H 0.4270 -0.1968 -0.0324 0.220 Uiso 1 1 calc R . . C140 C 0.3757(14) -0.2170(11) -0.1372(16) 0.157(10) Uani 1 1 d D . . H14A H 0.4218 -0.2130 -0.1580 0.189 Uiso 1 1 calc R . . H14B H 0.3790 -0.2620 -0.1553 0.189 Uiso 1 1 calc R . . C141 C 0.3049(17) -0.171(2) -0.1728(13) 0.24(2) Uani 1 1 d D . . H14C H 0.3213 -0.1406 -0.1952 0.290 Uiso 1 1 calc R . . H14D H 0.2898 -0.1976 -0.2163 0.290 Uiso 1 1 calc R . . B1 B 0.2782(8) 0.4631(6) 0.5227(7) 0.032(3) Uani 1 1 d . . . B2 B 0.7757(8) 0.4793(6) 0.9576(7) 0.029(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0357(10) 0.0321(10) 0.0306(10) -0.0018(8) -0.0081(7) -0.0106(8) Co2 0.0334(10) 0.0226(10) 0.0281(9) 0.0038(7) -0.0098(7) -0.0086(8) Cl1 0.123(5) 0.110(5) 0.154(5) -0.036(4) 0.028(4) 0.006(4) Cl2 0.085(3) 0.117(4) 0.072(3) 0.018(3) 0.000(2) -0.050(3) Cl3 0.082(3) 0.061(3) 0.094(3) -0.004(2) 0.005(2) -0.026(2) Cl4 0.085(3) 0.076(3) 0.075(3) 0.012(2) -0.019(2) -0.049(2) Cl5 0.076(3) 0.084(3) 0.062(2) 0.023(2) -0.018(2) -0.053(2) Cl6 0.127(4) 0.114(4) 0.068(3) 0.038(3) -0.046(3) -0.087(3) O1 0.038(5) 0.038(5) 0.040(5) 0.002(4) -0.003(4) -0.023(4) O2 0.037(5) 0.023(5) 0.031(5) 0.002(4) -0.001(4) -0.005(4) N1 0.015(6) 0.047(7) 0.036(6) -0.007(5) -0.002(5) -0.005(6) N2 0.055(7) 0.031(7) 0.022(6) 0.006(5) -0.016(5) -0.015(6) N3 0.026(6) 0.051(7) 0.022(6) -0.008(5) -0.008(5) -0.010(5) N4 0.027(6) 0.033(7) 0.025(6) 0.011(5) -0.011(5) -0.008(5) N5 0.047(7) 0.026(7) 0.031(6) 0.009(5) -0.014(5) -0.018(6) N6 0.037(6) 0.029(7) 0.043(7) 0.009(5) -0.015(5) -0.020(5) C1 0.023(7) 0.046(9) 0.049(9) -0.007(7) -0.009(7) -0.009(7) C2 0.052(9) 0.036(8) 0.039(8) -0.006(6) -0.010(7) -0.017(7) C3 0.022(7) 0.052(10) 0.047(8) 0.001(7) 0.000(6) -0.019(7) C4 0.030(7) 0.043(8) 0.034(8) 0.001(6) -0.014(6) -0.008(6) C5 0.040(8) 0.018(7) 0.046(8) 0.001(6) -0.005(7) 0.001(6) C6 0.038(8) 0.033(8) 0.046(8) 0.004(6) -0.013(6) -0.009(6) C7 0.042(9) 0.035(9) 0.037(8) -0.003(6) 0.000(7) -0.010(8) C8 0.051(9) 0.029(9) 0.036(8) -0.008(6) -0.009(7) -0.013(8) C9 0.030(8) 0.045(9) 0.030(7) -0.001(6) -0.010(6) -0.006(7) C10 0.034(8) 0.051(10) 0.031(7) 0.001(7) -0.011(6) -0.020(7) C11 0.051(9) 0.044(10) 0.062(10) 0.001(8) -0.012(7) -0.017(8) C12 0.074(11) 0.045(11) 0.073(11) 0.009(8) -0.005(9) -0.027(10) C13 0.070(11) 0.044(11) 0.068(11) 0.028(9) -0.001(9) 0.000(8) C14 0.046(10) 0.081(13) 0.054(10) 0.023(10) -0.019(7) -0.018(10) C15 0.040(8) 0.032(9) 0.063(9) 0.005(7) -0.016(7) -0.020(7) C16 0.044(9) 0.051(10) 0.040(8) 0.002(7) -0.008(7) -0.013(8) C17 0.055(9) 0.062(11) 0.050(9) 0.004(8) -0.002(7) -0.018(9) C18 0.042(9) 0.123(16) 0.052(10) 0.019(10) -0.002(7) -0.040(10) C19 0.070(11) 0.054(11) 0.085(12) 0.012(10) -0.007(10) -0.041(10) C20 0.070(12) 0.098(15) 0.099(13) 0.014(11) 0.017(10) -0.053(11) C21 0.084(14) 0.094(16) 0.124(17) 0.027(13) 0.029(12) -0.039(13) C22 0.071(13) 0.093(15) 0.135(17) 0.029(14) -0.030(12) -0.043(12) C23 0.093(13) 0.053(12) 0.078(11) 0.026(9) -0.015(10) -0.035(10) C24 0.051(10) 0.083(13) 0.064(11) 0.026(10) -0.013(8) -0.023(10) C25 0.011(6) 0.031(8) 0.041(9) 0.012(7) -0.003(6) 0.005(6) C26 0.044(8) 0.031(8) 0.027(8) 0.009(6) -0.018(6) -0.022(7) C27 0.051(9) 0.036(9) 0.047(10) 0.009(7) -0.021(7) -0.023(7) C28 0.036(8) 0.036(9) 0.052(10) 0.004(8) -0.002(7) -0.014(7) C29 0.064(10) 0.071(11) 0.016(8) -0.012(7) 0.001(7) -0.028(8) C30 0.121(15) 0.118(17) 0.020(9) -0.028(11) 0.006(10) -0.066(14) C31 0.099(13) 0.058(11) 0.051(12) -0.020(9) 0.017(9) -0.045(10) C32 0.075(11) 0.031(10) 0.078(13) -0.006(8) 0.010(9) -0.025(8) C33 0.064(9) 0.039(9) 0.039(8) -0.009(8) 0.009(7) -0.026(8) C34 0.032(8) 0.041(9) 0.023(7) -0.002(6) -0.009(6) -0.012(7) C35 0.051(9) 0.029(9) 0.043(8) 0.003(7) -0.010(7) -0.009(8) C36 0.055(11) 0.039(9) 0.067(10) -0.012(8) -0.012(9) -0.009(9) C37 0.062(10) 0.055(12) 0.054(10) -0.024(8) 0.008(8) -0.011(10) C38 0.038(9) 0.058(11) 0.051(9) -0.008(8) 0.008(7) -0.016(8) C39 0.055(10) 0.040(8) 0.033(8) 0.004(7) -0.016(7) -0.017(8) C40 0.058(9) 0.027(8) 0.032(8) 