# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Christopher Kozak' _publ_contact_author_email CKOZAK@MUN.CA _publ_section_title ; Synthesis and Structure of Mono-, Bi- and Trimetallic Amine-bis(phenolate) Cobalt(II) complexes ; loop_ _publ_author_name 'Christopher Kozak' 'Julia Bobak' 'Uttam Kumar Das' 'Louise Dawe' 'Andreas Decken' 'Candace Fowler' 'Sarah E. Hann' ; F.Kerton ; 'Chad F. Petten' # Attachment 'Kozak_Compiled_CIF.cif' data_1CH3COCH3 _database_code_depnum_ccdc_archive 'CCDC 766019' _publ_section_abstract ; Please see full paper. ; # start Validation Reply Form _vrf_PLAT413_1CH3COCH3 ; PROBLEM: Short Inter XH3 .. XHn H58 .. H120 .. 1.86 Ang. RESPONSE: This alert results from H-atoms being introduced in calculated positions, and not from an incorrectly determined structure or inconsistent symmetry data. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C34 H54 O2 N2) Co (C3 H6 O)] (C3 H6 O)0.75' _chemical_formula_sum 'C39.25 H64.50 Co N2 O3.75' _chemical_formula_weight 683.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 23.579(3) _cell_length_b 23.671(3) _cell_length_c 14.476(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8080(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17565 _cell_measurement_theta_min 2.2227 _cell_measurement_theta_max 30.8409 _exptl_crystal_description Irregular _exptl_crystal_colour 'Dark Pink' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_correction_T_min 0.9330 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 67575 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.50 _reflns_number_total 16357 _reflns_number_gt 15568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1043P)^2^+4.2004P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(12) _refine_ls_number_reflns 16357 _refine_ls_number_parameters 848 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _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 0.367384(17) 0.361407(17) 0.49245(3) 0.02579(11) Uani 1 1 d . . . Co2 Co 0.545769(18) 0.107678(17) 0.62674(4) 0.02817(11) Uani 1 1 d . . . O1 O 0.32959(11) 0.35706(10) 0.37498(18) 0.0322(5) Uani 1 1 d . . . O2 O 0.33230(11) 0.40001(9) 0.59566(18) 0.0297(5) Uani 1 1 d . . . O3 O 0.49413(11) 0.07032(10) 0.54133(19) 0.0349(5) Uani 1 1 d . . . O4 O 0.53000(10) 0.17966(10) 0.68376(19) 0.0314(5) Uani 1 1 d . . . O5 O 0.41607(11) 0.43649(10) 0.4488(2) 0.0366(6) Uani 1 1 d . . . O6 O 0.50937(13) 0.07266(13) 0.7510(2) 0.0490(7) Uani 1 1 d . . . O7 O 0.1530(5) 0.5485(4) 0.4645(9) 0.127(6) Uani 0.50 1 d P . . O8 O 0.52823(16) 0.39453(17) 0.1113(3) 0.0689(11) Uani 1 1 d . . . N1 N 0.33580(12) 0.28082(11) 0.5342(2) 0.0264(5) Uani 1 1 d . . . N2 N 0.44783(12) 0.32384(12) 0.5260(2) 0.0299(6) Uani 1 1 d . . . N3 N 0.59358(11) 0.14696(10) 0.5177(2) 0.0251(6) Uani 1 1 d . . . N4 N 0.62604(13) 0.07035(12) 0.6590(2) 0.0338(7) Uani 1 1 d . . . C1 C 0.28589(15) 0.32437(14) 0.3520(2) 0.0279(7) Uani 1 1 d . . . C2 C 0.24177(15) 0.34497(14) 0.2938(2) 0.0286(7) Uani 1 1 d . . . C3 C 0.24147(16) 0.40677(15) 0.2619(3) 0.0352(7) Uani 1 1 d . . . C4 C 0.2418(2) 0.44583(15) 0.3473(3) 0.0456(10) Uani 1 1 d . . . H1 H 0.2220 0.4272 0.3984 0.055 Uiso 1 1 calc R . . H2 H 0.2226 0.4814 0.3322 0.055 Uiso 1 1 calc R . . H3 H 0.2811 0.4537 0.3654 0.055 Uiso 1 1 calc R . . C5 C 0.29314(19) 0.41841(19) 0.2020(3) 0.0451(9) Uani 1 1 d . . . H4 H 0.3049 0.4578 0.2098 0.054 Uiso 1 1 calc R . . H5 H 0.2836 0.4115 0.1371 0.054 Uiso 1 1 calc R . . H6 H 0.3242 0.3934 0.2205 0.054 Uiso 1 1 calc R . . C6 C 0.18877(18) 0.42161(18) 0.2057(3) 0.0434(9) Uani 1 1 d . . . H7 H 0.1590 0.4353 0.2472 0.052 Uiso 1 1 calc R . . H8 H 0.1753 0.3879 0.1731 0.052 Uiso 1 1 calc R . . H9 H 0.1982 0.4511 0.1607 0.052 Uiso 1 1 calc R . . C7 C 0.20015(14) 0.30680(14) 0.2637(3) 0.0292(7) Uani 1 1 d . . . H10 H 0.1721 0.3201 0.2219 0.035 Uiso 1 1 calc R . . C8 C 0.19770(15) 0.25037(14) 0.2917(3) 0.0315(7) Uani 1 1 d . . . C9 C 0.15621(16) 0.20822(15) 0.2472(3) 0.0341(8) Uani 1 1 d . . . C10 C 0.1061(3) 0.2369(2) 0.2027(8) 0.120(4) Uani 1 1 d . . . H11 H 0.0984 0.2727 0.2345 0.144 Uiso 1 1 calc R . . H12 H 0.0728 0.2124 0.2071 0.144 Uiso 1 1 calc R . . H13 H 0.1146 0.2445 0.1376 0.144 Uiso 1 1 calc R . . C11 C 0.1886(2) 0.1753(2) 0.1735(4) 0.0565(12) Uani 1 1 d . . . H14 H 0.2187 0.1992 0.1478 0.068 Uiso 1 1 calc R . . H15 H 0.1625 0.1642 0.1240 0.068 Uiso 1 1 calc R . . H16 H 0.2054 0.1415 0.2012 0.068 Uiso 1 1 calc R . . C12 C 0.1356(3) 0.1642(3) 0.3173(4) 0.081(2) Uani 1 1 d . . . H17 H 0.1272 0.1287 0.2852 0.097 Uiso 1 1 calc R . . H18 H 0.1012 0.1780 0.3479 0.097 Uiso 1 1 calc R . . H19 H 0.1652 0.1577 0.3636 0.097 Uiso 1 1 calc R . . C13 C 0.23822(15) 0.23307(13) 0.3555(3) 0.0311(7) Uani 1 1 d . . . H20 H 0.2364 0.1957 0.3792 0.037 Uiso 1 1 calc R . . C14 C 0.28116(15) 0.26850(13) 0.3858(2) 0.0293(7) Uani 1 1 d . . . C15 C 0.32575(15) 0.24557(13) 0.4504(3) 0.0304(7) Uani 1 1 d . . . H21 H 0.3143 0.2072 0.4703 0.037 Uiso 1 1 calc R . . H22 H 0.3619 0.2420 0.4160 0.037 Uiso 1 1 calc R . . C16 C 0.38080(14) 0.25460(14) 0.5913(3) 0.0313(7) Uani 1 1 d . . . H23 H 0.3731 0.2137 0.5981 0.038 Uiso 1 1 calc R . . H24 H 0.3806 0.2718 0.6537 0.038 Uiso 1 1 calc R . . C17 C 0.43816(15) 0.26296(14) 0.5473(3) 0.0328(7) Uani 1 1 d . . . H25 H 0.4681 0.2493 0.5898 0.039 Uiso 1 1 calc R . . H26 H 0.4405 0.2406 0.4897 0.039 Uiso 1 1 calc R . . C18 C 0.49120(16) 0.32910(16) 0.4534(3) 0.0393(8) Uani 1 1 d . . . H27 H 0.4728 0.3298 0.3927 0.047 Uiso 1 1 calc R . . H28 H 0.5172 0.2968 0.4567 0.047 Uiso 1 1 calc R . . H29 H 0.5125 0.3642 0.4624 0.047 Uiso 1 1 calc R . . C19 C 0.46869(16) 0.35346(15) 0.6099(3) 0.0353(8) Uani 1 1 d . . . H30 H 0.5102 0.3538 0.6098 0.042 Uiso 1 1 calc R . . H31 H 0.4551 0.3337 0.6651 0.042 Uiso 1 1 calc R . . H32 H 0.4545 0.3924 0.6102 0.042 Uiso 1 1 calc R . . C20 C 0.28211(14) 0.28904(14) 0.5853(3) 0.0285(7) Uani 1 1 d . . . H33 H 0.2658 0.2516 0.6002 0.034 Uiso 1 1 calc R . . H34 H 0.2548 0.3091 0.5449 0.034 Uiso 1 1 calc R . . C21 C 0.28941(14) 0.32228(14) 0.6738(2) 0.0283(7) Uani 1 1 d . . . C22 C 0.26912(15) 0.29832(14) 0.7549(3) 0.0309(7) Uani 1 1 d . . . H35 H 0.2523 0.2619 0.7525 0.037 Uiso 1 1 calc R . . C23 C 0.27256(17) 0.32590(16) 0.8393(3) 0.0362(8) Uani 1 1 d . . . C24 C 0.2496(2) 0.30057(18) 0.9297(3) 0.0457(10) Uani 1 1 d . . . C25 C 0.2154(2) 0.2475(2) 0.9127(3) 0.0527(11) Uani 1 1 d . . . H36 H 0.1979 0.2495 0.8513 0.063 Uiso 1 1 calc R . . H37 H 0.1857 0.2443 0.9597 0.063 Uiso 1 1 calc R . . H38 H 0.2404 0.2145 0.9159 0.063 Uiso 1 1 calc R . . C26 C 0.2983(2) 0.2888(2) 0.9958(4) 0.0608(12) Uani 1 1 d . . . H39 H 0.3326 0.2798 0.9604 0.073 Uiso 1 1 calc R . . H40 H 0.2885 0.2567 1.0356 0.073 Uiso 1 1 calc R . . H41 H 0.3053 0.3222 1.0341 0.073 Uiso 1 1 calc R . . C27 C 0.2091(2) 0.3431(2) 0.9766(3) 0.0568(12) Uani 1 1 d . . . H42 H 0.2100 0.3375 1.0436 0.068 Uiso 1 1 calc R . . H43 H 0.1704 0.3372 0.9538 0.068 Uiso 1 1 calc R . . H44 H 0.2212 0.3817 0.9620 0.068 Uiso 1 1 calc R . . C28 C 0.29808(16) 0.37889(16) 0.8393(3) 0.0350(8) Uani 1 1 d . . . H45 H 0.3024 0.3978 0.8968 0.042 Uiso 1 1 calc R . . C29 C 0.31778(15) 0.40601(14) 0.7599(3) 0.0302(7) Uani 1 1 d . . . C30 C 0.34149(16) 0.46671(15) 0.7652(3) 0.0355(8) Uani 1 1 d . . . C31 C 0.3448(2) 0.48880(18) 0.8646(3) 0.0493(10) Uani 1 1 d . . . H46 H 0.3818 0.4791 0.8911 0.059 Uiso 1 1 calc R . . H47 H 0.3146 0.4715 0.9016 0.059 Uiso 1 1 calc R . . H48 H 0.3400 0.5299 0.8646 0.059 Uiso 1 1 calc R . . C32 C 0.30030(18) 0.50560(15) 0.7112(3) 0.0408(9) Uani 1 1 d . . . H49 H 0.2712 0.5201 0.7533 0.049 Uiso 1 1 calc R . . H50 H 0.2821 0.4840 0.6616 0.049 Uiso 1 1 calc R . . H51 H 0.3215 0.5373 0.6846 0.049 Uiso 1 1 calc R . . C33 C 0.40117(17) 0.47055(16) 0.7237(3) 0.0412(9) Uani 1 1 d . . . H52 H 0.4224 0.5007 0.7547 0.049 Uiso 1 1 calc R . . H53 H 0.3984 0.4789 0.6576 0.049 Uiso 1 1 calc R . . H54 H 0.4209 0.4345 0.7324 0.049 Uiso 1 1 calc R . . C34 C 0.31402(14) 0.37655(14) 0.6738(3) 0.0287(7) Uani 1 1 d . . . C35 C 0.47625(15) 0.09448(14) 0.4629(2) 0.0297(7) Uani 1 1 d . . . C36 C 0.41888(16) 0.09043(15) 0.4334(3) 0.0320(7) Uani 1 1 d . . . C37 C 0.37559(15) 0.05479(15) 0.4876(3) 0.0339(7) Uani 1 1 d . . . C38 C 0.36885(17) 0.07860(17) 0.5863(3) 0.0390(8) Uani 1 1 d . . . H55 H 0.3755 0.1195 0.5856 0.047 Uiso 1 1 calc R . . H56 H 0.3964 0.0605 0.6274 0.047 Uiso 1 1 calc R . . H57 H 0.3304 0.0709 0.6087 0.047 Uiso 1 1 calc R . . C39 C 0.39656(18) -0.00681(15) 0.4910(3) 0.0434(9) Uani 1 1 d . . . H58 H 0.4381 -0.0074 0.4888 0.052 Uiso 1 1 calc R . . H59 H 0.3814 -0.0276 0.4379 0.052 Uiso 1 1 calc R . . H60 H 0.3836 -0.0246 0.5483 0.052 Uiso 1 1 calc R . . C40 C 0.31684(18) 0.0535(2) 0.4415(3) 0.0475(10) Uani 1 1 d . . . H61 H 0.2937 0.0847 0.4653 0.057 Uiso 1 1 calc R . . H62 H 0.2982 0.0175 0.4555 0.057 Uiso 1 1 calc R . . H63 H 0.3212 0.0574 0.3745 0.057 Uiso 1 1 calc R . . C41 C 0.40278(15) 0.11854(14) 0.3526(3) 0.0315(7) Uani 1 1 d . . . H64 H 0.3643 0.1161 0.3336 0.038 Uiso 1 1 calc R . . C42 C 0.44006(16) 0.14993(15) 0.2984(3) 0.0309(7) Uani 1 1 d . . . C43 C 0.42166(17) 0.18072(17) 0.2091(3) 0.0378(8) Uani 1 1 d . . . C44 C 0.35861(18) 0.1716(2) 0.1883(3) 0.0486(10) Uani 1 1 d . . . H65 H 0.3378 0.1668 0.2463 0.058 Uiso 1 1 calc R . . H66 H 0.3540 0.1377 0.1502 0.058 Uiso 1 1 calc R . . H67 H 0.3437 0.2044 0.1550 0.058 Uiso 1 1 calc R . . C45 C 0.4561(2) 0.1571(2) 0.1267(4) 0.0517(10) Uani 1 1 d . . . H68 H 0.4658 0.1175 0.1386 0.062 Uiso 1 1 calc R . . H69 H 0.4910 0.1792 0.1193 0.062 Uiso 1 1 calc R . . H70 H 0.4334 0.1597 0.0702 0.062 Uiso 1 1 calc R . . C46 C 0.4327(2) 0.24372(18) 0.2175(3) 0.0520(11) Uani 1 1 d . . . H71 H 0.4410 0.2594 0.1564 0.062 Uiso 1 1 calc R . . H72 H 0.4651 0.2501 0.2586 0.062 Uiso 1 1 calc R . . H73 H 0.3990 0.2623 0.2431 0.062 Uiso 1 1 calc R . . C47 C 0.49709(15) 0.15104(14) 0.3269(3) 0.0296(7) Uani 1 1 d . . . H74 H 0.5241 0.1710 0.2907 0.036 Uiso 1 1 calc R . . C48 C 0.51480(14) 0.12358(13) 0.4068(2) 0.0281(7) Uani 1 1 d . . . C49 C 0.57783(14) 0.12113(14) 0.4282(2) 0.0289(7) Uani 1 1 d . . . H75 H 0.5900 0.0811 0.4283 0.035 Uiso 1 1 calc R . . H76 H 0.5988 0.1407 0.3783 0.035 Uiso 1 1 calc R . . C50 C 0.65426(14) 0.13760(13) 0.5371(3) 0.0299(7) Uani 1 1 d . . . H77 H 0.6679 0.1666 0.5810 0.036 Uiso 1 1 calc R . . H78 H 0.6763 0.1413 0.4792 0.036 Uiso 1 1 calc R . . C51 C 0.66373(15) 0.07933(15) 0.5779(3) 0.0345(7) Uani 1 1 d . . . H79 H 0.6558 0.0502 0.5305 0.041 Uiso 1 1 calc R . . H80 H 0.7038 0.0754 0.5972 0.041 Uiso 1 1 calc R . . C52 C 0.62249(19) 0.00947(16) 0.6791(4) 0.0463(10) Uani 1 1 d . . . H81 H 0.5910 -0.0071 0.6442 0.056 Uiso 1 1 calc R . . H82 H 0.6161 0.0039 0.7454 0.056 Uiso 1 1 calc R . . H83 H 0.6580 -0.0089 0.6611 0.056 Uiso 1 1 calc R . . C53 C 0.64893(18) 0.09948(17) 0.7417(3) 0.0386(8) Uani 1 1 d . . . H84 H 0.6725 0.0731 0.7772 0.046 Uiso 1 1 calc R . . H85 H 0.6175 0.1127 0.7803 0.046 Uiso 1 1 calc R . . H86 H 0.6720 0.1318 0.7224 0.046 Uiso 1 1 calc R . . C54 C 0.58211(14) 0.20875(13) 0.5114(2) 0.0264(7) Uani 1 1 d . . . H87 H 0.5424 0.2142 0.4910 0.032 Uiso 1 1 calc R . . H88 H 0.6070 0.2251 0.4633 0.032 Uiso 1 1 calc R . . C55 C 0.59102(14) 0.24127(13) 0.6003(2) 0.0262(6) Uani 1 1 d . . . C56 C 0.62419(14) 0.29019(14) 0.5959(3) 0.0285(7) Uani 1 1 d . . . H89 H 0.6443 0.2988 0.5408 0.034 Uiso 1 1 calc R . . C57 C 0.62800(15) 0.32644(15) 0.6718(3) 0.0304(7) Uani 1 1 d . . . C58 C 0.66016(17) 0.38286(15) 0.6668(3) 0.0371(8) Uani 1 1 d . . . C59 C 0.6904(3) 0.3917(2) 0.5754(5) 0.083(2) Uani 1 1 d . . . H90 H 0.7287 0.3757 0.5789 0.100 Uiso 1 1 calc R . . H91 H 0.6929 0.4323 0.5622 0.100 Uiso 1 1 calc R . . H92 H 0.6692 0.3729 0.5260 0.100 Uiso 1 1 calc R . . C60 C 0.6186(3) 0.4313(2) 0.6790(7) 0.088(2) Uani 1 1 d . . . H93 H 0.6043 0.4430 0.6184 0.106 Uiso 1 1 calc R . . H94 H 0.6379 0.4632 0.7086 0.106 Uiso 1 1 calc R . . H95 H 0.5869 0.4189 0.7178 0.106 Uiso 1 1 calc R . . C61 C 0.7047(3) 0.3857(3) 0.7426(5) 0.084(2) Uani 1 1 d . . . H96 H 0.7365 0.4093 0.7221 0.101 Uiso 1 1 calc R . . H97 H 0.7185 0.3475 0.7562 0.101 Uiso 1 1 calc R . . H98 H 0.6879 0.4020 0.7984 0.101 Uiso 1 1 calc R . . C62 C 0.59795(16) 0.31121(14) 0.7509(3) 0.0328(7) Uani 1 1 d . . . H99 H 0.6002 0.3356 0.8029 0.039 Uiso 1 1 calc R . . C63 C 0.56486(16) 0.26274(14) 0.7590(3) 0.0316(7) Uani 1 1 d . . . C64 C 0.53108(17) 0.24994(16) 0.8472(3) 0.0362(8) Uani 1 1 d . . . C65 C 0.5404(2) 0.2943(2) 0.9224(3) 0.0511(11) Uani 1 1 d . . . H100 H 0.5483 0.3309 0.8938 0.061 Uiso 1 1 calc R . . H101 H 0.5726 0.2831 0.9611 0.061 Uiso 1 1 calc R . . H102 H 0.5062 0.2971 0.9607 0.061 Uiso 1 1 calc R . . C66 C 0.54807(18) 0.19273(18) 0.8886(3) 0.0418(9) Uani 1 1 d . . . H106 H 0.5879 0.1849 0.8740 0.050 Uiso 1 1 calc R . . H107 H 0.5240 0.1630 0.8626 0.050 Uiso 1 1 calc R . . H108 H 0.5432 0.1939 0.9558 0.050 Uiso 1 1 calc R . . C67 C 0.46714(19) 0.2491(2) 0.8256(3) 0.0481(10) Uani 1 1 d . . . H103 H 0.4515 0.2871 0.8334 0.058 Uiso 1 1 calc R . . H104 H 0.4480 0.2230 0.8678 0.058 Uiso 1 1 calc R . . H105 H 0.4613 0.2366 0.7617 0.058 Uiso 1 1 calc R . . C68 C 0.56181(14) 0.22621(13) 0.6814(2) 0.0269(6) Uani 1 1 d . . . C69 C 0.41382(18) 0.48743(16) 0.4483(3) 0.0390(8) Uani 1 1 d . . . C70 C 0.4649(3) 0.5216(2) 0.4187(5) 0.0667(15) Uani 1 1 d . . . H109 H 0.4649 0.5579 0.4514 0.080 Uiso 1 1 calc R . . H110 H 0.4631 0.5284 0.3520 0.080 Uiso 1 1 calc R . . H111 H 0.4996 0.5007 0.4336 0.080 Uiso 1 1 calc R . . C71 C 0.3628(2) 0.5191(2) 0.4756(4) 0.0589(13) Uani 1 1 d . . . H112 H 0.3614 0.5549 0.4418 0.071 Uiso 1 1 calc R . . H113 H 0.3640 0.5266 0.5422 0.071 Uiso 1 1 calc R . . H114 H 0.3290 0.4967 0.4611 0.071 Uiso 1 1 calc R . . C72 C 0.4832(2) 0.0337(2) 0.7811(4) 0.0535(12) Uani 1 1 d . . . C73 C 0.4712(3) -0.0161(2) 0.7229(5) 0.0740(17) Uani 1 1 d . . . H115 H 0.5014 -0.0206 0.6770 0.089 Uiso 1 1 calc R . . H116 H 0.4348 -0.0110 0.6914 0.089 Uiso 1 1 calc R . . H117 H 0.4695 -0.0500 0.7619 0.089 Uiso 1 1 calc R . . C74 C 0.4665(3) 0.0340(3) 0.8809(6) 0.099(3) Uani 1 1 d . . . H118 H 0.4317 0.0119 0.8890 0.119 Uiso 1 1 calc R . . H119 H 0.4598 0.0730 0.9010 0.119 Uiso 1 1 calc R . . H120 H 0.4970 0.0174 0.9180 0.119 Uiso 1 1 calc R . . C75 C 0.1779(3) 0.5909(3) 0.4454(6) 0.0367(16) Uani 0.50 1 d P . . C76 C 0.2299(3) 0.6038(3) 0.4947(6) 0.0423(17) Uani 0.50 1 d P . . H121 H 0.2339 0.6449 0.5008 0.051 Uiso 0.50 1 calc PR . . H122 H 0.2624 0.5887 0.4603 0.051 Uiso 0.50 1 calc PR . . H123 H 0.2287 0.5866 0.5562 0.051 Uiso 0.50 1 calc PR . . C77 C 0.1561(4) 0.6300(4) 0.3741(8) 0.055(3) Uani 0.50 1 d P . . H124 H 0.1878 0.6515 0.3477 0.066 Uiso 0.50 1 calc PR . . H125 H 0.1288 0.6561 0.4021 0.066 Uiso 0.50 1 calc PR . . H126 H 0.1374 0.6083 0.3251 0.066 Uiso 0.50 1 calc PR . . C78 C 0.47904(19) 0.39807(17) 0.1362(4) 0.0463(9) Uani 1 1 d . . . C79 C 0.4313(2) 0.3905(3) 0.0698(4) 0.0629(13) Uani 1 1 d . . . H127 H 0.3989 0.4134 0.0896 0.075 Uiso 1 1 calc R . . H128 H 0.4203 0.3506 0.0681 0.075 Uiso 1 1 calc R . . H129 H 0.4434 0.4025 0.0081 0.075 Uiso 1 1 calc R . . C80 C 0.4637(3) 0.4103(3) 0.2340(4) 0.0670(14) Uani 1 1 d . . . H130 H 0.4271 0.3928 0.2484 0.080 Uiso 1 1 calc R . . H131 H 0.4610 0.4513 0.2429 0.080 Uiso 1 1 calc R . . H132 H 0.4929 0.3949 0.2750 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0235(2) 0.02819(19) 0.0256(2) 0.00151(17) -0.00150(19) 0.00079(15) Co2 0.0268(2) 0.0301(2) 0.0276(2) 0.00366(18) -0.0023(2) -0.00210(16) O1 0.0315(13) 0.0360(12) 0.0292(13) 0.0052(9) -0.0081(11) -0.0067(10) O2 0.0331(12) 0.0272(10) 0.0289(12) 0.0014(9) 0.0017(10) 0.0006(9) O3 0.0361(13) 0.0377(12) 0.0310(14) 0.0080(10) -0.0059(11) -0.0073(10) O4 0.0304(12) 0.0324(11) 0.0314(13) 0.0027(10) 0.0033(11) -0.0037(9) O5 0.0386(14) 0.0330(12) 0.0382(15) 0.0031(10) 0.0005(12) -0.0066(10) O6 0.0494(17) 0.0511(16) 0.0467(18) 0.0196(14) 0.0052(15) -0.0047(13) O7 0.119(8) 0.083(5) 0.179(12) 0.088(7) -0.097(9) -0.068(6) O8 0.052(2) 0.091(3) 0.063(3) -0.013(2) -0.0027(19) 0.0098(18) N1 0.0270(13) 0.0267(12) 0.0255(14) -0.0005(10) 0.0004(11) 0.0028(10) N2 0.0258(13) 0.0355(14) 0.0283(15) 0.0031(11) -0.0004(11) -0.0011(11) N3 0.0224(13) 0.0257(12) 0.0270(15) 0.0007(10) -0.0005(11) 0.0027(9) N4 0.0339(15) 0.0328(14) 0.0348(17) 0.0030(12) -0.0069(13) -0.0022(11) C1 0.0262(15) 0.0323(15) 0.0251(16) -0.0029(12) 0.0013(13) -0.0011(13) C2 0.0309(17) 0.0328(15) 0.0222(15) 0.0019(12) 0.0016(13) 0.0001(13) C3 0.0393(19) 0.0348(16) 0.0315(18) 0.0053(14) -0.0048(16) -0.0033(14) C4 0.064(3) 0.0294(17) 0.044(2) 0.0048(16) -0.007(2) 0.0003(17) C5 0.043(2) 0.056(2) 0.036(2) 0.0135(17) 0.0007(18) -0.0060(18) C6 0.040(2) 0.044(2) 0.047(2) 0.0162(17) -0.0067(19) 0.0000(16) C7 0.0262(15) 0.0349(15) 0.0263(16) -0.0021(13) 0.0011(13) 0.0004(12) C8 0.0288(17) 0.0359(17) 0.0298(18) -0.0064(13) 0.0006(14) 0.0001(13) C9 0.0320(18) 0.0359(16) 0.034(2) -0.0072(14) -0.0015(15) -0.0035(13) C10 0.074(4) 0.053(3) 0.232(11) -0.046(5) -0.098(6) 0.017(3) C11 0.066(3) 0.055(2) 0.048(3) -0.022(2) 0.012(2) -0.018(2) C12 0.090(4) 0.111(5) 0.041(3) -0.013(3) 0.009(3) -0.071(4) C13 0.0314(17) 0.0254(14) 0.0364(19) -0.0025(13) 0.0035(15) 0.0028(12) C14 0.0325(17) 0.0276(15) 0.0277(17) 0.0002(12) 0.0027(14) 0.0058(13) C15 0.0341(17) 0.0260(14) 0.0311(17) -0.0033(13) -0.0009(15) 0.0027(13) C16 0.0290(16) 0.0313(16) 0.0335(19) 0.0053(13) -0.0044(14) 0.0006(13) C17 0.0270(16) 0.0311(16) 0.040(2) 0.0030(14) -0.0047(15) 0.0051(13) C18 0.0280(17) 0.0457(19) 0.044(2) 0.0078(17) 0.0099(17) 0.0061(14) C19 0.0311(17) 0.0405(17) 0.034(2) 0.0019(14) -0.0087(15) 0.0027(14) C20 0.0234(15) 0.0306(15) 0.0316(17) -0.0002(13) 0.0018(14) 0.0009(12) C21 0.0250(15) 0.0332(15) 0.0267(17) -0.0021(13) 0.0008(13) -0.0010(12) C22 0.0281(17) 0.0347(16) 0.0300(18) 0.0018(13) -0.0015(14) -0.0061(13) C23 0.038(2) 0.0409(18) 0.0296(19) 0.0069(14) -0.0021(15) -0.0070(15) C24 0.057(3) 0.053(2) 0.0271(19) 0.0050(16) -0.0016(18) -0.016(2) C25 0.066(3) 0.056(2) 0.036(2) 0.0062(18) 0.004(2) -0.020(2) C26 0.072(3) 0.071(3) 0.040(2) 0.015(2) -0.009(3) -0.009(2) C27 0.060(3) 0.076(3) 0.034(2) 0.003(2) 0.012(2) -0.014(2) C28 0.0364(19) 0.0408(18) 0.0277(18) -0.0035(14) -0.0025(15) -0.0045(15) C29 0.0292(16) 0.0320(15) 0.0294(17) -0.0021(13) -0.0011(14) -0.0002(13) C30 0.0357(19) 0.0320(16) 0.039(2) -0.0019(14) 0.0000(16) -0.0003(13) C31 0.061(3) 0.043(2) 0.043(2) -0.0094(18) -0.001(2) -0.0154(19) C32 0.046(2) 0.0304(16) 0.047(2) -0.0032(15) -0.0048(18) 0.0033(15) C33 0.040(2) 0.0363(18) 0.047(2) -0.0004(16) -0.0026(18) -0.0106(15) C34 0.0259(15) 0.0288(15) 0.0313(18) -0.0011(13) 0.0005(14) 0.0018(12) C35 0.0313(17) 0.0291(14) 0.0287(17) 0.0022(12) -0.0039(14) -0.0053(13) C36 0.0326(18) 0.0364(16) 0.0271(17) -0.0014(13) -0.0003(14) -0.0051(14) C37 0.0335(17) 0.0386(16) 0.0296(17) 0.0034(15) 0.0019(16) -0.0119(13) C38 0.042(2) 0.045(2) 0.0299(19) 0.0029(15) 0.0043(16) -0.0114(16) C39 0.051(2) 0.0343(16) 0.045(2) 0.0005(17) -0.002(2) -0.0166(16) C40 0.032(2) 0.068(3) 0.042(2) 0.004(2) -0.0009(18) -0.0155(18) C41 0.0283(17) 0.0373(16) 0.0287(18) -0.0016(14) -0.0053(14) -0.0010(13) C42 0.0312(17) 0.0348(16) 0.0267(17) -0.0012(13) -0.0013(14) -0.0015(13) C43 0.0389(19) 0.050(2) 0.0242(18) 0.0051(15) -0.0031(15) 0.0019(16) C44 0.039(2) 0.065(3) 0.041(2) 0.010(2) -0.0086(19) 0.0024(19) C45 0.056(3) 0.070(3) 0.029(2) 0.008(2) 0.003(2) 0.011(2) C46 0.062(3) 0.050(2) 0.044(2) 0.0155(19) -0.013(2) -0.005(2) C47 0.0288(16) 0.0333(16) 0.0267(17) 0.0005(13) 0.0012(13) -0.0028(13) C48 0.0285(17) 0.0302(14) 0.0256(16) -0.0022(13) 0.0007(14) -0.0044(13) C49 0.0254(16) 0.0344(15) 0.0268(17) -0.0055(13) -0.0002(13) 0.0000(13) C50 0.0243(16) 0.0308(15) 0.0346(19) -0.0020(13) -0.0046(14) 0.0004(12) C51 0.0291(17) 0.0368(17) 0.037(2) -0.0008(14) -0.0038(15) 0.0044(14) C52 0.046(2) 0.0355(18) 0.057(3) 0.0129(18) -0.007(2) 0.0035(16) C53 0.0366(19) 0.0441(19) 0.035(2) 0.0009(15) -0.0108(17) 0.0011(15) C54 0.0282(15) 0.0270(14) 0.0241(17) 0.0025(11) 0.0015(13) 0.0007(11) C55 0.0248(15) 0.0286(14) 0.0251(16) -0.0016(12) -0.0025(12) 0.0038(12) C56 0.0271(16) 0.0312(15) 0.0271(17) 0.0011(12) 0.0025(13) 0.0001(12) C57 0.0302(17) 0.0320(16) 0.0290(18) -0.0030(13) -0.0019(14) 0.0001(13) C58 0.041(2) 0.0340(17) 0.036(2) -0.0048(14) 0.0020(17) -0.0080(15) C59 0.111(5) 0.069(3) 0.070(4) -0.018(3) 0.041(4) -0.051(3) C60 0.075(4) 0.035(2) 0.155(8) 0.002(3) 0.019(4) -0.005(2) C61 0.100(5) 0.073(4) 0.079(5) 0.004(3) -0.030(4) -0.040(3) C62 0.0366(18) 0.0343(16) 0.0275(17) -0.0041(13) -0.0011(15) 0.0014(13) C63 0.0352(18) 0.0333(16) 0.0264(17) -0.0001(13) 0.0022(15) 0.0053(13) C64 0.0370(18) 0.0437(18) 0.0278(18) 0.0013(15) 0.0056(16) 0.0063(15) C65 0.067(3) 0.056(2) 0.030(2) -0.0076(18) 0.013(2) 0.001(2) C66 0.049(2) 0.049(2) 0.0279(19) 0.0078(16) 0.0084(17) 0.0003(17) C67 0.041(2) 0.064(3) 0.040(2) 0.0069(19) 0.0131(19) 0.0054(19) C68 0.0223(14) 0.0292(14) 0.0292(17) 0.0015(12) -0.0017(13) 0.0011(12) C69 0.051(2) 0.0401(18) 0.0257(18) 0.0043(14) -0.0053(17) -0.0101(16) C70 0.072(3) 0.057(3) 0.071(4) 0.001(3) 0.010(3) -0.031(3) C71 0.074(3) 0.045(2) 0.057(3) 0.006(2) -0.001(3) 0.014(2) C72 0.045(2) 0.050(2) 0.065(3) 0.024(2) -0.007(2) -0.0053(18) C73 0.083(4) 0.067(3) 0.072(4) 0.022(3) -0.028(3) -0.026(3) C74 0.110(5) 0.072(4) 0.115(6) 0.051(4) 0.065(5) 0.020(4) C75 0.040(4) 0.022(3) 0.048(4) 0.000(3) -0.006(3) 0.004(3) C76 0.037(4) 0.053(4) 0.037(4) 0.012(4) 0.010(4) 0.007(3) C77 0.033(4) 0.069(5) 0.063(6) 0.035(5) -0.014(4) -0.019(4) C78 0.047(2) 0.047(2) 0.045(2) 0.0019(18) 0.002(2) 0.0025(17) C79 0.052(3) 0.090(4) 0.047(3) -0.001(2) -0.004(2) -0.001(2) C80 0.065(3) 0.096(4) 0.040(3) 0.007(3) 0.000(2) -0.011(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 O1 1.923(3) . ? Co1 O2 1.937(3) . ? Co1 N1 2.135(3) . ? Co1 N2 2.150(3) . ? Co1 O5 2.208(2) . ? Co2 O4 1.929(3) . ? Co2 O3 1.947(3) . ? Co2 N4 2.140(3) . ? Co2 N3 2.151(3) . ? Co2 O6 2.159(3) . ? O1 C1 1.331(4) . ? O2 C34 1.332(4) . ? O3 C35 1.339(4) . ? O4 C68 1.333(4) . ? O5 C69 1.207(4) . ? O6 C72 1.191(5) . ? O7 C75 1.195(10) . ? O8 C78 1.217(6) . ? N1 C20 1.479(4) . ? N1 C16 1.482(4) . ? N1 C15 1.491(4) . ? N2 C18 1.472(5) . ? N2 C19 1.487(5) . ? N2 C17 1.492(4) . ? N3 C50 1.475(4) . ? N3 C49 1.480(4) . ? N3 C54 1.490(4) . ? N4 C52 1.473(5) . ? N4 C53 1.484(5) . ? N4 C51 1.487(5) . ? C1 C14 1.414(5) . ? C1 C2 1.425(5) . ? C2 C7 1.403(5) . ? C2 C3 1.534(5) . ? C3 C5 1.521(6) . ? C3 C6 1.526(5) . ? C3 C4 1.543(6) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.397(5) . ? C7 H10 0.9500 . ? C8 C13 1.391(5) . ? C8 C9 1.539(5) . ? C9 C10 1.507(7) . ? C9 C11 1.525(6) . ? C9 C12 1.535(7) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.386(5) . ? C13 H20 0.9500 . ? C14 C15 1.508(5) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.508(5) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 H27 0.9800 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C19 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C20 C21 1.513(5) . ? C20 H33 0.9900 . ? C20 H34 0.9900 . ? C21 C22 1.390(5) . ? C21 C34 1.410(5) . ? C22 C23 1.387(5) . ? C22 H35 0.9500 . ? C23 C28 1.391(5) . ? C23 C24 1.539(5) . ? C24 C25 1.512(6) . ? C24 C26 1.521(7) . ? C24 C27 1.544(7) . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C26 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C27 H44 0.9800 . ? C28 C29 1.396(5) . ? C28 H45 0.9500 . ? C29 C34 1.431(5) . ? C29 C30 1.544(5) . ? C30 C31 1.533(6) . ? C30 C33 1.533(6) . ? C30 C32 1.550(5) . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? C33 H52 0.9800 . ? C33 H53 0.9800 . ? C33 H54 0.9800 . ? C35 C48 1.401(5) . ? C35 C36 1.422(5) . ? C36 C41 1.398(5) . ? C36 C37 1.539(5) . ? C37 C40 1.538(5) . ? C37 C39 1.540(5) . ? C37 C38 1.545(6) . ? C38 H55 0.9800 . ? C38 H56 0.9800 . ? C38 H57 0.9800 . ? C39 H58 0.9800 . ? C39 H59 0.9800 . ? C39 H60 0.9800 . ? C40 H61 0.9800 . ? C40 H62 0.9800 . ? C40 H63 0.9800 . ? C41 C42 1.392(5) . ? C41 H64 0.9500 . ? C42 C47 1.407(5) . ? C42 C43 1.546(5) . ? C43 C46 1.519(6) . ? C43 C44 1.532(6) . ? C43 C45 1.547(6) . ? C44 H65 0.9800 . ? C44 H66 0.9800 . ? C44 H67 0.9800 . ? C45 H68 0.9800 . ? C45 H69 0.9800 . ? C45 H70 0.9800 . ? C46 H71 0.9800 . ? C46 H72 0.9800 . ? C46 H73 0.9800 . ? C47 C48 1.391(5) . ? C47 H74 0.9500 . ? C48 C49 1.519(5) . ? C49 H75 0.9900 . ? C49 H76 0.9900 . ? C50 C51 1.517(5) . ? C50 H77 0.9900 . ? C50 H78 0.9900 . ? C51 H79 0.9900 . ? C51 H80 0.9900 . ? C52 H81 0.9800 . ? C52 H82 0.9800 . ? C52 H83 0.9800 . ? C53 H84 0.9800 . ? C53 H85 0.9800 . ? C53 H86 0.9800 . ? C54 C55 1.515(4) . ? C54 H87 0.9900 . ? C54 H88 0.9900 . ? C55 C56 1.399(5) . ? C55 C68 1.407(5) . ? C56 C57 1.397(5) . ? C56 H89 0.9500 . ? C57 C62 1.394(5) . ? C57 C58 1.538(5) . ? C58 C59 1.518(7) . ? C58 C60 1.518(7) . ? C58 C61 1.521(8) . ? C59 H90 0.9800 . ? C59 H91 0.9800 . ? C59 H92 0.9800 . ? C60 H93 0.9800 . ? C60 H94 0.9800 . ? C60 H95 0.9800 . ? C61 H96 0.9800 . ? C61 H97 0.9800 . ? C61 H98 0.9800 . ? C62 C63 1.392(5) . ? C62 H99 0.9500 . ? C63 C68 1.419(5) . ? C63 C64 1.535(5) . ? C64 C65 1.528(6) . ? C64 C66 1.534(5) . ? C64 C67 1.540(6) . ? C65 H100 0.9800 . ? C65 H101 0.9800 . ? C65 H102 0.9800 . ? C66 H106 0.9800 . ? C66 H107 0.9800 . ? C66 H108 0.9800 . ? C67 H103 0.9800 . ? C67 H104 0.9800 . ? C67 H105 0.9800 . ? C69 C71 1.471(7) . ? C69 C70 1.512(6) . ? C70 H109 0.9800 . ? C70 H110 0.9800 . ? C70 H111 0.9800 . ? C71 H112 0.9800 . ? C71 H113 0.9800 . ? C71 H114 0.9800 . ? C72 C73 1.478(8) . ? C72 C74 1.497(9) . ? C73 H115 0.9800 . ? C73 H116 0.9800 . ? C73 H117 0.9800 . ? C74 H118 0.9800 . ? C74 H119 0.9800 . ? C74 H120 0.9800 . ? C75 C76 1.453(12) . ? C75 C77 1.478(11) . ? C76 H121 0.9800 . ? C76 H122 0.9800 . ? C76 H123 0.9800 . ? C77 H124 0.9800 . ? C77 H125 0.9800 . ? C77 H126 0.9800 . ? C78 C80 1.490(7) . ? C78 C79 1.490(7) . ? C79 H127 0.9800 . ? C79 H128 0.9800 . ? C79 H129 0.9800 . ? C80 H130 0.9800 . ? C80 H131 0.9800 . ? C80 H132 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 120.64(11) . . ? O1 Co1 N1 92.33(11) . . ? O2 Co1 N1 93.12(10) . . ? O1 Co1 N2 125.90(12) . . ? O2 Co1 N2 113.43(11) . . ? N1 Co1 N2 82.79(11) . . ? O1 Co1 O5 91.77(10) . . ? O2 Co1 O5 93.62(10) . . ? N1 Co1 O5 168.94(10) . . ? N2 Co1 O5 86.49(11) . . ? O4 Co2 O3 123.51(11) . . ? O4 Co2 N4 116.22(12) . . ? O3 Co2 N4 120.25(12) . . ? O4 Co2 N3 91.91(10) . . ? O3 Co2 N3 93.32(11) . . ? N4 Co2 N3 82.82(11) . . ? O4 Co2 O6 84.60(12) . . ? O3 Co2 O6 96.10(12) . . ? N4 Co2 O6 90.66(12) . . ? N3 Co2 O6 170.36(12) . . ? C1 O1 Co1 127.6(2) . . ? C34 O2 Co1 126.6(2) . . ? C35 O3 Co2 122.8(2) . . ? C68 O4 Co2 127.6(2) . . ? C69 O5 Co1 141.5(3) . . ? C72 O6 Co2 143.9(4) . . ? C20 N1 C16 112.9(3) . . ? C20 N1 C15 110.1(3) . . ? C16 N1 C15 109.5(3) . . ? C20 N1 Co1 108.82(19) . . ? C16 N1 Co1 106.40(19) . . ? C15 N1 Co1 109.0(2) . . ? C18 N2 C19 108.3(3) . . ? C18 N2 C17 109.6(3) . . ? C19 N2 C17 109.7(3) . . ? C18 N2 Co1 114.6(2) . . ? C19 N2 Co1 106.3(2) . . ? C17 N2 Co1 108.1(2) . . ? C50 N3 C49 110.4(3) . . ? C50 N3 C54 109.6(2) . . ? C49 N3 C54 107.8(3) . . ? C50 N3 Co2 107.7(2) . . ? C49 N3 Co2 109.4(2) . . ? C54 N3 Co2 111.96(19) . . ? C52 N4 C53 108.4(3) . . ? C52 N4 C51 109.3(3) . . ? C53 N4 C51 110.7(3) . . ? C52 N4 Co2 113.4(2) . . ? C53 N4 Co2 107.8(2) . . ? C51 N4 Co2 107.3(2) . . ? O1 C1 C14 121.2(3) . . ? O1 C1 C2 120.9(3) . . ? C14 C1 C2 117.8(3) . . ? C7 C2 C1 118.3(3) . . ? C7 C2 C3 121.2(3) . . ? C1 C2 C3 120.5(3) . . ? C5 C3 C6 107.8(3) . . ? C5 C3 C2 109.9(3) . . ? C6 C3 C2 112.6(3) . . ? C5 C3 C4 110.1(3) . . ? C6 C3 C4 107.1(3) . . ? C2 C3 C4 109.3(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 123.7(3) . . ? C8 C7 H10 118.2 . . ? C2 C7 H10 118.2 . . ? C13 C8 C7 116.5(3) . . ? C13 C8 C9 121.6(3) . . ? C7 C8 C9 121.6(3) . . ? C10 C9 C11 108.9(5) . . ? C10 C9 C12 109.9(6) . . ? C11 C9 C12 105.9(4) . . ? C10 C9 C8 112.6(3) . . ? C11 C9 C8 107.8(3) . . ? C12 C9 C8 111.4(3) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C14 C13 C8 122.3(3) . . ? C14 C13 H20 118.9 . . ? C8 C13 H20 118.9 . . ? C13 C14 C1 120.9(3) . . ? C13 C14 C15 119.2(3) . . ? C1 C14 C15 119.7(3) . . ? N1 C15 C14 114.4(3) . . ? N1 C15 H21 108.7 . . ? C14 C15 H21 108.7 . . ? N1 C15 H22 108.7 . . ? C14 C15 H22 108.7 . . ? H21 C15 H22 107.6 . . ? N1 C16 C17 110.6(3) . . ? N1 C16 H23 109.5 . . ? C17 C16 H23 109.5 . . ? N1 C16 H24 109.5 . . ? C17 C16 H24 109.5 . . ? H23 C16 H24 108.1 . . ? N2 C17 C16 110.6(3) . . ? N2 C17 H25 109.5 . . ? C16 C17 H25 109.5 . . ? N2 C17 H26 109.5 . . ? C16 C17 H26 109.5 . . ? H25 C17 H26 108.1 . . ? N2 C18 H27 109.5 . . ? N2 C18 H28 109.5 . . ? H27 C18 H28 109.5 . . ? N2 C18 H29 109.5 . . ? H27 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? N2 C19 H30 109.5 . . ? N2 C19 H31 109.5 . . ? H30 C19 H31 109.5 . . ? N2 C19 H32 109.5 . . ? H30 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? N1 C20 C21 113.2(3) . . ? N1 C20 H33 108.9 . . ? C21 C20 H33 108.9 . . ? N1 C20 H34 108.9 . . ? C21 C20 H34 108.9 . . ? H33 C20 H34 107.7 . . ? C22 C21 C34 120.9(3) . . ? C22 C21 C20 117.7(3) . . ? C34 C21 C20 121.4(3) . . ? C23 C22 C21 122.2(3) . . ? C23 C22 H35 118.9 . . ? C21 C22 H35 118.9 . . ? C22 C23 C28 116.7(3) . . ? C22 C23 C24 123.0(3) . . ? C28 C23 C24 120.3(4) . . ? C25 C24 C26 110.7(4) . . ? C25 C24 C23 111.9(4) . . ? C26 C24 C23 109.9(4) . . ? C25 C24 C27 106.5(4) . . ? C26 C24 C27 108.1(4) . . ? C23 C24 C27 109.7(4) . . ? C24 C25 H36 109.5 . . ? C24 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? C24 C25 H38 109.5 . . ? H36 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C24 C26 H39 109.5 . . ? C24 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? C24 C26 H41 109.5 . . ? H39 C26 H41 109.5 . . ? H40 C26 H41 109.5 . . ? C24 C27 H42 109.5 . . ? C24 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? C24 C27 H44 109.5 . . ? H42 C27 H44 109.5 . . ? H43 C27 H44 109.5 . . ? C23 C28 C29 124.0(4) . . ? C23 C28 H45 118.0 . . ? C29 C28 H45 118.0 . . ? C28 C29 C34 118.2(3) . . ? C28 C29 C30 120.5(3) . . ? C34 C29 C30 121.3(3) . . ? C31 C30 C33 107.5(3) . . ? C31 C30 C29 112.5(3) . . ? C33 C30 C29 111.6(3) . . ? C31 C30 C32 107.6(3) . . ? C33 C30 C32 110.0(3) . . ? C29 C30 C32 107.5(3) . . ? C30 C31 H46 109.5 . . ? C30 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? C30 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? C30 C32 H49 109.5 . . ? C30 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? C30 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? C30 C33 H52 109.5 . . ? C30 C33 H53 109.5 . . ? H52 C33 H53 109.5 . . ? C30 C33 H54 109.5 . . ? H52 C33 H54 109.5 . . ? H53 C33 H54 109.5 . . ? O2 C34 C21 120.8(3) . . ? O2 C34 C29 121.1(3) . . ? C21 C34 C29 118.0(3) . . ? O3 C35 C48 119.8(3) . . ? O3 C35 C36 121.7(3) . . ? C48 C35 C36 118.4(3) . . ? C41 C36 C35 118.6(3) . . ? C41 C36 C37 120.5(3) . . ? C35 C36 C37 120.9(3) . . ? C40 C37 C36 112.8(3) . . ? C40 C37 C39 106.5(3) . . ? C36 C37 C39 108.8(3) . . ? C40 C37 C38 108.4(3) . . ? C36 C37 C38 109.9(3) . . ? C39 C37 C38 110.4(3) . . ? C37 C38 H55 109.5 . . ? C37 C38 H56 109.5 . . ? H55 C38 H56 109.5 . . ? C37 C38 H57 109.5 . . ? H55 C38 H57 109.5 . . ? H56 C38 H57 109.5 . . ? C37 C39 H58 109.5 . . ? C37 C39 H59 109.5 . . ? H58 C39 H59 109.5 . . ? C37 C39 H60 109.5 . . ? H58 C39 H60 109.5 . . ? H59 C39 H60 109.5 . . ? C37 C40 H61 109.5 . . ? C37 C40 H62 109.5 . . ? H61 C40 H62 109.5 . . ? C37 C40 H63 109.5 . . ? H61 C40 H63 109.5 . . ? H62 C40 H63 109.5 . . ? C42 C41 C36 123.6(3) . . ? C42 C41 H64 118.2 . . ? C36 C41 H64 118.2 . . ? C41 C42 C47 116.7(3) . . ? C41 C42 C43 123.0(3) . . ? C47 C42 C43 120.3(3) . . ? C46 C43 C44 108.7(4) . . ? C46 C43 C42 110.3(3) . . ? C44 C43 C42 111.7(3) . . ? C46 C43 C45 109.1(4) . . ? C44 C43 C45 107.9(4) . . ? C42 C43 C45 109.1(3) . . ? C43 C44 H65 109.5 . . ? C43 C44 H66 109.5 . . ? H65 C44 H66 109.5 . . ? C43 C44 H67 109.5 . . ? H65 C44 H67 109.5 . . ? H66 C44 H67 109.5 . . ? C43 C45 H68 109.5 . . ? C43 C45 H69 109.5 . . ? H68 C45 H69 109.5 . . ? C43 C45 H70 109.5 . . ? H68 C45 H70 109.5 . . ? H69 C45 H70 109.5 . . ? C43 C46 H71 109.5 . . ? C43 C46 H72 109.5 . . ? H71 C46 H72 109.5 . . ? C43 C46 H73 109.5 . . ? H71 C46 H73 109.5 . . ? H72 C46 H73 109.5 . . ? C48 C47 C42 121.4(3) . . ? C48 C47 H74 119.3 . . ? C42 C47 H74 119.3 . . ? C47 C48 C35 121.2(3) . . ? C47 C48 C49 118.8(3) . . ? C35 C48 C49 119.8(3) . . ? N3 C49 C48 114.1(3) . . ? N3 C49 H75 108.7 . . ? C48 C49 H75 108.7 . . ? N3 C49 H76 108.7 . . ? C48 C49 H76 108.7 . . ? H75 C49 H76 107.6 . . ? N3 C50 C51 110.7(3) . . ? N3 C50 H77 109.5 . . ? C51 C50 H77 109.5 . . ? N3 C50 H78 109.5 . . ? C51 C50 H78 109.5 . . ? H77 C50 H78 108.1 . . ? N4 C51 C50 110.4(3) . . ? N4 C51 H79 109.6 . . ? C50 C51 H79 109.6 . . ? N4 C51 H80 109.6 . . ? C50 C51 H80 109.6 . . ? H79 C51 H80 108.1 . . ? N4 C52 H81 109.5 . . ? N4 C52 H82 109.5 . . ? H81 C52 H82 109.5 . . ? N4 C52 H83 109.5 . . ? H81 C52 H83 109.5 . . ? H82 C52 H83 109.5 . . ? N4 C53 H84 109.5 . . ? N4 C53 H85 109.5 . . ? H84 C53 H85 109.5 . . ? N4 C53 H86 109.5 . . ? H84 C53 H86 109.5 . . ? H85 C53 H86 109.5 . . ? N3 C54 C55 114.9(3) . . ? N3 C54 H87 108.5 . . ? C55 C54 H87 108.5 . . ? N3 C54 H88 108.5 . . ? C55 C54 H88 108.5 . . ? H87 C54 H88 107.5 . . ? C56 C55 C68 121.5(3) . . ? C56 C55 C54 117.3(3) . . ? C68 C55 C54 120.8(3) . . ? C57 C56 C55 120.6(3) . . ? C57 C56 H89 119.7 . . ? C55 C56 H89 119.7 . . ? C62 C57 C56 117.0(3) . . ? C62 C57 C58 120.9(3) . . ? C56 C57 C58 121.9(3) . . ? C59 C58 C60 107.5(5) . . ? C59 C58 C61 107.4(5) . . ? C60 C58 C61 109.2(5) . . ? C59 C58 C57 113.1(3) . . ? C60 C58 C57 109.4(4) . . ? C61 C58 C57 110.1(4) . . ? C58 C59 H90 109.5 . . ? C58 C59 H91 109.5 . . ? H90 C59 H91 109.5 . . ? C58 C59 H92 109.5 . . ? H90 C59 H92 109.5 . . ? H91 C59 H92 109.5 . . ? C58 C60 H93 109.5 . . ? C58 C60 H94 109.5 . . ? H93 C60 H94 109.5 . . ? C58 C60 H95 109.5 . . ? H93 C60 H95 109.5 . . ? H94 C60 H95 109.5 . . ? C58 C61 H96 109.5 . . ? C58 C61 H97 109.5 . . ? H96 C61 H97 109.5 . . ? C58 C61 H98 109.5 . . ? H96 C61 H98 109.5 . . ? H97 C61 H98 109.5 . . ? C63 C62 C57 124.6(3) . . ? C63 C62 H99 117.7 . . ? C57 C62 H99 117.7 . . ? C62 C63 C68 117.6(3) . . ? C62 C63 C64 121.6(3) . . ? C68 C63 C64 120.8(3) . . ? C65 C64 C66 106.8(4) . . ? C65 C64 C63 112.5(3) . . ? C66 C64 C63 111.3(3) . . ? C65 C64 C67 107.1(4) . . ? C66 C64 C67 108.9(3) . . ? C63 C64 C67 110.0(3) . . ? C64 C65 H100 109.5 . . ? C64 C65 H101 109.5 . . ? H100 C65 H101 109.5 . . ? C64 C65 H102 109.5 . . ? H100 C65 H102 109.5 . . ? H101 C65 H102 109.5 . . ? C64 C66 H106 109.5 . . ? C64 C66 H107 109.5 . . ? H106 C66 H107 109.5 . . ? C64 C66 H108 109.5 . . ? H106 C66 H108 109.5 . . ? H107 C66 H108 109.5 . . ? C64 C67 H103 109.5 . . ? C64 C67 H104 109.5 . . ? H103 C67 H104 109.5 . . ? C64 C67 H105 109.5 . . ? H103 C67 H105 109.5 . . ? H104 C67 H105 109.5 . . ? O4 C68 C55 120.4(3) . . ? O4 C68 C63 120.8(3) . . ? C55 C68 C63 118.7(3) . . ? O5 C69 C71 122.9(4) . . ? O5 C69 C70 120.1(4) . . ? C71 C69 C70 117.1(4) . . ? C69 C70 H109 109.5 . . ? C69 C70 H110 109.5 . . ? H109 C70 H110 109.5 . . ? C69 C70 H111 109.5 . . ? H109 C70 H111 109.5 . . ? H110 C70 H111 109.5 . . ? C69 C71 H112 109.5 . . ? C69 C71 H113 109.5 . . ? H112 C71 H113 109.5 . . ? C69 C71 H114 109.5 . . ? H112 C71 H114 109.5 . . ? H113 C71 H114 109.5 . . ? O6 C72 C73 120.6(5) . . ? O6 C72 C74 119.0(5) . . ? C73 C72 C74 120.2(5) . . ? C72 C73 H115 109.5 . . ? C72 C73 H116 109.5 . . ? H115 C73 H116 109.5 . . ? C72 C73 H117 109.5 . . ? H115 C73 H117 109.5 . . ? H116 C73 H117 109.5 . . ? C72 C74 H118 109.5 . . ? C72 C74 H119 109.5 . . ? H118 C74 H119 109.5 . . ? C72 C74 H120 109.5 . . ? H118 C74 H120 109.5 . . ? H119 C74 H120 109.5 . . ? O7 C75 C76 118.5(8) . . ? O7 C75 C77 121.2(8) . . ? C76 C75 C77 120.3(7) . . ? C75 C76 H121 109.5 . . ? C75 C76 H122 109.5 . . ? H121 C76 H122 109.5 . . ? C75 C76 H123 109.5 . . ? H121 C76 H123 109.5 . . ? H122 C76 H123 109.5 . . ? C75 C77 H124 109.5 . . ? C75 C77 H125 109.5 . . ? H124 C77 H125 109.5 . . ? C75 C77 H126 109.5 . . ? H124 C77 H126 109.5 . . ? H125 C77 H126 109.5 . . ? O8 C78 C80 121.7(5) . . ? O8 C78 C79 121.4(5) . . ? C80 C78 C79 116.9(4) . . ? C78 C79 H127 109.5 . . ? C78 C79 H128 109.5 . . ? H127 C79 H128 109.5 . . ? C78 C79 H129 109.5 . . ? H127 C79 H129 109.5 . . ? H128 C79 H129 109.5 . . ? C78 C80 H130 109.5 . . ? C78 C80 H131 109.5 . . ? H130 C80 H131 109.5 . . ? C78 C80 H132 109.5 . . ? H130 C80 H132 109.5 . . ? H131 C80 H132 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.569 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.075 #===END data_1CH3OH _database_code_depnum_ccdc_archive 'CCDC 766020' #TrackingRef 'Kozak_Compiled_CIF.cif' # start Validation Reply Form _vrf_PLAT417_1CH3OH ; PROBLEM: Short Inter D-H..H-D H125 .. H129 .. 1.54 Ang. RESPONSE: These are methanolic (lattice solvent) protons that were introduced in difference map positions, and refined on a riding model. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C34 H54 O2 N2) Co (C H3 O H)] (C H3 O H)2.5 ' _chemical_formula_sum 'C37.50 H68 Co N2 O5.50' _chemical_formula_weight 693.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.902(2) _cell_length_b 15.3466(15) _cell_length_c 19.850(3) _cell_angle_alpha 74.869(10) _cell_angle_beta 89.538(13) _cell_angle_gamma 67.524(9) _cell_volume 4028.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 16160 _cell_measurement_theta_min 1.9180 _cell_measurement_theta_max 30.8064 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Pink' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_correction_T_min 0.9324 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 35216 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.50 _reflns_number_total 16429 _reflns_number_gt 13925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'DIRDIF99-ORIENT (Beurskens, et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0703P)^2^+3.7829P] 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 0.0012(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16429 _refine_ls_number_parameters 831 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1674 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.53348(3) 0.87544(3) 0.23986(2) 0.02963(12) Uani 1 1 d . . . Co2 Co 1.09565(3) 0.65459(3) 0.28110(2) 0.02864(12) Uani 1 1 d . . . O1 O 0.45605(15) 0.84771(15) 0.17739(11) 0.0324(5) Uani 1 1 d . . . O2 O 0.47025(15) 0.92270(15) 0.31840(11) 0.0334(5) Uani 1 1 d . . . O3 O 1.08131(15) 0.53946(15) 0.26264(10) 0.0312(5) Uani 1 1 d . . . O4 O 0.99160(15) 0.76919(15) 0.29537(10) 0.0315(5) Uani 1 1 d . . . O5 O 0.50023(16) 1.02391(16) 0.17764(12) 0.0370(5) Uani 1 1 d . . . H109 H 0.5199 1.0565 0.1953 0.044 Uiso 1 1 d . . . O6 O 1.12160(17) 0.58429(17) 0.39197(11) 0.0400(5) Uani 1 1 d . . . H113 H 1.1643 0.5285 0.4078 0.048 Uiso 1 1 d . . . O7 O 0.59396(19) 0.9893(2) 0.36039(13) 0.0523(7) Uani 1 1 d . . . H117 H 0.5498 0.9724 0.3513 0.062 Uiso 1 1 d . . . O8 O 0.5742(2) 1.12649(19) 0.23945(13) 0.0509(6) Uani 1 1 d . . . H121 H 0.5730 1.0956 0.2801 0.061 Uiso 1 1 d . . . O9 O 1.2452(2) 0.4013(2) 0.45774(16) 0.0686(8) Uani 1 1 d . . . H125 H 1.2656 0.3853 0.4177 0.081 Uiso 1 1 d . . . O10 O 1.3733(3) 0.3289(3) 0.37239(18) 0.0843(11) Uani 1 1 d . . . H129 H 1.3184 0.3188 0.3712 0.100 Uiso 1 1 d . . . O11 O 1.25799(19) 0.4115(2) 0.25403(16) 0.0590(7) Uani 1 1 d . . . H133 H 1.2004 0.4454 0.2556 0.071 Uiso 1 1 d . . . N1 N 0.59155(18) 0.72712(18) 0.30541(13) 0.0302(5) Uani 1 1 d . . . N2 N 0.68271(18) 0.83576(19) 0.21619(13) 0.0329(6) Uani 1 1 d . . . N3 N 1.08548(17) 0.72244(18) 0.16897(13) 0.0289(5) Uani 1 1 d . . . N4 N 1.23452(18) 0.66606(19) 0.27922(13) 0.0307(5) Uani 1 1 d . . . C1 C 0.4688(2) 0.7610(2) 0.16805(15) 0.0294(6) Uani 1 1 d . . . C2 C 0.4420(2) 0.7529(2) 0.10160(15) 0.0316(6) Uani 1 1 d . . . C3 C 0.3971(3) 0.8446(2) 0.03896(16) 0.0381(7) Uani 1 1 d . . . C4 C 0.2994(3) 0.9145(3) 0.0561(2) 0.0469(9) Uani 1 1 d . . . H1 H 0.2537 0.8818 0.0642 0.056 Uiso 1 1 calc R . . H2 H 0.2720 0.9741 0.0167 0.056 Uiso 1 1 calc R . . H3 H 0.3105 0.9322 0.0984 0.056 Uiso 1 1 calc R . . C5 C 0.4662(3) 0.8986(3) 0.02278(18) 0.0433(8) Uani 1 1 d . . . H4 H 0.4390 0.9539 -0.0195 0.052 Uiso 1 1 calc R . . H5 H 0.5301 0.8532 0.0151 0.052 Uiso 1 1 calc R . . H6 H 0.4738 0.9230 0.0624 0.052 Uiso 1 1 calc R . . C6 C 0.3766(3) 0.8202(3) -0.02797(19) 0.0570(11) Uani 1 1 d . . . H7 H 0.3516 0.8805 -0.0669 0.068 Uiso 1 1 calc R . . H8 H 0.3279 0.7911 -0.0207 0.068 Uiso 1 1 calc R . . H9 H 0.4371 0.7736 -0.0391 0.068 Uiso 1 1 calc R . . C7 C 0.4548(2) 0.6604(2) 0.09588(15) 0.0338(7) Uani 1 1 d . . . H10 H 0.4365 0.6557 0.0517 0.041 Uiso 1 1 calc R . . C8 C 0.4928(2) 0.5746(2) 0.15094(16) 0.0339(7) Uani 1 1 d . . . C9 C 0.5049(3) 0.4742(2) 0.14196(17) 0.0424(8) Uani 1 1 d . . . C10 C 0.4231(4) 0.4850(3) 0.0910(2) 0.0774(16) Uani 1 1 d . . . H11 H 0.3687 0.4785 0.1170 0.093 Uiso 1 1 calc R . . H12 H 0.4473 0.4336 0.0668 0.093 Uiso 1 1 calc R . . H13 H 0.4007 0.5496 0.0566 0.093 Uiso 1 1 calc R . . C11 C 0.6047(4) 0.4285(3) 0.1150(3) 0.0823(17) Uani 1 1 d . . . H14 H 0.5974 0.4491 0.0636 0.099 Uiso 1 1 calc R . . H15 H 0.6288 0.3567 0.1317 0.099 Uiso 1 1 calc R . . H16 H 0.6512 0.4504 0.1325 0.099 Uiso 1 1 calc R . . C12 C 0.5011(3) 0.4042(3) 0.21088(18) 0.0471(9) Uani 1 1 d . . . H17 H 0.4395 0.4338 0.2301 0.057 Uiso 1 1 calc R . . H18 H 0.5559 0.3910 0.2443 0.057 Uiso 1 1 calc R . . H19 H 0.5054 0.3424 0.2028 0.057 Uiso 1 1 calc R . . C13 C 0.5197(2) 0.5838(2) 0.21441(15) 0.0329(7) Uani 1 1 d . . . H20 H 0.5477 0.5265 0.2528 0.040 Uiso 1 1 calc R . . C14 C 0.5073(2) 0.6744(2) 0.22396(15) 0.0304(6) Uani 1 1 d . . . C15 C 0.5246(2) 0.6790(2) 0.29749(16) 0.0322(6) Uani 1 1 d . . . H21 H 0.4610 0.7148 0.3130 0.039 Uiso 1 1 calc R . . H22 H 0.5516 0.6113 0.3291 0.039 Uiso 1 1 calc R . . C16 C 0.6883(2) 0.6758(2) 0.28423(18) 0.0364(7) Uani 1 1 d . . . H23 H 0.6804 0.6551 0.2421 0.044 Uiso 1 1 calc R . . H24 H 0.7260 0.6162 0.3225 0.044 Uiso 1 1 calc R . . C17 C 0.7430(2) 0.7429(2) 0.26821(18) 0.0385(7) Uani 1 1 d . . . H25 H 0.7586 0.7566 0.3118 0.046 Uiso 1 1 calc R . . H26 H 0.8052 0.7105 0.2496 0.046 Uiso 1 1 calc R . . C18 C 0.6850(2) 0.8208(3) 0.14526(17) 0.0395(7) Uani 1 1 d . . . H27 H 0.6447 0.8828 0.1109 0.047 Uiso 1 1 calc R . . H28 H 0.6595 0.7708 0.1448 0.047 Uiso 1 1 calc R . . H29 H 0.7524 0.7991 0.1331 0.047 Uiso 1 1 calc R . . C19 C 0.7241(2) 0.9093(3) 0.21593(19) 0.0413(8) Uani 1 1 d . . . H30 H 0.6853 0.9711 0.1809 0.050 Uiso 1 1 calc R . . H31 H 0.7917 0.8851 0.2043 0.050 Uiso 1 1 calc R . . H32 H 0.7227 0.9204 0.2624 0.050 Uiso 1 1 calc R . . C20 C 0.6015(2) 0.7288(2) 0.37977(16) 0.0337(7) Uani 1 1 d . . . H33 H 0.6402 0.7676 0.3834 0.040 Uiso 1 1 calc R . . H34 H 0.6375 0.6609 0.4097 0.040 Uiso 1 1 calc R . . C21 C 0.5043(2) 0.7721(2) 0.40652(15) 0.0331(7) Uani 1 1 d . . . C22 C 0.4756(2) 0.7150(2) 0.46199(16) 0.0362(7) Uani 1 1 d . . . H35 H 0.5196 0.6495 0.4839 0.043 Uiso 1 1 calc R . . C23 C 0.3850(2) 0.7507(2) 0.48613(16) 0.0361(7) Uani 1 1 d . . . C24 C 0.3502(3) 0.6872(2) 0.54554(16) 0.0410(8) Uani 1 1 d . . . C25 C 0.4351(3) 0.5940(3) 0.58572(19) 0.0517(10) Uani 1 1 d . . . H36 H 0.4638 0.5534 0.5541 0.062 Uiso 1 1 calc R . . H37 H 0.4114 0.5571 0.6246 0.062 Uiso 1 1 calc R . . H38 H 0.4846 0.6114 0.6043 0.062 Uiso 1 1 calc R . . C26 C 0.3019(3) 0.7440(3) 0.5975(2) 0.0567(10) Uani 1 1 d . . . H39 H 0.3435 0.7745 0.6106 0.068 Uiso 1 1 calc R . . H40 H 0.2928 0.6989 0.6395 0.068 Uiso 1 1 calc R . . H41 H 0.2383 0.7951 0.5758 0.068 Uiso 1 1 calc R . . C27 C 0.2769(4) 0.6568(4) 0.5146(2) 0.0652(12) Uani 1 1 d . . . H42 H 0.2609 0.6104 0.5518 0.078 Uiso 1 1 calc R . . H43 H 0.3054 0.6255 0.4780 0.078 Uiso 1 1 calc R . . H44 H 0.2173 0.7151 0.4943 0.078 Uiso 1 1 calc R . . C28 C 0.3228(2) 0.8468(2) 0.45141(16) 0.0354(7) Uani 1 1 d . . . H45 H 0.2599 0.8724 0.4668 0.042 Uiso 1 1 calc R . . C29 C 0.3471(2) 0.9080(2) 0.39548(16) 0.0324(6) Uani 1 1 d . . . C30 C 0.2728(2) 1.0121(2) 0.35836(17) 0.0360(7) Uani 1 1 d . . . C31 C 0.1808(3) 1.0424(3) 0.3968(2) 0.0522(10) Uani 1 1 d . . . H46 H 0.1996 1.0345 0.4459 0.063 Uiso 1 1 calc R . . H47 H 0.1454 1.0008 0.3947 0.063 Uiso 1 1 calc R . . H48 H 0.1388 1.1112 0.3743 0.063 Uiso 1 1 calc R . . C32 C 0.3170(3) 1.0881(2) 0.35578(19) 0.0411(8) Uani 1 1 d . . . H49 H 0.3385 1.0835 0.4036 0.049 Uiso 1 1 calc R . . H50 H 0.2677 1.1541 0.3340 0.049 Uiso 1 1 calc R . . H51 H 0.3730 1.0752 0.3281 0.049 Uiso 1 1 calc R . . C33 C 0.2430(3) 1.0144(3) 0.28411(19) 0.0469(9) Uani 1 1 d . . . H52 H 0.2014 0.9777 0.2864 0.056 Uiso 1 1 calc R . . H53 H 0.3016 0.9845 0.2619 0.056 Uiso 1 1 calc R . . H54 H 0.2071 1.0827 0.2565 0.056 Uiso 1 1 calc R . . C34 C 0.4403(2) 0.8695(2) 0.37231(15) 0.0325(7) Uani 1 1 d . . . C35 C 1.0164(2) 0.5507(2) 0.21068(15) 0.0285(6) Uani 1 1 d . . . C36 C 0.9490(2) 0.5043(2) 0.22228(16) 0.0302(6) Uani 1 1 d . . . C37 C 0.9519(2) 0.4328(2) 0.29331(17) 0.0357(7) Uani 1 1 d . . . C38 C 1.0479(3) 0.3414(2) 0.3067(2) 0.0460(8) Uani 1 1 d . . . H55 H 1.0512 0.3089 0.2697 0.055 Uiso 1 1 calc R . . H56 H 1.0505 0.2960 0.3524 0.055 Uiso 1 1 calc R . . H57 H 1.1032 0.3612 0.3064 0.055 Uiso 1 1 calc R . . C39 C 0.9475(2) 0.4792(2) 0.35378(17) 0.0378(7) Uani 1 1 d . . . H58 H 0.8862 0.5371 0.3469 0.045 Uiso 1 1 calc R . . H59 H 1.0027 0.4988 0.3546 0.045 Uiso 1 1 calc R . . H60 H 0.9507 0.4314 0.3984 0.045 Uiso 1 1 calc R . . C40 C 0.8677(3) 0.3977(3) 0.29674(19) 0.0444(8) Uani 1 1 d . . . H61 H 0.8703 0.3563 0.3441 0.053 Uiso 1 1 calc R . . H62 H 0.8740 0.3597 0.2629 0.053 Uiso 1 1 calc R . . H63 H 0.8052 0.4547 0.2853 0.053 Uiso 1 1 calc R . . C41 C 0.8845(2) 0.5210(2) 0.16530(16) 0.0323(6) Uani 1 1 d . . . H64 H 0.8394 0.4902 0.1730 0.039 Uiso 1 1 calc R . . C42 C 0.8813(2) 0.5799(2) 0.09766(16) 0.0323(7) Uani 1 1 d . . . C43 C 0.8105(2) 0.5912(2) 0.03706(17) 0.0362(7) Uani 1 1 d . . . C44 C 0.7056(3) 0.6301(4) 0.0547(2) 0.0642(12) Uani 1 1 d . . . H65 H 0.6859 0.6985 0.0556 0.077 Uiso 1 1 calc R . . H66 H 0.7006 0.5902 0.1008 0.077 Uiso 1 1 calc R . . H67 H 0.6628 0.6268 0.0191 0.077 Uiso 1 1 calc R . . C45 C 0.8166(4) 0.6627(4) -0.0306(2) 0.0728(14) Uani 1 1 d . . . H68 H 0.8001 0.6440 -0.0709 0.087 Uiso 1 1 calc R . . H69 H 0.8830 0.6609 -0.0318 0.087 Uiso 1 1 calc R . . H70 H 0.7705 0.7293 -0.0326 0.087 Uiso 1 1 calc R . . C46 C 0.8348(3) 0.4925(3) 0.0230(2) 0.0558(10) Uani 1 1 d . . . H71 H 0.7836 0.4976 -0.0103 0.067 Uiso 1 1 calc R . . H72 H 0.8391 0.4431 0.0670 0.067 Uiso 1 1 calc R . . H73 H 0.8975 0.4729 0.0031 0.067 Uiso 1 1 calc R . . C47 C 0.9487(2) 0.6231(2) 0.08786(16) 0.0314(6) Uani 1 1 d . . . H74 H 0.9495 0.6634 0.0427 0.038 Uiso 1 1 calc R . . C48 C 1.0153(2) 0.6090(2) 0.14269(15) 0.0291(6) Uani 1 1 d . . . C49 C 1.0913(2) 0.6513(2) 0.12908(15) 0.0309(6) Uani 1 1 d . . . H75 H 1.1567 0.5969 0.1411 0.037 Uiso 1 1 calc R . . H76 H 1.0848 0.6846 0.0783 0.037 Uiso 1 1 calc R . . C50 C 1.1694(2) 0.7517(2) 0.15610(16) 0.0328(7) Uani 1 1 d . . . H77 H 1.1525 0.8174 0.1632 0.039 Uiso 1 1 calc R . . H78 H 1.1844 0.7555 0.1070 0.039 Uiso 1 1 calc R . . C51 C 1.2581(2) 0.6776(2) 0.20577(16) 0.0333(7) Uani 1 1 d . . . H79 H 1.2793 0.6135 0.1952 0.040 Uiso 1 1 calc R . . H80 H 1.3124 0.7001 0.1991 0.040 Uiso 1 1 calc R . . C52 C 1.3139(2) 0.5783(2) 0.32465(17) 0.0379(7) Uani 1 1 d . . . H81 H 1.3160 0.5195 0.3127 0.045 Uiso 1 1 calc R . . H82 H 1.3017 0.5725 0.3739 0.045 Uiso 1 1 calc R . . H83 H 1.3764 0.5847 0.3174 0.045 Uiso 1 1 calc R . . C53 C 1.2280(2) 0.7528(2) 0.30181(18) 0.0382(7) Uani 1 1 d . . . H84 H 1.2118 0.7444 0.3504 0.046 Uiso 1 1 calc R . . H85 H 1.1770 0.8120 0.2713 0.046 Uiso 1 1 calc R . . H86 H 1.2908 0.7595 0.2987 0.046 Uiso 1 1 calc R . . C54 C 0.9913(2) 0.8083(2) 0.14703(15) 0.0311(6) Uani 1 1 d . . . H87 H 0.9374 0.7854 0.1554 0.037 Uiso 1 1 calc R . . H88 H 0.9871 0.8389 0.0960 0.037 Uiso 1 1 calc R . . C55 C 0.9779(2) 0.8846(2) 0.18512(15) 0.0299(6) Uani 1 1 d . . . C56 C 0.9676(2) 0.9785(2) 0.14658(16) 0.0345(7) Uani 1 1 d . . . H89 H 0.9707 0.9920 0.0973 0.041 Uiso 1 1 calc R . . C57 C 0.9529(2) 1.0529(2) 0.17834(17) 0.0379(7) Uani 1 1 d . . . C58 C 0.9472(3) 1.1536(3) 0.13513(19) 0.0472(9) Uani 1 1 d . . . C59 C 1.0448(4) 1.1373(3) 0.0992(3) 0.0756(14) Uani 1 1 d . . . H90 H 1.0697 1.0726 0.0905 0.091 Uiso 1 1 calc R . . H91 H 1.0934 1.1409 0.1302 0.091 Uiso 1 1 calc R . . H92 H 1.0320 1.1883 0.0546 0.091 Uiso 1 1 calc R . . C60 C 0.8663(4) 1.1989(3) 0.0775(2) 0.0788(15) Uani 1 1 d . . . H93 H 0.8907 1.1795 0.0354 0.095 Uiso 1 1 calc R . . H94 H 0.8409 1.2705 0.0672 0.095 Uiso 1 1 calc R . . H95 H 0.8139 1.1764 0.0919 0.095 Uiso 1 1 calc R . . C61 C 0.9468(5) 1.2187(4) 0.1787(3) 0.097(2) Uani 1 1 d . . . H96 H 0.8793 1.2569 0.1855 0.117 Uiso 1 1 calc R . . H97 H 0.9770 1.2635 0.1551 0.117 Uiso 1 1 calc R . . H98 H 0.9837 1.1789 0.2244 0.117 Uiso 1 1 calc R . . C62 C 0.9441(2) 1.0305(2) 0.24977(17) 0.0361(7) Uani 1 1 d . . . H99 H 0.9315 1.0812 0.2720 0.043 Uiso 1 1 calc R . . C63 C 0.9527(2) 0.9382(2) 0.29129(16) 0.0318(6) Uani 1 1 d . . . C64 C 0.9408(2) 0.9204(2) 0.37055(16) 0.0364(7) Uani 1 1 d . . . C65 C 0.9094(3) 1.0151(3) 0.39334(19) 0.0493(9) Uani 1 1 d . . . H100 H 0.8482 1.0635 0.3659 0.059 Uiso 1 1 calc R . . H101 H 0.9602 1.0414 0.3854 0.059 Uiso 1 1 calc R . . H102 H 0.8998 1.0007 0.4433 0.059 Uiso 1 1 calc R . . C66 C 0.8619(2) 0.8791(3) 0.38855(18) 0.0434(8) Uani 1 1 d . . . H103 H 0.7988 0.9279 0.3641 0.052 Uiso 1 1 calc R . . H104 H 0.8578 0.8639 0.4393 0.052 Uiso 1 1 calc R . . H105 H 0.8788 0.8191 0.3737 0.052 Uiso 1 1 calc R . . C67 C 1.0383(2) 0.8487(3) 0.41307(17) 0.0399(8) Uani 1 1 d . . . H106 H 1.0871 0.8776 0.4033 0.048 Uiso 1 1 calc R . . H107 H 1.0604 0.7871 0.3999 0.048 Uiso 1 1 calc R . . H108 H 1.0298 0.8355 0.4632 0.048 Uiso 1 1 calc R . . C68 C 0.9746(2) 0.8612(2) 0.25867(16) 0.0300(6) Uani 1 1 d . . . C69 C 0.4027(3) 1.0883(3) 0.14828(19) 0.0458(8) Uani 1 1 d . . . H110 H 0.3663 1.1163 0.1841 0.055 Uiso 1 1 calc R . . H111 H 0.3706 1.0514 0.1319 0.055 Uiso 1 1 calc R . . H112 H 0.4042 1.1413 0.1087 0.055 Uiso 1 1 calc R . . C70 C 1.0507(3) 0.6031(3) 0.44054(18) 0.0512(9) Uani 1 1 d . . . H114 H 1.0751 0.6216 0.4780 0.061 Uiso 1 1 calc R . . H115 H 1.0382 0.5439 0.4608 0.061 Uiso 1 1 calc R . . H116 H 0.9900 0.6568 0.4162 0.061 Uiso 1 1 calc R . . C71 C 0.6015(3) 0.9788(3) 0.4333(2) 0.0557(10) Uani 1 1 d . . . H118 H 0.5399 1.0221 0.4457 0.067 Uiso 1 1 calc R . . H119 H 0.6546 0.9964 0.4456 0.067 Uiso 1 1 calc R . . H120 H 0.6152 0.9105 0.4591 0.067 Uiso 1 1 calc R . . C72 C 0.6609(3) 1.1448(3) 0.2287(2) 0.0532(10) Uani 1 1 d . . . H122 H 0.6581 1.1810 0.1796 0.064 Uiso 1 1 calc R . . H123 H 0.7179 1.0823 0.2399 0.064 Uiso 1 1 calc R . . H124 H 0.6664 1.1839 0.2593 0.064 Uiso 1 1 calc R . . C73 C 1.2020(4) 0.3328(4) 0.4837(3) 0.0923(19) Uani 1 1 d . . . H126 H 1.2348 0.2741 0.4679 0.111 Uiso 1 1 calc R . . H127 H 1.1326 0.3625 0.4662 0.111 Uiso 1 1 calc R . . H128 H 1.2087 0.3145 0.5351 0.111 Uiso 1 1 calc R . . C74 C 1.4460(3) 0.2354(3) 0.3807(3) 0.0685(12) Uani 1 1 d . . . H130 H 1.4289 0.2047 0.3481 0.082 Uiso 1 1 calc R . . H131 H 1.4515 0.1951 0.4289 0.082 Uiso 1 1 calc R . . H132 H 1.5084 0.2409 0.3708 0.082 Uiso 1 1 calc R . . C75 C 1.2565(3) 0.3626(3) 0.2025(2) 0.0638(12) Uani 1 1 d . . . H134 H 1.1888 0.3825 0.1835 0.077 Uiso 1 1 calc R . . H135 H 1.2853 0.2914 0.2239 0.077 Uiso 1 1 calc R . . H136 H 1.2941 0.3802 0.1645 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0284(2) 0.0313(2) 0.0281(2) -0.00787(17) 0.00263(16) -0.01089(18) Co2 0.0301(2) 0.0322(2) 0.0261(2) -0.00850(17) 0.00483(16) -0.01459(18) O1 0.0336(11) 0.0310(11) 0.0302(11) -0.0053(9) -0.0016(9) -0.0121(9) O2 0.0349(11) 0.0320(11) 0.0332(11) -0.0092(9) 0.0058(9) -0.0132(10) O3 0.0333(11) 0.0308(11) 0.0293(11) -0.0077(9) 0.0012(9) -0.0128(9) O4 0.0357(11) 0.0325(11) 0.0272(10) -0.0068(9) 0.0089(9) -0.0154(9) O5 0.0374(12) 0.0346(12) 0.0369(12) -0.0070(9) 0.0013(9) -0.0138(10) O6 0.0441(13) 0.0439(13) 0.0285(11) -0.0046(10) 0.0052(10) -0.0174(11) O7 0.0536(15) 0.0784(19) 0.0402(14) -0.0230(13) 