0.004(6) -0.012(6) -0.026(7) C41 0.038(8) 0.039(8) 0.017(6) -0.005(5) -0.004(6) -0.013(6) C42 0.029(7) 0.021(8) 0.041(8) -0.002(6) -0.003(6) -0.007(6) C43 0.042(8) 0.032(8) 0.041(8) 0.010(6) -0.016(6) -0.013(6) C44 0.053(9) 0.034(8) 0.019(7) 0.009(6) -0.009(6) -0.016(7) C45 0.056(8) 0.034(8) 0.036(8) 0.006(6) -0.018(6) -0.025(7) C46 0.042(8) 0.034(9) 0.028(7) 0.003(6) -0.006(7) -0.022(7) C47 0.024(7) 0.027(8) 0.030(7) 0.001(6) -0.003(6) -0.004(6) C48 0.038(8) 0.026(8) 0.038(8) 0.010(6) -0.014(7) -0.009(7) C49 0.052(9) 0.050(10) 0.022(7) 0.013(7) -0.020(6) -0.029(8) C50 0.062(10) 0.038(10) 0.060(9) 0.013(7) -0.040(7) -0.015(9) C51 0.064(10) 0.038(10) 0.060(10) 0.015(7) -0.031(8) -0.002(8) C52 0.062(11) 0.042(10) 0.069(10) 0.039(9) -0.010(9) 0.002(8) C53 0.037(9) 0.048(11) 0.098(12) 0.048(10) -0.035(8) -0.011(9) C54 0.065(10) 0.057(11) 0.070(10) 0.035(8) -0.051(9) -0.034(9) C55 0.044(8) 0.025(8) 0.026(7) 0.001(6) -0.014(6) -0.005(7) C56 0.023(7) 0.028(8) 0.047(8) -0.002(6) -0.001(6) -0.001(6) C57 0.030(7) 0.044(9) 0.043(8) -0.002(6) 0.004(6) -0.019(7) C58 0.050(9) 0.033(9) 0.049(9) 0.004(7) -0.007(7) -0.019(8) C59 0.067(10) 0.056(11) 0.055(9) 0.003(7) 0.013(8) -0.039(8) C60 0.086(12) 0.075(12) 0.062(10) -0.006(10) 0.015(9) -0.061(11) C61 0.088(12) 0.057(12) 0.071(11) 0.014(9) -0.014(10) -0.049(11) C62 0.097(13) 0.051(12) 0.079(12) -0.018(9) 0.028(10) -0.033(10) C63 0.089(12) 0.050(11) 0.071(11) 0.013(9) 0.018(9) -0.035(10) C64 0.053(8) 0.040(9) 0.011(7) 0.012(6) -0.015(6) -0.023(7) C65 0.045(8) 0.012(7) 0.042(9) 0.004(6) -0.011(6) -0.010(6) C66 0.059(8) 0.036(8) 0.006(7) 0.002(6) -0.006(6) -0.017(7) C67 0.048(9) 0.053(10) 0.028(8) 0.007(8) -0.009(6) -0.020(8) C68 0.097(12) 0.046(10) 0.035(9) -0.001(8) -0.010(8) -0.015(9) C69 0.137(15) 0.059(12) 0.017(8) -0.013(8) -0.017(9) -0.018(11) C70 0.099(13) 0.034(10) 0.063(12) -0.011(8) 0.005(10) -0.020(9) C71 0.062(10) 0.067(12) 0.043(10) 0.017(8) -0.020(8) -0.013(9) C72 0.043(8) 0.024(8) 0.040(8) -0.014(7) -0.008(7) 0.006(7) C73 0.049(9) 0.024(8) 0.017(7) 0.004(6) -0.024(6) -0.018(7) C74 0.047(9) 0.030(9) 0.053(9) 0.000(7) -0.007(7) -0.014(8) C75 0.067(11) 0.008(8) 0.067(10) 0.009(7) -0.012(8) 0.008(8) C76 0.062(12) 0.043(11) 0.052(10) 0.007(8) 0.005(8) 0.018(9) C77 0.043(9) 0.071(12) 0.024(8) 0.006(7) -0.005(7) -0.002(9) C78 0.029(8) 0.065(10) 0.029(7) 0.002(7) -0.014(6) -0.025(8) C79 0.020(7) 0.035(8) 0.024(7) -0.007(6) -0.006(5) -0.011(6) C80 0.045(9) 0.028(8) 0.025(7) -0.003(6) 0.002(6) -0.011(7) C81 0.040(8) 0.053(9) 0.043(8) -0.013(7) 0.005(7) -0.025(8) C82 0.071(11) 0.041(9) 0.052(9) 0.001(7) -0.008(8) -0.032(9) C83 0.056(10) 0.061(10) 0.032(8) 0.003(7) -0.011(7) -0.032(8) C84 0.043(8) 0.037(8) 0.029(7) -0.008(6) -0.002(6) -0.013(7) C85 0.033(8) 0.041(8) 0.021(7) 0.005(6) -0.012(6) -0.020(6) C86 0.037(8) 0.034(8) 0.035(8) 0.003(7) -0.010(7) -0.012(7) C87 0.058(10) 0.042(9) 0.036(8) -0.009(7) -0.004(7) -0.025(8) C88 0.031(8) 0.067(10) 0.044(9) 0.006(8) 0.003(6) -0.017(8) C89 0.036(9) 0.048(9) 0.057(9) -0.009(8) -0.004(7) -0.016(7) C90 0.043(9) 0.045(9) 0.042(8) -0.002(7) -0.006(7) -0.023(8) C91 0.017(7) 0.033(8) 0.041(9) 0.006(6) 0.000(5) -0.004(6) C92 0.030(7) 0.028(7) 0.035(8) 0.008(6) -0.009(6) -0.007(6) C93 0.039(8) 0.045(9) 0.035(8) 0.012(7) -0.008(6) -0.014(7) C94 0.044(8) 0.035(8) 0.040(9) -0.008(6) -0.004(6) -0.019(7) C95 0.036(8) 0.032(8) 0.044(9) 0.010(7) -0.002(6) -0.017(6) C96 0.039(8) 0.030(8) 0.047(8) 0.000(7) 0.003(6) -0.017(7) C97 0.036(8) 0.033(8) 0.022(7) 0.004(6) 0.000(6) -0.018(7) C98 0.038(8) 0.035(8) 0.027(8) -0.007(6) 0.000(6) -0.018(7) C99 0.043(8) 0.046(9) 0.020(7) 0.016(7) -0.014(7) -0.018(7) C100 0.039(9) 0.040(9) 0.037(9) 0.016(7) -0.018(7) -0.025(7) C101 0.040(8) 0.037(8) 0.038(9) 0.007(7) -0.009(7) -0.002(7) C102 0.035(8) 0.063(9) 0.022(7) 0.011(7) -0.009(7) -0.023(8) C103 0.032(8) 0.028(7) 0.026(8) 0.001(5) 0.004(6) -0.012(6) C104 0.032(8) 0.055(9) 0.042(9) 0.011(7) -0.006(7) -0.014(7) C105 0.056(10) 0.054(9) 0.029(7) 0.011(7) -0.020(8) -0.033(8) C106 0.022(8) 0.040(8) 0.067(11) 0.014(7) -0.011(7) -0.014(7) C107 0.037(9) 0.051(9) 0.040(9) -0.006(7) 0.004(7) -0.004(7) C108 0.042(9) 0.040(8) 0.028(7) -0.013(6) -0.006(7) -0.019(7) C109 0.049(8) 0.039(8) 0.018(7) 0.001(6) -0.010(6) -0.035(7) C110 0.048(8) 0.032(8) 0.016(6) -0.001(6) -0.005(6) -0.018(7) C111 0.083(12) 0.050(10) 0.040(8) -0.009(8) 0.002(8) -0.046(9) C112 0.082(12) 0.048(10) 0.030(8) 0.005(7) -0.004(8) -0.032(9) C113 0.055(9) 0.036(8) 0.017(7) 0.001(6) -0.006(6) -0.012(7) C114 0.053(9) 0.045(8) 0.015(7) 0.006(6) -0.013(6) -0.025(7) C115 0.050(8) 0.038(8) 0.034(8) 0.005(6) -0.005(6) -0.022(7) C116 0.030(7) 0.040(8) 0.034(8) -0.001(7) 0.003(6) -0.009(6) C117 0.037(8) 0.046(9) 0.038(8) -0.016(8) -0.007(6) -0.020(7) C118 0.033(8) 0.039(10) 0.092(14) -0.030(9) 0.007(8) -0.015(7) C119 0.052(9) 0.052(10) 0.061(11) -0.002(8) -0.002(8) -0.028(8) C120 0.053(9) 0.051(10) 0.037(8) 0.002(8) -0.013(6) -0.027(7) C121 0.044(8) 0.023(7) 0.027(7) 0.007(6) -0.002(6) -0.013(6) C122 0.038(8) 0.037(8) 0.028(7) 0.005(6) -0.005(6) -0.019(7) C123 0.042(9) 0.028(8) 0.033(7) 0.014(6) -0.012(6) -0.019(7) C124 0.044(9) 0.035(8) 0.029(8) 0.015(7) -0.003(6) 0.003(7) C125 0.048(9) 0.035(8) 0.032(7) 0.015(6) -0.015(7) -0.014(8) C126 0.027(8) 0.026(7) 0.027(7) 0.009(6) -0.007(6) -0.009(6) C127 0.067(10) 0.062(11) 0.094(12) 0.019(9) -0.012(9) -0.032(9) C128 0.104(14) 0.065(12) 0.127(15) -0.011(10) 0.023(11) -0.055(11) C129 0.093(12) 0.109(14) 0.098(13) 0.054(11) -0.057(10) -0.073(11) C130 0.17(2) 0.15(2) 0.110(18) 0.005(15) 0.026(17) -0.046(19) C131 0.27(4) 0.40(5) 0.23(3) -0.22(3) 0.13(3) -0.27(4) C132 0.39(5) 0.39(5) 0.090(18) -0.06(2) 0.06(2) -0.33(4) C133 0.12(2) 0.14(2) 0.20(3) -0.07(2) -0.04(2) -0.020(17) C134 0.11(2) 0.56(7) 0.14(2) -0.07(3) 0.020(19) -0.18(3) C135 0.24(3) 0.51(6) 0.12(2) 0.12(3) -0.08(2) -0.29(4) C136 0.30(5) 0.073(18) 0.20(3) 0.026(19) -0.14(3) -0.04(2) C137 0.17(3) 0.10(2) 0.28(4) 0.01(2) 0.02(3) -0.07(2) C138 0.17(3) 0.43(6) 0.047(15) -0.03(2) 0.019(17) -0.01(3) C139 0.23(3) 0.17(3) 0.14(2) -0.03(2) -0.08(2) -0.09(2) C140 0.14(2) 0.13(2) 0.21(3) -0.05(2) 0.05(2) -0.074(19) C141 0.14(3) 0.49(7) 0.15(3) 0.14(4) -0.03(2) -0.15(4) B1 0.042(9) 0.027(8) 0.027(8) 0.000(7) -0.008(7) -0.016(7) B2 0.045(9) 0.038(9) 0.016(7) 0.002(6) -0.017(7) -0.030(8) _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 O1 1.888(8) . ? Co1 N2 1.984(10) . ? Co1 N3 2.012(9) . ? Co1 N1 2.018(9) . ? Co2 O2 1.853(7) . ? Co2 N4 2.008(9) . ? Co2 N6 2.010(9) . ? Co2 N5 2.012(10) . ? Cl1 C127 1.735(15) . ? Cl2 C127 1.717(14) . ? Cl3 C128 1.742(15) . ? Cl4 C128 1.719(15) . ? Cl5 C129 1.761(14) . ? Cl6 C129 1.730(14) . ? O1 C34 1.308(13) . ? O2 C73 1.334(13) . ? N1 C7 1.286(14) . ? N1 C1 1.467(14) . ? N2 C16 1.312(15) . ? N2 C3 1.485(14) . ? N3 C25 1.294(13) . ? N3 C5 1.508(14) . ? N4 C46 1.290(13) . ? N4 C40 1.476(13) . ? N5 C55 1.278(14) . ? N5 C42 1.484(13) . ? N6 C64 1.290(13) . ? N6 C44 1.494(14) . ? C1 C2 1.532(15) . ? C1 C6 1.533(15) . ? C2 C3 1.541(15) . ? C3 C4 1.534(15) . ? C4 C5 1.540(15) . ? C5 C6 1.515(15) . ? C7 C8 1.410(16) . ? C8 C9 1.314(15) . ? C9 C10 1.482(16) . ? C10 C15 1.388(15) . ? C10 C11 1.402(16) . ? C11 C12 1.340(17) . ? C12 C13 1.392(19) . ? C13 C14 1.382(19) . ? C14 C15 1.377(17) . ? C16 C17 1.469(17) . ? C17 C18 1.390(18) . ? C18 C19 1.45(2) . ? C19 C20 1.371(19) . ? C19 C24 1.431(19) . ? C20 C21 1.40(2) . ? C21 C22 1.40(2) . ? C22 C23 1.38(2) . ? C23 C24 1.376(19) . ? C25 C26 1.410(15) . ? C26 C27 1.351(15) . ? C27 C28 1.507(16) . ? C28 C29 1.394(16) . ? C28 C33 1.397(16) . ? C29 C30 1.38(2) . ? C30 C31 1.35(2) . ? C31 C32 1.379(18) . ? C32 C33 1.382(16) . ? C34 C39 1.409(16) . ? C34 C35 1.424(16) . ? C35 C36 1.373(17) . ? C36 C37 1.373(18) . ? C37 C38 1.397(18) . ? C38 C39 1.346(16) . ? C40 C41 1.515(15) . ? C40 C45 1.537(14) . ? C41 C42 1.542(14) . ? C42 C43 1.512(15) . ? C43 C44 1.540(15) . ? C44 C45 1.538(15) . ? C46 C47 1.424(15) . ? C47 C48 1.336(14) . ? C48 C49 1.450(15) . ? C49 