0.0106(11) -0.0383(15) O8 0.0599(16) 0.0490(15) 0.0473(15) -0.0152(12) 0.0020(12) -0.0238(13) O9 0.0658(19) 0.0619(19) 0.0603(18) -0.0025(15) 0.0048(15) -0.0154(16) O10 0.086(2) 0.074(2) 0.069(2) -0.0270(18) 0.0027(18) -0.0009(19) O11 0.0428(14) 0.0600(17) 0.078(2) -0.0388(15) 0.0037(13) -0.0110(13) N1 0.0273(13) 0.0325(13) 0.0286(13) -0.0092(10) 0.0020(10) -0.0089(11) N2 0.0307(13) 0.0375(14) 0.0330(14) -0.0125(11) 0.0058(11) -0.0146(12) N3 0.0287(13) 0.0343(13) 0.0287(12) -0.0110(10) 0.0083(10) -0.0164(11) N4 0.0283(13) 0.0352(14) 0.0320(13) -0.0109(11) 0.0055(10) -0.0151(11) C1 0.0278(15) 0.0317(15) 0.0298(15) -0.0079(12) 0.0043(12) -0.0132(13) C2 0.0325(16) 0.0344(16) 0.0276(15) -0.0034(12) 0.0043(12) -0.0162(13) C3 0.0457(19) 0.0407(18) 0.0287(16) -0.0003(13) -0.0020(14) -0.0238(16) C4 0.0411(19) 0.043(2) 0.048(2) 0.0050(16) -0.0080(16) -0.0195(17) C5 0.049(2) 0.046(2) 0.0336(17) 0.0026(15) 0.0031(15) -0.0270(17) C6 0.084(3) 0.052(2) 0.0346(19) 0.0013(16) -0.0120(19) -0.035(2) C7 0.0391(17) 0.0412(17) 0.0223(14) -0.0070(12) 0.0048(12) -0.0182(15) C8 0.0416(18) 0.0345(16) 0.0271(15) -0.0097(13) 0.0100(13) -0.0161(14) C9 0.061(2) 0.0367(18) 0.0304(16) -0.0126(14) 0.0112(15) -0.0181(17) C10 0.127(4) 0.049(2) 0.062(3) -0.013(2) -0.029(3) -0.042(3) C11 0.110(4) 0.056(3) 0.098(4) -0.043(3) 0.067(3) -0.038(3) C12 0.071(3) 0.0367(18) 0.0391(19) -0.0132(15) 0.0111(17) -0.0258(18) C13 0.0388(17) 0.0326(16) 0.0250(14) -0.0060(12) 0.0077(12) -0.0130(14) C14 0.0292(15) 0.0357(16) 0.0260(14) -0.0078(12) 0.0052(12) -0.0130(13) C15 0.0336(16) 0.0328(16) 0.0293(15) -0.0079(12) 0.0037(12) -0.0127(13) C16 0.0277(15) 0.0349(17) 0.0406(18) -0.0116(14) 0.0050(13) -0.0053(13) C17 0.0251(15) 0.0441(19) 0.0405(18) -0.0109(15) 0.0019(13) -0.0078(14) C18 0.0368(17) 0.0469(19) 0.0368(17) -0.0171(15) 0.0080(14) -0.0151(16) C19 0.0352(17) 0.045(2) 0.050(2) -0.0187(16) 0.0086(15) -0.0200(16) C20 0.0334(16) 0.0337(16) 0.0283(15) -0.0074(12) -0.0010(12) -0.0078(14) C21 0.0339(16) 0.0343(16) 0.0254(14) -0.0072(12) -0.0022(12) -0.0081(13) C22 0.0424(18) 0.0312(16) 0.0254(15) -0.0060(12) -0.0013(13) -0.0054(14) C23 0.0454(19) 0.0319(16) 0.0269(15) -0.0079(12) 0.0035(13) -0.0108(15) C24 0.053(2) 0.0379(18) 0.0259(15) -0.0035(13) 0.0063(14) -0.0146(16) C25 0.065(2) 0.041(2) 0.0335(18) -0.0004(15) 0.0091(17) -0.0116(19) C26 0.076(3) 0.048(2) 0.040(2) -0.0091(17) 0.0255(19) -0.021(2) C27 0.081(3) 0.076(3) 0.041(2) 0.003(2) 0.001(2) -0.045(3) C28 0.0397(17) 0.0355(17) 0.0313(16) -0.0113(13) 0.0080(13) -0.0140(14) C29 0.0346(16) 0.0291(15) 0.0300(15) -0.0084(12) 0.0037(12) -0.0089(13) C30 0.0351(17) 0.0304(16) 0.0393(17) -0.0061(13) 0.0071(14) -0.0120(14) C31 0.042(2) 0.0340(18) 0.066(3) -0.0020(17) 0.0146(18) -0.0075(16) C32 0.0425(19) 0.0317(17) 0.0465(19) -0.0100(14) 0.0064(15) -0.0126(15) C33 0.046(2) 0.0373(18) 0.049(2) -0.0016(15) -0.0062(16) -0.0139(16) C34 0.0360(16) 0.0348(16) 0.0261(14) -0.0081(12) 0.0029(12) -0.0136(14) C35 0.0299(15) 0.0294(15) 0.0280(14) -0.0096(12) 0.0041(12) -0.0124(13) C36 0.0319(15) 0.0289(15) 0.0308(15) -0.0110(12) 0.0082(12) -0.0115(13) C37 0.0382(17) 0.0337(16) 0.0369(17) -0.0088(13) 0.0099(13) -0.0170(14) C38 0.050(2) 0.0332(17) 0.050(2) -0.0067(15) 0.0130(17) -0.0149(16) C39 0.0400(18) 0.0400(18) 0.0327(16) -0.0080(14) 0.0071(14) -0.0166(15) C40 0.054(2) 0.046(2) 0.0427(19) -0.0112(16) 0.0144(16) -0.0306(18) C41 0.0339(16) 0.0327(16) 0.0363(16) -0.0143(13) 0.0084(13) -0.0166(14) C42 0.0336(16) 0.0344(16) 0.0310(15) -0.0134(13) 0.0030(12) -0.0127(14) C43 0.0365(17) 0.0406(18) 0.0362(17) -0.0155(14) 0.0018(13) -0.0170(15) C44 0.043(2) 0.094(3) 0.063(3) -0.046(3) 0.0014(19) -0.019(2) C45 0.090(3) 0.083(3) 0.048(2) 0.006(2) -0.028(2) -0.053(3) C46 0.061(2) 0.053(2) 0.053(2) -0.0285(19) -0.0080(19) -0.013(2) C47 0.0332(16) 0.0331(16) 0.0286(15) -0.0108(12) 0.0050(12) -0.0125(13) C48 0.0310(15) 0.0310(15) 0.0282(14) -0.0110(12) 0.0075(12) -0.0138(13) C49 0.0360(16) 0.0356(16) 0.0263(14) -0.0106(12) 0.0096(12) -0.0185(14) C50 0.0320(16) 0.0425(17) 0.0290(15) -0.0099(13) 0.0089(12) -0.0204(14) C51 0.0306(16) 0.0407(17) 0.0321(16) -0.0117(13) 0.0098(12) -0.0169(14) C52 0.0347(17) 0.0387(18) 0.0368(17) -0.0088(14) -0.0003(13) -0.0118(15) C53 0.0370(17) 0.0445(19) 0.0406(18) -0.0194(15) 0.0059(14) -0.0193(15) C54 0.0334(16) 0.0341(16) 0.0259(14) -0.0069(12) 0.0017(12) -0.0144(13) C55 0.0280(15) 0.0329(16) 0.0288(15) -0.0096(12) 0.0015(12) -0.0112(13) C56 0.0383(17) 0.0352(17) 0.0288(15) -0.0047(13) -0.0002(13) -0.0160(14) C57 0.0427(18) 0.0347(17) 0.0355(17) -0.0070(13) -0.0009(14) -0.0164(15) C58 0.060(2) 0.0352(18) 0.045(2) -0.0033(15) -0.0069(17) -0.0224(17) C59 0.092(4) 0.058(3) 0.079(3) -0.005(2) 0.012(3) -0.041(3) C60 0.113(4) 0.049(3) 0.061(3) 0.004(2) -0.029(3) -0.030(3) C61 0.192(7) 0.056(3) 0.056(3) -0.002(2) -0.018(3) -0.071(4) C62 0.0390(17) 0.0347(17) 0.0352(17) -0.0117(13) 0.0002(13) -0.0137(14) C63 0.0295(15) 0.0350(16) 0.0299(15) -0.0106(13) 0.0035(12) -0.0105(13) C64 0.0367(17) 0.0406(18) 0.0296(16) -0.0122(14) 0.0039(13) -0.0114(15) C65 0.058(2) 0.047(2) 0.0413(19) -0.0221(17) 0.0110(17) -0.0133(18) C66 0.0389(18) 0.056(2) 0.0340(17) -0.0155(16) 0.0126(14) -0.0161(17) C67 0.0425(19) 0.048(2) 0.0316(16) -0.0117(14) 0.0026(14) -0.0197(16) C68 0.0271(15) 0.0330(16) 0.0307(15) -0.0085(12) 0.0051(12) -0.0131(13) C69 0.0403(19) 0.0388(19) 0.043(2) -0.0002(15) 0.0001(15) -0.0070(16) C70 0.074(3) 0.058(2) 0.0315(18) -0.0145(16) 0.0207(17) -0.035(2) C71 0.052(2) 0.073(3) 0.041(2) -0.0197(19) 0.0058(17) -0.021(2) C72 0.069(3) 0.050(2) 0.049(2) -0.0139(18) 0.0045(19) -0.033(2) C73 0.077(3) 0.080(4) 0.095(4) 0.028(3) -0.027(3) -0.038(3) C74 0.065(3) 0.055(3) 0.087(3) -0.024(2) -0.003(2) -0.023(2) C75 0.073(3) 0.062(3) 0.070(3) -0.038(2) 0.027(2) -0.028(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 Co1 O1 1.930(2) . ? Co1 O2 1.972(2) . ? Co1 N1 2.142(3) . ? Co1 N2 2.153(3) . ? Co1 O5 2.154(2) . ? Co2 O4 1.935(2) . ? Co2 O3 1.982(2) . ? Co2 N4 2.142(2) . ? Co2 O6 2.147(2) . ? Co2 N3 2.176(2) . ? O1 C1 1.333(3) . ? O2 C34 1.351(4) . ? O3 C35 1.351(3) . ? O4 C68 1.335(4) . ? O5 C69 1.430(4) . ? O5 H109 0.8142 . ? O6 C70 1.423(4) . ? O6 H113 0.8261 . ? O7 C71 1.414(4) . ? O7 H117 0.8296 . ? O8 C72 1.428(5) . ? O8 H121 0.8261 . ? O9 C73 1.420(6) . ? O9 H125 0.9081 . ? O10 C74 1.396(5) . ? O10 H129 0.8920 . ? O11 C75 1.423(5) . ? O11 H133 0.8212 . ? N1 C16 1.473(4) . ? N1 C15 1.481(4) . ? N1 C20 1.493(4) . ? N2 C17 1.474(4) . ? N2 C19 1.477(4) . ? N2 C18 1.482(4) . ? N3 C54 1.480(4) . ? N3 C50 1.481(4) . ? N3 C49 1.484(4) . ? N4 C51 1.478(4) . ? N4 C52 1.480(4) . ? N4 C53 1.482(4) . ? C1 C14 1.408(4) . ? C1 C2 1.431(4) . ? C2 C7 1.392(4) . ? C2 C3 1.535(4) . ? C3 C6 1.534(5) . ? C3 C5 1.536(5) . ? C3 C4 1.541(5) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.393(4) . ? C7 H10 0.9500 . ? C8 C13 1.384(4) . ? C8 C9 1.538(4) . ? C9 C12 1.520(5) . ? C9 C10 1.521(5) . ? C9 C11 1.541(6) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.394(4) . ? C13 H20 0.9500 . ? C14 C15 1.508(4) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.516(5) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 H27 0.9800 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C19 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C20 C21 1.502(4) . ? C20 H33 0.9900 . ? C20 H34 0.9900 . ? C21 C22 1.392(4) . ? C21 C34 1.413(4) . ? C22 C23 1.384(5) . ? C22 H35 0.9500 . ? C23 C28 1.394(4) . ? C23 C24 1.544(5) . ? C24 C26 1.522(5) . ? C24 C25 1.524(5) . ? C24 C27 1.529(5) . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C26 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C27 H44 0.9800 . ? C28 C29 1.398(4) . ? C28 H45 0.9500 . ? C29 C34 1.412(4) . ? C29 C30 1.538(4) . ? C30 C33 1.530(5) . ? C30 C32 1.533(4) . ? C30 C31 1.536(5) . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? C33 H52 0.9800 . ? C33 H53 0.9800 . ? C33 H54 0.9800 . ? C35 C48 1.408(4) . ? C35 C36 1.424(4) . ? C36 C41 1.395(4) . ? C36 C37 1.533(4) . ? C37 C38 1.536(5) . ? C37 C39 1.537(4) . ? C37 C40 1.538(5) . ? C38 H55 0.9800 . ? C38 H56 0.9800 . ? C38 H57 0.9800 . ? C39 H58 0.9800 . ? C39 H59 0.9800 . ? C39 H60 0.9800 . ? C40 H61 0.9800 . ? C40 H62 0.9800 . ? C40 H63 0.9800 . ? C41 C42 1.399(4) . ? C41 H64 0.9500 . ? C42 C47 1.388(4) . ? C42 C43 1.537(4) . ? C43 C46 1.518(5) . ? C43 C44 1.520(5) . ? C43 C45 1.523(5) . ? C44 H65 0.9800 . ? C44 H66 0.9800 . ? C44 H67 0.9800 . ? C45 H68 0.9800 . ? C45 H69 0.9800 . ? C45 H70 0.9800 . ? C46 H71 0.9800 . ? C46 H72 0.9800 . ? C46 H73 0.9800 . ? C47 C48 1.395(4) . ? C47 H74 0.9500 . ? C48 C49 1.498(4) . ? C49 H75 0.9900 . ? C49 H76 0.9900 . ? C50 C51 1.516(4) . ? C50 H77 0.9900 . ? C50 H78 0.9900 . ? C51 H79 0.9900 . ? C51 H80 0.9900 . ? C52 H81 0.9800 . ? C52 H82 0.9800 . ? C52 H83 0.9800 . ? C53 H84 0.9800 . ? C53 H85 0.9800 . ? C53 H86 0.9800 . ? C54 C55 1.504(4) . ? C54 H87 0.9900 . ? C54 H88 0.9900 . ? C55 C56 1.394(4) . ? C55 C68 1.415(4) . ? C56 C57 1.390(4) . ? C56 H89 0.9500 . ? C57 C62 1.387(4) . ? C57 C58 1.529(5) . ? C58 C61 1.482(6) . ? C58 C60 1.488(5) . ? C58 C59 1.576(6) . ? C59 H90 0.9800 . ? C59 H91 0.9800 . ? C59 H92 0.9800 . ? C60 H93 0.9800 . ? C60 H94 0.9800 . ? C60 H95 0.9800 . ? C61 H96 0.9800 . ? C61 H97 0.9800 . ? C61 H98 0.9800 . ? C62 C63 1.399(4) . ? C62 H99 0.9500 . ? C63 C68 1.422(4) . ? C63 C64 1.546(4) . ? C64 C67 1.532(5) . ? C64 C65 1.534(5) . ? C64 C66 1.536(5) . ? C65 H100 0.9800 . ? C65 H101 0.9800 . ? C65 H102 0.9800 . ? C66 H103 0.9800 . ? C66 H104 0.9800 . ? C66 H105 0.9800 . ? C67 H106 0.9800 . ? C67 H107 0.9800 . ? C67 H108 0.9800 . ? C69 H110 0.9800 . ? C69 H111 0.9800 . ? C69 H112 0.9800 . ? C70 H114 0.9800 . ? C70 H115 0.9800 . ? C70 H116 0.9800 . ? C71 H118 0.9800 . ? C71 H119 0.9800 . ? C71 H120 0.9800 . ? C72 H122 0.9800 . ? C72 H123 0.9800 . ? C72 H124 0.9800 . ? C73 H126 0.9800 . ? C73 H127 0.9800 . ? C73 H128 0.9800 . ? C74 H130 0.9800 . ? C74 H131 0.9800 . ? C74 H132 0.9800 . ? C75 H134 0.9800 . ? C75 H135 0.9800 . ? C75 H136 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 117.11(9) . . ? O1 Co1 N1 92.89(9) . . ? O2 Co1 N1 90.77(9) . . ? O1 Co1 N2 112.44(9) . . ? O2 Co1 N2 130.18(9) . . ? N1 Co1 N2 81.83(10) . . ? O1 Co1 O5 95.18(9) . . ? O2 Co1 O5 90.91(9) . . ? N1 Co1 O5 169.93(9) . . ? N2 Co1 O5 89.50(9) . . ? O4 Co2 O3 126.29(9) . . ? O4 Co2 N4 113.03(9) . . ? O3 Co2 N4 120.53(9) . . ? O4 Co2 O6 90.97(9) . . ? O3 Co2 O6 90.98(9) . . ? N4 Co2 O6 91.88(9) . . ? O4 Co2 N3 92.73(9) . . ? O3 Co2 N3 90.57(9) . . ? N4 Co2 N3 82.39(9) . . ? O6 Co2 N3 174.06(9) . . ? C1 O1 Co1 128.01(18) . . ? C34 O2 Co1 124.89(19) . . ? C35 O3 Co2 121.12(18) . . ? C68 O4 Co2 123.91(18) . . ? C69 O5 Co1 121.1(2) . . ? C69 O5 H109 104.7 . . ? Co1 O5 H109 115.8 . . ? C70 O6 Co2 125.1(2) . . ? C70 O6 H113 109.4 . . ? Co2 O6 H113 120.6 . . ? C71 O7 H117 108.0 . . ? C72 O8 H121 113.5 . . ? C73 O9 H125 99.8 . . ? C74 O10 H129 103.1 . . ? C75 O11 H133 104.8 . . ? C16 N1 C15 111.0(2) . . ? C16 N1 C20 109.9(2) . . ? C15 N1 C20 109.8(2) . . ? C16 N1 Co1 107.97(19) . . ? C15 N1 Co1 109.68(18) . . ? C20 N1 Co1 108.49(18) . . ? C17 N2 C19 108.6(2) . . ? C17 N2 C18 109.9(2) . . ? C19 N2 C18 108.4(3) . . ? C17 N2 Co1 108.12(19) . . ? C19 N2 Co1 115.36(19) . . ? C18 N2 Co1 106.41(18) . . ? C54 N3 C50 111.5(2) . . ? C54 N3 C49 109.3(2) . . ? C50 N3 C49 108.9(2) . . ? C54 N3 Co2 109.21(17) . . ? C50 N3 Co2 107.44(17) . . ? C49 N3 Co2 110.46(18) . . ? C51 N4 C52 108.6(2) . . ? C51 N4 C53 110.4(2) . . ? C52 N4 C53 108.4(2) . . ? C51 N4 Co2 106.19(17) . . ? C52 N4 Co2 113.40(19) . . ? C53 N4 Co2 109.86(18) . . ? O1 C1 C14 120.8(3) . . ? O1 C1 C2 121.3(3) . . ? C14 C1 C2 117.8(3) . . ? C7 C2 C1 118.4(3) . . ? C7 C2 C3 121.0(3) . . ? C1 C2 C3 120.5(3) . . ? C6 C3 C2 112.6(3) . . ? C6 C3 C5 107.5(3) . . ? C2 C3 C5 110.4(3) . . ? C6 C3 C4 107.7(3) . . ? C2 C3 C4 109.6(3) . . ? C5 C3 C4 109.0(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 124.1(3) . . ? C2 C7 H10 118.0 . . ? C8 C7 H10 118.0 . . ? C13 C8 C7 116.6(3) . . ? C13 C8 C9 121.4(3) . . ? C7 C8 C9 122.0(3) . . ? C12 C9 C10 106.7(3) . . ? C12 C9 C8 111.7(3) . . ? C10 C9 C8 110.9(3) . . ? C12 C9 C11 108.5(3) . . ? C10 C9 C11 110.2(4) . . ? C8 C9 C11 108.9(3) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 122.2(3) . . ? C8 C13 H20 118.9 . . ? C14 C13 H20 118.9 . . ? C13 C14 C1 120.9(3) . . ? C13 C14 C15 118.1(3) . . ? C1 C14 C15 120.6(3) . . ? N1 C15 C14 114.7(3) . . ? N1 C15 H21 108.6 . . ? C14 C15 H21 108.6 . . ? N1 C15 H22 108.6 . . ? C14 C15 H22 108.6 . . ? H21 C15 H22 107.6 . . ? N1 C16 C17 110.0(3) . . ? N1 C16 H23 109.7 . . ? C17 C16 H23 109.7 . . ? N1 C16 H24 109.7 . . ? C17 C16 H24 109.7 . . ? H23 C16 H24 108.2 . . ? N2 C17 C16 109.7(2) . . ? N2 C17 H25 109.7 . . ? C16 C17 H25 109.7 . . ? N2 C17 H26 109.7 . . ? C16 C17 H26 109.7 . . ? H25 C17 H26 108.2 . . ? N2 C18 H27 109.5 . . ? N2 C18 H28 109.5 . . ? H27 C18 H28 109.5 . . ? N2 C18 H29 109.5 . . ? H27 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? N2 C19 H30 109.5 . . ? N2 C19 H31 109.5 . . ? H30 C19 H31 109.5 . . ? N2 C19 H32 109.5 . . ? H30 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? N1 C20 C21 112.3(2) . . ? N1 C20 H33 109.1 . . ? C21 C20 H33 109.1 . . ? N1 C20 H34 109.1 . . ? C21 C20 H34 109.1 . . ? H33 C20 H34 107.9 . . ? C22 C21 C34 120.4(3) . . ? C22 C21 C20 120.2(3) . . ? C34 C21 C20 119.3(3) . . ? C23 C22 C21 122.0(3) . . ? C23 C22 H35 119.0 . . ? C21 C22 H35 119.0 . . ? C22 C23 C28 116.6(3) . . ? C22 C23 C24 122.8(3) . . ? C28 C23 C24 120.5(3) . . ? C26 C24 C25 108.0(3) . . ? C26 C24 C27 109.0(4) . . ? C25 C24 C27 107.8(3) . . ? C26 C24 C23 110.7(3) . . ? C25 C24 C23 111.4(3) . . ? C27 C24 C23 109.8(3) . . ? C24 C25 H36 109.5 . . ? C24 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? C24 C25 H38 109.5 . . ? H36 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C24 C26 H39 109.5 . . ? C24 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? C24 C26 H41 109.5 . . ? H39 C26 H41 109.5 . . ? H40 C26 H41 109.5 . . ? C24 C27 H42 109.5 . . ? C24 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? C24 C27 H44 109.5 . . ? H42 C27 H44 109.5 . . ? H43 C27 H44 109.5 . . ? C23 C28 C29 124.2(3) . . ? C23 C28 H45 117.9 . . ? C29 C28 H45 117.9 . . ? C28 C29 C34 117.8(3) . . ? C28 C29 C30 120.9(3) . . ? C34 C29 C30 121.2(3) . . ? C33 C30 C32 110.5(3) . . ? C33 C30 C31 108.7(3) . . ? C32 C30 C31 106.3(3) . . ? C33 C30 C29 108.4(3) . . ? C32 C30 C29 110.7(3) . . ? C31 C30 C29 112.2(3) . . ? C30 C31 H46 109.5 . . ? C30 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? C30 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? C30 C32 H49 109.5 . . ? C30 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? C30 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? C30 C33 H52 109.5 . . ? C30 C33 H53 109.5 . . ? H52 C33 H53 109.5 . . ? C30 C33 H54 109.5 . . ? H52 C33 H54 109.5 . . ? H53 C33 H54 109.5 . . ? O2 C34 C29 122.2(3) . . ? O2 C34 C21 118.9(3) . . ? C29 C34 C21 118.9(3) . . ? O3 C35 C48 119.6(3) . . ? O3 C35 C36 121.9(3) . . ? C48 C35 C36 118.4(3) . . ? C41 C36 C35 117.6(3) . . ? C41 C36 C37 121.1(3) . . ? C35 C36 C37 121.2(3) . . ? C36 C37 C38 109.2(3) . . ? C36 C37 C39 111.5(3) . . ? C38 C37 C39 107.9(3) . . ? C36 C37 C40 112.9(3) . . ? C38 C37 C40 107.4(3) . . ? C39 C37 C40 107.6(3) . . ? C37 C38 H55 109.5 . . ? C37 C38 H56 109.5 . . ? H55 C38 H56 109.5 . . ? C37 C38 H57 109.5 . . ? H55 C38 H57 109.5 . . ? H56 C38 H57 109.5 . . ? C37 C39 H58 109.5 . . ? C37 C39 H59 109.5 . . ? H58 C39 H59 109.5 . . ? C37 C39 H60 109.5 . . ? H58 C39 H60 109.5 . . ? H59 C39 H60 109.5 . . ? C37 C40 H61 109.5 . . ? C37 C40 H62 109.5 . . ? H61 C40 H62 109.5 . . ? C37 C40 H63 109.5 . . ? H61 C40 H63 109.5 . . ? H62 C40 H63 109.5 . . ? C36 C41 C42 124.8(3) . . ? C36 C41 H64 117.6 . . ? C42 C41 H64 117.6 . . ? C47 C42 C41 116.3(3) . . ? C47 C42 C43 122.2(3) . . ? C41 C42 C43 121.4(3) . . ? C46 C43 C44 109.2(3) . . ? C46 C43 C45 107.8(3) . . ? C44 C43 C45 107.2(4) . . ? C46 C43 C42 109.7(3) . . ? C44 C43 C42 110.8(3) . . ? C45 C43 C42 112.0(3) . . ? C43 C44 H65 109.5 . . ? C43 C44 H66 109.5 . . ? H65 C44 H66 109.5 . . ? C43 C44 H67 109.5 . . ? H65 C44 H67 109.5 . . ? H66 C44 H67 109.5 . . ? C43 C45 H68 109.5 . . ? C43 C45 H69 109.5 . . ? H68 C45 H69 109.5 . . ? C43 C45 H70 109.5 . . ? H68 C45 H70 109.5 . . ? H69 C45 H70 109.5 . . ? C43 C46 H71 109.5 . . ? C43 C46 H72 109.5 . . ? H71 C46 H72 109.5 . . ? C43 C46 H73 109.5 . . ? H71 C46 H73 109.5 . . ? H72 C46 H73 109.5 . . ? C42 C47 C48 121.7(3) . . ? C42 C47 H74 119.2 . . ? C48 C47 H74 119.2 . . ? C47 C48 C35 121.3(3) . . ? C47 C48 C49 120.1(3) . . ? C35 C48 C49 118.5(3) . . ? N3 C49 C48 114.2(2) . . ? N3 C49 H75 108.7 . . ? C48 C49 H75 108.7 . . ? N3 C49 H76 108.7 . . ? C48 C49 H76 108.7 . . ? H75 C49 H76 107.6 . . ? N3 C50 C51 110.1(2) . . ? N3 C50 H77 109.6 . . ? C51 C50 H77 109.6 . . ? N3 C50 H78 109.6 . . ? C51 C50 H78 109.6 . . ? H77 C50 H78 108.1 . . ? N4 C51 C50 110.2(2) . . ? N4 C51 H79 109.6 . . ? C50 C51 H79 109.6 . . ? N4 C51 H80 109.6 . . ? C50 C51 H80 109.6 . . ? H79 C51 H80 108.1 . . ? N4 C52 H81 109.5 . . ? N4 C52 H82 109.5 . . ? H81 C52 H82 109.5 . . ? N4 C52 H83 109.5 . . ? H81 C52 H83 109.5 . . ? H82 C52 H83 109.5 . . ? N4 C53 H84 109.5 . . ? N4 C53 H85 109.5 . . ? H84 C53 H85 109.5 . . ? N4 C53 H86 109.5 . . ? H84 C53 H86 109.5 . . ? H85 C53 H86 109.5 . . ? N3 C54 C55 113.4(2) . . ? N3 C54 H87 108.9 . . ? C55 C54 H87 108.9 . . ? N3 C54 H88 108.9 . . ? C55 C54 H88 108.9 . . ? H87 C54 H88 107.7 . . ? C56 C55 C68 120.9(3) . . ? C56 C55 C54 118.9(3) . . ? C68 C55 C54 120.3(3) . . ? C57 C56 C55 121.7(3) . . ? C57 C56 H89 119.1 . . ? C55 C56 H89 119.1 . . ? C62 C57 C56 116.6(3) . . ? C62 C57 C58 123.0(3) . . ? C56 C57 C58 120.4(3) . . ? C61 C58 C60 114.1(4) . . ? C61 C58 C57 113.1(3) . . ? C60 C58 C57 110.9(3) . . ? C61 C58 C59 103.7(4) . . ? C60 C58 C59 106.6(4) . . ? C57 C58 C59 107.6(3) . . ? C58 C59 H90 109.5 . . ? C58 C59 H91 109.5 . . ? H90 C59 H91 109.5 . . ? C58 C59 H92 109.5 . . ? H90 C59 H92 109.5 . . ? H91 C59 H92 109.5 . . ? C58 C60 H93 109.5 . . ? C58 C60 H94 109.5 . . ? H93 C60 H94 109.5 . . ? C58 C60 H95 109.5 . . ? H93 C60 H95 109.5 . . ? H94 C60 H95 109.5 . . ? C58 C61 H96 109.5 . . ? C58 C61 H97 109.5 . . ? H96 C61 H97 109.5 . . ? C58 C61 H98 109.5 . . ? H96 C61 H98 109.5 . . ? H97 C61 H98 109.5 . . ? C57 C62 C63 124.4(3) . . ? C57 C62 H99 117.8 . . ? C63 C62 H99 117.8 . . ? C62 C63 C68 118.0(3) . . ? C62 C63 C64 120.7(3) . . ? C68 C63 C64 121.3(3) . . ? C67 C64 C65 107.4(3) . . ? C67 C64 C66 110.2(3) . . ? C65 C64 C66 107.1(3) . . ? C67 C64 C63 109.7(3) . . ? C65 C64 C63 112.5(3) . . ? C66 C64 C63 109.9(3) . . ? C64 C65 H100 109.5 . . ? C64 C65 H101 109.5 . . ? H100 C65 H101 109.5 . . ? C64 C65 H102 109.5 . . ? H100 C65 H102 109.5 . . ? H101 C65 H102 109.5 . . ? C64 C66 H103 109.5 . . ? C64 C66 H104 109.5 . . ? H103 C66 H104 109.5 . . ? C64 C66 H105 109.5 . . ? H103 C66 H105 109.5 . . ? H104 C66 H105 109.5 . . ? C64 C67 H106 109.5 . . ? C64 C67 H107 109.5 . . ? H106 C67 H107 109.5 . . ? C64 C67 H108 109.5 . . ? H106 C67 H108 109.5 . . ? H107 C67 H108 109.5 . . ? O4 C68 C55 120.0(3) . . ? O4 C68 C63 121.9(3) . . ? C55 C68 C63 118.1(3) . . ? O5 C69 H110 109.5 . . ? O5 C69 H111 109.5 . . ? H110 C69 H111 109.5 . . ? O5 C69 H112 109.5 . . ? H110 C69 H112 109.5 . . ? H111 C69 H112 109.5 . . ? O6 C70 H114 109.5 . . ? O6 C70 H115 109.5 . . ? H114 C70 H115 109.5 . . ? O6 C70 H116 109.5 . . ? H114 C70 H116 109.5 . . ? H115 C70 H116 109.5 . . ? O7 C71 H118 109.5 . . ? O7 C71 H119 109.5 . . ? H118 C71 H119 109.5 . . ? O7 C71 H120 109.5 . . ? H118 C71 H120 109.5 . . ? H119 C71 H120 109.5 . . ? O8 C72 H122 109.5 . . ? O8 C72 H123 109.5 . . ? H122 C72 H123 109.5 . . ? O8 C72 H124 109.5 . . ? H122 C72 H124 109.5 . . ? H123 C72 H124 109.5 . . ? O9 C73 H126 109.5 . . ? O9 C73 H127 109.5 . . ? H126 C73 H127 109.5 . . ? O9 C73 H128 109.5 . . ? H126 C73 H128 109.5 . . ? H127 C73 H128 109.5 . . ? O10 C74 H130 109.5 . . ? O10 C74 H131 109.5 . . ? H130 C74 H131 109.5 . . ? O10 C74 H132 109.5 . . ? H130 C74 H132 109.5 . . ? H131 C74 H132 109.5 . . ? O11 C75 H134 109.5 . . ? O11 C75 H135 109.5 . . ? H134 C75 H135 109.5 . . ? O11 C75 H136 109.5 . . ? H134 C75 H136 109.5 . . ? H135 C75 H136 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.054 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.070 #===END data_1C3H6O _database_code_depnum_ccdc_archive 'CCDC 766021' #TrackingRef 'Kozak_Compiled_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C34 H54 O2 N2) Co (C3 H6 O), 0.25(C3 H6 O)' _chemical_formula_sum 'C37.75 H61.50 Co N2 O3.25' _chemical_formula_weight 654.35 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 23.496(3) _cell_length_b 23.319(3) _cell_length_c 14.4917(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7940.3(16) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 30445 _cell_measurement_theta_min 1.9410 _cell_measurement_theta_max 30.9201 _exptl_crystal_description Irregular _exptl_crystal_colour Pink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 68663 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 26.50 _reflns_number_total 16419 _reflns_number_gt 15587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1033P)^2^+3.3656P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(13) _refine_ls_number_reflns 16419 _refine_ls_number_parameters 848 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.13474(2) 0.86090(2) 0.16791(4) 0.03959(13) Uani 1 1 d . . . Co2 Co 0.45318(2) 0.899451(19) 0.03983(4) 0.03467(12) Uani 1 1 d . . . O1 O 0.16989(13) 0.89987(11) 0.0652(2) 0.0428(6) Uani 1 1 d . . . O2 O 0.17310(13) 0.85870(12) 0.2850(2) 0.0462(7) Uani 1 1 d . . . O3 O 0.50721(12) 0.93471(11) 0.12311(18) 0.0395(6) Uani 1 1 d . . . O4 O 0.47061(12) 0.82834(11) -0.02140(19) 0.0408(6) Uani 1 1 d . A . O5 O 0.08874(15) 0.94161(14) 0.2002(2) 0.0592(8) Uani 1 1 d . B . O6 O 0.48564(14) 0.94789(13) -0.0810(2) 0.0532(7) Uani 1 1 d . . . O7 O 0.6694(4) 0.9335(4) 0.6920(10) 0.112(4) Uani 0.50 1 d P . . N1 N 0.16563(14) 0.77886(13) 0.1288(2) 0.0377(7) Uani 1 1 d . . . N2 N 0.05410(14) 0.82350(16) 0.1374(3) 0.0483(8) Uani 1 1 d . . . N3 N 0.40643(13) 0.85786(11) 0.14771(19) 0.0320(6) Uani 1 1 d . . . N4 N 0.37235(15) 0.93594(14) 0.0090(2) 0.0416(7) Uani 1 1 d . . . C1 C 0.18686(17) 0.87563(17) -0.0119(3) 0.0402(8) Uani 1 1 d . . . C2 C 0.18275(19) 0.90470(17) -0.0987(3) 0.0451(9) Uani 1 1 d . . . C3 C 0.1597(2) 0.96706(18) -0.1025(4) 0.0543(11) Uani 1 1 d . . . C4 C 0.1975(3) 1.0056(2) -0.0444(4) 0.0674(14) Uani 1 1 d . . . H1 H 0.1831 1.0065 0.0191 0.081 Uiso 1 1 calc R . . H2 H 0.1972 1.0445 -0.0700 0.081 Uiso 1 1 calc R . . H3 H 0.2364 0.9906 -0.0447 0.081 Uiso 1 1 calc R . . C5 C 0.0986(2) 0.9684(2) -0.0676(4) 0.0646(13) Uani 1 1 d . . . H4 H 0.0725 0.9622 -0.1193 0.078 Uiso 1 1 calc R . . H5 H 0.0908 1.0057 -0.0392 0.078 Uiso 1 1 calc R . . H6 H 0.0932 0.9380 -0.0216 0.078 Uiso 1 1 calc R . . C6 C 0.1595(3) 0.9905(2) -0.2025(4) 0.0733(15) Uani 1 1 d . . . H7 H 0.1958 1.0097 -0.2150 0.088 Uiso 1 1 calc R . . H8 H 0.1283 1.0180 -0.2097 0.088 Uiso 1 1 calc R . . H9 H 0.1544 0.9587 -0.2459 0.088 Uiso 1 1 calc R . . C7 C 0.2017(2) 0.8783(2) -0.1770(3) 0.0557(11) Uani 1 1 d . . . H10 H 0.1989 0.8986 -0.2338 0.067 Uiso 1 1 calc R . . C8 C 0.2250(3) 0.8226(2) -0.1781(3) 0.0609(12) Uani 1 1 d . . . C9 C 0.2463(4) 0.7973(3) -0.2695(4) 0.090(2) Uani 1 1 d . . . C10 C 0.1969(4) 0.7889(3) -0.3329(5) 0.114(3) Uani 1 1 d . . . H11 H 0.1801 0.7510 -0.3223 0.137 Uiso 1 1 calc R . . H12 H 0.2099 0.7917 -0.3970 0.137 Uiso 1 1 calc R . . H13 H 0.1683 0.8186 -0.3211 0.137 Uiso 1 1 calc R . . C11 C 0.2883(4) 0.8391(4) -0.3147(4) 0.110(3) Uani 1 1 d . . . H14 H 0.2675 0.8655 -0.3550 0.132 Uiso 1 1 calc R . . H15 H 0.3161 0.8175 -0.3513 0.132 Uiso 1 1 calc R . . H16 H 0.3081 0.8609 -0.2668 0.132 Uiso 1 1 calc R . . C12 C 0.2782(5) 0.7418(3) -0.2532(5) 0.128(4) Uani 1 1 d . . . H17 H 0.3189 0.7499 -0.2461 0.154 Uiso 1 1 calc R . . H18 H 0.2725 0.7161 -0.3059 0.154 Uiso 1 1 calc R . . H19 H 0.2639 0.7234 -0.1970 0.154 Uiso 1 1 calc R . . C13 C 0.2293(2) 0.79569(18) -0.0946(3) 0.0493(10) Uani 1 1 d . . . H20 H 0.2455 0.7584 -0.0929 0.059 Uiso 1 1 calc R . . C14 C 0.21128(18) 0.82001(16) -0.0125(3) 0.0401(8) Uani 1 1 d . . . C15 C 0.21879(16) 0.78696(16) 0.0762(3) 0.0390(8) Uani 1 1 d . . . H21 H 0.2350 0.7488 0.0616 0.047 Uiso 1 1 calc R . . H22 H 0.2466 0.8075 0.1156 0.047 Uiso 1 1 calc R . . C16 C 0.12017(18) 0.75204(17) 0.0730(3) 0.0446(9) Uani 1 1 d . . . H23 H 0.1276 0.7104 0.0668 0.053 Uiso 1 1 calc R . . H24 H 0.1198 0.7691 0.0104 0.053 Uiso 1 1 calc R . . C17 C 0.06257(19) 0.76149(19) 0.1192(3) 0.0508(10) Uani 1 1 d . . . H25 H 0.0318 0.7471 0.0787 0.061 Uiso 1 1 calc R . . H26 H 0.0610 0.7399 0.1780 0.061 Uiso 1 1 calc R . . C18 C 0.0324(2) 0.8523(2) 0.0528(4) 0.0529(10) Uani 1 1 d . . . H27 H 0.0100 0.8859 0.0703 0.064 Uiso 1 1 calc R . . H28 H 0.0085 0.8255 0.0181 0.064 Uiso 1 1 calc R . . H29 H 0.0646 0.8643 0.0144 0.064 Uiso 1 1 calc R . . C19 C 0.0119(2) 0.8318(3) 0.2118(4) 0.0632(12) Uani 1 1 d . . . H30 H 0.0140 0.7996 0.2551 0.076 Uiso 1 1 calc R . . H31 H -0.0263 0.8336 0.1851 0.076 Uiso 1 1 calc R . . H32 H 0.0201 0.8676 0.2445 0.076 Uiso 1 1 calc R . . C20 C 0.17687(19) 0.74435(17) 0.2131(3) 0.0437(9) Uani 1 1 d . . . H33 H 0.1893 0.7056 0.1940 0.052 Uiso 1 1 calc R . . H34 H 0.1407 0.7400 0.2476 0.052 Uiso 1 1 calc R . . C21 C 0.22043(18) 0.76871(17) 0.2764(3) 0.0411(8) Uani 1 1 d . . . C22 C 0.26438(18) 0.73251(16) 0.3072(3) 0.0428(9) Uani 1 1 d . . . H35 H 0.2668 0.6947 0.2830 0.051 Uiso 1 1 calc R . . C23 C 0.30379(17) 0.75009(16) 0.3710(3) 0.0412(8) Uani 1 1 d . . . C24 C 0.34601(19) 0.70734(17) 0.4157(3) 0.0458(9) Uani 1 1 d . . . C25 C 0.3680(3) 0.6656(3) 0.3465(4) 0.088(2) Uani 1 1 d . . . H36 H 0.3428 0.6322 0.3441 0.106 Uiso 1 1 calc R . . H37 H 0.4064 0.6534 0.3641 0.106 Uiso 1 1 calc R . . H38 H 0.3693 0.6839 0.2856 0.106 Uiso 1 1 calc R . . C26 C 0.3948(3) 0.7370(3) 