C54 1.394(16) . ? C49 C50 1.415(16) . ? C50 C51 1.356(16) . ? C51 C52 1.400(18) . ? C52 C53 1.388(18) . ? C53 C54 1.321(17) . ? C55 C56 1.461(16) . ? C56 C57 1.305(15) . ? C57 C58 1.480(16) . ? C58 C59 1.372(16) . ? C58 C63 1.375(17) . ? C59 C60 1.387(18) . ? C60 C61 1.381(19) . ? C61 C62 1.374(19) . ? C62 C63 1.364(18) . ? C64 C65 1.428(15) . ? C65 C66 1.345(14) . ? C66 C67 1.438(16) . ? C67 C72 1.366(16) . ? C67 C68 1.402(16) . ? C68 C69 1.388(18) . ? C69 C70 1.356(18) . ? C70 C71 1.390(18) . ? C71 C72 1.389(16) . ? C73 C74 1.392(15) . ? C73 C78 1.404(15) . ? C74 C75 1.388(16) . ? C75 C76 1.372(18) . ? C76 C77 1.410(19) . ? C77 C78 1.385(16) . ? C79 C80 1.381(15) . ? C79 C84 1.403(15) . ? C79 B1 1.670(17) . ? C80 C81 1.380(16) . ? C81 C82 1.408(17) . ? C82 C83 1.365(17) . ? C83 C84 1.406(16) . ? C85 C90 1.387(15) . ? C85 C86 1.398(15) . ? C85 B1 1.649(17) . ? C86 C87 1.393(16) . ? C87 C88 1.353(16) . ? C88 C89 1.391(16) . ? C89 C90 1.364(16) . ? C91 C92 1.398(14) . ? C91 C96 1.404(15) . ? C91 B1 1.632(17) . ? C92 C93 1.440(15) . ? C93 C94 1.359(15) . ? C94 C95 1.368(15) . ? C95 C96 1.397(15) . ? C97 C98 1.403(14) . ? C97 C102 1.420(15) . ? C97 B1 1.651(17) . ? C98 C99 1.396(15) . ? C99 C100 1.364(15) . ? C100 C101 1.385(15) . ? C101 C102 1.367(15) . ? C103 C108 1.362(14) . ? C103 C104 1.419(15) . ? C103 B2 1.687(17) . ? C104 C105 1.390(15) . ? C105 C106 1.382(15) . ? C106 C107 1.394(16) . ? C107 C108 1.398(16) . ? C109 C114 1.383(15) . ? C109 C110 1.404(15) . ? C109 B2 1.639(17) . ? C110 C111 1.405(16) . ? C111 C112 1.411(18) . ? C112 C113 1.359(16) . ? C113 C114 1.398(15) . ? C115 C116 1.406(15) . ? C115 C120 1.438(16) . ? C115 B2 1.644(17) . ? C116 C117 1.428(16) . ? C117 C118 1.369(17) . ? C118 C119 1.372(18) . ? C119 C120 1.377(17) . ? C121 C126 1.414(14) . ? C121 C122 1.417(15) . ? C121 B2 1.608(17) . ? C122 C123 1.415(15) . ? C123 C124 1.360(15) . ? C124 C125 1.400(16) . ? C125 C126 1.399(15) . ? C130 C135 1.48(3) . ? C130 C131 1.50(2) . ? C131 C132 1.55(3) . ? C132 C133 1.43(3) . ? C133 C134 1.54(3) . ? C134 C135 1.50(3) . ? C136 C141 1.47(3) . ? C136 C137 1.53(3) . ? C137 C138 1.42(3) . ? C138 C139 1.46(3) . ? C139 C140 1.54(3) . ? C140 C141 1.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N2 115.4(4) . . ? O1 Co1 N3 122.6(4) . . ? N2 Co1 N3 96.6(4) . . ? O1 Co1 N1 124.0(4) . . ? N2 Co1 N1 94.5(4) . . ? N3 Co1 N1 97.4(4) . . ? O2 Co2 N4 125.6(3) . . ? O2 Co2 N6 122.2(4) . . ? N4 Co2 N6 98.7(4) . . ? O2 Co2 N5 114.2(4) . . ? N4 Co2 N5 93.6(4) . . ? N6 Co2 N5 95.2(4) . . ? C34 O1 Co1 126.0(7) . . ? C73 O2 Co2 131.4(7) . . ? C7 N1 C1 119.1(10) . . ? C7 N1 Co1 128.2(8) . . ? C1 N1 Co1 112.0(7) . . ? C16 N2 C3 114.0(10) . . ? C16 N2 Co1 132.5(9) . . ? C3 N2 Co1 113.0(7) . . ? C25 N3 C5 119.2(9) . . ? C25 N3 Co1 129.7(8) . . ? C5 N3 Co1 110.9(7) . . ? C46 N4 C40 118.4(9) . . ? C46 N4 Co2 129.3(8) . . ? C40 N4 Co2 111.6(7) . . ? C55 N5 C42 118.3(10) . . ? C55 N5 Co2 128.7(8) . . ? C42 N5 Co2 113.0(7) . . ? C64 N6 C44 119.0(9) . . ? C64 N6 Co2 130.4(8) . . ? C44 N6 Co2 110.6(7) . . ? N1 C1 C2 109.1(10) . . ? N1 C1 C6 111.7(9) . . ? C2 C1 C6 110.8(9) . . ? C1 C2 C3 115.1(9) . . ? N2 C3 C4 109.9(9) . . ? N2 C3 C2 110.3(9) . . ? C4 C3 C2 109.5(10) . . ? C3 C4 C5 115.6(9) . . ? N3 C5 C6 110.5(9) . . ? N3 C5 C4 109.0(9) . . ? C6 C5 C4 111.5(9) . . ? C5 C6 C1 115.2(10) . . ? N1 C7 C8 125.7(12) . . ? C9 C8 C7 123.1(12) . . ? C8 C9 C10 126.0(12) . . ? C15 C10 C11 117.4(12) . . ? C15 C10 C9 120.5(11) . . ? C11 C10 C9 122.1(11) . . ? C12 C11 C10 122.0(13) . . ? C11 C12 C13 119.4(14) . . ? C14 C13 C12 120.9(13) . . ? C15 C14 C13 118.4(13) . . ? C14 C15 C10 121.9(12) . . ? N2 C16 C17 121.3(12) . . ? C18 C17 C16 121.6(14) . . ? C17 C18 C19 128.1(14) . . ? C20 C19 C24 118.1(15) . . ? C20 C19 C18 119.2(16) . . ? C24 C19 C18 122.5(14) . . ? C19 C20 C21 120.6(16) . . ? C22 C21 C20 119.6(16) . . ? C23 C22 C21 121.3(17) . . ? C24 C23 C22 118.4(16) . . ? C23 C24 C19 121.9(14) . . ? N3 C25 C26 123.2(10) . . ? C27 C26 C25 121.4(11) . . ? C26 C27 C28 126.6(11) . . ? C29 C28 C33 119.9(12) . . ? C29 C28 C27 119.2(12) . . ? C33 C28 C27 120.9(11) . . ? C30 C29 C28 118.8(13) . . ? C31 C30 C29 121.3(13) . . ? C30 C31 C32 120.7(14) . . ? C31 C32 C33 119.7(14) . . ? C32 C33 C28 119.6(12) . . ? O1 C34 C39 126.2(11) . . ? O1 C34 C35 118.7(11) . . ? C39 C34 C35 115.0(11) . . ? C36 C35 C34 120.8(12) . . ? C35 C36 C37 122.2(13) . . ? C36 C37 C38 118.0(13) . . ? C39 C38 C37 120.5(13) . . ? C38 C39 C34 123.6(12) . . ? N4 C40 C41 110.8(9) . . ? N4 C40 C45 111.1(9) . . ? C41 C40 C45 111.6(9) . . ? C40 C41 C42 113.7(9) . . ? N5 C42 C43 111.2(9) . . ? N5 C42 C41 109.6(9) . . ? C43 C42 C41 110.4(9) . . ? C42 C43 C44 115.0(9) . . ? N6 C44 C45 111.8(9) . . ? N6 C44 C43 110.5(9) . . ? C45 C44 C43 110.0(9) . . ? C40 C45 C44 114.1(9) . . ? N4 C46 C47 124.6(10) . . ? C48 C47 C46 122.6(11) . . ? C47 C48 C49 128.2(11) . . ? C54 C49 C50 115.6(12) . . ? C54 C49 C48 120.7(12) . . ? C50 C49 C48 123.7(11) . . ? C51 C50 C49 123.0(12) . . ? C50 C51 C52 117.4(13) . . ? C53 C52 C51 121.1(12) . . ? C54 C53 C52 119.3(12) . . ? C53 C54 C49 123.5(13) . . ? N5 C55 C56 125.1(11) . . ? C57 C56 C55 122.9(11) . . ? C56 C57 C58 129.9(11) . . ? C59 C58 C63 118.4(12) . . ? C59 C58 C57 120.0(12) . . ? C63 C58 C57 121.6(12) . . ? C58 C59 C60 121.4(13) . . ? C61 C60 C59 118.0(13) . . ? C62 C61 C60 121.2(14) . . ? C63 C62 C61 119.0(14) . . ? C62 C63 C58 121.7(13) . . ? N6 C64 C65 125.0(10) . . ? C66 C65 C64 122.5(10) . . ? C65 C66 C67 127.2(11) . . ? C72 C67 C68 118.6(12) . . ? C72 C67 C66 121.6(11) . . ? C68 C67 C66 119.7(12) . . ? C69 C68 C67 121.7(13) . . ? C70 C69 C68 118.5(12) . . ? C69 C70 C71 120.8(13) . . ? C72 C71 C70 120.3(12) . . ? C67 C72 C71 120.0(12) . . ? O2 C73 C74 119.2(11) . . ? O2 C73 C78 123.1(10) . . ? C74 C73 C78 117.7(11) . . ? C75 C74 C73 120.6(12) . . ? C76 C75 C74 121.9(12) . . ? C75 C76 C77 118.4(12) . . ? C78 C77 C76 119.8(13) . . ? C77 C78 C73 121.6(12) . . ? C80 C79 C84 114.6(10) . . ? C80 C79 B1 125.9(10) . . ? C84 C79 B1 119.5(10) . . ? C81 C80 C79 124.8(11) . . ? C80 C81 C82 119.0(12) . . ? C83 C82 C81 118.6(12) . . ? C82 C83 C84 120.7(12) . . ? C79 C84 C83 122.2(11) . . ? C90 C85 C86 113.8(10) . . ? C90 C85 B1 124.9(10) . . ? C86 C85 B1 121.2(10) . . ? C87 C86 C85 123.5(11) . . ? C88 C87 C86 119.6(12) . . ? C87 C88 C89 119.2(12) . . ? C90 C89 C88 119.7(12) . . ? C89 C90 C85 124.1(12) . . ? C92 C91 C96 115.4(10) . . ? C92 C91 B1 125.3(10) . . ? C96 C91 B1 119.3(10) . . ? C91 C92 C93 122.1(11) . . ? C94 C93 C92 118.5(11) . . ? C93 C94 C95 121.6(11) . . ? C94 C95 C96 119.4(11) . . ? C95 C96 C91 122.8(11) . . ? C98 C97 C102 113.5(10) . . ? C98 C97 B1 127.8(10) . . ? C102 C97 B1 118.7(9) . . ? C99 C98 C97 122.9(11) . . ? C100 C99 C98 120.9(10) . . ? C99 C100 C101 118.4(11) . . ? C102 C101 C100 120.7(11) . . ? C101 C102 C97 123.6(11) . . ? C108 C103 C104 115.9(10) . . ? C108 C103 B2 119.8(10) . . ? C104 C103 B2 124.3(10) . . ? C105 C104 C103 121.8(11) . . ? C106 C105 C104 120.9(11) . . ? C105 C106 C107 117.8(11) . . ? C106 C107 C108 120.3(11) . . ? C103 C108 C107 123.2(11) . . ? C114 C109 C110 114.4(10) . . ? C114 C109 B2 119.9(10) . . ? C110 C109 B2 125.7(11) . . ? C109 C110 C111 122.8(11) . . ? C110 C111 C112 119.8(12) . . ? C113 C112 C111 118.0(12) . . ? C112 C113 C114 120.9(12) . . ? C109 C114 C113 124.0(11) . . ? C116 C115 C120 115.2(11) . . ? C116 C115 B2 125.9(10) . . ? C120 C115 B2 118.9(10) . . ? C115 C116 C117 123.2(11) . . ? C118 C117 C116 117.9(12) . . ? C117 C118 C119 121.0(12) . . ? C118 C119 C120 121.7(13) . . ? C119 C120 C115 120.9(12) . . ? C126 C121 C122 114.4(10) . . ? C126 C121 B2 120.5(10) . . ? C122 C121 B2 124.8(10) . . ? C123 C122 C121 122.2(11) . . ? C124 C123 C122 120.9(11) . . ? C123 C124 C125 119.3(11) . . ? C126 C125 C124 119.6(11) . . ? C125 C126 C121 123.4(10) . . ? Cl2 C127 Cl1 111.9(8) . . ? Cl4 C128 Cl3 115.5(9) . . ? Cl6 C129 Cl5 111.5(8) . . ? C135 C130 C131 115.2(17) . . ? C130 C131 C132 115.3(19) . . ? C133 