0.4637(8) 0.141(5) Uani 1 1 d . . . H39 H 0.4264 0.7421 0.4203 0.169 Uiso 1 1 calc R . . H40 H 0.4074 0.7137 0.5161 0.169 Uiso 1 1 calc R . . H41 H 0.3822 0.7746 0.4860 0.169 Uiso 1 1 calc R . . C27 C 0.3134(3) 0.6738(2) 0.4888(4) 0.0742(16) Uani 1 1 d . . . H42 H 0.3159 0.6939 0.5480 0.089 Uiso 1 1 calc R . . H43 H 0.3300 0.6354 0.4951 0.089 Uiso 1 1 calc R . . H44 H 0.2734 0.6704 0.4704 0.089 Uiso 1 1 calc R . . C28 C 0.30141(18) 0.80740(16) 0.3992(3) 0.0410(8) Uani 1 1 d . . . H45 H 0.3294 0.8207 0.4415 0.049 Uiso 1 1 calc R . . C29 C 0.26010(18) 0.84623(18) 0.3686(3) 0.0421(8) Uani 1 1 d . . . C30 C 0.2599(2) 0.90777(18) 0.4032(3) 0.0497(10) Uani 1 1 d . . . C31 C 0.3131(2) 0.9235(2) 0.4585(4) 0.0639(13) Uani 1 1 d . . . H46 H 0.3067 0.9151 0.5240 0.077 Uiso 1 1 calc R . . H47 H 0.3212 0.9645 0.4510 0.077 Uiso 1 1 calc R . . H48 H 0.3455 0.9011 0.4362 0.077 Uiso 1 1 calc R . . C32 C 0.2070(3) 0.9181(2) 0.4634(3) 0.0641(13) Uani 1 1 d . . . H49 H 0.1755 0.9313 0.4245 0.077 Uiso 1 1 calc R . . H50 H 0.2156 0.9473 0.5100 0.077 Uiso 1 1 calc R . . H51 H 0.1962 0.8822 0.4941 0.077 Uiso 1 1 calc R . . C33 C 0.2599(2) 0.94918(18) 0.3196(3) 0.0562(11) Uani 1 1 d . . . H52 H 0.2992 0.9582 0.3023 0.067 Uiso 1 1 calc R . . H53 H 0.2399 0.9846 0.3362 0.067 Uiso 1 1 calc R . . H54 H 0.2405 0.9309 0.2674 0.067 Uiso 1 1 calc R . . C34 C 0.21693(18) 0.82582(16) 0.3096(3) 0.0397(8) Uani 1 1 d . . . C35 C 0.52372(17) 0.91051(15) 0.2027(2) 0.0355(7) Uani 1 1 d . . . C36 C 0.58151(17) 0.91499(16) 0.2335(3) 0.0374(8) Uani 1 1 d . . . C37 C 0.62530(17) 0.95080(17) 0.1790(3) 0.0430(8) Uani 1 1 d . . . C38 C 0.63429(18) 0.92367(19) 0.0840(3) 0.0473(9) Uani 1 1 d . . . H55 H 0.6652 0.8956 0.0874 0.057 Uiso 1 1 calc R . . H56 H 0.6442 0.9536 0.0393 0.057 Uiso 1 1 calc R . . H57 H 0.5992 0.9044 0.0645 0.057 Uiso 1 1 calc R . . C39 C 0.60377(19) 1.01264(17) 0.1704(3) 0.0490(9) Uani 1 1 d . . . H58 H 0.5810 1.0164 0.1140 0.059 Uiso 1 1 calc R . . H59 H 0.6363 1.0389 0.1675 0.059 Uiso 1 1 calc R . . H60 H 0.5802 1.0221 0.2241 0.059 Uiso 1 1 calc R . . C40 C 0.6835(2) 0.9524(2) 0.2269(3) 0.0556(11) Uani 1 1 d . . . H61 H 0.6849 0.9851 0.2692 0.067 Uiso 1 1 calc R . . H62 H 0.7135 0.9563 0.1804 0.067 Uiso 1 1 calc R . . H63 H 0.6892 0.9168 0.2616 0.067 Uiso 1 1 calc R . . C41 C 0.59723(17) 0.88622(16) 0.3136(3) 0.0384(8) Uani 1 1 d . . . H64 H 0.6358 0.8882 0.3328 0.046 Uiso 1 1 calc R . . C42 C 0.55883(17) 0.85427(16) 0.3677(3) 0.0373(8) Uani 1 1 d . . . C43 C 0.57769(19) 0.82297(18) 0.4553(3) 0.0454(9) Uani 1 1 d . . . C44 C 0.6408(2) 0.8316(2) 0.4771(3) 0.0572(11) Uani 1 1 d . . . H65 H 0.6632 0.8014 0.4470 0.069 Uiso 1 1 calc R . . H66 H 0.6466 0.8296 0.5440 0.069 Uiso 1 1 calc R . . H67 H 0.6531 0.8691 0.4544 0.069 Uiso 1 1 calc R . . C45 C 0.5428(2) 0.8457(2) 0.5376(4) 0.0594(11) Uani 1 1 d . . . H68 H 0.5628 0.8781 0.5659 0.071 Uiso 1 1 calc R . . H69 H 0.5380 0.8151 0.5833 0.071 Uiso 1 1 calc R . . H70 H 0.5053 0.8584 0.5159 0.071 Uiso 1 1 calc R . . C46 C 0.5674(3) 0.7587(2) 0.4448(4) 0.0617(12) Uani 1 1 d . . . H71 H 0.5290 0.7493 0.4666 0.074 Uiso 1 1 calc R . . H72 H 0.5955 0.7375 0.4815 0.074 Uiso 1 1 calc R . . H73 H 0.5710 0.7479 0.3797 0.074 Uiso 1 1 calc R . . C47 C 0.50302(18) 0.85372(16) 0.3390(3) 0.0392(8) Uani 1 1 d . . . H74 H 0.4758 0.8335 0.3750 0.047 Uiso 1 1 calc R . . C48 C 0.48467(17) 0.88180(15) 0.2588(2) 0.0372(8) Uani 1 1 d . . . C49 C 0.42236(16) 0.88428(16) 0.2375(2) 0.0348(7) Uani 1 1 d . . . H75 H 0.4013 0.8645 0.2874 0.042 Uiso 1 1 calc R . . H76 H 0.4102 0.9249 0.2372 0.042 Uiso 1 1 calc R . . C50 C 0.34534(16) 0.86627(15) 0.1281(3) 0.0365(7) Uani 1 1 d . . . H77 H 0.3231 0.8614 0.1856 0.044 Uiso 1 1 calc R . . H78 H 0.3324 0.8371 0.0832 0.044 Uiso 1 1 calc R . . C51 C 0.33504(17) 0.92536(17) 0.0893(3) 0.0429(8) Uani 1 1 d . . . H79 H 0.2947 0.9289 0.0703 0.051 Uiso 1 1 calc R . . H80 H 0.3426 0.9544 0.1375 0.051 Uiso 1 1 calc R . . C52 C 0.3742(2) 0.99813(18) -0.0090(4) 0.0553(11) Uani 1 1 d . . . H81 H 0.3686 1.0190 0.0489 0.066 Uiso 1 1 calc R . . H82 H 0.3440 1.0084 -0.0526 0.066 Uiso 1 1 calc R . . H83 H 0.4113 1.0083 -0.0354 0.066 Uiso 1 1 calc R . . C53 C 0.34992(19) 0.90696(19) -0.0743(3) 0.0467(9) Uani 1 1 d . . . H84 H 0.3624 0.9277 -0.1295 0.056 Uiso 1 1 calc R . . H85 H 0.3082 0.9064 -0.0720 0.056 Uiso 1 1 calc R . . H86 H 0.3643 0.8675 -0.0766 0.056 Uiso 1 1 calc R . . C54 C 0.41979(17) 0.79590(14) 0.1524(3) 0.0367(8) Uani 1 1 d . . . H87 H 0.3956 0.7781 0.2004 0.044 Uiso 1 1 calc R . . H88 H 0.4599 0.7914 0.1720 0.044 Uiso 1 1 calc R . . C55 C 0.41133(16) 0.76369(15) 0.0632(3) 0.0368(8) Uani 1 1 d . A . C56 C 0.3438(2) 0.61923(17) -0.0070(3) 0.0489(10) Uani 1 1 d . . . C57 C 0.37907(17) 0.71308(16) 0.0656(3) 0.0389(8) Uani 1 1 d . . . H89 H 0.3591 0.7034 0.1204 0.047 Uiso 1 1 calc R A . C58 C 0.37572(19) 0.67676(17) -0.0106(3) 0.0435(9) Uani 1 1 d . A . C59 C 0.3140(6) 0.6087(5) 0.0891(8) 0.068(3) Uani 0.50 1 d P A 1 C60 C 0.2948(7) 0.6189(6) -0.0783(10) 0.082(4) Uani 0.50 1 d P A 1 C61 C 0.3850(7) 0.5704(5) -0.0245(14) 0.090(5) Uani 0.50 1 d P A 1 C62 C 0.2857(6) 0.6299(6) 0.0330(19) 0.110(7) Uani 0.50 1 d P A 2 C63 C 0.3359(10) 0.5950(7) -0.1031(11) 0.102(6) Uani 0.50 1 d P A 2 C64 C 0.3838(8) 0.5775(5) 0.0473(17) 0.109(7) Uani 0.50 1 d P A 2 C65 C 0.4054(2) 0.69311(17) -0.0896(3) 0.0486(9) Uani 1 1 d . . . H90 H 0.4039 0.6684 -0.1418 0.058 Uiso 1 1 calc R A . C66 C 0.4371(2) 0.74351(17) -0.0968(3) 0.0452(9) Uani 1 1 d . A . C67 C 0.4704(2) 0.7575(2) -0.1849(3) 0.0554(11) Uani 1 1 d . . . C68 C 0.4609(4) 0.7124(3) -0.2613(4) 0.090(2) Uani 1 1 d . A . H91 H 0.4893 0.6819 -0.2554 0.108 Uiso 1 1 calc R . . H92 H 0.4645 0.7307 -0.3219 0.108 Uiso 1 1 calc R . . H93 H 0.4227 0.6960 -0.2550 0.108 Uiso 1 1 calc R . . C69 C 0.5345(2) 0.7618(3) -0.1644(4) 0.0660(13) Uani 1 1 d . A . H94 H 0.5441 0.8014 -0.1482 0.079 Uiso 1 1 calc R . . H95 H 0.5561 0.7503 -0.2192 0.079 Uiso 1 1 calc R . . H96 H 0.5441 0.7364 -0.1128 0.079 Uiso 1 1 calc R . . C70 C 0.4509(2) 0.8158(2) -0.2246(3) 0.0622(13) Uani 1 1 d . A . H97 H 0.4197 0.8096 -0.2683 0.075 Uiso 1 1 calc R . . H98 H 0.4829 0.8342 -0.2564 0.075 Uiso 1 1 calc R . . H99 H 0.4378 0.8405 -0.1742 0.075 Uiso 1 1 calc R . . C71 C 0.44029(17) 0.78016(15) -0.0183(3) 0.0371(8) Uani 1 1 d . . . C72 C 0.0909(9) 1.0483(4) 0.1661(10) 0.163(7) Uani 0.75 1 d P B 3 H100 H 0.1048 1.0532 0.1029 0.196 Uiso 0.75 1 calc PR B 3 H101 H 0.1012 1.0820 0.2029 0.196 Uiso 0.75 1 calc PR B 3 H102 H 0.0494 1.0440 0.1653 0.196 Uiso 0.75 1 calc PR B 3 C75 C 0.0332(11) 0.9848(14) 0.323(2) 0.100(10) Uani 0.25 1 d P B 4 H103 H 0.0209 1.0220 0.2987 0.120 Uiso 0.25 1 calc PR B 4 H104 H 0.0336 0.9862 0.3906 0.120 Uiso 0.25 1 calc PR B 4 H105 H 0.0068 0.9549 0.3025 0.120 Uiso 0.25 1 calc PR B 4 C73 C 0.1166(4) 0.9971(3) 0.2068(6) 0.092(2) Uani 1 1 d . . . C74 C 0.0930(4) 0.9712(3) 0.2877(5) 0.089(2) Uani 1 1 d . B . C76 C 0.5446(3) 0.9487(3) -0.2255(4) 0.0722(15) Uani 1 1 d . . . H106 H 0.5455 0.9092 -0.2485 0.087 Uiso 1 1 calc R . . H107 H 0.5791 0.9688 -0.2452 0.087 Uiso 1 1 calc R . . H108 H 0.5111 0.9684 -0.2505 0.087 Uiso 1 1 calc R . . C77 C 0.5415(2) 0.9482(3) -0.1225(4) 0.0646(13) Uani 1 1 d . . . H109 H 0.5708 0.9242 -0.0907 0.077 Uiso 1 1 calc R . . C78 C 0.5227(3) 0.9974(2) -0.0725(4) 0.0680(15) Uani 1 1 d . . . H110 H 0.5127 1.0321 -0.1083 0.082 Uiso 1 1 calc R . . H111 H 0.5402 1.0049 -0.0116 0.082 Uiso 1 1 calc R . . C79 C 0.6659(13) 0.8683(10) 0.8249(14) 0.163(11) Uani 0.50 1 d P . . H112 H 0.7010 0.8737 0.8602 0.195 Uiso 0.50 1 calc PR . . H113 H 0.6520 0.8290 0.8335 0.195 Uiso 0.50 1 calc PR . . H114 H 0.6370 0.8954 0.8466 0.195 Uiso 0.50 1 calc PR . . C80 C 0.6769(8) 0.8781(8) 0.7291(12) 0.099(5) Uani 0.50 1 d P . . H115 H 0.6591 0.8480 0.6893 0.119 Uiso 0.50 1 calc PR . . C81 C 0.7236(8) 0.9029(7) 0.6872(12) 0.099(5) Uani 0.50 1 d P . . H116 H 0.7356 0.8876 0.6265 0.119 Uiso 0.50 1 calc PR . . H117 H 0.7550 0.9163 0.7272 0.119 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 Co1 0.0427(3) 0.0380(2) 0.0380(3) -0.0014(2) 0.0007(2) 0.0011(2) Co2 0.0424(2) 0.0315(2) 0.0301(2) 0.00116(19) 0.0005(2) -0.00447(19) O1 0.0524(16) 0.0313(12) 0.0447(16) 0.0000(10) 0.0056(12) 0.0013(11) O2 0.0533(17) 0.0427(15) 0.0427(15) -0.0032(12) -0.0004(13) 0.0086(12) O3 0.0485(15) 0.0392(13) 0.0307(12) 0.0051(11) -0.0018(11) -0.0075(11) O4 0.0475(14) 0.0390(13) 0.0360(13) -0.0002(11) 0.0050(11) -0.0073(11) O5 0.0636(19) 0.0536(17) 0.060(2) -0.0128(15) -0.0015(16) 0.0195(15) O6 0.0676(19) 0.0483(16) 0.0438(16) 0.0080(13) 0.0060(14) -0.0159(14) O7 0.085(6) 0.087(6) 0.163(11) 0.026(7) 0.002(7) 0.020(5) N1 0.0425(16) 0.0329(14) 0.0377(16) 0.0010(12) 0.0008(13) -0.0046(13) N2 0.0434(18) 0.0491(19) 0.052(2) 0.0061(16) -0.0008(15) -0.0033(15) N3 0.0358(15) 0.0305(14) 0.0299(15) -0.0014(11) 0.0031(11) 0.0020(11) N4 0.0535(19) 0.0363(16) 0.0350(16) 0.0059(13) -0.0010(13) -0.0010(14) C1 0.044(2) 0.0368(18) 0.040(2) 0.0014(15) 0.0006(16) -0.0073(16) C2 0.051(2) 0.0373(19) 0.047(2) 0.0068(16) -0.0008(18) 0.0031(16) C3 0.065(3) 0.038(2) 0.061(3) 0.0129(19) 0.004(2) 0.0030(19) C4 0.075(3) 0.043(2) 0.084(4) 0.014(2) -0.003(3) -0.003(2) C5 0.062(3) 0.050(3) 0.082(4) 0.017(2) 0.006(3) 0.019(2) C6 0.087(4) 0.055(3) 0.077(4) 0.026(3) 0.007(3) 0.012(3) C7 0.072(3) 0.054(2) 0.041(2) 0.0112(19) -0.004(2) 0.011(2) C8 0.085(3) 0.059(3) 0.038(2) -0.004(2) -0.001(2) 0.019(3) C9 0.152(7) 0.081(4) 0.036(2) -0.003(2) 0.001(3) 0.037(4) C10 0.190(9) 0.093(5) 0.058(4) -0.026(4) 0.006(5) -0.006(5) C11 0.142(7) 0.139(7) 0.048(3) 0.015(4) 0.026(4) 0.042(6) C12 0.237(11) 0.096(5) 0.051(3) -0.016(3) 0.022(5) 0.077(6) C13 0.061(3) 0.043(2) 0.044(2) 0.0016(17) 0.0033(19) 0.0105(18) C14 0.047(2) 0.0352(18) 0.0380(19) -0.0008(15) -0.0008(16) -0.0003(16) C15 0.0377(19) 0.0374(18) 0.0420(19) 0.0029(16) 0.0029(16) 0.0024(15) C16 0.050(2) 0.0361(19) 0.047(2) -0.0019(16) -0.0063(17) -0.0049(17) C17 0.048(2) 0.052(2) 0.052(2) 0.002(2) -0.0069(19) -0.0075(19) C18 0.052(2) 0.052(2) 0.055(3) 0.003(2) -0.008(2) -0.0003(19) C19 0.054(3) 0.075(3) 0.061(3) 0.004(3) 0.011(2) -0.004(2) C20 0.053(2) 0.0389(19) 0.0391(19) 0.0041(16) 0.0016(17) -0.0086(17) C21 0.049(2) 0.0372(18) 0.0372(19) 0.0022(15) 0.0039(16) -0.0006(16) C22 0.057(2) 0.0313(17) 0.040(2) 0.0050(15) 0.0010(17) -0.0012(16) C23 0.049(2) 0.0369(18) 0.0381(19) 0.0066(15) 0.0041(16) 0.0003(16) C24 0.051(2) 0.0412(19) 0.045(2) 0.0078(17) -0.0010(18) 0.0012(17) C25 0.106(5) 0.107(5) 0.052(3) 0.017(3) 0.016(3) 0.065(4) C26 0.100(5) 0.061(3) 0.260(12) 0.057(5) -0.114(7) -0.020(4) C27 0.099(4) 0.064(3) 0.059(3) 0.024(3) 0.019(3) 0.027(3) C28 0.053(2) 0.0394(19) 0.0308(17) 0.0010(15) 0.0006(16) 0.0037(16) C29 0.050(2) 0.044(2) 0.0331(18) -0.0015(16) 0.0014(16) 0.0040(17) C30 0.070(3) 0.045(2) 0.0348(19) -0.0083(16) -0.0004(19) 0.0089(19) C31 0.089(4) 0.049(3) 0.054(3) -0.018(2) -0.013(3) 0.000(2) C32 0.086(4) 0.066(3) 0.040(2) -0.005(2) 0.005(2) 0.020(3) C33 0.083(3) 0.038(2) 0.047(2) -0.0034(18) -0.003(2) 0.003(2) C34 0.052(2) 0.0388(19) 0.0285(17) 0.0018(14) 0.0039(16) 0.0022(16) C35 0.046(2) 0.0316(16) 0.0284(16) -0.0035(13) -0.0019(14) -0.0054(15) C36 0.045(2) 0.0349(17) 0.0322(17) -0.0022(14) 0.0033(15) -0.0028(15) C37 0.048(2) 0.0422(19) 0.039(2) -0.0007(16) 0.0020(17) -0.0119(16) C38 0.053(2) 0.050(2) 0.039(2) 0.0022(18) 0.0051(18) -0.0094(18) C39 0.057(2) 0.044(2) 0.046(2) -0.0028(19) 0.006(2) -0.0187(17) C40 0.049(2) 0.068(3) 0.049(2) 0.003(2) 0.0014(19) -0.021(2) C41 0.043(2) 0.0411(18) 0.0313(17) -0.0022(15) -0.0024(15) -0.0047(16) C42 0.047(2) 0.0342(17) 0.0310(17) -0.0026(14) 0.0008(15) -0.0042(15) C43 0.052(2) 0.048(2) 0.0366(19) 0.0036(16) -0.0023(17) 0.0008(18) C44 0.064(3) 0.062(3) 0.045(2) 0.009(2) -0.014(2) -0.004(2) C45 0.069(3) 0.076(3) 0.0330(19) 0.002(2) 0.002(2) 0.000(2) C46 0.084(3) 0.050(2) 0.052(3) 0.013(2) -0.006(2) -0.007(2) C47 0.049(2) 0.0372(18) 0.0309(17) -0.0025(14) 0.0013(16) -0.0029(16) C48 0.050(2) 0.0318(16) 0.0299(17) -0.0046(14) 0.0021(15) -0.0038(15) C49 0.0404(19) 0.0343(17) 0.0296(16) -0.0046(14) 0.0039(14) -0.0029(15) C50 0.0361(18) 0.0388(18) 0.0346(17) -0.0009(14) 0.0019(15) -0.0017(14) C51 0.042(2) 0.043(2) 0.043(2) -0.0031(17) 0.0019(16) 0.0073(17) C52 0.066(3) 0.039(2) 0.061(3) 0.008(2) -0.006(2) 0.0046(19) C53 0.049(2) 0.051(2) 0.040(2) -0.0002(17) -0.0075(18) -0.0016(18) C54 0.0458(19) 0.0288(16) 0.0355(19) 0.0044(13) 0.0025(15) -0.0006(14) C55 0.0413(18) 0.0315(16) 0.0377(19) -0.0010(13) -0.0012(14) 0.0005(14) C56 0.063(3) 0.0325(19) 0.052(2) -0.0067(18) 0.003(2) -0.0124(19) C57 0.0447(19) 0.0318(17) 0.040(2) -0.0003(14) -0.0009(15) -0.0022(15) C58 0.053(2) 0.0324(18) 0.045(2) -0.0057(16) 0.0000(18) -0.0066(16) C59 0.095(9) 0.046(5) 0.064(6) -0.002(5) 0.017(6) -0.035(6) C60 0.095(9) 0.073(8) 0.077(8) -0.006(7) -0.007(7) -0.050(7) C61 0.099(10) 0.045(6) 0.124(13) -0.031(8) 0.038(10) -0.009(6) C62 0.069(8) 0.061(7) 0.20(2) -0.031(11) 0.030(12) -0.036(6) C63 0.155(16) 0.077(9) 0.073(9) -0.025(7) -0.001(10) -0.066(10) C64 0.111(11) 0.039(6) 0.178(18) 0.036(9) -0.065(14) -0.029(7) C65 0.067(3) 0.041(2) 0.037(2) -0.0115(17) 0.0024(19) -0.0086(19) C66 0.065(3) 0.0401(19) 0.0310(18) -0.0028(15) 0.0032(18) -0.0050(18) C67 0.072(3) 0.059(3) 0.035(2) -0.0104(19) 0.016(2) -0.013(2) C68 0.149(6) 0.075(4) 0.047(3) -0.027(3) 0.037(3) -0.034(4) C69 0.070(3) 0.074(3) 0.054(3) -0.003(2) 0.029(2) 0.001(3) C70 0.087(4) 0.062(3) 0.038(2) 0.007(2) 0.006(2) -0.016(3) C71 0.047(2) 0.0286(16) 0.0353(18) -0.0038(14) 0.0005(15) 0.0007(15) C72 0.31(2) 0.060(5) 0.121(10) -0.005(6) 0.041(13) 0.034(9) C75 0.070(14) 0.13(2) 0.102(19) -0.085(19) 0.017(14) 0.013(15) C73 0.112(5) 0.048(3) 0.116(6) -0.011(3) -0.004(4) 0.011(3) C74 0.118(5) 0.075(4) 0.073(4) -0.030(3) -0.001(4) 0.026(4) C76 0.087(4) 0.082(4) 0.048(3) 0.013(3) 0.011(3) -0.009(3) C77 0.072(3) 0.075(3) 0.047(3) 0.014(2) 0.003(2) -0.011(3) C78 0.099(4) 0.050(2) 0.055(3) 0.011(2) 0.000(3) -0.029(3) C79 0.27(3) 0.134(17) 0.088(13) -0.017(12) -0.028(17) 0.079(19) C80 0.108(12) 0.096(10) 0.094(11) -0.005(9) -0.023(9) -0.010(9) C81 0.120(12) 0.092(10) 0.084(10) -0.001(7) -0.002(9) 0.018(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 O2 1.922(3) . ? Co1 O1 1.930(3) . ? Co1 N1 2.123(3) . ? Co1 N2 2.132(4) . ? Co1 O5 2.220(3) . ? Co2 O4 1.925(3) . ? Co2 O3 1.935(3) . ? Co2 N4 2.129(4) . ? Co2 N3 2.143(3) . ? Co2 O6 2.219(3) . ? O1 C1 1.314(5) . ? O2 C34 1.332(5) . ? O3 C35 1.341(4) . ? O4 C71 1.331(5) . ? O5 C74 1.448(7) . ? O5 C73 1.453(8) . ? O6 C77 1.444(6) . ? O6 C78 1.450(5) . ? O7 C80 1.410(19) . ? O7 C81 1.461(19) . ? N1 C15 1.476(5) . ? N1 C16 1.479(5) . ? N1 C20 1.486(5) . ? N2 C19 1.476(6) . ? N2 C17 1.483(6) . ? N2 C18 1.487(6) . ? N3 C50 1.477(5) . ? N3 C54 1.480(4) . ? N3 C49 1.487(4) . ? N4 C52 1.474(5) . ? N4 C51 1.478(5) . ? N4 C53 1.481(5) . ? C1 C14 1.418(5) . ? C1 C2 1.432(6) . ? C2 C7 1.365(7) . ? C2 C3 1.553(6) . ? C3 C4 1.519(8) . ? C3 C5 1.522(7) . ? C3 C6 1.548(7) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.411(7) . ? C7 H10 0.9500 . ? C8 C13 1.367(6) . ? C8 C9 1.534(7) . ? C9 C10 1.492(12) . ? C9 C12 1.515(9) . ? C9 C11 1.534(12) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.384(6) . ? C13 H20 0.9500 . ? C14 C15 1.510(5) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.527(6) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 H27 0.9800 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C19 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C20 C21 1.487(6) . ? C20 H33 0.9900 . ? C20 H34 0.9900 . ? C21 C22 1.407(6) . ? C21 C34 1.418(6) . ? C22 C23 1.372(6) . ? C22 H35 0.9500 . ? C23 C28 1.399(5) . ? C23 C24 1.548(6) . ? C24 C25 1.490(7) . ? C24 C26 1.509(8) . ? C24 C27 1.524(7) . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C26 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C27 H44 0.9800 . ? C28 C29 1.400(6) . ? C28 H45 0.9500 . ? C29 C34 1.410(6) . ? C29 C30 1.520(6) . ? C30 C31 1.530(7) . ? C30 C32 1.538(7) . ? C30 C33 1.550(6) . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? C33 H52 0.9800 . ? C33 H53 0.9800 . ? C33 H54 0.9800 . ? C35 C48 1.397(5) . ? C35 C36 1.433(6) . ? C36 C41 1.391(5) . ? C36 C37 1.542(5) . ? C37 C38 1.530(6) . ? C37 C39 1.533(6) . ? C37 C40 1.533(6) . ? C38 H55 0.9800 . ? C38 H56 0.9800 . ? C38 H57 0.9800 . ? C39 H58 0.9800 . ? C39 H59 0.9800 . ? C39 H60 0.9800 . ? C40 H61 0.9800 . ? C40 H62 0.9800 . ? C40 H63 0.9800 . ? C41 C42 1.409(5) . ? C41 H64 0.9500 . ? C42 C47 1.376(6) . ? C42 C43 1.530(5) . ? C43 C46 1.526(6) . ? C43 C44 1.530(6) . ? C43 C45 1.542(6) . ? C44 H65 0.9800 . ? C44 H66 0.9800 . ? C44 H67 0.9800 . ? C45 H68 0.9800 . ? C45 H69 0.9800 . ? C45 H70 0.9800 . ? C46 H71 0.9800 . ? C46 H72 0.9800 . ? C46 H73 0.9800 . ? C47 C48 1.402(5) . ? C47 H74 0.9500 . ? C48 C49 1.497(6) . ? C49 H75 0.9900 . ? C49 H76 0.9900 . ? C50 C51 1.508(5) . ? C50 H77 0.9900 . ? C50 H78 0.9900 . ? C51 H79 0.9900 . ? C51 H80 0.9900 . ? C52 H81 0.9800 . ? C52 H82 0.9800 . ? C52 H83 0.9800 . ? C53 H84 0.9800 . ? C53 H85 0.9800 . ? C53 H86 0.9800 . ? C54 C55 1.509(5) . ? C54 H87 0.9900 . ? C54 H88 0.9900 . ? C55 C57 1.403(5) . ? C55 C71 1.416(5) . ? C56 C62 1.503(16) . ? C56 C63 1.514(14) . ? C56 C61 1.516(15) . ? C56 C58 1.538(5) . ? C56 C60 1.546(15) . ? C56 C64 1.565(14) . ? C56 C59 1.578(12) . ? C57 C58 1.394(5) . ? C57 H89 0.9500 . ? C58 C65 1.394(6) . ? C65 C66 1.395(6) . ? C65 H90 0.9500 . ? C66 C71 1.425(5) . ? C66 C67 1.532(6) . ? C67 C69 1.537(8) . ? C67 C68 1.544(6) . ? C67 C70 1.544(8) . ? C68 H91 0.9800 . ? C68 H92 0.9800 . ? C68 H93 0.9800 . ? C69 H94 0.9800 . ? C69 H95 0.9800 . ? C69 H96 0.9800 . ? C70 H97 0.9800 . ? C70 H98 0.9800 . ? C70 H99 0.9800 . ? C72 C73 1.462(14) . ? C72 H100 0.9800 . ? C72 H101 0.9800 . ? C72 H102 0.9800 . ? C75 C74 1.53(2) . ? C75 H103 0.9800 . ? C75 H104 0.9800 . ? C75 H105 0.9800 . ? C73 C74 1.430(11) . ? C76 C77 1.495(7) . ? C76 H106 0.9800 . ? C76 H107 0.9800 . ? C76 H108 0.9800 . ? C77 C78 1.427(8) . ? C77 H109 1.0000 . ? C78 H110 0.9900 . ? C78 H111 0.9900 . ? C79 C80 1.43(3) . ? C79 H112 0.9800 . ? C79 H113 0.9800 . ? C79 H114 0.9800 . ? C80 C81 1.38(2) . ? C80 H115 1.0000 . ? C81 H116 0.9900 . ? C81 H117 0.9900 . ? 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 119.55(13) . . ? O2 Co1 N1 92.93(12) . . ? O1 Co1 N1 94.14(12) . . ? O2 Co1 N2 126.05(14) . . ? O1 Co1 N2 114.40(14) . . ? N1 Co1 N2 83.10(13) . . ? O2 Co1 O5 93.72(12) . . ? O1 Co1 O5 88.38(13) . . ? N1 Co1 O5 170.58(13) . . ? N2 Co1 O5 87.58(14) . . ? O4 Co2 O3 120.93(12) . . ? O4 Co2 N4 115.94(13) . . ? O3 Co2 N4 123.13(13) . . ? O4 Co2 N3 93.18(11) . . ? O3 Co2 N3 94.22(11) . . ? N4 Co2 N3 82.91(12) . . ? O4 Co2 O6 90.10(12) . . ? O3 Co2 O6 92.88(11) . . ? N4 Co2 O6 86.42(12) . . ? N3 Co2 O6 169.23(12) . . ? C1 O1 Co1 125.7(2) . . ? C34 O2 Co1 127.8(2) . . ? C35 O3 Co2 123.2(2) . . ? C71 O4 Co2 126.7(2) . . ? C74 O5 C73 59.1(5) . . ? C74 O5 Co1 123.7(3) . . ? C73 O5 Co1 123.3(4) . . ? C77 O6 C78 59.1(4) . . ? C77 O6 Co2 130.1(3) . . ? C78 O6 Co2 123.0(3) . . ? C80 O7 C81 57.5(10) . . ? C15 N1 C16 112.5(3) . . ? C15 N1 C20 110.1(3) . . ? C16 N1 C20 110.4(3) . . ? C15 N1 Co1 108.2(2) . . ? C16 N1 Co1 106.3(2) . . ? C20 N1 Co1 109.2(2) . . ? C19 N2 C17 110.3(4) . . ? C19 N2 C18 108.2(4) . . ? C17 N2 C18 109.8(4) . . ? C19 N2 Co1 113.1(3) . . ? C17 N2 Co1 108.5(3) . . ? C18 N2 Co1 106.9(3) . . ? C50 N3 C54 110.2(3) . . ? C50 N3 C49 111.0(3) . . ? C54 N3 C49 108.1(3) . . ? C50 N3 Co2 107.3(2) . . ? C54 N3 Co2 111.5(2) . . ? C49 N3 Co2 108.8(2) . . ? C52 N4 C51 108.8(3) . . ? C52 N4 C53 108.3(3) . . ? C51 N4 C53 110.8(3) . . ? C52 N4 Co2 113.8(3) . . ? C51 N4 Co2 107.3(2) . . ? C53 N4 Co2 107.8(3) . . ? O1 C1 C14 121.5(4) . . ? O1 C1 C2 121.5(3) . . ? C14 C1 C2 117.0(4) . . ? C7 C2 C1 119.7(4) . . ? C7 C2 C3 120.4(4) . . ? C1 C2 C3 119.9(4) . . ? C4 C3 C5 110.8(5) . . ? C4 C3 C6 108.1(4) . . ? C5 C3 C6 107.6(4) . . ? C4 C3 C2 109.3(4) . . ? C5 C3 C2 109.6(4) . . ? C6 C3 C2 111.4(4) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 123.4(4) . . ? C2 C7 H10 118.3 . . ? C8 C7 H10 118.3 . . ? C13 C8 C7 116.2(4) . . ? C13 C8 C9 124.3(4) . . ? C7 C8 C9 119.4(4) . . ? C10 C9 C12 111.7(7) . . ? C10 C9 C8 109.2(7) . . ? C12 C9 C8 110.8(5) . . ? C10 C9 C11 108.6(6) . . ? C12 C9 C11 106.9(8) . . ? C8 C9 C11 109.5(6) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 123.4(4) . . ? C8 C13 H20 118.3 . . ? C14 C13 H20 118.3 . . ? C13 C14 C1 120.3(4) . . ? C13 C14 C15 119.2(3) . . ? C1 C14 C15 120.6(3) . . ? N1 C15 C14 114.0(3) . . ? N1 C15 H21 108.8 . . ? C14 C15 H21 108.8 . . ? N1 C15 H22 108.8 . . ? C14 C15 H22 108.8 . . ? H21 C15 H22 107.6 . . ? N1 C16 C17 109.8(3) . . ? N1 C16 H23 109.7 . . ? C17 C16 H23 109.7 . . ? N1 C16 H24 109.7 . . ? C17 C16 H24 109.7 . . ? H23 C16 H24 108.2 . . ? N2 C17 C16 109.7(3) . . ? N2 C17 H25 109.7 . . ? C16 C17 H25 109.7 . . ? N2 C17 H26 109.7 . . ? C16 C17 H26 109.7 . . ? H25 C17 H26 108.2 . . ? N2 C18 H27 109.5 . . ? N2 C18 H28 109.5 . . ? H27 C18 H28 109.5 . . ? N2 C18 H29 109.5 . . ? H27 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? N2 C19 H30 109.5 . . ? N2 C19 H31 109.5 . . ? H30 C19 H31 109.5 . . ? N2 C19 H32 109.5 . . ? H30 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? N1 C20 C21 115.0(3) . . ? N1 C20 H33 108.5 . . ? C21 C20 H33 108.5 . . ? N1 C20 H34 108.5 . . ? C21 C20 H34 108.5 . . ? H33 C20 H34 107.5 . . ? C22 C21 C34 119.9(4) . . ? C22 C21 C20 118.2(4) . . ? C34 C21 C20 121.9(4) . . ? C23 C22 C21 122.0(4) . . ? C23 C22 H35 119.0 . . ? C21 C22 H35 119.0 . . ? C22 C23 C28 117.1(4) . . ? C22 C23 C24 121.5(4) . . ? C28 C23 C24 121.3(4) . . ? C25 C24 C26 110.3(7) . . ? C25 C24 C27 107.9(5) . . ? C26 C24 C27 107.2(6) . . ? C25 C24 C23 111.2(4) . . ? C26 C24 C23 112.6(4) . . ? C27 C24 C23 107.4(4) . . ? C24 C25 H36 109.5 . . ? C24 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? C24 C25 H38 109.5 . . ? H36 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C24 C26 H39 109.5 . . ? C24 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? C24 C26 H41 109.5 . . ? H39 C26 H41 109.5 . . ? H40 C26 H41 109.5 . . ? C24 C27 H42 109.5 . . ? C24 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? C24 C27 H44 109.5 . . ? H42 C27 H44 109.5 . . ? H43 C27 H44 109.5 . . ? C23 C28 C29 123.6(4) . . ? C23 C28 H45 118.2 . . ? C29 C28 H45 118.2 . . ? C28 C29 C34 118.2(4) . . ? C28 C29 C30 120.6(4) . . ? C34 C29 C30 121.1(4) . . ? C29 C30 C31 113.4(4) . . ? C29 C30 C32 109.7(4) . . ? C31 C30 C32 109.0(4) . . ? C29 C30 C33 109.3(3) . . ? C31 C30 C33 105.1(4) . . ? C32 C30 C33 110.2(4) . . ? C30 C31 H46 109.5 . . ? C30 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? C30 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? C30 C32 H49 109.5 . . ? C30 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? C30 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? C30 C33 H52 109.5 . . ? C30 C33 H53 109.5 . . ? H52 C33 H53 109.5 . . ? C30 C33 H54 109.5 . . ? H52 C33 H54 109.5 . . ? H53 C33 H54 109.5 . . ? O2 C34 C29 121.6(3) . . ? O2 C34 C21 119.7(4) . . ? C29 C34 C21 118.8(4) . . ? O3 C35 C48 120.8(3) . . ? O3 C35 C36 120.7(3) . . ? C48 C35 C36 118.5(3) . . ? C41 C36 C35 118.4(3) . . ? C41 C36 C37 120.7(4) . . ? C35 C36 C37 120.8(3) . . ? C38 C37 C39 111.2(4) . . ? C38 C37 C40 107.1(4) . . ? C39 C37 C40 108.0(3) . . ? C38 C37 C36 109.2(3) . . ? C39 C37 C36 109.3(3) . . ? C40 C37 C36 112.1(4) . . ? C37 C38 H55 109.5 . . ? C37 C38 H56 109.5 . . ? H55 C38 H56 109.5 . . ? C37 C38 H57 109.5 . . ? H55 C38 H57 109.5 . . ? H56 C38 H57 109.5 . . ? C37 C39 H58 109.5 . . ? C37 C39 H59 109.5 . . ? H58 C39 H59 109.5 . . ? C37 C39 H60 109.5 . . ? H58 C39 H60 109.5 . . ? H59 C39 H60 109.5 . . ? C37 C40 H61 109.5 . . ? C37 C40 H62 109.5 . . ? H61 C40 H62 109.5 . . ? C37 C40 H63 109.5 . . ? H61 C40 H63 109.5 . . ? H62 C40 H63 109.5 . . ? C36 C41 C42 123.3(4) . . ? C36 C41 H64 118.3 . . ? C42 C41 H64 118.3 . . ? C47 C42 C41 116.6(4) . . ? C47 C42 C43 121.5(4) . . ? C41 C42 C43 121.9(4) . . ? C46 C43 C44 107.7(4) . . ? C46 C43 C42 109.9(3) . . ? C44 C43 C42 112.9(4) . . ? C46 C43 C45 109.3(4) . . ? C44 C43 C45 108.1(4) . . ? C42 C43 C45 108.9(3) . . ? C43 C44 H65 109.5 . . ? C43 C44 H66 109.5 . . ? H65 C44 H66 109.5 . . ? C43 C44 H67 109.5 . . ? H65 C44 H67 109.5 . . ? H66 C44 H67 109.5 . . ? C43 C45 H68 109.5 . . ? C43 C45 H69 109.5 . . ? H68 C45 H69 109.5 . . ? C43 C45 H70 109.5 . . ? H68 C45 H70 109.5 . . ? H69 C45 H70 109.5 . . ? C43 C46 H71 109.5 . . ? C43 C46 H72 109.5 . . ? H71 C46 H72 109.5 . . ? C43 C46 H73 109.5 . . ? H71 C46 H73 109.5 . . ? H72 C46 H73 109.5 . . ? C42 C47 C48 122.6(4) . . ? C42 C47 H74 118.7 . . ? C48 C47 H74 118.7 . . ? C35 C48 C47 120.3(4) . . ? C35 C48 C49 120.3(3) . . ? C47 C48 C49 119.3(3) . . ? N3 C49 C48 114.2(3) . . ? N3 C49 H75 108.7 . . ? C48 C49 H75 108.7 . . ? N3 C49 H76 108.7 . . ? C48 C49 H76 108.7 . . ? H75 C49 H76 107.6 . . ? N3 C50 C51 110.4(3) . . ? N3 C50 H77 109.6 . . ? C51 C50 H77 109.6 . . ? N3 C50 H78 109.6 . . ? C51 C50 H78 109.6 . . ? H77 C50 H78 108.1 . . ? N4 C51 C50 110.5(3) . . ? N4 C51 H79 109.5 . . ? C50 C51 H79 109.5 . . ? N4 C51 H80 109.5 . . ? C50 C51 H80 109.5 . . ? H79 C51 H80 108.1 . . ? N4 C52 H81 109.5 . . ? N4 C52 H82 109.5 . . ? H81 C52 H82 109.5 . . ? N4 C52 H83 109.5 . . ? H81 C52 H83 109.5 . . ? H82 C52 H83 109.5 . . ? N4 C53 H84 109.5 . . ? N4 C53 H85 109.5 . . ? H84 C53 H85 109.5 . . ? N4 C53 H86 109.5 . . ? H84 C53 H86 109.5 . . ? H85 C53 H86 109.5 . . ? N3 C54 C55 114.8(3) . . ? N3 C54 H87 108.6 . . ? C55 C54 H87 108.6 . . ? N3 C54 H88 108.6 . . ? C55 C54 H88 108.6 . . ? H87 C54 H88 107.6 . . ? C57 C55 C71 120.6(3) . . ? C57 C55 C54 117.9(3) . . ? C71 C55 C54 121.1(3) . . ? C62 C56 C63 107.8(13) . . ? C62 C56 C61 140.3(9) . . ? C63 C56 C61 69.1(12) . . ? C62 C56 C58 108.2(6) . . ? C63 C56 C58 110.7(6) . . ? C61 C56 C58 109.7(6) . . ? C62 C56 C60 65.4(12) . . ? C63 C56 C60 45.0(9) . . ? C61 C56 C60 111.1(10) . . ? C58 C56 C60 110.1(6) . . ? C62 C56 C64 117.0(14) . . ? C63 C56 C64 107.7(13) . . ? C61 C56 C64 40.0(10) . . ? C58 C56 C64 105.5(5) . . ? C60 C56 C64 141.2(8) . . ? C62 C56 C59 44.2(10) . . ? C63 C56 C59 134.4(8) . . ? C61 C56 C59 108.4(9) . . ? C58 C56 C59 112.5(5) . . ? C60 C56 C59 105.1(8) . . ? C64 C56 C59 74.1(11) . . ? C58 C57 C55 121.4(4) . . ? C58 C57 H89 119.3 . . ? C55 C57 H89 119.3 . . ? C57 C58 C65 117.2(4) . . ? C57 C58 C56 122.0(4) . . ? C65 C58 C56 120.7(4) . . ? C58 C65 C66 124.0(4) . . ? C58 C65 H90 118.0 . . ? C66 C65 H90 118.0 . . ? C65 C66 C71 118.3(4) . . ? C65 C66 C67 121.0(4) . . ? C71 C66 C67 120.7(4) . . ? C66 C67 C69 110.7(4) . . ? C66 C67 C68 112.1(4) . . ? C69 C67 C68 109.0(5) . . ? C66 C67 C70 110.3(4) . . ? C69 C67 C70 107.8(4) . . ? C68 C67 C70 106.8(5) . . ? C67 C68 H91 109.5 . . ? C67 C68 H92 109.5 . . ? H91 C68 H92 109.5 . . ? C67 C68 H93 109.5 . . ? H91 C68 H93 109.5 . . ? H92 C68 H93 109.5 . . ? C67 C69 H94 109.5 . . ? C67 C69 H95 109.5 . . ? H94 C69 H95 109.5 . . ? C67 C69 H96 109.5 . . ? H94 C69 H96 109.5 . . ? H95 C69 H96 109.5 . . ? C67 C70 H97 109.5 . . ? C67 C70 H98 109.5 . . ? H97 C70 H98 109.5 . . ? C67 C70 H99 109.5 . . ? H97 C70 H99 109.5 . . ? H98 C70 H99 109.5 . . ? O4 C71 C55 120.9(3) . . ? O4 C71 C66 120.5(3) . . ? C55 C71 C66 118.5(3) . . ? C73 C72 H100 109.5 . . ? C73 C72 H101 109.5 . . ? H100 C72 H101 109.5 . . ? C73 C72 H102 109.5 . . ? H100 C72 H102 109.5 . . ? H101 C72 H102 109.5 . . ? C74 C75 H103 109.5 . . ? C74 C75 H104 109.5 . . ? H103 C75 H104 109.5 . . ? C74 C75 H105 109.5 . . ? H103 C75 H105 109.5 . . ? H104 C75 H105 109.5 . . ? C74 C73 O5 60.3(4) . . ? C74 C73 C72 121.0(9) . . ? O5 C73 C72 121.0(10) . . ? C73 C74 O5 60.7(4) . . ? C73 C74 C75 122.9(16) . . ? O5 C74 C75 109.2(11) . . ? C77 C76 H106 109.5 . . ? C77 C76 H107 109.5 . . ? H106 C76 H107 109.5 . . ? C77 C76 H108 109.5 . . ? H106 C76 H108 109.5 . . ? H107 C76 H108 109.5 . . ? C78 C77 O6 60.7(3) . . ? C78 C77 C76 121.0(5) . . ? O6 C77 C76 117.3(5) . . ? C78 C77 H109 115.5 . . ? O6 C77 H109 115.5 . . ? C76 C77 H109 115.5 . . ? C77 C78 O6 60.3(3) . . ? C77 C78 H110 117.7 . . ? O6 C78 H110 117.7 . . ? C77 C78 H111 117.7 . . ? O6 C78 H111 117.7 . . ? H110 C78 H111 114.9 . . ? C80 C79 H112 109.5 . . ? C80 C79 H113 109.5 . . ? H112 C79 H113 109.5 . . ? C80 C79 H114 109.5 . . ? H112 C79 H114 109.5 . . ? H113 C79 H114 109.5 . . ? C81 C80 O7 63.2(11) . . ? C81 C80 C79 130(2) . . ? O7 C80 C79 119.6(17) . . ? C81 C80 H115 111.8 . . ? O7 C80 H115 111.8 . . ? C79 C80 H115 111.8 . . ? C80 C81 O7 59.4(11) . . ? C80 C81 H116 117.8 . . ? O7 C81 H116 117.8 . . ? C80 C81 H117 117.8 . . ? O7 C81 H117 117.8 . . ? H116 C81 H117 115.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.725 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.072 #===END data_1CH3OH/H2O _database_code_depnum_ccdc_archive 'CCDC 766022' _publ_section_abstract ; Please see full paper. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C34 H54 N2 O2) (H2 O) Co][(C34 H54 N2 O2) (C H4 O) Co](C H4 O)3' _chemical_formula_sum 'C72 H126 Co2 N4 O9' _chemical_formula_weight 1309.68 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.764(6) _cell_length_b 13.592(6) _cell_length_c 22.443(10) _cell_angle_alpha 96.005(9) _cell_angle_beta 102.272(6) _cell_angle_gamma 95.489(11) _cell_volume 3756(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14505 _cell_measurement_theta_min 2.0678 _cell_measurement_theta_max 30.9599 _exptl_crystal_description Irregular _exptl_crystal_colour Pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9716 _exptl_absorpt_correction_T_min 0.9430 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 33698 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.50 _reflns_number_total 14811 _reflns_number_gt 11848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1601P)^2^+6.0386P] 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 14811 _refine_ls_number_parameters 785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.3009 _refine_ls_wR_factor_gt 0.2781 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.05608(5) 0.65190(5) 0.63011(3) 0.03342(19) Uani 1 1 d . . . Co2 Co 0.63710(5) 0.88115(5) 0.81896(3) 0.03329(19) Uani 1 1 d . . . O1 O 0.1017(2) 0.5242(2) 0.65322(14) 0.0328(7) Uani 1 1 d . . . O2 O 0.1481(3) 0.7765(2) 0.63924(15) 0.0365(7) Uani 1 1 d . . . O3 O 0.6941(3) 0.8949(2) 0.74692(15) 0.0369(7) Uani 1 1 d . . . O4 O 0.7118(3) 0.8184(2) 0.88806(14) 0.0356(7) Uani 1 1 d . . . O5 O 0.1081(3) 0.6274(3) 0.54466(15) 0.0432(8) Uani 1 1 d . . . H121 H 0.0619 0.6135 0.5016 0.052 Uiso 1 1 d . . . H122 H 0.1821 0.6711 0.5408 0.052 Uiso 1 1 d . . . O6 O 0.7149(3) 1.0258(3) 0.86513(16) 0.0424(8) Uani 1 1 d . . . O7 O 0.6155(3) 0.8596(3) 0.97814(17) 0.0480(9) Uani 1 1 d . . . O8 O 0.2782(3) 0.9556(3) 1.01356(18) 0.0534(10) Uani 1 1 d . . . O9 O -0.0230(4) 0.3820(3) 0.57519(18) 0.0599(11) Uani 1 1 d . . . N1 N 0.0124(3) 0.6872(3) 0.71592(18) 0.0332(8) Uani 1 1 d . . . N2 N -0.1102(3) 0.6613(3) 0.59272(19) 0.0409(9) Uani 1 1 d . . . N3 N 0.5398(3) 0.7433(3) 0.77790(18) 0.0351(8) Uani 1 1 d . . . N4 N 0.4832(3) 0.9317(3) 0.81476(19) 0.0405(9) Uani 1 1 d . . . C1 C 0.1515(3) 0.5147(3) 0.7113(2) 0.0300(9) Uani 1 1 d . . . C2 C 0.2486(4) 0.4713(3) 0.7252(2) 0.0333(9) Uani 1 1 d . . . C3 C 0.3045(4) 0.4319(3) 0.6746(2) 0.0344(10) Uani 1 1 d . . . C4 C 0.3199(4) 0.5117(4) 0.6324(2) 0.0374(10) Uani 1 1 d . . . H1 H 0.3896 0.5525 0.6488 0.045 Uiso 1 1 calc R . . H2 H 0.2617 0.5541 0.6304 0.045 Uiso 1 1 calc R . . H3 H 0.3181 0.4792 0.5910 0.045 Uiso 1 1 calc R . . C5 C 0.2364(5) 0.3388(4) 0.6369(3) 0.0470(12) Uani 1 1 d . . . H4 H 0.1847 0.3581 0.6024 0.056 Uiso 1 1 calc R . . H5 H 0.1971 0.3037 0.6630 0.056 Uiso 1 1 calc R . . H6 H 0.2835 0.2949 0.6211 0.056 Uiso 1 1 calc R . . C6 C 0.4163(4) 0.4025(4) 0.7009(2) 0.0453(12) Uani 1 1 d . . . H7 H 0.4094 0.3320 0.7070 0.054 Uiso 1 1 calc R . . H8 H 0.4481 0.4434 0.7403 0.054 Uiso 1 1 calc R . . H9 H 0.4630 0.4131 0.6721 0.054 Uiso 1 1 calc R . . C7 C 0.2945(4) 0.4674(3) 0.7869(2) 0.0352(10) Uani 1 1 d . . . H10 H 0.3603 0.4391 0.7964 0.042 Uiso 1 1 calc R . . C8 C 0.2504(4) 0.5021(3) 0.8355(2) 0.0336(9) Uani 1 1 d . . . C9 C 0.3047(4) 0.5001(4) 0.9031(2) 0.0396(11) Uani 1 1 d . . . C10 C 0.4097(4) 0.4537(4) 0.9118(2) 0.0426(11) Uani 1 1 d . . . H11 H 0.4702 0.5057 0.9151 0.051 Uiso 1 1 calc R . . H12 H 0.4068 0.4039 0.8764 0.051 Uiso 1 1 calc R . . H13 H 0.4199 0.4216 0.9494 0.051 Uiso 1 1 calc R . . C11 C 0.2270(4) 0.4420(4) 0.9343(2) 0.0461(12) Uani 1 1 d . . . H14 H 0.2380 0.3715 0.9305 0.055 Uiso 1 1 calc R . . H15 H 0.1523 0.4487 0.9144 0.055 Uiso 1 1 calc R . . H16 H 0.2410 0.4688 0.9779 0.055 Uiso 1 1 calc R . . C12 C 0.3295(5) 0.6080(4) 0.9365(2) 0.0467(12) Uani 1 1 d . . . H17 H 0.2677 0.6254 0.9531 0.056 Uiso 1 1 calc R . . H18 H 0.3430 0.6540 0.9074 0.056 Uiso 1 1 calc R . . H19 H 0.3936 0.6129 0.9702 0.056 Uiso 1 1 calc R . . C13 C 0.1545(4) 0.5440(3) 0.8206(2) 0.0354(10) Uani 1 1 d . . . H20 H 0.1221 0.5691 0.8526 0.042 Uiso 1 1 calc R . . C14 C 0.1049(4) 0.5499(3) 0.7598(2) 0.0331(9) Uani 1 1 d . . . C15 C 0.0014(4) 0.5962(4) 0.7457(2) 0.0356(10) Uani 1 1 d . . . H21 H -0.0553 0.5470 0.7183 0.043 Uiso 1 1 calc R . . H22 H -0.0223 0.6127 0.7844 0.043 Uiso 1 1 calc R . . C16 C -0.0926(4) 0.7282(4) 0.7013(2) 0.0393(11) Uani 1 1 d . . . H23 H -0.0804 0.7984 0.6937 0.047 Uiso 1 1 calc R . . H24 H -0.1278 0.7265 0.7365 0.047 Uiso 1 1 calc R . . C17 C -0.1650(4) 0.6668(4) 0.6446(3) 0.0450(12) Uani 1 1 d . . . H25 H -0.1842 0.5986 0.6539 0.054 Uiso 1 1 calc R . . H26 H -0.2327 0.6972 0.6329 0.054 Uiso 1 1 calc R . . C18 C -0.1602(5) 0.5754(5) 0.5461(3) 0.0571(15) Uani 1 1 d . . . H27 H -0.1904 0.5223 0.5661 0.069 Uiso 1 1 calc R . . H28 H -0.1053 0.5506 0.5258 0.069 Uiso 1 1 calc R . . H29 H -0.2179 0.5962 0.5155 0.069 Uiso 1 1 calc R . . C19 C -0.1191(5) 0.7532(4) 0.5631(3) 0.0498(13) Uani 1 1 d . . . H30 H -0.1156 0.7387 0.5199 0.060 Uiso 1 1 calc R . . H31 H -0.0596 0.8041 0.5843 0.060 Uiso 1 1 calc R . . H32 H -0.1881 0.7776 0.5654 0.060 Uiso 1 1 calc R . . C20 C 0.0982(4) 0.7614(3) 0.7564(2) 0.0340(10) Uani 1 1 d . . . H33 H 0.1670 0.7317 0.7634 0.041 Uiso 1 1 calc R . . H34 H 0.0792 0.7750 0.7967 0.041 Uiso 1 1 calc R . . C21 C 0.1163(4) 0.8599(3) 0.7314(2) 0.0324(9) Uani 1 1 d . . . C22 C 0.1164(3) 0.9483(4) 0.7692(2) 0.0346(10) Uani 1 1 d . . . H35 H 0.0982 0.9448 0.8079 0.042 Uiso 1 1 calc R . . C23 C 0.1420(4) 1.0401(4) 0.7522(2) 0.0362(10) Uani 1 1 d . . . C24 C 0.1496(4) 1.1396(4) 0.7936(2) 0.0405(11) Uani 1 1 d . . . C25 C 0.1228(6) 1.1224(4) 0.8546(3) 0.0643(19) Uani 1 1 d . . . H36 H 0.1889 1.1141 0.8842 0.077 Uiso 1 1 calc R . . H37 H 0.0711 1.0622 0.8489 0.077 Uiso 1 1 calc R . . H38 H 0.0910 1.1798 0.8703 0.077 Uiso 1 1 calc R . . C26 C 0.2645(4) 1.1922(4) 0.8058(2) 0.0441(12) Uani 1 1 d . . . H39 H 0.2700 1.2356 0.7741 0.053 Uiso 1 1 calc R . . H40 H 0.3150 1.1424 0.8047 0.053 Uiso 1 1 calc R . . H41 H 0.2823 1.2323 0.8463 0.053 Uiso 1 1 calc R . . C27 C 0.0732(5) 1.2092(4) 0.7624(3) 0.0574(15) Uani 1 1 d . . . H42 H 0.0027 1.1970 0.7728 0.069 Uiso 1 1 calc R . . H43 H 0.0643 1.1962 0.7177 0.069 Uiso 1 1 calc R . . H44 H 0.1037 1.2786 0.7767 0.069 Uiso 1 1 calc R . . C28 C 0.1652(4) 1.0409(4) 0.6939(2) 0.0384(10) Uani 1 1 d . . . H45 H 0.1801 1.1035 0.6803 0.046 Uiso 1 1 calc R . . C29 C 0.1678(4) 0.9545(4) 0.6546(2) 0.0363(10) Uani 1 1 d . . . C30 C 0.1982(5) 0.9633(4) 0.5926(2) 0.0443(12) Uani 1 1 d . . . C31 C 0.2146(6) 1.0720(4) 0.5806(3) 0.0564(15) Uani 1 1 d . . . H46 H 0.2901 1.0997 0.5978 0.068 Uiso 1 1 calc R . . H47 H 0.1672 1.1107 0.6001 0.068 Uiso 1 1 calc R . . H48 H 0.1972 1.0750 0.5362 0.068 Uiso 1 1 calc R . . C32 C 0.1074(5) 0.9090(4) 0.5403(2) 0.0527(14) Uani 1 1 d . . . H49 H 0.0563 0.9555 0.5261 0.063 Uiso 1 1 calc R . . H50 H 0.0696 0.8537 0.5552 0.063 Uiso 1 1 calc R . . H51 H 0.1380 0.8830 0.5062 0.063 Uiso 1 1 calc R . . C33 C 0.3038(5) 0.9197(5) 0.5925(3) 0.0505(13) Uani 1 1 d . . . H52 H 0.2882 0.8488 0.5763 0.061 Uiso 1 1 calc R . . H53 H 0.3477 0.9274 0.6346 0.061 Uiso 1 1 calc R . . H54 H 0.3434 0.9549 0.5666 0.061 Uiso 1 1 calc R . . C34 C 0.1428(3) 0.8617(3) 0.6743(2) 0.0325(9) Uani 1 1 d . . . C35 C 0.6495(4) 0.8558(4) 0.6897(2) 0.0333(9) Uani 1 1 d . . . C36 C 0.6624(4) 0.9063(4) 0.6394(2) 0.0388(11) Uani 1 1 d . . . C37 C 0.7336(5) 1.0063(4) 0.6502(2) 0.0459(12) Uani 1 1 d . . . C38 C 0.8489(4) 0.9964(4) 0.6853(3) 0.0463(12) Uani 1 1 d . . . H55 H 0.8535 1.0087 0.7296 0.056 Uiso 1 1 calc R . . H56 H 0.9004 1.0450 0.6739 0.056 Uiso 1 1 calc R . . H57 H 0.8662 0.9289 0.6747 0.056 Uiso 1 1 calc R . . C39 C 0.6845(5) 1.0856(4) 0.6868(3) 0.0501(13) Uani 1 1 d . . . H58 H 0.6362 1.1199 0.6581 0.060 Uiso 1 1 calc R . . H59 H 0.7426 1.1341 0.7124 0.060 Uiso 1 1 calc R . . H60 H 0.6436 1.0530 0.7132 0.060 Uiso 1 1 calc R . . C40 C 0.7434(6) 1.0454(4) 0.5901(3) 0.0593(16) Uani 1 1 d . . . H61 H 0.8049 1.0202 0.5764 0.071 Uiso 1 1 calc R . . H62 H 0.7546 1.1184 0.5966 0.071 Uiso 1 1 calc R . . H63 H 0.6770 1.0227 0.5587 0.071 Uiso 1 1 calc R . . C41 C 0.6102(4) 0.8625(4) 0.5802(2) 0.0429(11) Uani 1 1 d . . . H64 H 0.6187 0.8975 0.5467 0.051 Uiso 1 1 calc R . . C42 C 0.5466(4) 0.7709(4) 0.5672(2) 0.0422(11) Uani 1 1 d . . . C43 C 0.4889(4) 0.7242(4) 0.5015(2) 0.0466(12) Uani 1 1 d . . . C44 C 0.3685(5) 0.6940(6) 0.4977(3) 0.0662(18) Uani 1 1 d . . . H65 H 0.3577 0.6255 0.5072 0.079 Uiso 1 1 calc R . . H66 H 0.3272 0.6982 0.4561 0.079 Uiso 1 1 calc R . . H67 H 0.3437 0.7390 0.5274 0.079 Uiso 1 1 calc R . . C45 C 0.4981(7) 0.7947(6) 0.4543(3) 0.080(2) Uani 1 1 d . . . H68 H 0.4367 0.8336 0.4494 0.096 Uiso 1 1 calc R . . H69 H 0.4979 0.7562 0.4149 0.096 Uiso 1 1 calc R . . H70 H 0.5656 0.8399 0.4682 0.096 Uiso 1 1 calc R . . C46 C 0.5391(6) 0.6311(5) 0.4846(3) 0.0674(18) Uani 1 1 d . . . H71 H 0.5990 0.6491 0.4653 0.081 Uiso 1 1 calc R . . H72 H 0.4844 0.5833 0.4557 0.081 Uiso 1 1 calc R . . H73 H 0.5660 0.6009 0.5217 0.081 Uiso 1 1 calc R . . C47 C 0.5382(4) 0.7209(4) 0.6170(2) 0.0413(11) Uani 1 1 d . . . H74 H 0.4963 0.6574 0.6099 0.050 Uiso 1 1 calc R . . C48 C 0.5887(4) 0.7599(3) 0.6766(2) 0.0325(9) Uani 1 1 d . . . C49 C 0.5847(4) 0.6965(4) 0.7275(2) 0.0358(10) Uani 1 1 d . . . H75 H 0.5402 0.6322 0.7098 0.043 Uiso 1 1 calc R . . H76 H 0.6588 0.6820 0.7450 0.043 Uiso 1 1 calc R . . C50 C 0.4281(4) 0.7647(4) 0.7559(2) 0.0406(11) Uani 1 1 d . . . H77 H 0.3776 0.7030 0.7512 0.049 Uiso 1 1 calc R . . H78 H 0.4204 0.7887 0.7152 0.049 Uiso 1 1 calc R . . C51 C 0.4004(4) 0.8434(4) 0.8012(2) 0.0410(11) Uani 1 1 d . . . H79 H 0.3288 0.8636 0.7838 0.049 Uiso 1 1 calc R . . H80 H 0.3964 0.8154 0.8398 0.049 Uiso 1 1 calc R . . C52 C 0.4646(4) 0.9930(4) 0.7629(2) 0.0475(13) Uani 1 1 d . . . H81 H 0.4934 1.0627 0.7783 0.057 Uiso 1 1 calc R . . H82 H 0.3869 0.9886 0.7452 0.057 Uiso 1 1 calc R . . H83 H 0.5013 0.9681 0.7313 0.057 Uiso 1 1 calc R . . C53 C 0.4714(4) 0.9927(4) 0.8714(2) 0.0435(12) Uani 1 1 d . . . H84 H 0.4444 0.9491 0.8983 0.052 Uiso 1 1 calc R . . H85 H 0.4203 1.0407 0.8602 0.052 Uiso 1 1 calc R . . H86 H 0.5418 1.0286 0.8929 0.052 Uiso 1 1 calc R . . C54 C 0.5411(4) 0.6744(4) 0.8253(2) 0.0399(11) Uani 1 1 d . . . H87 H 0.4918 0.6128 0.8071 0.048 Uiso 1 1 calc R . . H88 H 0.5135 0.7063 0.8596 0.048 Uiso 1 1 calc R . . C55 C 0.6519(4) 0.6470(4) 0.8503(2) 0.0359(10) Uani 1 1 d . . . C56 C 0.6718(4) 0.5500(4) 0.8432(2) 0.0415(11) Uani 1 1 d . . . H89 H 0.6143 0.5004 0.8225 0.050 Uiso 1 1 calc R . . C57 C 0.7736(4) 0.5209(4) 0.8651(2) 0.0418(11) Uani 1 1 d . . . C58 C 0.7927(5) 0.4123(4) 0.8563(3) 0.0486(13) Uani 1 1 d . . . C59 C 0.7675(9) 0.3732(6) 0.7886(4) 0.093(3) Uani 1 1 d . . . H90 H 0.6912 0.3457 0.7753 0.112 Uiso 1 1 calc R . . H91 H 0.8127 0.3207 0.7816 0.112 Uiso 1 1 calc R . . H92 H 0.7822 0.4276 0.7650 0.112 Uiso 1 1 calc R . . C60 C 0.7237(8) 0.3535(6) 0.8896(5) 0.110(4) Uani 1 1 d . . . H93 H 0.7639 0.3517 0.9318 0.132 Uiso 1 1 calc R . . H94 H 0.7040 0.2854 0.8683 0.132 Uiso 1 1 calc R . . H95 H 0.6580 0.3850 0.8906 0.132 Uiso 1 1 calc R . . C61 C 0.9125(6) 0.3974(6) 0.8812(5) 0.087(2) Uani 1 1 d . . . H96 H 0.9520 0.4021 0.8484 0.104 Uiso 1 1 calc R . . H97 H 0.9160 0.3317 0.8952 0.104 Uiso 1 1 calc R . . H98 H 0.9452 0.4492 0.9157 0.104 Uiso 1 1 calc R . . C62 C 0.8554(4) 0.5981(4) 0.8942(2) 0.0415(11) Uani 1 1 d . . . H99 H 0.9258 0.5809 0.9090 0.050 Uiso 1 1 calc R . . C63 C 0.8401(4) 0.6981(4) 0.9028(2) 0.0382(10) Uani 1 1 d . . . C64 C 0.9341(4) 0.7773(4) 0.9357(2) 0.0385(11) Uani 1 1 d . . . C65 C 1.0410(5) 0.7352(5) 0.9515(3) 0.0602(16) Uani 1 1 d . . . H100 H 1.0508 0.7141 0.9926 0.072 Uiso 1 1 calc R . . H101 H 1.1001 0.7864 0.9510 0.072 Uiso 1 1 calc R . . H102 H 1.0411 0.6777 0.9213 0.072 Uiso 1 1 calc R . . C66 C 0.9098(5) 0.8249(5) 0.9952(3) 0.0552(15) Uani 1 1 d . . . H103 H 0.8704 0.8823 0.9869 0.066 Uiso 1 1 calc R . . H104 H 0.9777 0.8471 1.0255 0.066 Uiso 1 1 calc R . . H105 H 0.8656 0.7759 1.0115 0.066 Uiso 1 1 calc R . . C67 C 0.9492(5) 0.8580(5) 0.8940(3) 0.0533(14) Uani 1 1 d . . . H106 H 0.9997 0.8390 0.8687 0.064 Uiso 1 1 calc R . . H107 H 0.9783 0.9218 0.9195 0.064 Uiso 1 1 calc R . . H108 H 0.8794 0.8645 0.8673 0.064 Uiso 1 1 calc R . . C68 C 0.7348(4) 0.7237(4) 0.8807(2) 0.0356(10) Uani 1 1 d . . . C69 C 0.8138(4) 1.0717(4) 0.8544(3) 0.0477(12) Uani 1 1 d . . . H109 H 0.8751 1.0514 0.8828 0.057 Uiso 1 1 calc R . . H110 H 0.8158 1.1443 0.8611 0.057 Uiso 1 1 calc R . . H111 H 0.8182 1.0509 0.8120 0.057 Uiso 1 1 calc R . . C70 C 0.6114(5) 0.7809(5) 1.0146(2) 0.0506(13) Uani 1 1 d . . . H112 H 0.5366 0.7623 1.0171 0.061 Uiso 1 1 calc R . . H113 H 0.6560 0.8027 1.0559 0.061 Uiso 1 1 calc R . . H114 H 0.6389 0.7233 0.9958 0.061 Uiso 1 1 calc R . . C71 C 0.3269(6) 0.8769(5) 0.9873(3) 0.0649(17) Uani 1 1 d . . . H115 H 0.3195 0.8187 1.0091 0.078 Uiso 1 1 calc R . . H116 H 0.4037 0.8987 0.9909 0.078 Uiso 1 1 calc R . . H117 H 0.2910 0.8590 0.9438 0.078 Uiso 1 1 calc R . . C72 C -0.0669(6) 0.3134(6) 0.6092(3) 0.077(2) Uani 1 1 d . . . H118 H -0.1331 0.3352 0.6188 0.092 Uiso 1 1 calc R . . H119 H -0.0143 0.3100 0.6475 0.092 Uiso 1 1 calc R . . H120 H -0.0837 0.2474 0.5849 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0322(4) 0.0356(4) 0.0335(3) 0.0020(3) 0.0095(3) 0.0070(3) Co2 0.0307(4) 0.0385(4) 0.0325(3) 0.0027(3) 0.0113(2) 0.0062(3) O1 0.0348(17) 0.0301(16) 0.0346(16) 0.0022(12) 0.0105(13) 0.0050(12) O2 0.0416(18) 0.0356(18) 0.0336(17) -0.0008(13) 0.0137(14) 0.0052(14) O3 0.0369(18) 0.0385(18) 0.0348(17) -0.0004(13) 0.0115(13) 0.0003(14) O4 0.0366(17) 0.0383(18) 0.0332(16) 0.0015(13) 0.0102(13) 0.0083(13) O5 0.051(2) 0.047(2) 0.0321(17) 0.0012(14) 0.0096(15) 0.0134(16) O6 0.0416(19) 0.042(2) 0.0443(19) 0.0019(15) 0.0126(15) 0.0048(15) O7 0.059(2) 0.047(2) 0.047(2) 0.0115(16) 0.0246(17) 0.0140(17) O8 0.060(2) 0.055(2) 0.047(2) -0.0040(17) 0.0204(18) 0.0092(18) O9 0.080(3) 0.045(2) 0.044(2) 0.0078(17) -0.0054(19) -0.002(2) N1 0.0271(19) 0.036(2) 0.039(2) 0.0046(16) 0.0129(15) 0.0062(15) N2 0.033(2) 0.044(2) 0.043(2) -0.0011(18) 0.0063(17) 0.0075(17) N3 0.0291(19) 0.043(2) 0.035(2) 0.0052(16) 0.0105(15) 0.0040(16) N4 0.038(2) 0.050(3) 0.035(2) 0.0009(18) 0.0119(17) 0.0105(18) C1 0.031(2) 0.031(2) 0.031(2) 0.0070(17) 0.0129(17) 0.0016(17) C2 0.031(2) 0.033(2) 0.039(2) 0.0046(18) 0.0144(18) 0.0025(17) C3 0.036(2) 0.034(2) 0.034(2) -0.0008(18) 0.0112(18) 0.0078(18) C4 0.036(2) 0.043(3) 0.036(2) 0.0018(19) 0.0150(19) 0.0049(19) C5 0.058(3) 0.041(3) 0.045(3) -0.004(2) 0.022(2) 0.007(2) C6 0.048(3) 0.052(3) 0.042(3) 0.007(2) 0.017(2) 0.019(2) C7 0.034(2) 0.033(2) 0.041(2) 0.0034(18) 0.0143(19) 0.0039(18) C8 0.035(2) 0.030(2) 0.036(2) 0.0040(17) 0.0139(18) -0.0010(18) C9 0.043(3) 0.044(3) 0.032(2) 0.0023(19) 0.0106(19) 0.004(2) C10 0.040(3) 0.047(3) 0.039(3) 0.006(2) 0.007(2) 0.004(2) C11 0.049(3) 0.050(3) 0.040(3) 0.008(2) 0.015(2) 0.002(2) C12 0.053(3) 0.047(3) 0.040(3) 0.001(2) 0.015(2) 0.001(2) C13 0.032(2) 0.037(3) 0.040(2) 0.0011(19) 0.0165(19) 0.0011(18) C14 0.032(2) 0.036(2) 0.035(2) 0.0072(18) 0.0146(18) 0.0067(18) C15 0.033(2) 0.041(3) 0.038(2) 0.0064(19) 0.0181(19) 0.0036(19) C16 0.035(2) 0.045(3) 0.042(3) 0.004(2) 0.015(2) 0.009(2) C17 0.026(2) 0.051(3) 0.056(3) 0.001(2) 0.009(2) 0.006(2) C18 0.039(3) 0.062(4) 0.061(4) -0.010(3) -0.005(2) 0.014(3) C19 0.046(3) 0.054(3) 0.049(3) 0.009(2) 0.005(2) 0.015(2) C20 0.035(2) 0.036(2) 0.031(2) 0.0023(18) 0.0124(18) 0.0012(18) C21 0.030(2) 0.035(2) 0.033(2) 0.0018(17) 0.0082(17) 0.0029(17) C22 0.025(2) 0.045(3) 0.034(2) 0.0002(19) 0.0125(17) 0.0025(18) C23 0.034(2) 0.043(3) 0.033(2) 0.0001(19) 0.0141(18) 0.0027(19) C24 0.041(3) 0.036(3) 0.046(3) -0.003(2) 0.019(2) 0.003(2) C25 0.099(5) 0.048(3) 0.050(3) -0.017(3) 0.047(3) -0.013(3) C26 0.052(3) 0.036(3) 0.043(3) -0.003(2) 0.012(2) 0.001(2) C27 0.052(3) 0.044(3) 0.070(4) -0.012(3) 0.009(3) 0.013(2) C28 0.035(2) 0.049(3) 0.033(2) 0.004(2) 0.0126(19) 0.005(2) C29 0.034(2) 0.042(3) 0.034(2) 0.0006(19) 0.0133(18) -0.0001(19) C30 0.060(3) 0.041(3) 0.036(3) 0.005(2) 0.021(2) 0.006(2) C31 0.092(5) 0.042(3) 0.038(3) 0.003(2) 0.025(3) 0.000(3) C32 0.075(4) 0.045(3) 0.038(3) 0.005(2) 0.016(3) 0.000(3) C33 0.059(3) 0.059(4) 0.040(3) 0.006(2) 0.027(2) 0.007(3) C34 0.028(2) 0.035(2) 0.035(2) -0.0009(18) 0.0096(17) 0.0049(17) C35 0.031(2) 0.041(3) 0.030(2) 0.0009(18) 0.0111(17) 0.0081(18) C36 0.040(3) 0.042(3) 0.039(3) 0.004(2) 0.019(2) 0.009(2) C37 0.056(3) 0.041(3) 0.045(3) 0.005(2) 0.022(2) 0.004(2) C38 0.047(3) 0.042(3) 0.052(3) 0.003(2) 0.021(2) -0.004(2) C39 0.062(4) 0.046(3) 0.049(3) 0.008(2) 0.022(3) 0.013(3) C40 0.088(5) 0.043(3) 0.051(3) 0.008(2) 0.031(3) -0.007(3) C41 0.040(3) 0.054(3) 0.040(3) 0.006(2) 0.018(2) 0.012(2) C42 0.037(3) 0.053(3) 0.038(3) 0.001(2) 0.012(2) 0.012(2) C43 0.044(3) 0.061(3) 0.036(3) -0.001(2) 0.011(2) 0.011(2) C44 0.048(3) 0.095(5) 0.047(3) -0.021(3) 0.008(3) 0.008(3) C45 0.097(6) 0.095(6) 0.038(3) 0.009(3) -0.002(3) 0.001(4) C46 0.069(4) 0.082(5) 0.045(3) -0.016(3) 0.002(3) 0.027(3) C47 0.038(3) 0.052(3) 0.036(2) -0.003(2) 0.015(2) 0.004(2) C48 0.031(2) 0.038(2) 0.033(2) 0.0051(18) 0.0137(17) 0.0079(18) C49 0.037(2) 0.036(3) 0.037(2) 0.0024(19) 0.0150(19) 0.0051(19) C50 0.025(2) 0.053(3) 0.044(3) 0.002(2) 0.0095(19) 0.007(2) C51 0.029(2) 0.051(3) 0.044(3) 0.002(2) 0.0125(19) 0.008(2) C52 0.043(3) 0.060(4) 0.043(3) 0.012(2) 0.010(2) 0.020(2) C53 0.038(3) 0.053(3) 0.045(3) 0.001(2) 0.018(2) 0.018(2) C54 0.038(3) 0.045(3) 0.037(2) 0.004(2) 0.014(2) 0.000(2) C55 0.036(2) 0.041(3) 0.033(2) 0.0041(19) 0.0127(18) 0.0029(19) C56 0.045(3) 0.043(3) 0.036(2) 0.001(2) 0.013(2) -0.003(2) C57 0.048(3) 0.040(3) 0.042(3) 0.005(2) 0.021(2) 0.009(2) C58 0.054(3) 0.040(3) 0.056(3) 0.004(2) 0.022(3) 0.007(2) C59 0.147(8) 0.061(5) 0.075(5) -0.005(4) 0.026(5) 0.037(5) C60 0.133(8) 0.053(5) 0.190(11) 0.041(5) 0.117(8) 0.034(5) C61 0.070(5) 0.052(4) 0.144(8) 0.018(4) 0.030(5) 0.018(3) C62 0.042(3) 0.044(3) 0.042(3) 0.005(2) 0.015(2) 0.012(2) C63 0.038(3) 0.049(3) 0.032(2) 0.009(2) 0.0148(19) 0.011(2) C64 0.031(2) 0.048(3) 0.039(3) 0.002(2) 0.0132(19) 0.010(2) C65 0.040(3) 0.066(4) 0.068(4) -0.007(3) 0.003(3) 0.012(3) C66 0.050(3) 0.073(4) 0.039(3) -0.008(3) 0.010(2) 0.003(3) C67 0.039(3) 0.067(4) 0.055(3) 0.011(3) 0.017(2) -0.002(3) C68 0.035(2) 0.044(3) 0.031(2) 0.0068(19) 0.0133(18) 0.0058(19) C69 0.046(3) 0.044(3) 0.049(3) -0.002(2) 0.012(2) -0.006(2) C70 0.055(3) 0.066(4) 0.036(3) 0.018(2) 0.016(2) 0.009(3) C71 0.070(4) 0.059(4) 0.071(4) -0.009(3) 0.039(3) 0.004(3) C72 0.072(5) 0.078(5) 0.070(5) 0.020(4) -0.001(4) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.932(3) . ? Co1 O1 1.968(3) . ? Co1 N2 2.131(4) . ? Co1 N1 2.136(4) . ? Co1 O5 2.163(4) . ? Co2 O3 1.928(3) . ? Co2 O4 1.961(3) . ? Co2 N4 2.129(4) . ? Co2 N3 2.147(4) . ? Co2 O6 2.165(4) . ? O1 C1 1.349(5) . ? O2 C34 1.345(5) . ? O3 C35 1.321(5) . ? O4 C68 1.348(6) . ? O5 H121 1.0079 . ? O5 H122 1.0906 . ? O6 C69 1.432(6) . ? O7 C70 1.415(6) . ? O8 C71 1.425(7) . ? O9 C72 1.414(8) . ? N1 C15 1.475(6) . ? N1 C16 1.486(6) . ? N1 C20 1.489(6) . ? N2 C18 1.478(7) . ? N2 C19 1.478(7) . ? N2 C17 1.479(7) . ? N3 C50 1.474(6) . ? N3 C49 1.486(6) . ? N3 C54 1.489(6) . ? N4 C51 1.482(7) . ? N4 C53 1.487(6) . ? N4 C52 1.492(7) . ? C1 C14 1.408(6) . ? C1 C2 1.412(6) . ? C2 C7 1.394(7) . ? C2 C3 1.541(6) . ? C3 C5 1.525(7) . ? C3 C6 1.532(7) . ? C3 C4 1.538(7) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.390(6) . ? C7 H10 0.9500 . ? C8 C13 1.391(7) . ? C8 C9 1.532(7) . ? C9 C10 1.519(7) . ? C9 C11 1.536(7) . ? C9 C12 1.548(7) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.391(7) . ? C13 H20 0.9500 . ? C14 C15 1.505(6) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.517(7) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 H27 0.9800 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C19 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C20 C21 1.521(6) . ? C20 H33 0.9900 . ? C20 H34 0.9900 . ? C21 C34 1.394(6) . ? C21 C22 1.396(6) . ? C22 C23 1.373(7) . ? C22 H35 0.9500 . ? C23 C28 1.402(6) . ? C23 C24 1.542(7) . ? C24 C25 1.515(7) . ? C24 C26 1.524(7) . ? C24 C27 1.537(8) . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C26 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C27 H44 0.9800 . ? C28 C29 1.400(7) . ? C28 H45 0.9500 . ? C29 C34 1.411(7) . ? C29 C30 1.535(6) . ? C30 C33 1.523(8) . ? C30 C32 1.530(8) . ? C30 C31 1.532(8) . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? C33 H52 0.9800 . ? C33 H53 0.9800 . ? C33 H54 0.9800 . ? C35 C36 1.413(7) . ? C35 C48 1.420(7) . ? C36 C41 1.394(7) . ? C36 C37 1.528(7) . ? C37 C40 1.525(7) . ? C37 C38 1.540(8) . ? C37 C39 1.547(7) . ? C38 H55 0.9800 . ? C38 H56 0.9800 . ? C38 H57 0.9800 . ? C39 H58 0.9800 . ? C39 H59 0.9800 . ? C39 H60 0.9800 . ? C40 H61 0.9800 . ? C40 H62 0.9800 . ? C40 H63 0.9800 . ? C41 C42 1.387(8) . ? C41 H64 0.9500 . ? C42 C47 1.385(7) . ? C42 C43 1.540(7) . ? C43 C45 1.517(9) . ? C43 C46 1.521(8) . ? C43 C44 1.535(8) . ? C44 H65 0.9800 . ? C44 H66 0.9800 . ? C44 H67 0.9800 . ? C45 H68 0.9800 . ? C45 H69 0.9800 . ? C45 H70 0.9800 . ? C46 H71 0.9800 . ? C46 H72 0.9800 . ? C46 H73 0.9800 . ? C47 C48 1.380(7) . ? C47 H74 0.9500 . ? C48 C49 1.508(6) . ? C49 H75 0.9900 . ? C49 H76 0.9900 . ? C50 C51 1.518(7) . ? C50 H77 0.9900 . ? C50 H78 0.9900 . ? C51 H79 0.9900 . ? C51 H80 0.9900 . ? C52 H81 0.9800 . ? C52 H82 0.9800 . ? C52 H83 0.9800 . ? C53 H84 0.9800 . ? C53 H85 0.9800 . ? C53 H86 0.9800 . ? C54 C55 1.503(7) . ? C54 H87 0.9900 . ? C54 H88 0.9900 . ? C55 C56 1.366(7) . ? C55 C68 1.417(7) . ? C56 C57 1.398(7) . ? C56 H89 0.9500 . ? C57 C62 1.406(7) . ? C57 C58 1.518(7) . ? C58 C60 1.498(9) . ? C58 C59 1.512(9) . ? C58 C61 1.553(9) . ? C59 H90 0.9800 . ? C59 H91 0.9800 . ? C59 H92 0.9800 . ? C60 H93 0.9800 . ? C60 H94 0.9800 . ? C60 H95 0.9800 . ? C61 H96 0.9800 . ? C61 H97 0.9800 . ? C61 H98 0.9800 . ? C62 C63 1.390(7) . ? C62 H99 0.9500 . ? C63 C68 1.420(7) . ? C63 C64 1.535(7) . ? C64 C65 1.517(7) . ? C64 C66 1.528(7) . ? C64 C67 1.538(8) . ? C65 H100 0.9800 . ? C65 H101 0.9800 . ? C65 H102 0.9800 . ? C66 H103 0.9800 . ? C66 H104 0.9800 . ? C66 H105 0.9800 . ? C67 H106 0.9800 . ? C67 H107 0.9800 . ? C67 H108 0.9800 . ? C69 H109 0.9800 . ? C69 H110 0.9800 . ? C69 H111 0.9800 . ? C70 H112 0.9800 . ? C70 H113 0.9800 . ? C70 H114 0.9800 . ? C71 H115 0.9800 . ? C71 H116 0.9800 . ? C71 H117 0.9800 . ? C72 H118 0.9800 . ? C72 H119 0.9800 . ? C72 H120 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O1 126.43(14) . . ? O2 Co1 N2 113.94(16) . . ? O1 Co1 N2 119.62(15) . . ? O2 Co1 N1 93.02(14) . . ? O1 Co1 N1 91.78(14) . . ? N2 Co1 N1 83.47(15) . . ? O2 Co1 O5 82.44(14) . . ? O1 Co1 O5 90.91(13) . . ? N2 Co1 O5 98.35(15) . . ? N1 Co1 O5 175.47(15) . . ? O3 Co2 O4 122.26(14) . . ? O3 Co2 N4 114.50(15) . . ? O4 Co2 N4 123.15(15) . . ? O3 Co2 N3 92.69(14) . . ? O4 Co2 N3 91.75(15) . . ? N4 Co2 N3 82.39(16) . . ? O3 Co2 O6 93.38(14) . . ? O4 Co2 O6 89.80(14) . . ? N4 Co2 O6 89.94(15) . . ? N3 Co2 O6 171.70(14) . . ? C1 O1 Co1 121.7(3) . . ? C34 O2 Co1 127.0(3) . . ? C35 O3 Co2 127.4(3) . . ? C68 O4 Co2 121.8(3) . . ? Co1 O5 H121 128.0 . . ? Co1 O5 H122 117.8 . . ? H121 O5 H122 105.5 . . ? C69 O6 Co2 123.0(3) . . ? C15 N1 C16 110.6(4) . . ? C15 N1 C20 109.6(4) . . ? C16 N1 C20 111.7(4) . . ? C15 N1 Co1 109.7(3) . . ? C16 N1 Co1 106.2(3) . . ? C20 N1 Co1 109.0(3) . . ? C18 N2 C19 108.3(4) . . ? C18 N2 C17 110.9(4) . . ? C19 N2 C17 109.6(4) . . ? C18 N2 Co1 112.0(3) . . ? C19 N2 Co1 108.7(3) . . ? C17 N2 Co1 107.2(3) . . ? C50 N3 C49 112.2(4) . . ? C50 N3 C54 108.8(4) . . ? C49 N3 C54 108.8(4) . . ? C50 N3 Co2 108.1(3) . . ? C49 N3 Co2 109.8(3) . . ? C54 N3 Co2 109.2(3) . . ? C51 N4 C53 108.3(4) . . ? C51 N4 C52 109.4(4) . . ? C53 N4 C52 108.5(4) . . ? C51 N4 Co2 108.2(3) . . ? C53 N4 Co2 115.4(3) . . ? C52 N4 Co2 106.9(3) . . ? O1 C1 C14 118.6(4) . . ? O1 C1 C2 122.3(4) . . ? C14 C1 C2 119.1(4) . . ? C7 C2 C1 117.6(4) . . ? C7 C2 C3 120.5(4) . . ? C1 C2 C3 121.9(4) . . ? C5 C3 C6 107.1(4) . . ? C5 C3 C4 109.9(4) . . ? C6 C3 C4 107.2(4) . . ? C5 C3 C2 109.4(4) . . ? C6 C3 C2 112.5(4) . . ? C4 C3 C2 110.7(4) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 124.4(4) . . ? C8 C7 H10 117.8 . . ? C2 C7 H10 117.8 . . ? C7 C8 C13 116.9(4) . . ? C7 C8 C9 123.2(4) . . ? C13 C8 C9 119.9(4) . . ? C10 C9 C8 113.5(4) . . ? C10 C9 C11 108.8(4) . . ? C8 C9 C11 109.6(4) . . ? C10 C9 C12 108.1(4) . . ? C8 C9 C12 109.2(4) . . ? C11 C9 C12 107.6(4) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 121.3(4) . . ? C8 C13 H20 119.4 . . ? C14 C13 H20 119.4 . . ? C13 C14 C1 120.8(4) . . ? C13 C14 C15 119.6(4) . . ? C1 C14 C15 119.6(4) . . ? N1 C15 C14 112.7(4) . . ? N1 C15 H21 109.0 . . ? C14 C15 H21 109.0 . . ? N1 C15 H22 109.0 . . ? C14 C15 H22 109.0 . . ? H21 C15 H22 107.8 . . ? N1 C16 C17 109.5(4) . . ? N1 C16 H23 109.8 . . ? C17 C16 H23 109.8 . . ? N1 C16 H24 109.8 . . ? C17 C16 H24 109.8 . . ? H23 C16 H24 108.2 . . ? N2 C17 C16 110.7(4) . . ? N2 C17 H25 109.5 . . ? C16 C17 H25 109.5 . . ? N2 C17 H26 109.5 . . ? C16 C17 H26 109.5 . . ? H25 C17 H26 108.1 . . ? N2 C18 H27 109.5 . . ? N2 C18 H28 109.5 . . ? H27 C18 H28 109.5 . . ? N2 C18 H29 109.5 . . ? H27 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? N2 C19 H30 109.5 . . ? N2 C19 H31 109.5 . . ? H30 C19 H31 109.5 . . ? N2 C19 H32 109.5 . . ? H30 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? N1 C20 C21 114.8(4) . . ? N1 C20 H33 108.6 . . ? C21 C20 H33 108.6 . . ? N1 C20 H34 108.6 . . ? C21 C20 H34 108.6 . . ? H33 C20 H34 107.5 . . ? C34 C21 C22 120.9(4) . . ? C34 C21 C20 120.2(4) . . ? C22 C21 C20 118.6(4) . . ? C23 C22 C21 122.0(4) . . ? C23 C22 H35 119.0 . . ? C21 C22 H35 119.0 . . ? C22 C23 C28 116.6(4) . . ? C22 C23 C24 124.0(4) . . ? C28 C23 C24 119.4(4) . . ? C25 C24 C26 108.8(5) . . ? C25 C24 C27 109.0(5) . . ? C26 C24 C27 107.7(5) . . ? C25 C24 C23 111.1(4) . . ? C26 C24 C23 109.0(4) . . ? C27 C24 C23 111.3(4) . . ? C24 C25 H36 109.5 . . ? C24 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? C24 C25 H38 109.5 . . ? H36 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C24 C26 H39 109.5 . . ? C24 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? C24 C26 H41 109.5 . . ? H39 C26 H41 109.5 . . ? H40 C26 H41 109.5 . . ? C24 C27 H42 109.5 . . ? C24 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? C24 C27 H44 109.5 . . ? H42 C27 H44 109.5 . . ? H43 C27 H44 109.5 . . ? C29 C28 C23 123.7(5) . . ? C29 C28 H45 118.2 . . ? C23 C28 H45 118.2 . . ? C28 C29 C34 117.9(4) . . ? C28 C29 C30 119.7(4) . . ? C34 C29 C30 122.4(4) . . ? C33 C30 C32 110.9(5) . . ? C33 C30 C31 107.7(5) . . ? C32 C30 C31 107.2(5) . . ? C33 C30 C29 109.3(4) . . ? C32 C30 C29 109.8(4) . . ? C31 C30 C29 111.9(4) . . ? C30 C31 H46 109.5 . . ? C30 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? C30 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? C30 C32 H49 109.5 . . ? C30 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? C30 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? C30 C33 H52 109.5 . . ? C30 C33 H53 109.5 . . ? H52 C33 H53 109.5 . . ? C30 C33 H54 109.5 . . ? H52 C33 H54 109.5 . . ? H53 C33 H54 109.5 . . ? O2 C34 C21 120.9(4) . . ? O2 C34 C29 120.2(4) . . ? C21 C34 C29 118.9(4) . . ? O3 C35 C36 121.5(4) . . ? O3 C35 C48 120.9(4) . . ? C36 C35 C48 117.6(4) . . ? C41 C36 C35 118.7(5) . . ? C41 C36 C37 121.3(5) . . ? C35 C36 C37 120.1(4) . . ? C40 C37 C36 112.1(5) . . ? C40 C37 C38 107.0(5) . . ? C36 C37 C38 110.6(4) . . ? C40 C37 C39 107.0(5) . . ? C36 C37 C39 110.1(4) . . ? C38 C37 C39 109.9(5) . . ? C37 C38 H55 109.5 . . ? C37 C38 H56 109.5 . . ? H55 C38 H56 109.5 . . ? C37 C38 H57 109.5 . . ? H55 C38 H57 109.5 . . ? H56 C38 H57 109.5 . . ? C37 C39 H58 109.5 . . ? C37 C39 H59 109.5 . . ? H58 C39 H59 109.5 . . ? C37 C39 H60 109.5 . . ? H58 C39 H60 109.5 . . ? H59 C39 H60 109.5 . . ? C37 C40 H61 109.5 . . ? C37 C40 H62 109.5 . . ? H61 C40 H62 109.5 . . ? C37 C40 H63 109.5 . . ? H61 C40 H63 109.5 . . ? H62 C40 H63 109.5 . . ? C42 C41 C36 124.0(5) . . ? C42 C41 H64 118.0 . . ? C36 C41 H64 118.0 . . ? C47 C42 C41 116.4(5) . . ? C47 C42 C43 120.4(5) . . ? C41 C42 C43 123.2(5) . . ? C45 C43 C46 108.4(5) . . ? C45 C43 C44 108.0(5) . . ? C46 C43 C44 108.3(5) . . ? C45 C43 C42 112.4(5) . . ? C46 C43 C42 109.1(5) . . ? C44 C43 C42 110.6(4) . . ? C43 C44 H65 109.5 . . ? C43 C44 H66 109.5 . . ? H65 C44 H66 109.5 . . ? C43 C44 H67 109.5 . . ? H65 C44 H67 109.5 . . ? H66 C44 H67 109.5 . . ? C43 C45 H68 109.5 . . ? C43 C45 H69 109.5 . . ? H68 C45 H69 109.5 . . ? C43 C45 H70 109.5 . . ? H68 C45 H70 109.5 . . ? H69 C45 H70 109.5 . . ? C43 C46 H71 109.5 . . ? C43 C46 H72 109.5 . . ? H71 C46 H72 109.5 . . ? C43 C46 H73 109.5 . . ? H71 C46 H73 109.5 . . ? H72 C46 H73 109.5 . . ? C48 C47 C42 122.3(5) . . ? C48 C47 H74 118.8 . . ? C42 C47 H74 118.8 . . ? C47 C48 C35 120.9(4) . . ? C47 C48 C49 119.0(4) . . ? C35 C48 C49 120.0(4) . . ? N3 C49 C48 113.8(4) . . ? N3 C49 H75 108.8 . . ? C48 C49 H75 108.8 . . ? N3 C49 H76 108.8 . . ? C48 C49 H76 108.8 . . ? H75 C49 H76 107.7 . . ? N3 C50 C51 110.0(4) . . ? N3 C50 H77 109.7 . . ? C51 C50 H77 109.7 . . ? N3 C50 H78 109.7 . . ? C51 C50 H78 109.7 . . ? H77 C50 H78 108.2 . . ? N4 C51 C50 110.4(4) . . ? N4 C51 H79 109.6 . . ? C50 C51 H79 109.6 . . ? N4 C51 H80 109.6 . . ? C50 C51 H80 109.6 . . ? H79 C51 H80 108.1 . . ? N4 C52 H81 109.5 . . ? N4 C52 H82 109.5 . . ? H81 C52 H82 109.5 . . ? N4 C52 H83 109.5 . . ? H81 C52 H83 109.5 . . ? H82 C52 H83 109.5 . . ? N4 C53 H84 109.5 . . ? N4 C53 H85 109.5 . . ? H84 C53 H85 109.5 . . ? N4 C53 H86 109.5 . . ? H84 C53 H86 109.5 . . ? H85 C53 H86 109.5 . . ? N3 C54 C55 112.9(4) . . ? N3 C54 H87 109.0 . . ? C55 C54 H87 109.0 . . ? N3 C54 H88 109.0 . . ? C55 C54 H88 109.0 . . ? H87 C54 H88 107.8 . . ? C56 C55 C68 121.0(5) . . ? C56 C55 C54 120.3(4) . . ? C68 C55 C54 118.7(4) . . ? C55 C56 C57 122.5(5) . . ? C55 C56 H89 118.8 . . ? C57 C56 H89 118.8 . . ? C56 C57 C62 115.8(5) . . ? C56 C57 C58 121.0(5) . . ? C62 C57 C58 123.2(5) . . ? C60 C58 C59 111.1(7) . . ? C60 C58 C57 108.8(5) . . ? C59 C58 C57 110.2(5) . . ? C60 C58 C61 108.7(6) . . ? C59 C58 C61 105.6(6) . . ? C57 C58 C61 112.4(5) . . ? C58 C59 H90 109.5 . . ? C58 C59 H91 109.5 . . ? H90 C59 H91 109.5 . . ? C58 C59 H92 109.5 . . ? H90 C59 H92 109.5 . . ? H91 C59 H92 109.5 . . ? C58 C60 H93 109.5 . . ? C58 C60 H94 109.5 . . ? H93 C60 H94 109.5 . . ? C58 C60 H95 109.5 . . ? H93 C60 H95 109.5 . . ? H94 C60 H95 109.5 . . ? C58 C61 H96 109.5 . . ? C58 C61 H97 109.5 . . ? H96 C61 H97 109.5 . . ? C58 C61 H98 109.5 . . ? H96 C61 H98 109.5 . . ? H97 C61 H98 109.5 . . ? C63 C62 C57 124.3(5) . . ? C63 C62 H99 117.8 . . ? C57 C62 H99 117.8 . . ? C62 C63 C68 117.8(5) . . ? C62 C63 C64 120.7(4) . . ? C68 C63 C64 121.5(4) . . ? C65 C64 C66 108.4(5) . . ? C65 C64 C63 112.9(4) . . ? C66 C64 C63 109.4(4) . . ? C65 C64 C67 106.7(5) . . ? C66 C64 C67 109.6(5) . . ? C63 C64 C67 109.9(4) . . ? C64 C65 H100 109.5 . . ? C64 C65 H101 109.5 . . ? H100 C65 H101 109.5 . . ? C64 C65 H102 109.5 . . ? H100 C65 H102 109.5 . . ? H101 C65 H102 109.5 . . ? C64 C66 H103 109.5 . . ? C64 C66 H104 109.5 . . ? H103 C66 H104 109.5 . . ? C64 C66 H105 109.5 . . ? H103 C66 H105 109.5 . . ? H104 C66 H105 109.5 . . ? C64 C67 H106 109.5 . . ? C64 C67 H107 109.5 . . ? H106 C67 H107 109.5 . . ? C64 C67 H108 109.5 . . ? H106 C67 H108 109.5 . . ? H107 C67 H108 109.5 . . ? O4 C68 C55 119.5(4) . . ? O4 C68 C63 122.0(4) . . ? C55 C68 C63 118.6(5) . . ? O6 C69 H109 109.5 . . ? O6 C69 H110 109.5 . . ? H109 C69 H110 109.5 . . ? O6 C69 H111 109.5 . . ? H109 C69 H111 109.5 . . ? H110 C69 H111 109.5 . . ? O7 C70 H112 109.5 . . ? O7 C70 H113 109.5 . . ? H112 C70 H113 109.5 . . ? O7 C70 H114 109.5 . . ? H112 C70 H114 109.5 . . ? H113 C70 H114 109.5 . . ? O8 C71 H115 109.5 . . ? O8 C71 H116 109.5 . . ? H115 C71 H116 109.5 . . ? O8 C71 H117 109.5 . . ? H115 C71 H117 109.5 . . ? H116 C71 H117 109.5 . . ? O9 C72 H118 109.5 . . ? O9 C72 H119 109.5 . . ? H118 C72 H119 109.5 . . ? O9 C72 H120 109.5 . . ? H118 C72 H120 109.5 . . ? H119 C72 H120 109.5 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.498 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.104 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 766023' #TrackingRef 'C002843F_Compiled_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H66 Co N2 O2' _chemical_formula_sum 'C40 H66 Co N2 O2' _chemical_formula_weight 665.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 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 10.833(2) _cell_length_b 30.704(7) _cell_length_c 11.725(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.829(4) _cell_angle_gamma 90.00 _cell_volume 3895.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used 8301 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.47 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7805 _exptl_absorpt_correction_T_max 0.8709 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 198(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15018 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8666 _reflns_number_gt 6879 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.1206P)^2^+0.7947P] 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 8666 _refine_ls_number_parameters 473 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.75519(3) 0.066500(9) 0.06186(2) 0.03255(10) Uani 1 1 d . . . N1 N 0.60496(16) 0.09578(6) 0.13131(14) 0.0348(4) Uani 1 1 d . . . N2 N 0.74064(19) 0.01810(6) 0.18617(14) 0.0402(4) Uani 1 1 d . . . O1 O 0.87414(13) 0.10964(5) 0.09641(11) 0.0344(3) Uani 1 1 d . . . O2 O 0.67693(15) 0.04959(5) -0.07927(12) 0.0459(4) Uani 1 1 d . . . C1 C 0.86311(19) 0.14017(6) 0.17791(16) 0.0306(4) Uani 1 1 d . . . C2 C 0.97058(19) 0.15779(7) 0.23520(18) 0.0345(4) Uani 1 1 d . . . C3 C 0.9548(2) 0.18810(8) 0.3212(2) 0.0435(5) Uani 1 1 d . . . H3 H 1.0270 0.2001 0.3585 0.052 Uiso 1 1 calc R . . C4 C 0.8413(2) 0.20213(8) 0.3566(2) 0.0469(6) Uani 1 1 d . . . C5 C 0.7381(2) 0.18539(8) 0.2966(2) 0.0447(6) Uani 1 1 d . . . H5 H 0.6585 0.1947 0.3169 0.054 Uiso 1 1 calc R . . C6 C 0.74643(19) 0.15549(7) 0.20799(17) 0.0351(5) Uani 1 1 d . . . C7 C 0.6299(2) 0.14334(7) 0.13967(19) 0.0391(5) Uani 1 1 d . . . H7A H 0.5590 0.1575 0.1746 0.047 Uiso 1 1 calc R . . H7B H 0.6350 0.1552 0.0615 0.047 Uiso 1 1 calc R . . C8 C 0.5931(2) 0.07509(9) 0.24311(18) 0.0462(6) Uani 1 1 d . . . H8A H 0.5084 0.0797 0.2689 0.055 Uiso 1 1 calc R . . H8B H 0.6520 0.0887 0.2998 0.055 Uiso 1 1 calc R . . C9 C 0.6195(2) 0.02631(9) 0.2357(2) 0.0503(6) Uani 1 1 d . . . H9A H 0.6193 0.0134 0.3130 0.060 Uiso 1 1 calc R . . H9B H 0.5534 0.0121 0.1877 0.060 Uiso 1 1 calc R . . C10 C 0.8436(2) 0.02295(7) 0.27518(17) 0.0421(5) Uani 1 1 d D . . H10A H 0.8354 0.0518 0.3119 0.050 Uiso 1 1 calc R . . H10B H 0.9228 0.0229 0.2365 0.050 Uiso 1 1 calc R . . C11 C 0.8509(3) -0.01135(9) 0.3678(2) 0.0604(7) Uani 1 1 d D . . H11A H 0.7739 -0.0114 0.4082 0.091 Uiso 1 1 calc R . . H11B H 0.9204 -0.0049 0.4217 0.091 Uiso 1 1 calc R . . H11C H 0.8631 -0.0400 0.3334 0.091 Uiso 1 1 calc R . . C12 C 0.7415(3) -0.02548(8) 0.1307(2) 0.0642(8) Uani 1 1 d D . . H12A H 0.6690 -0.0278 0.0764 0.077 Uiso 1 1 calc R . . H12B H 0.7335 -0.0482 0.1898 0.077 Uiso 1 1 calc R . . C13 C 0.8559(4) -0.03376(10) 0.0686(3) 0.0884(12) Uani 1 1 d D . . H13A H 0.8630 -0.0119 0.0083 0.133 Uiso 1 1 calc R . . H13B H 0.8518 -0.0629 0.0345 0.133 Uiso 1 1 calc R . . H13C H 0.9280 -0.0319 0.1222 0.133 Uiso 1 1 calc R . . C14 C 0.4934(2) 0.08725(9) 0.05575(18) 0.0422(5) Uani 1 1 d . . . H14A H 0.4231 0.1040 0.0843 0.051 Uiso 1 1 calc R . . H14B H 0.4724 0.0559 0.0600 0.051 Uiso 1 1 calc R . . C15 C 0.5998(2) 0.07852(8) -0.13057(18) 0.0418(5) Uani 1 1 d . . . C16 C 0.6071(2) 0.08837(9) -0.24798(19) 0.0508(6) Uani 1 1 d . . . C17 C 0.5238(3) 0.11817(9) -0.2962(2) 0.0573(7) Uani 1 1 d . . . H17 H 0.5294 0.1250 -0.3748 0.069 Uiso 1 1 calc R . . C18 C 0.4323(3) 0.13871(9) -0.2361(2) 0.0514(6) Uani 1 1 d . A . C19 C 0.4278(2) 0.12892(8) -0.12045(19) 0.0458(6) Uani 1 1 d . . . H19 H 0.3678 0.1427 -0.0763 0.055 Uiso 1 1 calc R . . C20 C 0.5096(2) 0.09935(8) -0.06862(18) 0.0402(5) Uani 1 1 d . . . C21 C 1.1010(2) 0.14336(8) 0.2036(2) 0.0414(5) Uani 1 1 d . . . C22 C 1.1170(2) 0.15112(9) 0.0764(2) 0.0513(6) Uani 1 1 d . . . H22A H 1.0528 0.1353 0.0316 0.077 Uiso 1 1 calc R . . H22B H 1.1986 0.1407 0.0561 0.077 Uiso 1 1 calc R . . H22C H 1.1100 0.1823 0.0599 0.077 Uiso 1 1 calc R . . C23 C 1.2026(2) 0.16980(10) 0.2684(3) 0.0605(7) Uani 1 1 d . . . H23A H 1.1889 0.2009 0.2543 0.091 Uiso 1 1 calc R . . H23B H 1.2835 0.1614 0.2417 0.091 Uiso 1 1 calc R . . H23C H 1.2000 0.1639 0.3504 0.091 Uiso 1 1 calc R . . C24 C 1.1197(2) 0.09425(8) 0.2320(2) 0.0467(6) Uani 1 1 d D . . H24A H 1.0577 0.0772 0.1860 0.056 Uiso 1 1 calc R . . H24B H 1.2025 0.0854 0.2085 0.056 Uiso 1 1 calc R . . C25 C 1.1089(3) 0.08283(10) 0.3553(2) 0.0653(8) Uani 1 1 d D . . H25A H 1.1799 0.0947 0.4001 0.098 Uiso 1 1 calc R . . H25B H 1.1073 0.0511 0.3638 0.098 Uiso 1 1 calc R . . H25C H 1.0324 0.0952 0.3827 0.098 Uiso 1 1 calc R . . C26 C 0.8329(3) 0.23544(10) 0.4536(3) 0.0690(9) Uani 1 1 d . . . C29 C 0.9413(4) 0.23043(17) 0.5447(4) 0.1016(14) Uani 1 1 d D . . C27 C 0.7115(4) 0.23151(16) 0.5131(4) 0.1188(18) Uani 1 1 d . . . H27A H 0.7066 0.2027 0.5488 0.178 Uiso 1 1 calc R . . H27B H 0.6422 0.2351 0.4569 0.178 Uiso 1 1 calc R . . H27C H 0.7076 0.2541 0.5718 0.178 Uiso 1 1 calc R . . C28 C 0.8440(5) 0.28181(13) 0.4058(4) 0.1103(15) Uani 1 1 d D . . C30 C 0.9297(13) 0.1874(3) 0.5977(11) 0.165(7) Uani 0.40 1 d PD . . H30A H 0.8427 0.1784 0.5934 0.247 Uiso 0.40 1 calc PR . . H30B H 0.9595 0.1889 0.6779 0.247 Uiso 0.40 1 calc PR . . H30C H 0.9790 0.1662 0.5572 0.247 Uiso 0.40 1 calc PR . . C30' C 0.7277(7) 0.2929(2) 0.3433(6) 0.067(2) Uani 0.38 1 d PD . . H30D H 0.7291 0.3237 0.3211 0.100 Uiso 0.38 1 calc PR . . H30E H 0.6584 0.2878 0.3923 0.100 Uiso 0.38 1 calc PR . . H30F H 0.7178 0.2748 0.2747 0.100 Uiso 0.38 1 calc PR . . C30" C 0.9616(10) 0.2876(4) 0.3490(12) 0.111(8) Uani 0.22 1 d PD . . H30G H 0.9946 0.2590 0.3290 0.166 Uiso 0.22 1 calc PR . . H30H H 1.0212 0.3026 0.4009 0.166 Uiso 0.22 1 calc PR . . H30I H 0.9470 0.3050 0.2795 0.166 Uiso 0.22 1 calc PR . . C31 C 0.7025(3) 0.06591(13) -0.3203(2) 0.0780(10) Uani 1 1 d . . . C32 C 0.6671(4) 0.01525(12) -0.3302(3) 0.0966(13) Uani 1 1 d . . . H32A H 0.7398 -0.0014 -0.3509 0.145 Uiso 1 1 calc R . . H32B H 0.6006 0.0114 -0.3890 0.145 Uiso 1 1 calc R . . H32C H 0.6395 0.0049 -0.2566 0.145 Uiso 1 1 calc R . . C33 C 0.7025(5) 0.08451(17) -0.4423(3) 0.1191(18) Uani 1 1 d . . . H33A H 0.7377 0.1139 -0.4399 0.179 Uiso 1 1 calc R . . H33B H 0.6176 0.0857 -0.4750 0.179 Uiso 1 1 calc R . . H33C H 0.7524 0.0658 -0.4896 0.179 Uiso 1 1 calc R . . C34 C 0.8317(4) 0.06453(18) -0.2688(4) 0.1128(17) Uani 1 1 d D . . H34A H 0.8338 0.0457 -0.2001 0.135 Uiso 1 1 calc R . . H34B H 0.8868 0.0514 -0.3243 0.135 Uiso 1 1 calc R . . C35 C 0.8774(4) 0.10729(18) -0.2374(5) 0.142(2) Uani 1 1 d D . . H35A H 0.8835 0.1251 -0.3063 0.214 Uiso 1 1 calc R . . H35B H 0.9592 0.1046 -0.1986 0.214 Uiso 1 1 calc R . . H35C H 0.8204 0.1212 -0.1861 0.214 Uiso 1 1 calc R . . C36 C 0.3374(3) 0.16900(10) -0.2963(2) 0.0675(8) Uani 1 1 d D . . C37 C 0.2541(8) 0.1418(3) -0.3811(6) 0.108(3) Uani 0.63 1 d PDU A 1 H37A H 0.2057 0.1614 -0.4317 0.162 Uiso 0.63 1 calc PR A 1 H37B H 0.1981 0.1236 -0.3384 0.162 Uiso 0.63 1 calc PR A 1 H37C H 0.3061 0.1231 -0.4268 0.162 Uiso 0.63 1 calc PR A 1 C38 C 0.2412(6) 0.1886(2) -0.2164(5) 0.0760(18) Uani 0.63 1 d PDU A 1 H38A H 0.2845 0.2032 -0.1518 0.114 Uiso 0.63 1 calc PR A 1 H38B H 0.1895 0.1652 -0.1878 0.114 Uiso 0.63 1 calc PR A 1 H38C H 0.1891 0.2096 -0.2591 0.114 Uiso 0.63 1 calc PR A 1 C39 C 0.4105(7) 0.2039(2) -0.3586(6) 0.109(3) Uani 0.63 1 d PD A 1 C40 C 0.4480(7) 0.2344(2) -0.2652(8) 0.152(4) Uani 0.63 1 d PDU A 1 H40A H 0.3886 0.2327 -0.2050 0.229 Uiso 0.63 1 calc PR A 1 H40B H 0.4497 0.2642 -0.2952 0.229 Uiso 0.63 1 calc PR A 1 H40C H 0.5304 0.2265 -0.2337 0.229 Uiso 0.63 1 calc PR A 1 C37' C 0.2139(9) 0.1433(5) -0.3065(15) 0.143(6) Uani 0.37 1 d PDU A 2 H37D H 0.2314 0.1120 -0.3116 0.215 Uiso 0.37 1 calc PR A 2 H37E H 0.1660 0.1526 -0.3753 0.215 Uiso 0.37 1 calc PR A 2 H37F H 0.1662 0.1489 -0.2391 0.215 Uiso 0.37 1 calc PR A 2 C38' C 0.3036(15) 0.2066(4) -0.2155(10) 0.125(5) Uani 0.37 1 d PDU A 2 H38D H 0.2713 0.1945 -0.1456 0.188 Uiso 0.37 1 calc PR A 2 H38E H 0.2406 0.2252 -0.2538 0.188 Uiso 0.37 1 calc PR A 2 H38F H 0.3775 0.2240 -0.1961 0.188 Uiso 0.37 1 calc PR A 2 C39' C 0.3704(11) 0.1785(4) -0.4218(6) 0.096(4) Uani 0.37 1 d PD A 2 C40' C 0.3509(16) 0.2262(4) -0.4175(19) 0.191(7) Uani 0.37 1 d PDU A 2 H40D H 0.4090 0.2407 -0.4666 0.286 Uiso 0.37 1 calc PR A 2 H40E H 0.3649 0.2365 -0.3388 0.286 Uiso 0.37 1 calc PR A 2 H40F H 0.2660 0.2331 -0.4444 0.286 Uiso 0.37 1 calc PR A 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 0.03762(17) 0.03470(16) 0.02496(15) -0.00146(11) -0.00223(11) -0.00152(13) N1 0.0326(9) 0.0449(10) 0.0268(8) -0.0008(7) -0.0010(7) -0.0040(8) N2 0.0543(12) 0.0349(9) 0.0305(9) 0.0006(7) -0.0073(8) -0.0113(9) O1 0.0360(8) 0.0351(7) 0.0323(7) -0.0074(6) 0.0045(6) -0.0014(7) O2 0.0531(10) 0.0532(9) 0.0302(7) -0.0087(7) -0.0080(7) 0.0106(8) C1 0.0362(11) 0.0280(9) 0.0276(9) 0.0001(7) 0.0023(8) 0.0005(9) C2 0.0331(11) 0.0336(10) 0.0370(11) -0.0033(8) 0.0026(9) -0.0016(9) C3 0.0387(12) 0.0459(13) 0.0458(12) -0.0127(10) 0.0001(10) -0.0078(11) C4 0.0491(14) 0.0439(13) 0.0480(13) -0.0172(10) 0.0059(11) -0.0030(12) C5 0.0373(12) 0.0514(13) 0.0457(13) -0.0142(10) 0.0052(10) 0.0037(11) C6 0.0339(11) 0.0368(11) 0.0343(10) -0.0049(8) 0.0005(9) 0.0023(10) C7 0.0328(11) 0.0467(12) 0.0374(11) -0.0086(9) -0.0013(9) 0.0067(10) C8 0.0380(12) 0.0728(17) 0.0279(10) 0.0044(10) 0.0023(9) -0.0041(12) C9 0.0468(14) 0.0604(15) 0.0431(13) 0.0150(11) -0.0047(11) -0.0181(13) C10 0.0495(13) 0.0428(12) 0.0330(11) -0.0002(9) -0.0078(10) -0.0030(11) C11 0.0737(19) 0.0637(17) 0.0428(13) 0.0137(12) -0.0071(13) 0.0049(15) C12 0.107(2) 0.0354(12) 0.0481(14) -0.0043(10) -0.0163(15) -0.0180(15) C13 0.146(4) 0.0543(17) 0.0640(19) -0.0214(15) -0.010(2) 0.027(2) C14 0.0318(11) 0.0597(15) 0.0345(11) -0.0001(10) -0.0043(9) -0.0045(11) C15 0.0471(13) 0.0480(12) 0.0293(10) -0.0063(9) -0.0079(9) 0.0002(11) C16 0.0613(16) 0.0598(15) 0.0305(11) -0.0065(10) -0.0048(11) 0.0108(14) C17 0.0723(18) 0.0688(17) 0.0301(11) -0.0004(11) -0.0047(12) 0.0108(15) C18 0.0554(15) 0.0545(15) 0.0430(13) 0.0023(11) -0.0110(11) 0.0053(13) C19 0.0409(12) 0.0562(14) 0.0393(12) -0.0024(10) -0.0076(10) 0.0016(12) C20 0.0371(12) 0.0509(13) 0.0317(11) -0.0029(9) -0.0054(9) -0.0052(11) C21 0.0304(11) 0.0455(12) 0.0482(13) -0.0049(10) 0.0010(9) 0.0003(10) C22 0.0383(13) 0.0563(15) 0.0605(15) 0.0015(12) 0.0159(11) 0.0018(12) C23 0.0356(13) 0.0643(17) 0.082(2) -0.0184(15) 0.0026(13) -0.0082(13) C24 0.0361(12) 0.0472(13) 0.0563(14) -0.0055(11) -0.0037(10) 0.0058(11) C25 0.0688(18) 0.0659(17) 0.0588(17) 0.0065(14) -0.0199(14) 0.0004(16) C26 0.0618(18) 0.0707(19) 0.0752(19) -0.0426(16) 0.0112(15) -0.0074(16) C29 0.094(3) 0.135(4) 0.074(2) -0.066(2) -0.011(2) -0.002(3) C27 0.098(3) 0.151(4) 0.111(3) -0.091(3) 0.046(2) -0.030(3) C28 0.151(4) 0.061(2) 0.120(4) -0.039(2) 0.027(3) -0.013(3) C30 0.109(10) 0.26(2) 0.123(12) -0.055(13) -0.005(9) 0.011(13) C30' 0.117(7) 0.044(4) 0.039(3) 0.002(3) -0.002(4) 0.031(4) C30" 0.22(2) 0.035(7) 0.071(10) -0.022(6) -0.038(13) 0.007(11) C31 0.085(2) 0.119(3) 0.0302(13) 0.0005(14) 0.0055(14) 0.037(2) C32 0.121(3) 0.093(3) 0.078(2) -0.008(2) 0.030(2) 0.047(3) C33 0.166(4) 0.156(4) 0.0372(16) 0.011(2) 0.028(2) 0.078(4) C34 0.075(3) 0.182(5) 0.083(3) -0.006(3) 0.023(2) 0.000(3) C35 0.086(3) 0.145(5) 0.197(6) 0.002(4) 0.013(3) -0.007(3) C36 0.080(2) 0.0711(19) 0.0497(15) 0.0079(13) -0.0109(15) 0.0245(17) C37 0.125(6) 0.102(5) 0.089(5) -0.026(4) -0.072(5) 0.036(4) C38 0.084(4) 0.070(4) 0.073(3) 0.015(3) -0.007(3) 0.025(3) C39 0.111(6) 0.074(4) 0.139(7) 0.059(5) -0.021(5) 0.004(4) C40 0.101(5) 0.074(4) 0.276(12) 0.006(6) -0.058(6) -0.004(4) C37' 0.128(11) 0.097(9) 0.194(14) 0.037(10) -0.109(11) 0.003(8) C38' 0.136(12) 0.081(9) 0.153(11) 0.029(8) -0.044(10) 0.031(8) C39' 0.103(8) 0.095(8) 0.087(7) 0.042(6) -0.024(6) 0.015(7) C40' 0.105(10) 0.248(16) 0.221(17) -0.020(15) 0.029(11) 0.023(12) _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 1.8782(14) . ? Co1 O2 1.8942(15) . ? Co1 N1 2.0616(18) . ? Co1 N2 2.0929(18) . ? N1 C8 1.468(3) . ? N1 C14 1.486(3) . ? N1 C7 1.487(3) . ? N2 C9 1.482(3) . ? N2 C12 1.488(3) . ? N2 C10 1.497(3) . ? O1 C1 1.348(2) . ? O2 C15 1.341(3) . ? C1 C6 1.410(3) . ? C1 C2 1.422(3) . ? C2 C3 1.389(3) . ? C2 C21 1.543(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.390(3) . ? C4 C26 1.536(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C7 1.508(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.528(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.512(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.489(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C20 1.523(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.401(3) . ? C15 C16 1.415(3) . ? C16 C17 1.386(4) . ? C16 C31 1.533(4) . ? C17 C18 1.395(4) . ? C17 H17 0.9500 . ? C18 C19 1.392(3) . ? C18 C36 1.532(4) . ? C19 C20 1.387(3) . ? C19 H19 0.9500 . ? C21 C22 1.529(3) . ? C21 C23 1.538(3) . ? C21 C24 1.555(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.498(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.523(5) . ? C26 C28 1.537(5) . ? C26 C29 1.555(5) . ? C29 C30 1.468(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30' 1.467(4) . ? C28 C30" 1.477(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30' H30D 0.9800 . ? C30' H30E 0.9800 . ? C30' H30F 0.9800 . ? C30" H30G 0.9800 . ? C30" H30H 0.9800 . ? C30" H30I 0.9800 . ? C31 C34 1.497(6) . ? C31 C33 1.541(4) . ? C31 C32 1.605(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.444(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C39 1.539(4) . ? C36 C38' 1.549(5) . ? C36 C37' 1.554(5) . ? C36 C37 1.554(4) . ? C36 C38 1.556(4) . ? C36 C39' 1.559(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.482(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38' H38D 0.9800 . ? C38' H38E 0.9800 . ? C38' H38F 0.9800 . ? C39' C40' 1.482(4) . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 130.88(7) . . ? O1 Co1 N1 98.85(7) . . ? O2 Co1 N1 97.85(7) . . ? O1 Co1 N2 115.15(7) . . ? O2 Co1 N2 111.59(7) . . ? N1 Co1 N2 86.93(8) . . ? C8 N1 C14 110.60(17) . . ? C8 N1 C7 112.93(17) . . ? C14 N1 C7 110.62(17) . . ? C8 N1 Co1 105.63(14) . . ? C14 N1 Co1 108.80(13) . . ? C7 N1 Co1 108.04(12) . . ? C9 N2 C12 110.42(19) . . ? C9 N2 C10 110.71(17) . . ? C12 N2 C10 111.93(19) . . ? C9 N2 Co1 104.49(14) . . ? C12 N2 Co1 109.40(14) . . ? C10 N2 Co1 109.63(13) . . ? C1 O1 Co1 124.01(13) . . ? C15 O2 Co1 116.89(13) . . ? O1 C1 C6 121.42(18) . . ? O1 C1 C2 120.02(18) . . ? C6 C1 C2 118.56(18) . . ? C3 C2 C1 118.08(19) . . ? C3 C2 C21 120.90(19) . . ? C1 C2 C21 121.01(18) . . ? C4 C3 C2 124.6(2) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C3 C4 C5 116.0(2) . . ? C3 C4 C26 121.0(2) . . ? C5 C4 C26 123.0(2) . . ? C4 C5 C6 122.7(2) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 119.91(19) . . ? C5 C6 C7 118.42(19) . . ? C1 C6 C7 121.46(18) . . ? N1 C7 C6 114.99(18) . . ? N1 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N1 C8 C9 110.37(19) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N2 C9 C8 111.17(19) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C11 116.3(2) . . ? N2 C10 H10A 108.2 . . ? C11 C10 H10A 108.2 . . ? N2 C10 H10B 108.2 . . ? C11 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 113.0(2) . . ? N2 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N2 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C20 113.51(18) . . ? N1 C14 H14A 108.9 . . ? C20 C14 H14A 108.9 . . ? N1 C14 H14B 108.9 . . ? C20 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? O2 C15 C20 120.33(19) . . ? O2 C15 C16 121.0(2) . . ? C20 C15 C16 118.7(2) . . ? C17 C16 C15 118.2(2) . . ? C17 C16 C31 121.0(2) . . ? C15 C16 C31 120.9(2) . . ? C16 C17 C18 123.8(2) . . ? C16 C17 H17 118.1 . . ? C18 C17 H17 118.1 . . ? C19 C18 C17 117.0(2) . . ? C19 C18 C36 121.6(2) . . ? C17 C18 C36 121.3(2) . . ? C20 C19 C18 121.0(2) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 121.2(2) . . ? C19 C20 C14 118.5(2) . . ? C15 C20 C14 120.1(2) . . ? C22 C21 C23 106.6(2) . . ? C22 C21 C2 109.84(19) . . ? C23 C21 C2 111.80(19) . . ? C22 C21 C24 109.86(19) . . ? C23 C21 C24 108.9(2) . . ? C2 C21 C24 109.78(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C21 114.7(2) . . ? C25 C24 H24A 108.6 . . ? C21 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? C21 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C4 111.8(2) . . ? C27 C26 C28 109.0(3) . . ? C4 C26 C28 109.7(3) . . ? C27 C26 C29 108.5(3) . . ? C4 C26 C29 111.9(3) . . ? C28 C26 C29 105.8(3) . . ? C30 C29 C26 107.6(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? H30G C30" H30I 109.5 . . ? H30H C30" H30I 109.5 . . ? C34 C31 C16 115.6(3) . . ? C34 C31 C33 110.0(4) . . ? C16 C31 C33 112.2(3) . . ? C34 C31 C32 102.5(3) . . ? C16 C31 C32 108.1(3) . . ? C33 C31 C32 107.7(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C31 112.3(4) . . ? C35 C34 H34A 109.2 . . ? C31 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C31 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C18 C36 C39 107.0(3) . . ? C18 C36 C38' 110.2(6) . . ? C18 C36 C37' 106.4(5) . . ? C18 C36 C37 108.9(4) . . ? C39 C36 C37 111.5(5) . . ? C18 C36 C38 114.3(3) . . ? C39 C36 C38 113.1(4) . . ? C37 C36 C38 102.0(5) . . ? C18 C36 C39' 111.6(4) . . ? C37' C36 C39' 105.0(8) . . ? C38 C36 C39' 133.5(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C36 102.6(5) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C37' H37D 109.5 . . ? C36 C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C36 C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C36 C38' H38D 109.5 . . ? C36 C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C36 C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C40' C39' C36 96.5(11) . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.857 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.076 #===END data_3CH3OH _database_code_depnum_ccdc_archive 'CCDC 766024' #TrackingRef 'Kozak_Compiled_CIF.cif' # start Validation Reply Form _vrf_CHEMW03_3CH3OH ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: Three disordered toluene molecules were removed via the Platon Squeeze procedure.These were included in the formula for the calculation of intensive properties (for example, molecular weight and density). ; _vrf_PLAT220_3CH3OH ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.89 Ratio RESPONSE: This carbon is part of a terminal (2-methylbutan-2-yl), and does not indicate that an atom type has been incorrectly assigned. ; _vrf_PLAT222_3CH3OH ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.54 Ratio RESPONSE: This hydrogen was introduced in a calculated position, and neighbors a large carbon, which is part of a terminal (2-methylbutan-2-yl), and was refined on a riding model. ; _vrf_PLAT412_3CH3OH ; PROBLEM: Short Intra XH3 .. XHn H27 .. H61 .. 1.31 Ang. RESPONSE: This is a short H .. H contact involving CH3 H-atoms. While these are often the result of not optimal calculated positions, other orientations also produced shorter contacts with other CH3 H-atoms. ; _vrf_PLAT043_3CH3OH ; PROBLEM: Check Reported Molecular Weight ................ 1656.19 RESPONSE: Three disordered toluene molecules were removed via the Platon Squeeze procedure.These were included in the formula for the calculation of intensive properties (for example, molecular weight and density). ; _vrf_PLAT044_3CH3OH ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: Three disordered toluene molecules were removed via the Platon Squeeze procedure.These were included in the formula for the calculation of intensive properties (for example, molecular weight and density). ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C40 H58 N2 O2), 2Co, 2(C H3 O H), 3(C7 H8)' _chemical_formula_sum 'C103 H148 Co2 N4 O6' _chemical_formula_weight 1656.19 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.346(3) _cell_length_b 15.283(5) _cell_length_c 15.482(5) _cell_angle_alpha 100.085(3) _cell_angle_beta 97.893(3) _cell_angle_gamma 105.592(4) _cell_volume 2277.1(13) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7090 _cell_measurement_theta_min 1.7348 _cell_measurement_theta_max 29.6346 _exptl_crystal_description Chunk _exptl_crystal_colour Black _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9387 _exptl_absorpt_correction_T_min 0.8507 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 17963 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.1187 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9168 _reflns_number_gt 8618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1222P)^2^+0.9085P] 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 9168 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1794 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 -0.016 -0.018 -0.018 624 154 '3 Disordered Toluene' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 154 electrons per unit cell in one void (total volume 624 ^A^3); that is 154 electrons per formula unit (with Z=1 in this model). Disordered solvent lattice toluene molecules were present prior to the application of Squeeze, however, a satisfactory point atom model could not be achieved. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 0.93060(2) 0.399098(15) 0.963107(15) 0.01941(12) Uani 1 1 d . . . O1 O 0.81972(14) 0.40277(9) 1.05117(9) 0.0220(3) Uani 1 1 d . . . O2 O 0.76593(14) 0.33345(9) 0.87718(9) 0.0228(3) Uani 1 1 d . . . O3 O 0.91102(14) 0.51827(9) 0.94878(9) 0.0218(3) Uani 1 1 d . . . N1 N 0.97001(17) 0.28579(11) 0.98376(11) 0.0213(3) Uani 1 1 d . . . N2 N 1.03322(17) 0.39134(12) 0.86959(11) 0.0228(3) Uani 1 1 d . . . C1 C 0.7848(2) 0.33962(13) 1.10006(13) 0.0219(4) Uani 1 1 d . . . C2 C 0.6597(2) 0.32513(13) 1.13249(13) 0.0229(4) Uani 1 1 d . . . C3 C 0.5501(2) 0.37058(14) 1.10226(14) 0.0252(4) Uani 1 1 d . . . C4 C 0.5028(2) 0.33824(15) 0.99908(14) 0.0289(4) Uani 1 1 d . . . H1 H 0.4303 0.3659 0.9803 0.035 Uiso 1 1 calc R . . H2 H 0.5810 0.3631 0.9708 0.035 Uiso 1 1 calc R . . C5 C 0.4486(3) 0.23349(17) 0.96391(17) 0.0410(6) Uani 1 1 d . . . H3 H 0.4235 0.2194 0.8985 0.049 Uiso 1 1 calc R . . H4 H 0.3678 0.2083 0.9887 0.049 Uiso 1 1 calc R . . H5 H 0.5195 0.2051 0.9818 0.049 Uiso 1 1 calc R . . C6 C 0.6051(2) 0.47756(15) 1.12789(16) 0.0321(5) Uani 1 1 d . . . H6 H 0.6909 0.4982 1.1067 0.039 Uiso 1 1 calc R . . H7 H 0.6218 0.4987 1.1931 0.039 Uiso 1 1 calc R . . H8 H 0.5377 0.5039 1.1003 0.039 Uiso 1 1 calc R . . C7 C 0.4243(2) 0.34497(16) 1.14593(16) 0.0317(5) Uani 1 1 d . . . H9 H 0.3626 0.3806 1.1296 0.038 Uiso 1 1 calc R . . H10 H 0.4538 0.3598 1.2111 0.038 Uiso 1 1 calc R . . H11 H 0.3764 0.2782 1.1250 0.038 Uiso 1 1 calc R . . C8 C 0.6333(2) 0.26232(14) 1.18785(13) 0.0263(4) Uani 1 1 d . . . H12 H 0.5522 0.2551 1.2117 0.032 Uiso 1 1 calc R . . C9 C 0.7187(2) 0.20905(15) 1.21068(14) 0.0275(4) Uani 1 1 d . . . C10 C 0.6771(3) 0.13971(16) 1.27021(15) 0.0344(5) Uani 1 1 d . . . C11 C 0.5354(3) 0.06828(17) 1.22686(18) 0.0426(6) Uani 1 1 d . . . H13 H 0.5118 0.0243 1.2663 0.051 Uiso 1 1 calc R . . H14 H 0.4663 0.1022 1.2243 0.051 Uiso 1 1 calc R . . C12 C 0.5247(4) 0.0121(2) 1.1332(2) 0.0609(8) Uani 1 1 d . . . H15 H 0.4318 -0.0306 1.1117 0.073 Uiso 1 1 calc R . . H16 H 0.5903 -0.0237 1.1349 0.073 Uiso 1 1 calc R . . H17 H 0.5451 0.0546 1.0929 0.073 Uiso 1 1 calc R . . C13 C 0.6662(3) 0.1930(2) 1.36103(16) 0.0436(6) Uani 1 1 d . . . H18 H 0.5966 0.2249 1.3524 0.052 Uiso 1 1 calc R . . H19 H 0.7547 0.2389 1.3894 0.052 Uiso 1 1 calc R . . H20 H 0.6402 0.1491 1.3994 0.052 Uiso 1 1 calc R . . C14 C 0.7821(3) 0.0867(2) 1.28605(19) 0.0461(6) Uani 1 1 d . . . H21 H 0.7500 0.0414 1.3220 0.055 Uiso 1 1 calc R . . H22 H 0.8703 0.1309 1.3179 0.055 Uiso 1 1 calc R . . H23 H 0.7929 0.0540 1.2284 0.055 Uiso 1 1 calc R . . C15 C 0.8355(2) 0.22072(14) 1.17441(13) 0.0263(4) Uani 1 1 d . . . H24 H 0.8940 0.1840 1.1862 0.032 Uiso 1 1 calc R . . C16 C 0.8699(2) 0.28492(13) 1.12089(12) 0.0228(4) Uani 1 1 d . . . C17 C 0.9972(2) 0.29117(14) 1.08266(13) 0.0244(4) Uani 1 1 d . . . H25 H 1.0678 0.3507 1.1129 0.029 Uiso 1 1 calc R . . H26 H 1.0332 0.2397 1.0943 0.029 Uiso 1 1 calc R . . C18 C 1.0959(2) 0.28303(15) 0.94740(15) 0.0276(4) Uani 1 1 d . . . H27 H 1.1784 0.3186 0.9935 0.033 Uiso 1 1 calc R . . H28 H 1.0975 0.2178 0.9309 0.033 Uiso 1 1 calc R . . C19 C 1.0959(2) 0.32460(14) 0.86690(14) 0.0258(4) Uani 1 1 d . . . C20 C 1.1552(2) 0.29933(15) 0.79578(15) 0.0318(5) Uani 1 1 d . . . H29 H 1.2002 0.2527 0.7952 0.038 Uiso 1 1 calc R . . C21 C 1.1478(2) 0.34350(17) 0.72493(15) 0.0351(5) Uani 1 1 d . . . H30 H 1.1870 0.3270 0.6748 0.042 Uiso 1 1 calc R . . C22 C 1.0826(2) 0.41200(17) 0.72801(15) 0.0328(5) Uani 1 1 d . . . H31 H 1.0760 0.4425 0.6799 0.039 Uiso 1 1 calc R . . C23 C 1.0273(2) 0.43537(15) 0.80219(14) 0.0264(4) Uani 1 1 d . . . H32 H 0.9845 0.4833 0.8053 0.032 Uiso 1 1 calc R . . C24 C 0.8556(2) 0.19948(13) 0.93727(13) 0.0237(4) Uani 1 1 d . . . H33 H 0.8829 0.1441 0.9469 0.028 Uiso 1 1 calc R . . H34 H 0.7740 0.1991 0.9641 0.028 Uiso 1 1 calc R . . C25 C 0.8191(2) 0.19307(13) 0.83909(13) 0.0232(4) Uani 1 1 d . . . C26 C 0.8339(2) 0.12069(14) 0.77658(14) 0.0276(4) Uani 1 1 d . . . H35 H 0.8732 0.0764 0.7963 0.033 Uiso 1 1 calc R . . C27 C 0.7917(2) 0.11267(15) 0.68584(15) 0.0314(5) Uani 1 1 d . . . C28 C 0.8096(3) 0.03462(18) 0.61514(16) 0.0416(6) Uani 1 1 d . . . C29 C 0.8494(4) 0.0699(2) 0.5328(2) 0.0600(8) Uani 1 1 d . . . H36 H 0.8627 0.0178 0.4907 0.072 Uiso 1 1 calc R . . H37 H 0.7714 0.0865 0.5028 0.072 Uiso 1 1 calc R . . C30 C 0.9719(5) 0.1500(3) 0.5485(3) 0.0819(13) Uani 1 1 d . . . H38 H 1.0362 0.1494 0.6010 0.098 Uiso 1 1 calc R . . H39 H 0.9463 0.2076 0.5590 0.098 Uiso 1 1 calc R . . H40 H 1.0151 0.1464 0.4961 0.098 Uiso 1 1 calc R . . C31 C 0.9174(7) -0.0062(4) 0.6518(2) 0.121(2) Uani 1 1 d . . . H41 H 0.8945 -0.0718 0.6213 0.145 Uiso 1 1 calc R . . H42 H 0.9209 -0.0015 0.7161 0.145 Uiso 1 1 calc R . . H43 H 1.0066 0.0283 0.6419 0.145 Uiso 1 1 calc R . . C32 C 0.6731(6) -0.0420(3) 0.5824(4) 0.129(3) Uani 1 1 d . . . H44 H 0.6674 -0.0732 0.5205 0.155 Uiso 1 1 calc R . . H45 H 0.5980 -0.0145 0.5855 0.155 Uiso 1 1 calc R . . H46 H 0.6662 -0.0874 0.6204 0.155 Uiso 1 1 calc R . . C33 C 0.7271(2) 0.17655(16) 0.66161(14) 0.0311(5) Uani 1 1 d . . . H47 H 0.6918 0.1690 0.5999 0.037 Uiso 1 1 calc R . . C34 C 0.7104(2) 0.25104(15) 0.72165(14) 0.0270(4) Uani 1 1 d . . . C35 C 0.6230(2) 0.31052(16) 0.68980(14) 0.0313(5) Uani 1 1 d . . . C36 C 0.4902(2) 0.28649(18) 0.72719(17) 0.0386(5) Uani 1 1 d . . . H48 H 0.5144 0.3052 0.7933 0.046 Uiso 1 1 calc R . . H49 H 0.4327 0.3241 0.7067 0.046 Uiso 1 1 calc R . . C37 C 0.4053(3) 0.1841(2) 0.7005(2) 0.0520(7) Uani 1 1 d . . . H50 H 0.4629 0.1455 0.7161 0.062 Uiso 1 1 calc R . . H51 H 0.3698 0.1668 0.6358 0.062 Uiso 1 1 calc R . . H52 H 0.3288 0.1741 0.7322 0.062 Uiso 1 1 calc R . . C38 C 0.5866(3) 0.2918(2) 0.58739(17) 0.0471(7) Uani 1 1 d . . . H53 H 0.5235 0.2288 0.5640 0.056 Uiso 1 1 calc R . . H54 H 0.6701 0.2975 0.5628 0.056 Uiso 1 1 calc R . . H55 H 0.5429 0.3373 0.5700 0.056 Uiso 1 1 calc R . . C39 C 0.6941(3) 0.41577(17) 0.72309(17) 0.0390(5) Uani 1 1 d . . . H56 H 0.6299 0.4499 0.7072 0.047 Uiso 1 1 calc R . . H57 H 0.7737 0.4340 0.6951 0.047 Uiso 1 1 calc R . . H58 H 0.7240 0.4305 0.7882 0.047 Uiso 1 1 calc R . . C40 C 0.76514(19) 0.26171(13) 0.81353(13) 0.0224(4) Uani 1 1 d . . . C41 C 0.7774(3) 0.52509(19) 0.9573(2) 0.0435(6) Uani 1 1 d . . . H59 H 0.7407 0.4868 0.9981 0.052 Uiso 1 1 calc R . . H60 H 0.7165 0.5029 0.8985 0.052 Uiso 1 1 calc R . . H61 H 0.7837 0.5902 0.9812 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01897(18) 0.01744(17) 0.02162(18) 0.00195(11) 0.00389(11) 0.00668(12) O1 0.0231(7) 0.0190(6) 0.0262(7) 0.0053(5) 0.0070(5) 0.0087(5) O2 0.0211(7) 0.0220(6) 0.0233(7) -0.0007(5) 0.0024(5) 0.0081(5) O3 0.0198(7) 0.0205(6) 0.0243(7) 0.0027(5) 0.0023(5) 0.0074(5) N1 0.0210(8) 0.0208(8) 0.0226(8) 0.0023(6) 0.0043(6) 0.0085(6) N2 0.0202(8) 0.0212(8) 0.0246(8) 0.0009(6) 0.0038(6) 0.0052(6) C1 0.0240(10) 0.0187(8) 0.0211(9) 0.0023(7) 0.0021(7) 0.0060(7) C2 0.0257(10) 0.0214(9) 0.0219(9) 0.0043(7) 0.0042(7) 0.0083(7) C3 0.0229(9) 0.0235(9) 0.0302(10) 0.0072(8) 0.0046(8) 0.0081(8) C4 0.0251(10) 0.0320(10) 0.0297(10) 0.0107(8) 0.0025(8) 0.0077(8) C5 0.0438(14) 0.0353(12) 0.0354(12) 0.0014(10) -0.0019(10) 0.0067(10) C6 0.0289(11) 0.0250(10) 0.0445(12) 0.0072(9) 0.0090(9) 0.0109(8) C7 0.0285(11) 0.0343(11) 0.0374(11) 0.0114(9) 0.0116(9) 0.0129(9) C8 0.0299(10) 0.0270(10) 0.0246(9) 0.0075(8) 0.0077(8) 0.0102(8) C9 0.0360(11) 0.0263(10) 0.0234(9) 0.0088(8) 0.0066(8) 0.0121(9) C10 0.0484(14) 0.0356(11) 0.0302(11) 0.0171(9) 0.0158(10) 0.0204(10) C11 0.0545(16) 0.0335(12) 0.0469(14) 0.0194(11) 0.0194(12) 0.0135(11) C12 0.079(2) 0.0388(14) 0.0534(18) 0.0016(13) 0.0140(16) 0.0028(15) C13 0.0616(17) 0.0496(14) 0.0303(11) 0.0174(10) 0.0177(11) 0.0248(13) C14 0.0616(17) 0.0525(15) 0.0464(14) 0.0327(12) 0.0232(13) 0.0336(14) C15 0.0328(11) 0.0270(10) 0.0223(9) 0.0065(7) 0.0046(8) 0.0138(8) C16 0.0252(10) 0.0224(9) 0.0201(8) 0.0033(7) 0.0029(7) 0.0078(8) C17 0.0252(10) 0.0260(9) 0.0232(9) 0.0053(7) 0.0014(7) 0.0112(8) C18 0.0244(10) 0.0280(10) 0.0339(11) 0.0047(8) 0.0084(8) 0.0135(8) C19 0.0216(9) 0.0236(9) 0.0310(10) 0.0013(8) 0.0064(8) 0.0070(7) C20 0.0296(11) 0.0305(10) 0.0361(11) 0.0005(9) 0.0124(9) 0.0120(9) C21 0.0323(11) 0.0406(12) 0.0308(11) 0.0007(9) 0.0133(9) 0.0091(10) C22 0.0293(11) 0.0417(12) 0.0277(10) 0.0078(9) 0.0087(8) 0.0096(9) C23 0.0223(10) 0.0296(10) 0.0274(10) 0.0058(8) 0.0060(8) 0.0077(8) C24 0.0240(9) 0.0198(9) 0.0268(10) 0.0031(7) 0.0054(7) 0.0067(7) C25 0.0224(9) 0.0212(9) 0.0235(9) 0.0008(7) 0.0052(7) 0.0048(7) C26 0.0313(11) 0.0219(9) 0.0304(10) 0.0010(8) 0.0079(8) 0.0116(8) C27 0.0367(12) 0.0302(10) 0.0276(10) -0.0007(8) 0.0086(9) 0.0138(9) C28 0.0618(17) 0.0370(12) 0.0312(11) -0.0014(9) 0.0151(11) 0.0259(12) C29 0.086(2) 0.0549(17) 0.0457(16) 0.0042(13) 0.0254(16) 0.0299(17) C30 0.091(3) 0.066(2) 0.076(2) -0.0136(19) 0.048(2) 0.006(2) C31 0.230(7) 0.145(4) 0.0406(18) 0.003(2) 0.021(3) 0.157(5) C32 0.141(5) 0.066(3) 0.138(5) -0.054(3) 0.084(4) -0.017(3) C33 0.0332(11) 0.0371(11) 0.0219(9) -0.0005(8) 0.0031(8) 0.0144(9) C34 0.0237(10) 0.0310(10) 0.0257(10) 0.0014(8) 0.0037(8) 0.0111(8) C35 0.0336(11) 0.0366(11) 0.0256(10) 0.0030(8) 0.0012(8) 0.0183(9) C36 0.0309(12) 0.0429(13) 0.0410(12) -0.0030(10) 0.0016(10) 0.0199(10) C37 0.0350(13) 0.0504(15) 0.0605(17) -0.0107(13) 0.0100(12) 0.0104(12) C38 0.0591(17) 0.0597(16) 0.0283(11) 0.0049(11) -0.0017(11) 0.0359(14) C39 0.0428(13) 0.0373(12) 0.0399(12) 0.0106(10) 0.0013(10) 0.0187(10) C40 0.0200(9) 0.0217(9) 0.0239(9) -0.0007(7) 0.0048(7) 0.0069(7) C41 0.0397(14) 0.0409(13) 0.0502(15) 0.0083(11) 0.0090(11) 0.0136(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 O1 1.9013(15) . ? Co1 N2 1.9150(17) . ? Co1 O2 1.9157(15) . ? Co1 O3 1.9326(15) . ? Co1 N1 1.9505(17) . ? Co1 O3 1.9522(15) 2_767 ? Co1 Co1 2.9688(10) 2_767 ? O1 C1 1.334(2) . ? O2 C40 1.337(2) . ? O3 C41 1.436(3) . ? O3 Co1 1.9522(14) 2_767 ? N1 C18 1.496(2) . ? N1 C24 1.501(2) . ? N1 C17 1.502(3) . ? N2 C23 1.340(3) . ? N2 C19 1.346(3) . ? C1 C16 1.411(3) . ? C1 C2 1.428(3) . ? C2 C8 1.394(3) . ? C2 C3 1.542(3) . ? C3 C6 1.538(3) . ? C3 C7 1.538(3) . ? C3 C4 1.554(3) . ? C4 C5 1.517(3) . ? C4 H1 0.9900 . ? C4 H2 0.9900 . ? C5 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C7 H9 0.9800 . ? C7 H10 0.9800 . ? C7 H11 0.9800 . ? C8 C9 1.403(3) . ? C8 H12 0.9500 . ? C9 C15 1.383(3) . ? C9 C10 1.537(3) . ? C10 C13 1.531(3) . ? C10 C14 1.538(3) . ? C10 C11 1.551(4) . ? C11 C12 1.523(4) . ? C11 H13 0.9900 . ? C11 H14 0.9900 . ? C12 H15 0.9800 . ? C12 H16 0.9800 . ? C12 H17 0.9800 . ? C13 H18 0.9800 . ? C13 H19 0.9800 . ? C13 H20 0.9800 . ? C14 H21 0.9800 . ? C14 H22 0.9800 . ? C14 H23 0.9800 . ? C15 C16 1.398(3) . ? C15 H24 0.9500 . ? C16 C17 1.503(3) . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 C19 1.495(3) . ? C18 H27 0.9900 . ? C18 H28 0.9900 . ? C19 C20 1.379(3) . ? C20 C21 1.389(3) . ? C20 H29 0.9500 . ? C21 C22 1.387(3) . ? C21 H30 0.9500 . ? C22 C23 1.386(3) . ? C22 H31 0.9500 . ? C23 H32 0.9500 . ? C24 C25 1.494(3) . ? C24 H33 0.9900 . ? C24 H34 0.9900 . ? C25 C26 1.393(3) . ? C25 C40 1.403(3) . ? C26 C27 1.386(3) . ? C26 H35 0.9500 . ? C27 C33 1.397(3) . ? C27 C28 1.540(3) . ? C28 C31 1.510(5) . ? C28 C32 1.526(6) . ? C28 C29 1.533(4) . ? C29 C30 1.463(5) . ? C29 H36 0.9900 . ? C29 H37 0.9900 . ? C30 H38 0.9800 . ? C30 H39 0.9800 . ? C30 H40 0.9800 . ? C31 H41 0.9800 . ? C31 H42 0.9800 . ? C31 H43 0.9800 . ? C32 H44 0.9800 . ? C32 H45 0.9800 . ? C32 H46 0.9800 . ? C33 C34 1.403(3) . ? C33 H47 0.9500 . ? C34 C40 1.421(3) . ? C34 C35 1.537(3) . ? C35 C38 1.535(3) . ? C35 C39 1.537(3) . ? C35 C36 1.542(3) . ? C36 C37 1.525(4) . ? C36 H48 0.9900 . ? C36 H49 0.9900 . ? C37 H50 0.9800 . ? C37 H51 0.9800 . ? C37 H52 0.9800 . ? C38 H53 0.9800 . ? C38 H54 0.9800 . ? C38 H55 0.9800 . ? C39 H56 0.9800 . ? C39 H57 0.9800 . ? C39 H58 0.9800 . ? C41 H59 0.9800 . ? C41 H60 0.9800 . ? C41 H61 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N2 176.79(6) . . ? O1 Co1 O2 87.44(7) . . ? N2 Co1 O2 89.35(7) . . ? O1 Co1 O3 87.39(6) . . ? N2 Co1 O3 92.89(7) . . ? O2 Co1 O3 91.72(6) . . ? O1 Co1 N1 94.40(6) . . ? N2 Co1 N1 85.64(7) . . ? O2 Co1 N1 94.05(7) . . ? O3 Co1 N1 174.03(6) . . ? O1 Co1 O3 89.86(7) . 2_767 ? N2 Co1 O3 93.34(7) . 2_767 ? O2 Co1 O3 171.71(6) . 2_767 ? O3 Co1 O3 80.33(7) . 2_767 ? N1 Co1 O3 93.97(7) . 2_767 ? O1 Co1 Co1 88.21(4) . 2_767 ? N2 Co1 Co1 94.08(5) . 2_767 ? O2 Co1 Co1 132.09(4) . 2_767 ? O3 Co1 Co1 40.41(4) . 2_767 ? N1 Co1 Co1 133.86(5) . 2_767 ? O3 Co1 Co1 39.92(4) 2_767 2_767 ? C1 O1 Co1 126.55(12) . . ? C40 O2 Co1 119.46(12) . . ? C41 O3 Co1 112.14(14) . . ? C41 O3 Co1 118.89(14) . 2_767 ? Co1 O3 Co1 99.67(6) . 2_767 ? C18 N1 C24 108.99(15) . . ? C18 N1 C17 109.70(16) . . ? C24 N1 C17 110.16(15) . . ? C18 N1 Co1 106.76(12) . . ? C24 N1 Co1 112.34(12) . . ? C17 N1 Co1 108.83(11) . . ? C23 N2 C19 120.14(18) . . ? C23 N2 Co1 124.70(14) . . ? C19 N2 Co1 114.22(14) . . ? O1 C1 C16 121.04(18) . . ? O1 C1 C2 120.89(17) . . ? C16 C1 C2 118.07(17) . . ? C8 C2 C1 118.03(18) . . ? C8 C2 C3 119.75(18) . . ? C1 C2 C3 122.04(17) . . ? C6 C3 C7 105.42(17) . . ? C6 C3 C2 111.80(17) . . ? C7 C3 C2 112.79(17) . . ? C6 C3 C4 109.22(17) . . ? C7 C3 C4 108.66(17) . . ? C2 C3 C4 108.84(16) . . ? C5 C4 C3 114.99(18) . . ? C5 C4 H1 108.5 . . ? C3 C4 H1 108.5 . . ? C5 C4 H2 108.5 . . ? C3 C4 H2 108.5 . . ? H1 C4 H2 107.5 . . ? C4 C5 H3 109.5 . . ? C4 C5 H4 109.5 . . ? H3 C5 H4 109.5 . . ? C4 C5 H5 109.5 . . ? H3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C6 H6 109.5 . . ? C3 C6 H7 109.5 . . ? H6 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H6 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C7 H9 109.5 . . ? C3 C7 H10 109.5 . . ? H9 C7 H10 109.5 . . ? C3 C7 H11 109.5 . . ? H9 C7 H11 109.5 . . ? H10 C7 H11 109.5 . . ? C2 C8 C9 124.30(19) . . ? C2 C8 H12 117.8 . . ? C9 C8 H12 117.8 . . ? C15 C9 C8 116.43(19) . . ? C15 C9 C10 123.72(19) . . ? C8 C9 C10 119.8(2) . . ? C13 C10 C9 109.12(19) . . ? C13 C10 C14 108.3(2) . . ? C9 C10 C14 112.0(2) . . ? C13 C10 C11 108.2(2) . . ? C9 C10 C11 110.18(19) . . ? C14 C10 C11 108.9(2) . . ? C12 C11 C10 115.6(2) . . ? C12 C11 H13 108.4 . . ? C10 C11 H13 108.4 . . ? C12 C11 H14 108.4 . . ? C10 C11 H14 108.4 . . ? H13 C11 H14 107.4 . . ? C11 C12 H15 109.5 . . ? C11 C12 H16 109.5 . . ? H15 C12 H16 109.5 . . ? C11 C12 H17 109.5 . . ? H15 C12 H17 109.5 . . ? H16 C12 H17 109.5 . . ? C10 C13 H18 109.5 . . ? C10 C13 H19 109.5 . . ? H18 C13 H19 109.5 . . ? C10 C13 H20 109.5 . . ? H18 C13 H20 109.5 . . ? H19 C13 H20 109.5 . . ? C10 C14 H21 109.5 . . ? C10 C14 H22 109.5 . . ? H21 C14 H22 109.5 . . ? C10 C14 H23 109.5 . . ? H21 C14 H23 109.5 . . ? H22 C14 H23 109.5 . . ? C9 C15 C16 121.91(19) . . ? C9 C15 H24 119.0 . . ? C16 C15 H24 119.0 . . ? C15 C16 C1 121.11(18) . . ? C15 C16 C17 118.13(17) . . ? C1 C16 C17 120.71(17) . . ? N1 C17 C16 111.72(16) . . ? N1 C17 H25 109.3 . . ? C16 C17 H25 109.3 . . ? N1 C17 H26 109.3 . . ? C16 C17 H26 109.3 . . ? H25 C17 H26 107.9 . . ? C19 C18 N1 109.01(17) . . ? C19 C18 H27 109.9 . . ? N1 C18 H27 109.9 . . ? C19 C18 H28 109.9 . . ? N1 C18 H28 109.9 . . ? H27 C18 H28 108.3 . . ? N2 C19 C20 121.7(2) . . ? N2 C19 C18 113.87(17) . . ? C20 C19 C18 124.44(19) . . ? C19 C20 C21 118.6(2) . . ? C19 C20 H29 120.7 . . ? C21 C20 H29 120.7 . . ? C22 C21 C20 119.4(2) . . ? C22 C21 H30 120.3 . . ? C20 C21 H30 120.3 . . ? C23 C22 C21 119.2(2) . . ? C23 C22 H31 120.4 . . ? C21 C22 H31 120.4 . . ? N2 C23 C22 121.0(2) . . ? N2 C23 H32 119.5 . . ? C22 C23 H32 119.5 . . ? C25 C24 N1 112.48(16) . . ? C25 C24 H33 109.1 . . ? N1 C24 H33 109.1 . . ? C25 C24 H34 109.1 . . ? N1 C24 H34 109.1 . . ? H33 C24 H34 107.8 . . ? C26 C25 C40 122.03(19) . . ? C26 C25 C24 121.39(18) . . ? C40 C25 C24 116.55(17) . . ? C27 C26 C25 120.59(19) . . ? C27 C26 H35 119.7 . . ? C25 C26 H35 119.7 . . ? C26 C27 C33 116.76(18) . . ? C26 C27 C28 121.7(2) . . ? C33 C27 C28 121.5(2) . . ? C31 C28 C32 109.5(4) . . ? C31 C28 C29 108.2(3) . . ? C32 C28 C29 106.5(3) . . ? C31 C28 C27 111.9(2) . . ? C32 C28 C27 109.0(2) . . ? C29 C28 C27 111.5(2) . . ? C30 C29 C28 116.8(3) . . ? C30 C29 H36 108.1 . . ? C28 C29 H36 108.1 . . ? C30 C29 H37 108.1 . . ? C28 C29 H37 108.1 . . ? H36 C29 H37 107.3 . . ? C29 C30 H38 109.5 . . ? C29 C30 H39 109.5 . . ? H38 C30 H39 109.5 . . ? C29 C30 H40 109.5 . . ? H38 C30 H40 109.5 . . ? H39 C30 H40 109.5 . . ? C28 C31 H41 109.5 . . ? C28 C31 H42 109.5 . . ? H41 C31 H42 109.5 . . ? C28 C31 H43 109.5 . . ? H41 C31 H43 109.5 . . ? H42 C31 H43 109.5 . . ? C28 C32 H44 109.5 . . ? C28 C32 H45 109.5 . . ? H44 C32 H45 109.5 . . ? C28 C32 H46 109.5 . . ? H44 C32 H46 109.5 . . ? H45 C32 H46 109.5 . . ? C27 C33 C34 124.9(2) . . ? C27 C33 H47 117.6 . . ? C34 C33 H47 117.6 . . ? C33 C34 C40 116.70(19) . . ? C33 C34 C35 120.82(19) . . ? C40 C34 C35 122.13(17) . . ? C38 C35 C39 106.6(2) . . ? C38 C35 C34 112.17(18) . . ? C39 C35 C34 113.02(19) . . ? C38 C35 C36 109.2(2) . . ? C39 C35 C36 107.88(19) . . ? C34 C35 C36 107.79(19) . . ? C37 C36 C35 115.16(19) . . ? C37 C36 H48 108.5 . . ? C35 C36 H48 108.5 . . ? C37 C36 H49 108.5 . . ? C35 C36 H49 108.5 . . ? H48 C36 H49 107.5 . . ? C36 C37 H50 109.5 . . ? C36 C37 H51 109.5 . . ? H50 C37 H51 109.5 . . ? C36 C37 H52 109.5 . . ? H50 C37 H52 109.5 . . ? H51 C37 H52 109.5 . . ? C35 C38 H53 109.5 . . ? C35 C38 H54 109.5 . . ? H53 C38 H54 109.5 . . ? C35 C38 H55 109.5 . . ? H53 C38 H55 109.5 . . ? H54 C38 H55 109.5 . . ? C35 C39 H56 109.5 . . ? C35 C39 H57 109.5 . . ? H56 C39 H57 109.5 . . ? C35 C39 H58 109.5 . . ? H56 C39 H58 109.5 . . ? H57 C39 H58 109.5 . . ? O2 C40 C25 118.28(18) . . ? O2 C40 C34 123.13(18) . . ? C25 C40 C34 118.58(17) . . ? O3 C41 H59 109.5 . . ? O3 C41 H60 109.5 . . ? H59 C41 H60 109.5 . . ? O3 C41 H61 109.5 . . ? H59 C41 H61 109.5 . . ? H60 C41 H61 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.329 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.079 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 766025' #TrackingRef 'Kozak_Compiled_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H106.80 Co3 N4 O12.40' _chemical_formula_sum 'C64 H106.80 Co3 N4 O12.40' _chemical_formula_weight 1307.57 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.7690(9) _cell_length_b 17.4799(17) _cell_length_c 19.904(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.771(2) _cell_angle_gamma 90.00 _cell_volume 3398.