C132 C131 115.3(19) . . ? C132 C133 C134 116.4(17) . . ? C135 C134 C133 115.3(15) . . ? C130 C135 C134 116.2(17) . . ? C141 C136 C137 116.5(18) . . ? C138 C137 C136 119.7(17) . . ? C137 C138 C139 124.1(17) . . ? C138 C139 C140 117.1(16) . . ? C141 C140 C139 118.2(16) . . ? C136 C141 C140 121.2(18) . . ? C91 B1 C85 111.2(9) . . ? C91 B1 C97 108.1(9) . . ? C85 B1 C97 110.5(9) . . ? C91 B1 C79 109.5(9) . . ? C85 B1 C79 107.6(9) . . ? C97 B1 C79 109.9(9) . . ? C121 B2 C109 106.1(10) . . ? C121 B2 C115 110.6(9) . . ? C109 B2 C115 109.3(9) . . ? C121 B2 C103 114.5(9) . . ? C109 B2 C103 111.2(9) . . ? C115 B2 C103 105.2(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 N2 Co1 O1 C34 -171.8(8) . . . . ? N3 Co1 O1 C34 71.2(9) . . . . ? N1 Co1 O1 C34 -56.7(9) . . . . ? N4 Co2 O2 C73 -68.0(9) . . . . ? N6 Co2 O2 C73 64.2(9) . . . . ? N5 Co2 O2 C73 178.0(8) . . . . ? O1 Co1 N1 C7 -5.5(11) . . . . ? N2 Co1 N1 C7 119.3(10) . . . . ? N3 Co1 N1 C7 -143.4(10) . . . . ? O1 Co1 N1 C1 -176.4(7) . . . . ? N2 Co1 N1 C1 -51.6(7) . . . . ? N3 Co1 N1 C1 45.7(8) . . . . ? O1 Co1 N2 C16 -7.9(11) . . . . ? N3 Co1 N2 C16 123.0(10) . . . . ? N1 Co1 N2 C16 -139.0(10) . . . . ? O1 Co1 N2 C3 -179.4(6) . . . . ? N3 Co1 N2 C3 -48.4(7) . . . . ? N1 Co1 N2 C3 49.5(7) . . . . ? O1 Co1 N3 C25 -11.2(11) . . . . ? N2 Co1 N3 C25 -137.1(10) . . . . ? N1 Co1 N3 C25 127.5(10) . . . . ? O1 Co1 N3 C5 175.1(6) . . . . ? N2 Co1 N3 C5 49.2(7) . . . . ? N1 Co1 N3 C5 -46.2(7) . . . . ? O2 Co2 N4 C46 -3.8(11) . . . . ? N6 Co2 N4 C46 -144.5(9) . . . . ? N5 Co2 N4 C46 119.6(9) . . . . ? O2 Co2 N4 C40 -174.1(6) . . . . ? N6 Co2 N4 C40 45.2(7) . . . . ? N5 Co2 N4 C40 -50.7(7) . . . . ? O2 Co2 N5 C55 0.9(10) . . . . ? N4 Co2 N5 C55 -131.0(9) . . . . ? N6 Co2 N5 C55 129.9(9) . . . . ? O2 Co2 N5 C42 -177.5(6) . . . . ? N4 Co2 N5 C42 50.6(7) . . . . ? N6 Co2 N5 C42 -48.6(7) . . . . ? O2 Co2 N6 C64 -6.1(11) . . . . ? N4 Co2 N6 C64 136.3(10) . . . . ? N5 Co2 N6 C64 -129.2(10) . . . . ? O2 Co2 N6 C44 173.1(6) . . . . ? N4 Co2 N6 C44 -44.4(7) . . . . ? N5 Co2 N6 C44 50.1(7) . . . . ? C7 N1 C1 C2 -107.7(11) . . . . ? Co1 N1 C1 C2 64.1(10) . . . . ? C7 N1 C1 C6 129.4(11) . . . . ? Co1 N1 C1 C6 -58.7(10) . . . . ? N1 C1 C2 C3 -71.6(12) . . . . ? C6 C1 C2 C3 51.7(14) . . . . ? C16 N2 C3 C4 -113.1(10) . . . . ? Co1 N2 C3 C4 60.0(10) . . . . ? C16 N2 C3 C2 126.0(10) . . . . ? Co1 N2 C3 C2 -60.9(10) . . . . ? C1 C2 C3 N2 69.5(13) . . . . ? C1 C2 C3 C4 -51.5(13) . . . . ? N2 C3 C4 C5 -71.3(12) . . . . ? C2 C3 C4 C5 50.1(13) . . . . ? C25 N3 C5 C6 -113.6(11) . . . . ? Co1 N3 C5 C6 60.8(10) . . . . ? C25 N3 C5 C4 123.5(11) . . . . ? Co1 N3 C5 C4 -62.1(10) . . . . ? C3 C4 C5 N3 73.0(12) . . . . ? C3 C4 C5 C6 -49.3(13) . . . . ? N3 C5 C6 C1 -72.7(12) . . . . ? C4 C5 C6 C1 48.7(13) . . . . ? N1 C1 C6 C5 71.9(12) . . . . ? C2 C1 C6 C5 -50.0(13) . . . . ? C1 N1 C7 C8 173.8(10) . . . . ? Co1 N1 C7 C8 3.5(17) . . . . ? N1 C7 C8 C9 -173.9(11) . . . . ? C7 C8 C9 C10 174.8(10) . . . . ? C8 C9 C10 C15 -162.4(12) . . . . ? C8 C9 C10 C11 16.2(18) . . . . ? C15 C10 C11 C12 1.6(19) . . . . ? C9 C10 C11 C12 -177.0(12) . . . . ? C10 C11 C12 C13 -2(2) . . . . ? C11 C12 C13 C14 2(2) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 C10 0.5(19) . . . . ? C11 C10 C15 C14 -0.7(18) . . . . ? C9 C10 C15 C14 177.9(11) . . . . ? C3 N2 C16 C17 172.0(10) . . . . ? Co1 N2 C16 C17 0.6(17) . . . . ? N2 C16 C17 C18 -169.6(12) . . . . ? C16 C17 C18 C19 174.0(13) . . . . ? C17 C18 C19 C20 169.9(14) . . . . ? C17 C18 C19 C24 -15(2) . . . . ? C24 C19 C20 C21 4(2) . . . . ? C18 C19 C20 C21 179.3(15) . . . . ? C19 C20 C21 C22 -4(3) . . . . ? C20 C21 C22 C23 2(3) . . . . ? C21 C22 C23 C24 0(2) . . . . ? C22 C23 C24 C19 -1(2) . . . . ? C20 C19 C24 C23 -1(2) . . . . ? C18 C19 C24 C23 -176.8(13) . . . . ? C5 N3 C25 C26 178.9(10) . . . . ? Co1 N3 C25 C26 5.6(16) . . . . ? N3 C25 C26 C27 -176.0(11) . . . . ? C25 C26 C27 C28 177.1(10) . . . . ? C26 C27 C28 C29 179.3(11) . . . . ? C26 C27 C28 C33 -0.7(18) . . . . ? C33 C28 C29 C30 1.3(18) . . . . ? C27 C28 C29 C30 -178.7(12) . . . . ? C28 C29 C30 C31 -1(2) . . . . ? C29 C30 C31 C32 1(2) . . . . ? C30 C31 C32 C33 -2(2) . . . . ? C31 C32 C33 C28 1.9(19) . . . . ? C29 C28 C33 C32 -1.7(18) . . . . ? C27 C28 C33 C32 178.3(11) . . . . ? Co1 O1 C34 C39 -7.3(15) . . . . ? Co1 O1 C34 C35 171.1(7) . . . . ? O1 C34 C35 C36 179.1(10) . . . . ? C39 C34 C35 C36 -2.3(16) . . . . ? C34 C35 C36 C37 2.2(19) . . . . ? C35 C36 C37 C38 -1(2) . . . . ? C36 C37 C38 C39 -0.3(19) . . . . ? C37 C38 C39 C34 0.0(19) . . . . ? O1 C34 C39 C38 179.7(11) . . . . ? C35 C34 C39 C38 1.2(16) . . . . ? C46 N4 C40 C41 -106.5(11) . . . . ? Co2 N4 C40 C41 64.9(9) . . . . ? C46 N4 C40 C45 128.8(10) . . . . ? Co2 N4 C40 C45 -59.8(10) . . . . ? N4 C40 C41 C42 -72.5(11) . . . . ? C45 C40 C41 C42 52.0(12) . . . . ? C55 N5 C42 C43 -118.8(10) . . . . ? Co2 N5 C42 C43 59.8(10) . . . . ? C55 N5 C42 C41 118.9(10) . . . . ? Co2 N5 C42 C41 -62.5(9) . . . . ? C40 C41 C42 N5 70.4(12) . . . . ? C40 C41 C42 C43 -52.5(12) . . . . ? N5 C42 C43 C44 -69.0(12) . . . . ? C41 C42 C43 C44 52.8(12) . . . . ? C64 N6 C44 C45 -121.4(11) . . . . ? Co2 N6 C44 C45 59.2(10) . . . . ? C64 N6 C44 C43 115.6(10) . . . . ? Co2 N6 C44 C43 -63.7(9) . . . . ? C42 C43 C44 N6 72.0(12) . . . . ? C42 C43 C44 C45 -51.9(12) . . . . ? N4 C40 C45 C44 72.9(12) . . . . ? C41 C40 C45 C44 -51.4(13) . . . . ? N6 C44 C45 C40 -73.0(12) . . . . ? C43 C44 C45 C40 50.2(13) . . . . ? C40 N4 C46 C47 178.5(9) . . . . ? Co2 N4 C46 C47 8.9(16) . . . . ? N4 C46 C47 C48 173.7(11) . . . . ? C46 C47 C48 C49 -171.6(10) . . . . ? C47 C48 C49 C54 168.4(12) . . . . ? C47 C48 C49 C50 -11.4(19) . . . . ? C54 C49 C50 C51 -2.1(19) . . . . ? C48 C49 C50 C51 177.7(12) . . . . ? C49 C50 C51 C52 1(2) . . . . ? C50 C51 C52 C53 -2(2) . . . . ? C51 C52 C53 C54 3(2) . . . . ? C52 C53 C54 C49 -4(2) . . . . ? C50 C49 C54 C53 3(2) . . . . ? C48 C49 C54 C53 -176.5(12) . . . . ? C42 N5 C55 C56 -178.2(9) . . . . ? Co2 N5 C55 C56 3.4(16) . . . . ? N5 C55 C56 C57 170.0(11) . . . . ? C55 C56 C57 C58 -173.7(11) . . . . ? C56 C57 C58 C59 165.5(13) . . . . ? C56 C57 C58 C63 -14(2) . . . . ? C63 C58 C59 C60 5(2) . . . . ? C57 C58 C59 C60 -174.4(12) . . . . ? C58 C59 C60 C61 -4(2) . . . . ? C59 C60 C61 C62 2(2) . . . . ? C60 C61 C62 C63 -1(2) . . . . ? C61 C62 C63 C58 2(2) . . . . ? C59 C58 C63 C62 -4(2) . . . . ? C57 C58 C63 C62 175.4(13) . . . . ? C44 N6 C64 C65 178.2(10) . . . . ? Co2 N6 C64 C65 -2.6(17) . . . . ? N6 C64 C65 C66 176.6(11) . . . . ? C64 C65 C66 C67 178.4(11) . . . . ? C65 C66 C67 C72 -20.7(19) . . . . ? C65 C66 C67 C68 157.2(12) . . . . ? C72 C67 C68 C69 0(2) . . . . ? C66 C67 C68 C69 -177.9(13) . . . . ? C67 C68 C69 C70 2(2) . . . . ? C68 C69 C70 C71 -4(2) . . . . ? C69 C70 C71 C72 4(2) . . . . ? C68 C67 C72 C71 0.5(19) . . . . ? C66 C67 C72 C71 178.4(12) . . . . ? C70 C71 C72 C67 -3(2) . . . . ? Co2 O2 C73 C74 -165.9(8) . . . . ? Co2 O2 C73 C78 11.3(14) . . . . ? O2 C73 C74 C75 -179.3(10) . . . . ? C78 C73 C74 C75 3.4(16) . . . . ? C73 C74 C75 C76 -1.9(19) . . . . ? C74 C75 C76 C77 0(2) . . . . ? C75 C76 C77 C78 0.2(19) . . . . ? C76 C77 C78 C73 1.4(17) . . . . ? O2 C73 C78 C77 179.6(10) . . . . ? C74 C73 C78 C77 -3.2(15) . . . . ? C84 C79 C80 C81 2.9(16) . . . . ? B1 C79 C80 C81 -174.1(10) . . . . ? C79 C80 C81 C82 -0.8(17) . . . . ? C80 C81 C82 C83 -0.3(17) . . . . ? C81 C82 C83 C84 -0.9(18) . . . . ? C80 C79 C84 C83 -4.0(15) . . . . ? B1 C79 C84 C83 173.2(10) . . . . ? C82 C83 C84 C79 3.2(18) . . . . ? C90 C85 C86 C87 1.5(16) . . . . ? B1 C85 C86 C87 178.7(10) . . . . ? C85 C86 C87 C88 -3.2(18) . . . . ? C86 C87 C88 C89 3.6(18) . . . . ? C87 C88 C89 C90 -2.7(19) . . . . ? C88 C89 C90 C85 1.1(19) . . . . ? C86 C85 C90 C89 -0.5(17) . . . . ? B1 C85 C90 C89 -177.5(11) . . . . ? C96 C91 C92 C93 -2.4(15) . . . . ? B1 C91 C92 C93 179.6(10) . . . . ? C91 C92 C93 C94 -1.0(16) . . . . ? C92 C93 C94 C95 2.5(17) . . . . ? C93 C94 C95 C96 -0.6(17) . . . . ? C94 C95 C96 C91 -3.2(17) . . . . ? C92 C91 C96 C95 4.5(16) . . . . ? B1 C91 C96 C95 -177.4(10) . . . . ? C102 C97 C98 C99 -1.2(15) . . . . ? B1 C97 C98 C99 178.0(10) . . . . ? C97 C98 C99 C100 0.6(17) . . . . ? C98 C99 C100 C101 -0.7(17) . . . . ? C99 C100 C101 C102 1.4(17) . . . . ? C100 C101 C102 C97 -2.2(18) . . . . ? C98 C97 C102 C101 2.0(16) . . . . ? B1 C97 C102 C101 -177.3(10) . . . . ? C108 C103 C104 C105 1.8(17) . . . . ? B2 C103 C104 C105 -177.4(10) . . . . ? C103 C104 C105 C106 -4.5(18) . . . . ? C104 C105 C106 C107 4.9(17) . . . . ? C105 C106 C107 C108 -2.7(18) . . . . ? C104 C103 C108 C107 0.4(17) . . . . ? B2 C103 C108 C107 179.6(11) . . . . ? C106 C107 C108 C103 0.1(19) . . . . ? C114 C109 C110 C111 -1.2(15) . . . . ? B2 C109 C110 C111 179.1(10) . . . . ? C109 C110 C111 C112 1.4(17) . . . . ? C110 C111 C112 C113 0.0(17) . . . . ? C111 C112 C113 C114 -1.5(17) . . . . ? C110 C109 C114 C113 -0.3(16) . . . . ? B2 C109 C114 C113 179.4(10) . . . . ? C112 C113 C114 C109 1.7(17) . . . . ? C120 C115 C116 C117 -1.3(16) . . . . ? B2 C115 C116 C117 180.0(10) . . . . ? C115 C116 C117 C118 1.4(17) . . . . ? C116 C117 C118 C119 0.0(18) . . . . ? C117 C118 C119 C120 -1.4(19) . . . . ? C118 C119 C120 C115 1.5(19) . . . . ? C116 C115 C120 C119 -0.2(17) . . . . ? B2 C115 C120 C119 178.7(11) . . . . ? C126 C121 C122 C123 -1.5(15) . . . . ? B2 C121 C122 C123 172.8(10) . . . . ? C121 C122 C123 C124 4.4(16) . . . . ? C122 C123 C124 C125 -5.3(16) . . . . ? C123 C124 C125 C126 3.6(16) . . . . ? C124 C125 C126 C121 -0.9(16) . . . . ? C122 C121 C126 C125 -0.2(15) . . . . ? B2 C121 C126 C125 -174.8(9) . . . . ? C135 C130 C131 C132 41(4) . . . . ? C130 C131 C132 C133 -42(5) . . . . ? C131 C132 C133 C134 41(4) . . . . ? C132 C133 C134 C135 -40(4) . . . . ? C131 C130 C135 C134 -40(4) . . . . ? C133 C134 C135 C130 39(4) . . . . ? C141 C136 C137 C138 -16(5) . . . . ? C136 C137 C138 C139 6(6) . . . . ? C137 C138 C139 C140 0(5) . . . . ? C138 C139 C140 C141 5(4) . . . . ? C137 C136 C141 C140 22(5) . . . . ? C139 C140 C141 C136 -16(5) . . . . ? C92 C91 B1 C85 -112.5(11) . . . . ? C96 C91 B1 C85 69.6(13) . . . . ? C92 C91 B1 C97 126.0(11) . . . . ? C96 C91 B1 C97 -51.9(13) . . . . ? C92 C91 B1 C79 6.3(15) . . . . ? C96 C91 B1 C79 -171.6(9) . . . . ? C90 C85 B1 C91 -14.5(15) . . . . ? C86 C85 B1 C91 168.6(10) . . . . ? C90 C85 B1 C97 105.5(12) . . . . ? C86 C85 B1 C97 -71.3(13) . . . . ? C90 C85 B1 C79 -134.4(11) . . . . ? C86 C85 B1 C79 48.8(13) . . . . ? C98 C97 B1 C91 137.6(11) . . . . ? C102 C97 B1 C91 -43.2(13) . . . . ? C98 C97 B1 C85 15.7(15) . . . . ? C102 C97 B1 C85 -165.1(9) . . . . ? C98 C97 B1 C79 -103.0(12) . . . . ? C102 C97 B1 C79 76.2(12) . . . . ? C80 C79 B1 C91 101.7(12) . . . . ? C84 C79 B1 C91 -75.2(12) . . . . ? C80 C79 B1 C85 -137.4(10) . . . . ? C84 C79 B1 C85 45.8(13) . . . . ? C80 C79 B1 C97 -16.9(14) . . . . ? C84 C79 B1 C97 166.2(9) . . . . ? C126 C121 B2 C109 63.7(12) . . . . ? C122 C121 B2 C109 -110.3(11) . . . . ? C126 C121 B2 C115 -177.9(9) . . . . ? C122 C121 B2 C115 8.2(15) . . . . ? C126 C121 B2 C103 -59.3(13) . . . . ? C122 C121 B2 C103 126.7(11) . . . . ? C114 C109 B2 C121 38.2(13) . . . . ? C110 C109 B2 C121 -142.2(10) . . . . ? C114 C109 B2 C115 -81.1(13) . . . . ? C110 C109 B2 C115 98.5(12) . . . . ? C114 C109 B2 C103 163.2(9) . . . . ? C110 C109 B2 C103 -17.2(15) . . . . ? C116 C115 B2 C121 -116.7(12) . . . . ? C120 C115 B2 C121 64.6(13) . . . . ? C116 C115 B2 C109 -0.2(16) . . . . ? C120 C115 B2 C109 -179.0(10) . . . . ? C116 C115 B2 C103 119.3(12) . . . . ? C120 C115 B2 C103 -59.5(13) . . . . ? C108 C103 B2 C121 -173.6(10) . . . . ? C104 C103 B2 C121 5.6(15) . . . . ? C108 C103 B2 C109 66.2(13) . . . . ? C104 C103 B2 C109 -114.6(12) . . . . ? C108 C103 B2 C115 -52.0(13) . . . . ? C104 C103 B2 C115 127.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.721 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.721 _refine_diff_density_max 0.520 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.101