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 12285 _cell_measurement_theta_min 2.0848 _cell_measurement_theta_max 30.6963 _exptl_crystal_description Irregular _exptl_crystal_colour Purple _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.69 _exptl_crystal_size_min 0.68 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.7350 _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 30947 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7781 _reflns_number_gt 7348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0739P)^2^+2.4436P] 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 7781 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.61053(3) 0.157568(15) 0.147841(13) 0.02451(9) Uani 1 1 d . . . Co2 Co 0.5000 0.0000 0.0000 0.02697(11) Uani 1 2 d S . . O1 O 0.47297(14) 0.08314(8) 0.18106(7) 0.0265(3) Uani 1 1 d . . . O2 O 0.66448(14) 0.19910(8) 0.05849(7) 0.0265(3) Uani 1 1 d . . . O3 O 0.76570(15) 0.07841(9) 0.15315(8) 0.0319(3) Uani 1 1 d . . . O4 O 0.65067(18) 0.02272(11) 0.07159(8) 0.0406(4) Uani 1 1 d . . . O5 O 0.36105(16) 0.03975(9) 0.06902(8) 0.0359(3) Uani 1 1 d . . . O6 O 0.46363(18) -0.11294(9) 0.02994(8) 0.0376(4) Uani 1 1 d . . . O7 O 0.5425(16) 0.5038(9) 0.2444(8) 0.084(4) Uiso 0.20 1 d P . . N1 N 0.44989(16) 0.24797(9) 0.15427(8) 0.0251(3) Uani 1 1 d . . . N2 N 0.70017(18) 0.22633(11) 0.22667(9) 0.0312(4) Uani 1 1 d . . . C1 C 0.37891(19) 0.09697(11) 0.22846(10) 0.0253(4) Uani 1 1 d . . . C2 C 0.3581(2) 0.04526(12) 0.28221(10) 0.0300(4) Uani 1 1 d . . . C3 C 0.4382(2) -0.03039(13) 0.28801(12) 0.0355(5) Uani 1 1 d . . . C4 C 0.5937(3) -0.01606(16) 0.29070(14) 0.0460(6) Uani 1 1 d . . . H1 H 0.6149 0.0215 0.3259 0.055 Uiso 1 1 calc R . . H2 H 0.6237 0.0036 0.2472 0.055 Uiso 1 1 calc R . . H3 H 0.6413 -0.0641 0.3007 0.055 Uiso 1 1 calc R . . C5 C 0.4027(3) -0.08068(14) 0.22728(14) 0.0496(6) Uani 1 1 d . . . H4 H 0.4281 -0.0541 0.1859 0.059 Uiso 1 1 calc R . . H5 H 0.3041 -0.0911 0.2264 0.059 Uiso 1 1 calc R . . H6 H 0.4530 -0.1290 0.2306 0.059 Uiso 1 1 calc R . . C6 C 0.4024(3) -0.07538(16) 0.35136(14) 0.0469(6) Uani 1 1 d . . . H7 H 0.4582 -0.1219 0.3537 0.056 Uiso 1 1 calc R . . H8 H 0.3052 -0.0893 0.3498 0.056 Uiso 1 1 calc R . . H9 H 0.4210 -0.0438 0.3911 0.056 Uiso 1 1 calc R . . C7 C 0.2569(2) 0.06358(13) 0.32849(11) 0.0349(5) Uani 1 1 d . . . H10 H 0.2426 0.0296 0.3650 0.042 Uiso 1 1 calc R . . C8 C 0.1757(2) 0.12916(14) 0.32388(11) 0.0343(4) Uani 1 1 d . . . C9 C 0.0655(3) 0.14401(17) 0.37503(14) 0.0458(6) Uani 1 1 d . . . H11 H 0.0196 0.0958 0.3859 0.055 Uiso 1 1 calc R . . H12 H -0.0015 0.1802 0.3564 0.055 Uiso 1 1 calc R . . H13 H 0.1072 0.1656 0.4159 0.055 Uiso 1 1 calc R . . C10 C 0.1979(2) 0.17861(12) 0.27055(11) 0.0303(4) Uani 1 1 d . . . H14 H 0.1445 0.2238 0.2665 0.036 Uiso 1 1 calc R . . C11 C 0.2971(2) 0.16290(11) 0.22285(10) 0.0262(4) Uani 1 1 d . . . C12 C 0.3114(2) 0.21370(11) 0.16220(10) 0.0274(4) Uani 1 1 d . . . H15 H 0.2889 0.1834 0.1215 0.033 Uiso 1 1 calc R . . H16 H 0.2435 0.2556 0.1651 0.033 Uiso 1 1 calc R . . C13 C 0.4834(2) 0.29782(12) 0.21254(11) 0.0310(4) Uani 1 1 d . . . H17 H 0.4403 0.2769 0.2533 0.037 Uiso 1 1 calc R . . H18 H 0.4455 0.3496 0.2045 0.037 Uiso 1 1 calc R . . C14 C 0.6371(2) 0.30336(13) 0.22392(12) 0.0351(5) Uani 1 1 d . . . H19 H 0.6782 0.3332 0.1870 0.042 Uiso 1 1 calc R . . H20 H 0.6561 0.3307 0.2666 0.042 Uiso 1 1 calc R . . C15 C 0.6780(3) 0.18861(16) 0.29149(12) 0.0432(5) Uani 1 1 d . . . H21 H 0.7088 0.2224 0.3280 0.052 Uiso 1 1 calc R . . H22 H 0.7300 0.1407 0.2933 0.052 Uiso 1 1 calc R . . H23 H 0.5803 0.1776 0.2965 0.052 Uiso 1 1 calc R . . C16 C 0.8494(2) 0.23469(16) 0.21714(13) 0.0423(5) Uani 1 1 d . . . H24 H 0.8880 0.2670 0.2529 0.051 Uiso 1 1 calc R . . H25 H 0.8663 0.2584 0.1734 0.051 Uiso 1 1 calc R . . H26 H 0.8929 0.1842 0.2188 0.051 Uiso 1 1 calc R . . C17 C 0.4454(2) 0.29281(12) 0.09030(10) 0.0284(4) Uani 1 1 d . . . H27 H 0.3797 0.3354 0.0956 0.034 Uiso 1 1 calc R . . H28 H 0.4094 0.2592 0.0541 0.034 Uiso 1 1 calc R . . C18 C 0.5797(2) 0.32548(12) 0.06825(10) 0.0273(4) Uani 1 1 d . . . C19 C 0.5976(2) 0.40448(12) 0.06305(10) 0.0309(4) Uani 1 1 d . . . H29 H 0.5263 0.4378 0.0766 0.037 Uiso 1 1 calc R . . C20 C 0.7180(2) 0.43495(12) 0.03832(10) 0.0315(4) Uani 1 1 d . . . C21 C 0.7389(3) 0.52034(13) 0.03232(13) 0.0404(5) Uani 1 1 d . . . H30 H 0.6649 0.5471 0.0554 0.048 Uiso 1 1 calc R . . H31 H 0.7381 0.5349 -0.0152 0.048 Uiso 1 1 calc R . . H32 H 0.8270 0.5344 0.0529 0.048 Uiso 1 1 calc R . . C22 C 0.8188(2) 0.38408(12) 0.01763(10) 0.0308(4) Uani 1 1 d . . . H33 H 0.9006 0.4047 -0.0002 0.037 Uiso 1 1 calc R . . C23 C 0.8068(2) 0.30444(12) 0.02145(10) 0.0278(4) Uani 1 1 d . . . C24 C 0.9187(2) 0.25192(12) -0.00697(11) 0.0319(4) Uani 1 1 d . . . C25 C 1.0428(3) 0.29792(15) -0.03155(14) 0.0435(6) Uani 1 1 d . . . H34 H 1.0777 0.3303 0.0050 0.052 Uiso 1 1 calc R . . H35 H 1.0149 0.3301 -0.0696 0.052 Uiso 1 1 calc R . . H36 H 1.1148 0.2626 -0.0457 0.052 Uiso 1 1 calc R . . C26 C 0.8595(3) 0.20839(14) -0.06759(12) 0.0404(5) Uani 1 1 d . . . H37 H 0.8270 0.2450 -0.1015 0.049 Uiso 1 1 calc R . . H38 H 0.7829 0.1764 -0.0531 0.049 Uiso 1 1 calc R . . H39 H 0.9307 0.1759 -0.0869 0.049 Uiso 1 1 calc R . . C27 C 0.9732(2) 0.19550(15) 0.04564(13) 0.0426(5) Uani 1 1 d . . . H40 H 1.0477 0.1654 0.0265 0.051 Uiso 1 1 calc R . . H41 H 0.8992 0.1612 0.0592 0.051 Uiso 1 1 calc R . . H42 H 1.0074 0.2238 0.0849 0.051 Uiso 1 1 calc R . . C28 C 0.6847(2) 0.27479(11) 0.04938(10) 0.0261(4) Uani 1 1 d . . . C29 C 0.7500(2) 0.02517(12) 0.11146(11) 0.0311(4) Uani 1 1 d . . . C30 C 0.8590(3) -0.03601(17) 0.1111(2) 0.0659(9) Uani 1 1 d . . . H43 H 0.9468 -0.0139 0.1255 0.079 Uiso 1 1 calc R . . H44 H 0.8672 -0.0568 0.0656 0.079 Uiso 1 1 calc R . . H45 H 0.8337 -0.0771 0.1420 0.079 Uiso 1 1 calc R . . C31 C 0.2265(2) 0.01065(15) 0.08016(13) 0.0397(5) Uani 1 1 d . . . H46 H 0.1826 0.0406 0.1155 0.048 Uiso 1 1 calc R . . H47 H 0.2325 -0.0430 0.0941 0.048 Uiso 1 1 calc R . . H48 H 0.1722 0.0144 0.0385 0.048 Uiso 1 1 calc R . . C32 C 0.5613(4) -0.15756(15) 0.06413(17) 0.0610(9) Uani 1 1 d . . . H49 H 0.5148 -0.1940 0.0935 0.073 Uiso 1 1 calc R . . H50 H 0.6209 -0.1243 0.0913 0.073 Uiso 1 1 calc R . . H51 H 0.6165 -0.1855 0.0315 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02241(15) 0.02513(15) 0.02604(15) -0.00062(9) 0.00180(10) -0.00153(9) Co2 0.0289(2) 0.02197(19) 0.0301(2) -0.00336(13) 0.00481(15) -0.00252(14) O1 0.0259(7) 0.0242(7) 0.0297(7) -0.0010(5) 0.0069(5) 0.0000(5) O2 0.0288(7) 0.0209(6) 0.0301(7) -0.0004(5) 0.0048(5) -0.0030(5) O3 0.0281(7) 0.0341(8) 0.0336(7) -0.0009(6) 0.0005(6) -0.0003(6) O4 0.0392(9) 0.0480(9) 0.0346(8) -0.0037(7) -0.0001(7) -0.0136(7) O5 0.0300(8) 0.0408(8) 0.0372(8) -0.0090(7) 0.0073(6) -0.0068(6) O6 0.0473(9) 0.0248(7) 0.0405(8) 0.0011(6) -0.0034(7) -0.0067(6) N1 0.0247(8) 0.0238(8) 0.0269(8) -0.0006(6) 0.0025(6) -0.0025(6) N2 0.0284(9) 0.0348(9) 0.0303(8) -0.0047(7) -0.0029(7) -0.0023(7) C1 0.0230(9) 0.0252(9) 0.0279(9) -0.0010(7) 0.0023(7) -0.0022(7) C2 0.0297(10) 0.0279(9) 0.0326(10) 0.0036(8) 0.0040(8) 0.0001(8) C3 0.0351(11) 0.0305(11) 0.0411(12) 0.0086(9) 0.0079(9) 0.0061(9) C4 0.0369(12) 0.0470(13) 0.0543(15) 0.0186(12) 0.0089(11) 0.0114(11) C5 0.0667(18) 0.0268(11) 0.0553(15) 0.0013(10) 0.0043(13) 0.0062(11) C6 0.0464(14) 0.0398(13) 0.0549(15) 0.0209(11) 0.0124(12) 0.0083(10) C7 0.0339(11) 0.0379(11) 0.0331(10) 0.0076(9) 0.0071(8) 0.0025(9) C8 0.0302(10) 0.0397(12) 0.0331(10) 0.0018(9) 0.0070(8) 0.0028(9) C9 0.0380(13) 0.0560(15) 0.0438(13) 0.0065(11) 0.0161(10) 0.0111(11) C10 0.0248(9) 0.0311(10) 0.0351(10) 0.0010(8) 0.0033(8) 0.0023(8) C11 0.0237(9) 0.0245(9) 0.0304(9) -0.0003(7) 0.0018(7) -0.0021(7) C12 0.0229(9) 0.0258(9) 0.0335(10) 0.0022(7) 0.0009(7) 0.0008(7) C13 0.0308(10) 0.0290(10) 0.0334(10) -0.0067(8) 0.0041(8) -0.0014(8) C14 0.0340(11) 0.0330(11) 0.0381(11) -0.0064(9) 0.0008(9) -0.0063(9) C15 0.0495(14) 0.0503(14) 0.0298(11) 0.0016(10) -0.0044(10) -0.0096(11) C16 0.0310(11) 0.0489(14) 0.0468(13) -0.0094(11) -0.0035(9) -0.0077(10) C17 0.0260(9) 0.0271(9) 0.0321(10) 0.0053(7) 0.0034(7) 0.0023(7) C18 0.0262(9) 0.0269(9) 0.0288(9) 0.0007(7) 0.0042(7) -0.0011(7) C19 0.0352(11) 0.0262(9) 0.0314(10) -0.0003(8) 0.0050(8) 0.0025(8) C20 0.0397(11) 0.0249(9) 0.0301(10) 0.0001(7) 0.0032(8) -0.0036(8) C21 0.0500(14) 0.0260(10) 0.0454(13) 0.0005(9) 0.0063(11) -0.0047(10) C22 0.0320(10) 0.0296(10) 0.0310(10) 0.0003(8) 0.0033(8) -0.0078(8) C23 0.0283(9) 0.0288(10) 0.0263(9) -0.0013(7) 0.0026(7) -0.0021(8) C24 0.0290(10) 0.0299(10) 0.0369(11) -0.0005(8) 0.0084(8) -0.0007(8) C25 0.0367(12) 0.0414(13) 0.0530(14) -0.0019(11) 0.0194(11) -0.0039(10) C26 0.0397(12) 0.0398(12) 0.0420(12) -0.0115(10) 0.0087(10) 0.0010(10) C27 0.0322(11) 0.0476(14) 0.0482(13) 0.0081(11) 0.0080(10) 0.0076(10) C28 0.0292(9) 0.0228(9) 0.0263(9) -0.0007(7) 0.0022(7) -0.0033(7) C29 0.0293(10) 0.0263(9) 0.0378(10) 0.0026(8) 0.0066(8) 0.0005(8) C30 0.0503(16) 0.0401(15) 0.108(3) 0.0042(16) 0.0214(17) 0.0156(13) C31 0.0323(11) 0.0437(12) 0.0433(12) -0.0068(10) 0.0058(9) -0.0052(9) C32 0.087(2) 0.0312(13) 0.0636(18) 0.0056(11) -0.0338(17) -0.0054(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 O1 1.9899(14) . ? Co1 O2 1.9982(14) . ? Co1 O3 2.0540(15) . ? Co1 N2 2.1532(17) . ? Co1 N1 2.2319(17) . ? Co2 O5 2.0647(15) 3_655 ? Co2 O5 2.0647(15) . ? Co2 O4 2.0732(16) 3_655 ? Co2 O4 2.0732(16) . ? Co2 O6 2.0938(15) . ? Co2 O6 2.0939(15) 3_655 ? O1 C1 1.348(2) . ? O2 C28 1.350(2) . ? O3 C29 1.255(3) . ? O4 C29 1.246(3) . ? O5 C31 1.429(3) . ? O6 C32 1.402(3) . ? N1 C13 1.484(2) . ? N1 C12 1.490(2) . ? N1 C17 1.495(2) . ? N2 C15 1.468(3) . ? N2 C16 1.480(3) . ? N2 C14 1.482(3) . ? C1 C11 1.406(3) . ? C1 C2 1.417(3) . ? C2 C7 1.398(3) . ? C2 C3 1.540(3) . ? C3 C6 1.531(3) . ? C3 C5 1.531(4) . ? C3 C4 1.539(3) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.396(3) . ? C7 H10 0.9500 . ? C8 C10 1.388(3) . ? C8 C9 1.514(3) . ? C9 H11 0.9800 . ? C9 H12 0.9800 . ? C9 H13 0.9800 . ? C10 C11 1.393(3) . ? C10 H14 0.9500 . ? C11 C12 1.507(3) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 C14 1.518(3) . ? C13 H17 0.9900 . ? C13 H18 0.9900 . ? C14 H19 0.9900 . ? C14 H20 0.9900 . ? C15 H21 0.9800 . ? C15 H22 0.9800 . ? C15 H23 0.9800 . ? C16 H24 0.9800 . ? C16 H25 0.9800 . ? C16 H26 0.9800 . ? C17 C18 1.502(3) . ? C17 H27 0.9900 . ? C17 H28 0.9900 . ? C18 C19 1.396(3) . ? C18 C28 1.410(3) . ? C19 C20 1.388(3) . ? C19 H29 0.9500 . ? C20 C22 1.393(3) . ? C20 C21 1.511(3) . ? C21 H30 0.9800 . ? C21 H31 0.9800 . ? C21 H32 0.9800 . ? C22 C23 1.399(3) . ? C22 H33 0.9500 . ? C23 C28 1.421(3) . ? C23 C24 1.541(3) . ? C24 C27 1.529(3) . ? C24 C26 1.533(3) . ? C24 C25 1.540(3) . ? C25 H34 0.9800 . ? C25 H35 0.9800 . ? C25 H36 0.9800 . ? C26 H37 0.9800 . ? C26 H38 0.9800 . ? C26 H39 0.9800 . ? C27 H40 0.9800 . ? C27 H41 0.9800 . ? C27 H42 0.9800 . ? C29 C30 1.509(3) . ? C30 H43 0.9800 . ? C30 H44 0.9800 . ? C30 H45 0.9800 . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 136.11(6) . . ? O1 Co1 O3 92.50(6) . . ? O2 Co1 O3 95.00(6) . . ? O1 Co1 N2 113.12(6) . . ? O2 Co1 N2 109.65(6) . . ? O3 Co1 N2 92.63(7) . . ? O1 Co1 N1 88.01(6) . . ? O2 Co1 N1 89.31(6) . . ? O3 Co1 N1 173.19(6) . . ? N2 Co1 N1 80.93(6) . . ? O5 Co2 O5 180.00(6) 3_655 . ? O5 Co2 O4 86.86(7) 3_655 3_655 ? O5 Co2 O4 93.14(7) . 3_655 ? O5 Co2 O4 93.14(7) 3_655 . ? O5 Co2 O4 86.86(7) . . ? O4 Co2 O4 180.0 3_655 . ? O5 Co2 O6 89.30(7) 3_655 . ? O5 Co2 O6 90.70(7) . . ? O4 Co2 O6 83.88(7) 3_655 . ? O4 Co2 O6 96.12(7) . . ? O5 Co2 O6 90.71(7) 3_655 3_655 ? O5 Co2 O6 89.29(7) . 3_655 ? O4 Co2 O6 96.12(7) 3_655 3_655 ? O4 Co2 O6 83.88(7) . 3_655 ? O6 Co2 O6 180.0 . 3_655 ? C1 O1 Co1 125.81(12) . . ? C28 O2 Co1 121.08(12) . . ? C29 O3 Co1 112.45(14) . . ? C29 O4 Co2 169.74(17) . . ? C31 O5 Co2 126.69(14) . . ? C32 O6 Co2 123.08(16) . . ? C13 N1 C12 110.14(15) . . ? C13 N1 C17 111.19(16) . . ? C12 N1 C17 106.52(15) . . ? C13 N1 Co1 108.23(12) . . ? C12 N1 Co1 111.21(12) . . ? C17 N1 Co1 109.57(12) . . ? C15 N2 C16 108.32(19) . . ? C15 N2 C14 111.98(19) . . ? C16 N2 C14 108.40(18) . . ? C15 N2 Co1 109.05(14) . . ? C16 N2 Co1 110.70(14) . . ? C14 N2 Co1 108.39(13) . . ? O1 C1 C11 118.92(17) . . ? O1 C1 C2 121.33(18) . . ? C11 C1 C2 119.72(18) . . ? C7 C2 C1 117.46(19) . . ? C7 C2 C3 120.71(19) . . ? C1 C2 C3 121.76(18) . . ? C6 C3 C5 107.7(2) . . ? C6 C3 C4 106.9(2) . . ? C5 C3 C4 109.5(2) . . ? C6 C3 C2 112.42(19) . . ? C5 C3 C2 108.91(19) . . ? C4 C3 C2 111.28(19) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C8 C7 C2 123.4(2) . . ? C8 C7 H10 118.3 . . ? C2 C7 H10 118.3 . . ? C10 C8 C7 117.9(2) . . ? C10 C8 C9 121.8(2) . . ? C7 C8 C9 120.3(2) . . ? C8 C9 H11 109.5 . . ? C8 C9 H12 109.5 . . ? H11 C9 H12 109.5 . . ? C8 C9 H13 109.5 . . ? H11 C9 H13 109.5 . . ? H12 C9 H13 109.5 . . ? C8 C10 C11 121.0(2) . . ? C8 C10 H14 119.5 . . ? C11 C10 H14 119.5 . . ? C10 C11 C1 120.49(19) . . ? C10 C11 C12 120.15(18) . . ? C1 C11 C12 119.23(18) . . ? N1 C12 C11 114.55(16) . . ? N1 C12 H15 108.6 . . ? C11 C12 H15 108.6 . . ? N1 C12 H16 108.6 . . ? C11 C12 H16 108.6 . . ? H15 C12 H16 107.6 . . ? N1 C13 C14 111.18(17) . . ? N1 C13 H17 109.4 . . ? C14 C13 H17 109.4 . . ? N1 C13 H18 109.4 . . ? C14 C13 H18 109.4 . . ? H17 C13 H18 108.0 . . ? N2 C14 C13 110.95(17) . . ? N2 C14 H19 109.4 . . ? C13 C14 H19 109.4 . . ? N2 C14 H20 109.4 . . ? C13 C14 H20 109.4 . . ? H19 C14 H20 108.0 . . ? N2 C15 H21 109.5 . . ? N2 C15 H22 109.5 . . ? H21 C15 H22 109.5 . . ? N2 C15 H23 109.5 . . ? H21 C15 H23 109.5 . . ? H22 C15 H23 109.5 . . ? N2 C16 H24 109.5 . . ? N2 C16 H25 109.5 . . ? H24 C16 H25 109.5 . . ? N2 C16 H26 109.5 . . ? H24 C16 H26 109.5 . . ? H25 C16 H26 109.5 . . ? N1 C17 C18 115.61(16) . . ? N1 C17 H27 108.4 . . ? C18 C17 H27 108.4 . . ? N1 C17 H28 108.4 . . ? C18 C17 H28 108.4 . . ? H27 C17 H28 107.4 . . ? C19 C18 C28 120.65(18) . . ? C19 C18 C17 120.55(18) . . ? C28 C18 C17 118.71(18) . . ? C20 C19 C18 120.88(19) . . ? C20 C19 H29 119.6 . . ? C18 C19 H29 119.6 . . ? C19 C20 C22 117.77(19) . . ? C19 C20 C21 121.5(2) . . ? C22 C20 C21 120.7(2) . . ? C20 C21 H30 109.5 . . ? C20 C21 H31 109.5 . . ? H30 C21 H31 109.5 . . ? C20 C21 H32 109.5 . . ? H30 C21 H32 109.5 . . ? H31 C21 H32 109.5 . . ? C20 C22 C23 123.99(19) . . ? C20 C22 H33 118.0 . . ? C23 C22 H33 118.0 . . ? C22 C23 C28 117.10(18) . . ? C22 C23 C24 120.83(18) . . ? C28 C23 C24 121.99(18) . . ? C27 C24 C26 110.1(2) . . ? C27 C24 C25 106.65(19) . . ? C26 C24 C25 107.43(19) . . ? C27 C24 C23 112.01(18) . . ? C26 C24 C23 108.81(18) . . ? C25 C24 C23 111.77(18) . . ? C24 C25 H34 109.5 . . ? C24 C25 H35 109.5 . . ? H34 C25 H35 109.5 . . ? C24 C25 H36 109.5 . . ? H34 C25 H36 109.5 . . ? H35 C25 H36 109.5 . . ? C24 C26 H37 109.5 . . ? C24 C26 H38 109.5 . . ? H37 C26 H38 109.5 . . ? C24 C26 H39 109.5 . . ? H37 C26 H39 109.5 . . ? H38 C26 H39 109.5 . . ? C24 C27 H40 109.5 . . ? C24 C27 H41 109.5 . . ? H40 C27 H41 109.5 . . ? C24 C27 H42 109.5 . . ? H40 C27 H42 109.5 . . ? H41 C27 H42 109.5 . . ? O2 C28 C18 118.13(17) . . ? O2 C28 C23 122.36(18) . . ? C18 C28 C23 119.51(18) . . ? O4 C29 O3 122.3(2) . . ? O4 C29 C30 121.1(2) . . ? O3 C29 C30 116.6(2) . . ? C29 C30 H43 109.5 . . ? C29 C30 H44 109.5 . . ? H43 C30 H44 109.5 . . ? C29 C30 H45 109.5 . . ? H43 C30 H45 109.5 . . ? H44 C30 H45 109.5 . . ? O5 C31 H46 109.5 . . ? O5 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? O5 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? O6 C32 H49 109.5 . . ? O6 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? O6 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.865 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.072 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 766026' #TrackingRef 'Kozak_Compiled_CIF.cif' # start Validation Reply Form _vrf_PLAT770_5 ; PROBLEM: Suspect C-H Bond in CIF: C38 -- H65 .. 1.44 Ang. RESPONSE: C38 is the methy carbon in a methanol molecule while H65 is the alcoholic proton that was introduced in its difference map position and was allowed to refine positionally. There is no direct bond between C38 and H65. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C34 H54 O2 N2) Co]2 [Co (C H2 C O2)2 (C H3 O H)4] (C7 H8)2' _chemical_formula_sum 'C90 H146 Co3 N4 O12' _chemical_formula_weight 1652.96 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 11.027(3) _cell_length_b 22.278(5) _cell_length_c 20.267(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.692(5) _cell_angle_gamma 90.00 _cell_volume 4559(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20060 _cell_measurement_theta_min 2.6556 _cell_measurement_theta_max 30.8607 _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1782 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.9298 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 42832 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10466 _reflns_number_gt 9767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0995P)^2^+8.9219P] 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 10466 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1996 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.10209(4) 0.610545(18) 0.36456(2) 0.02062(13) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.5000 0.02096(15) Uani 1 2 d S . . O1 O 0.0772(2) 0.52530(10) 0.33012(11) 0.0237(4) Uani 1 1 d . . . O2 O 0.1530(2) 0.64904(9) 0.46088(11) 0.0234(4) Uani 1 1 d . . . O3 O -0.0963(2) 0.62681(10) 0.33279(12) 0.0253(4) Uani 1 1 d . . . O4 O -0.0822(2) 0.55993(10) 0.41557(12) 0.0313(5) Uani 1 1 d . . . O5 O 0.1140(4) 0.46852(16) 0.44699(19) 0.0611(10) Uani 1 1 d . . . O6 O -0.1376(3) 0.43326(15) 0.45387(16) 0.0595(10) Uani 1 1 d . . . N1 N 0.3182(2) 0.60135(11) 0.38871(13) 0.0219(5) Uani 1 1 d . . . N2 N 0.1132(2) 0.66928(12) 0.28312(14) 0.0253(5) Uani 1 1 d . . . C1 C 0.1305(3) 0.50514(13) 0.28499(16) 0.0221(6) Uani 1 1 d . . . C2 C 0.0538(3) 0.47645(14) 0.21898(17) 0.0243(6) Uani 1 1 d . . . C3 C -0.0908(3) 0.45831(16) 0.19929(18) 0.0309(7) Uani 1 1 d . . . C4 C -0.1786(3) 0.51419(19) 0.1874(2) 0.0417(9) Uani 1 1 d . . . H1 H -0.1822 0.5261 0.2331 0.050 Uiso 1 1 calc R . . H2 H -0.2682 0.5050 0.1521 0.050 Uiso 1 1 calc R . . H3 H -0.1415 0.5471 0.1693 0.050 Uiso 1 1 calc R . . C5 C -0.1021(4) 0.4198(2) 0.2594(2) 0.0463(10) Uani 1 1 d . . . H4 H -0.0323 0.4312 0.3058 0.056 Uiso 1 1 calc R . . H5 H -0.0923 0.3773 0.2499 0.056 Uiso 1 1 calc R . . H6 H -0.1889 0.4263 0.2608 0.056 Uiso 1 1 calc R . . C6 C -0.1460(4) 0.4201(2) 0.1306(2) 0.0465(10) Uani 1 1 d . . . H7 H -0.0742 0.3966 0.1265 0.056 Uiso 1 1 calc R . . H8 H -0.1853 0.4463 0.0885 0.056 Uiso 1 1 calc R . . H9 H -0.2139 0.3928 0.1330 0.056 Uiso 1 1 calc R . . C7 C 0.1155(3) 0.46530(14) 0.17195(17) 0.0270(6) Uani 1 1 d . . . H10 H 0.0635 0.4481 0.1264 0.032 Uiso 1 1 calc R . . C8 C 0.2487(3) 0.47776(14) 0.18727(17) 0.0257(6) Uani 1 1 d . . . C9 C 0.3029(3) 0.46945(15) 0.12916(18) 0.0302(7) Uani 1 1 d . . . C10 C 0.2587(5) 0.4097(2) 0.0908(3) 0.0649(15) Uani 1 1 d . . . H11 H 0.1731 0.3984 0.0912 0.078 Uiso 1 1 calc R . . H12 H 0.3246 0.3788 0.1157 0.078 Uiso 1 1 calc R . . H13 H 0.2499 0.4133 0.0409 0.078 Uiso 1 1 calc R . . C11 C 0.2443(7) 0.5188(3) 0.0726(3) 0.0768(18) Uani 1 1 d . . . H14 H 0.3072 0.5287 0.0512 0.092 Uiso 1 1 calc R . . H15 H 0.2270 0.5546 0.0956 0.092 Uiso 1 1 calc R . . H16 H 0.1613 0.5046 0.0349 0.092 Uiso 1 1 calc R . . C12 C 0.4503(5) 0.4735(3) 0.1583(3) 0.0706(17) Uani 1 1 d . . . H17 H 0.4765 0.5151 0.1556 0.085 Uiso 1 1 calc R . . H18 H 0.4831 0.4478 0.1297 0.085 Uiso 1 1 calc R . . H19 H 0.4881 0.4601 0.2086 0.085 Uiso 1 1 calc R . . C13 C 0.3237(3) 0.49999(13) 0.25526(18) 0.0257(6) Uani 1 1 d . . . H20 H 0.4160 0.5061 0.2693 0.031 Uiso 1 1 calc R . . C14 C 0.2668(3) 0.51361(13) 0.30361(17) 0.0235(6) Uani 1 1 d . . . C15 C 0.3489(3) 0.53801(14) 0.37706(16) 0.0237(6) Uani 1 1 d . . . H21 H 0.3358 0.5123 0.4135 0.028 Uiso 1 1 calc R . . H22 H 0.4435 0.5354 0.3852 0.028 Uiso 1 1 calc R . . C16 C 0.3504(3) 0.64315(14) 0.34094(16) 0.0252(6) Uani 1 1 d . . . H23 H 0.4247 0.6265 0.3311 0.030 Uiso 1 1 calc R . . H24 H 0.3793 0.6821 0.3658 0.030 Uiso 1 1 calc R . . C17 C 0.2327(3) 0.65321(15) 0.27038(16) 0.0255(6) Uani 1 1 d . . . H25 H 0.2530 0.6859 0.2433 0.031 Uiso 1 1 calc R . . H26 H 0.2151 0.6163 0.2409 0.031 Uiso 1 1 calc R . . C18 C -0.0054(3) 0.66304(18) 0.21488(18) 0.0341(7) Uani 1 1 d . . . H27 H -0.0817 0.6518 0.2255 0.041 Uiso 1 1 calc R . . H28 H 0.0103 0.6319 0.1851 0.041 Uiso 1 1 calc R . . H29 H -0.0235 0.7013 0.1889 0.041 Uiso 1 1 calc R . . C19 C 0.1211(4) 0.73244(15) 0.30741(19) 0.0332(7) Uani 1 1 d . . . H30 H 0.0316 0.7490 0.2919 0.040 Uiso 1 1 calc R . . H31 H 0.1716 0.7561 0.2863 0.040 Uiso 1 1 calc R . . H32 H 0.1655 0.7340 0.3601 0.040 Uiso 1 1 calc R . . C20 C 0.3999(3) 0.61610(14) 0.46538(16) 0.0243(6) Uani 1 1 d . . . H33 H 0.4946 0.6128 0.4740 0.029 Uiso 1 1 calc R . . H34 H 0.3820 0.5860 0.4963 0.029 Uiso 1 1 calc R . . C21 C 0.3752(3) 0.67788(14) 0.48782(16) 0.0236(6) Uani 1 1 d . . . C22 C 0.4761(3) 0.72113(15) 0.51037(16) 0.0264(6) Uani 1 1 d . . . H35 H 0.5593 0.7120 0.5092 0.032 Uiso 1 1 calc R . . C23 C 0.4563(3) 0.77690(15) 0.53432(16) 0.0270(6) Uani 1 1 d . . . C24 C 0.5621(3) 0.82651(15) 0.55913(17) 0.0291(7) Uani 1 1 d . . . C25 C 0.6908(3) 0.80736(17) 0.5532(2) 0.0354(7) Uani 1 1 d . . . H36 H 0.6705 0.7789 0.5132 0.042 Uiso 1 1 calc R . . H37 H 0.7494 0.7881 0.5982 0.042 Uiso 1 1 calc R . . H38 H 0.7348 0.8428 0.5442 0.042 Uiso 1 1 calc R . . C26 C 0.5095(4) 0.88249(16) 0.5124(2) 0.0355(8) Uani 1 1 d . . . H39 H 0.5327 0.8806 0.4706 0.043 Uiso 1 1 calc R . . H40 H 0.5492 0.9184 0.5408 0.043 Uiso 1 1 calc R . . H41 H 0.4130 0.8843 0.4960 0.043 Uiso 1 1 calc R . . C27 C 0.5936(4) 0.84257(17) 0.63795(19) 0.0363(8) Uani 1 1 d . . . H42 H 0.6859 0.8558 0.6615 0.044 Uiso 1 1 calc R . . H43 H 0.5802 0.8072 0.6630 0.044 Uiso 1 1 calc R . . H44 H 0.5348 0.8749 0.6397 0.044 Uiso 1 1 calc R . . C28 C 0.3326(3) 0.78769(14) 0.53611(16) 0.0262(6) Uani 1 1 d . . . H45 H 0.3188 0.8255 0.5536 0.031 Uiso 1 1 calc R . . C29 C 0.2282(3) 0.74675(14) 0.51405(16) 0.0247(6) Uani 1 1 d . . . C30 C 0.0971(3) 0.76187(15) 0.52032(18) 0.0277(6) Uani 1 1 d . . . C31 C 0.0967(4) 0.82602(16) 0.5482(2) 0.0344(7) Uani 1 1 d . . . H46 H 0.1527 0.8518 0.5329 0.041 Uiso 1 1 calc R . . H47 H 0.1312 0.8255 0.6009 0.041 Uiso 1 1 calc R . . H48 H 0.0060 0.8416 0.5285 0.041 Uiso 1 1 calc R . . C32 C -0.0198(3) 0.75798(17) 0.4471(2) 0.0364(8) Uani 1 1 d . . . H49 H -0.0342 0.7973 0.4234 0.044 Uiso 1 1 calc R . . H50 H -0.0995 0.7460 0.4539 0.044 Uiso 1 1 calc R . . H51 H -0.0006 0.7282 0.4170 0.044 Uiso 1 1 calc R . . C33 C 0.0750(4) 0.71847(17) 0.5730(2) 0.0418(9) Uani 1 1 d . . . H52 H 0.0257 0.6833 0.5466 0.050 Uiso 1 1 calc R . . H53 H 0.0242 0.7387 0.5966 0.050 Uiso 1 1 calc R . . H54 H 0.1607 0.7056 0.6094 0.050 Uiso 1 1 calc R . . C34 C 0.2495(3) 0.69045(14) 0.48739(16) 0.0232(6) Uani 1 1 d . . . C35 C -0.1477(3) 0.59395(14) 0.36498(17) 0.0242(6) Uani 1 1 d . . . C36 C -0.2963(4) 0.5964(2) 0.3392(3) 0.0465(10) Uani 1 1 d . . . H55 H -0.3277 0.6366 0.3204 0.056 Uiso 1 1 calc R . . H56 H -0.3213 0.5876 0.3794 0.056 Uiso 1 1 calc R . . H57 H -0.3366 0.5667 0.3009 0.056 Uiso 1 1 calc R . . C37 C 0.1688(4) 0.41217(17) 0.4500(2) 0.0404(8) Uani 1 1 d . . . H58 H 0.2556 0.4105 0.4905 0.049 Uiso 1 1 calc R . . H59 H 0.1791 0.4043 0.4049 0.049 Uiso 1 1 calc R . . H60 H 0.1105 0.3818 0.4566 0.049 Uiso 1 1 calc R . . C38 C -0.2590(4) 0.43946(19) 0.3972(2) 0.0420(9) Uani 1 1 d . . . H62 H -0.2555 0.4728 0.3664 0.050 Uiso 1 1 calc R . . H63 H -0.3268 0.4477 0.4158 0.050 Uiso 1 1 calc R . . H64 H -0.2811 0.4023 0.3689 0.050 Uiso 1 1 calc R . . C39 C 0.2569(6) 0.3241(3) 0.2961(3) 0.0687(15) Uani 1 1 d . . . H66 H 0.2066 0.3598 0.2721 0.082 Uiso 1 1 calc R . . H67 H 0.3056 0.3325 0.3476 0.082 Uiso 1 1 calc R . . H68 H 0.1958 0.2906 0.2901 0.082 Uiso 1 1 calc R . . C40 C 0.3526(4) 0.30802(18) 0.2635(2) 0.0441(9) Uani 1 1 d . . . C41 C 0.4778(5) 0.3306(3) 0.2911(3) 0.0746(17) Uani 1 1 d . . . H69 H 0.5063 0.3542 0.3337 0.090 Uiso 1 1 calc R . . C42 C 0.5652(5) 0.3201(3) 0.2581(4) 0.0845(19) Uani 1 1 d . . . H70 H 0.6510 0.3376 0.2774 0.101 Uiso 1 1 calc R . . C43 C 0.5275(5) 0.2844(2) 0.1978(3) 0.0633(13) Uani 1 1 d . . . H71 H 0.5862 0.2771 0.1749 0.076 Uiso 1 1 calc R . . C44 C 0.4054(6) 0.2599(2) 0.1719(3) 0.0643(13) Uani 1 1 d . . . H72 H 0.3786 0.2349 0.1305 0.077 Uiso 1 1 calc R . . C45 C 0.3190(5) 0.2703(2) 0.2040(3) 0.0601(13) Uani 1 1 d . . . H73 H 0.2346 0.2515 0.1852 0.072 Uiso 1 1 calc R . . H61 H 0.038(6) 0.452(3) 0.423(3) 0.073 Uiso 1 1 d . . . H65 H -0.186(6) 0.456(3) 0.471(3) 0.071 Uiso 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 0.0190(2) 0.0232(2) 0.0201(2) 0.00048(14) 0.00825(16) -0.00076(14) Co2 0.0202(3) 0.0225(3) 0.0209(3) 0.0009(2) 0.0090(2) -0.0013(2) O1 0.0235(10) 0.0262(11) 0.0252(10) -0.0028(8) 0.0136(9) -0.0017(8) O2 0.0220(10) 0.0253(10) 0.0242(10) -0.0026(8) 0.0105(8) -0.0052(8) O3 0.0219(10) 0.0283(11) 0.0265(11) 0.0039(9) 0.0106(9) 0.0017(8) O4 0.0367(12) 0.0293(12) 0.0263(11) 0.0055(9) 0.0110(10) 0.0030(10) O5 0.096(3) 0.055(2) 0.060(2) 0.0285(16) 0.060(2) 0.0424(19) O6 0.0563(19) 0.058(2) 0.0364(15) 0.0168(14) -0.0100(13) -0.0330(15) N1 0.0182(11) 0.0257(12) 0.0218(12) -0.0004(10) 0.0081(9) -0.0008(9) N2 0.0199(12) 0.0313(14) 0.0248(12) 0.0035(10) 0.0091(10) -0.0002(10) C1 0.0249(14) 0.0221(14) 0.0225(14) -0.0017(11) 0.0129(12) -0.0006(11) C2 0.0241(14) 0.0229(14) 0.0267(14) -0.0014(11) 0.0110(12) -0.0013(11) C3 0.0243(15) 0.0373(18) 0.0315(16) -0.0102(14) 0.0116(13) -0.0061(13) C4 0.0202(15) 0.048(2) 0.052(2) -0.0103(18) 0.0092(15) -0.0011(14) C5 0.0355(19) 0.053(2) 0.051(2) -0.0004(19) 0.0186(18) -0.0192(17) C6 0.0327(19) 0.059(3) 0.045(2) -0.0243(19) 0.0135(17) -0.0143(18) C7 0.0296(15) 0.0272(15) 0.0250(14) -0.0044(12) 0.0118(12) -0.0020(12) C8 0.0286(15) 0.0238(14) 0.0276(15) -0.0029(12) 0.0145(13) 0.0004(11) C9 0.0365(17) 0.0290(16) 0.0336(17) -0.0044(13) 0.0230(14) -0.0008(13) C10 0.072(3) 0.071(3) 0.078(3) -0.045(3) 0.058(3) -0.030(3) C11 0.112(5) 0.070(3) 0.081(4) 0.033(3) 0.073(4) 0.033(3) C12 0.043(2) 0.126(5) 0.055(3) -0.034(3) 0.032(2) -0.005(3) C13 0.0211(14) 0.0254(15) 0.0319(16) -0.0032(12) 0.0119(12) 0.0005(11) C14 0.0220(14) 0.0220(14) 0.0264(14) -0.0007(11) 0.0099(12) 0.0009(11) C15 0.0197(13) 0.0269(15) 0.0249(14) -0.0014(12) 0.0093(11) 0.0025(11) C16 0.0209(13) 0.0311(16) 0.0255(14) 0.0003(12) 0.0112(12) -0.0028(11) C17 0.0238(14) 0.0310(16) 0.0233(14) 0.0009(12) 0.0111(12) -0.0031(12) C18 0.0246(15) 0.049(2) 0.0254(15) 0.0116(14) 0.0064(13) 0.0000(14) C19 0.0400(18) 0.0308(17) 0.0354(17) 0.0073(14) 0.0219(15) 0.0056(14) C20 0.0186(13) 0.0303(15) 0.0213(14) -0.0010(11) 0.0052(11) 0.0001(11) C21 0.0228(14) 0.0274(15) 0.0205(13) -0.0008(11) 0.0086(11) -0.0029(11) C22 0.0233(14) 0.0316(16) 0.0230(14) -0.0010(12) 0.0078(11) -0.0032(12) C23 0.0271(15) 0.0301(16) 0.0225(14) 0.0002(12) 0.0089(12) -0.0070(12) C24 0.0269(15) 0.0308(16) 0.0260(15) 0.0006(12) 0.0068(12) -0.0067(12) C25 0.0272(16) 0.0366(18) 0.0371(18) 0.0009(15) 0.0074(14) -0.0076(14) C26 0.0317(17) 0.0340(18) 0.0385(18) 0.0077(14) 0.0117(15) -0.0064(13) C27 0.0374(18) 0.0373(18) 0.0300(17) -0.0037(14) 0.0093(14) -0.0122(15) C28 0.0290(15) 0.0259(15) 0.0239(14) -0.0031(11) 0.0109(12) -0.0051(12) C29 0.0250(14) 0.0275(15) 0.0225(13) -0.0016(11) 0.0105(12) -0.0034(11) C30 0.0275(15) 0.0286(15) 0.0305(15) -0.0051(12) 0.0154(13) -0.0023(12) C31 0.0358(18) 0.0329(17) 0.0383(18) -0.0077(14) 0.0189(15) -0.0007(14) C32 0.0254(16) 0.0403(19) 0.0419(19) -0.0105(15) 0.0120(15) 0.0029(14) C33 0.051(2) 0.0358(19) 0.056(2) 0.0025(17) 0.040(2) 0.0026(16) C34 0.0232(14) 0.0261(14) 0.0202(13) -0.0006(11) 0.0087(11) -0.0047(11) C35 0.0211(13) 0.0256(14) 0.0265(14) -0.0003(12) 0.0101(12) 0.0011(11) C36 0.0243(17) 0.054(2) 0.062(3) 0.019(2) 0.0188(17) 0.0030(16) C37 0.046(2) 0.038(2) 0.045(2) 0.0068(16) 0.0261(18) 0.0134(16) C38 0.0324(18) 0.047(2) 0.0342(18) 0.0054(16) 0.0007(15) -0.0106(16) C39 0.070(3) 0.070(3) 0.078(4) 0.025(3) 0.041(3) 0.013(3) C40 0.043(2) 0.0363(19) 0.049(2) 0.0107(17) 0.0142(18) 0.0044(16) C41 0.056(3) 0.086(4) 0.082(4) -0.045(3) 0.028(3) -0.031(3) C42 0.041(3) 0.111(5) 0.096(5) -0.027(4) 0.022(3) -0.020(3) C43 0.058(3) 0.055(3) 0.076(3) 0.001(3) 0.027(3) 0.021(2) C44 0.078(4) 0.057(3) 0.055(3) -0.009(2) 0.023(3) -0.007(3) C45 0.046(2) 0.073(3) 0.046(2) 0.003(2) 0.002(2) -0.014(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 Co1 O2 1.995(2) . ? Co1 O1 2.004(2) . ? Co1 O3 2.049(2) . ? Co1 N2 2.148(3) . ? Co1 N1 2.241(3) . ? Co2 O6 2.061(3) 3_566 ? Co2 O6 2.061(3) . ? Co2 O4 2.070(2) 3_566 ? Co2 O4 2.070(2) . ? Co2 O5 2.076(3) 3_566 ? Co2 O5 2.076(3) . ? O1 C1 1.347(3) . ? O2 C34 1.346(3) . ? O3 C35 1.257(4) . ? O4 C35 1.246(4) . ? O5 C37 1.384(5) . ? O5 H61 0.87(6) . ? O6 C38 1.377(4) . ? O6 H65 0.89(6) . ? N1 C16 1.486(4) . ? N1 C20 1.486(4) . ? N1 C15 1.492(4) . ? N2 C18 1.480(4) . ? N2 C19 1.482(4) . ? N2 C17 1.485(4) . ? C1 C14 1.408(4) . ? C1 C2 1.416(4) . ? C2 C7 1.398(4) . ? C2 C3 1.534(4) . ? C3 C6 1.534(5) . ? C3 C5 1.535(5) . ? C3 C4 1.536(5) . ? C4 H1 0.9800 . ? C4 H2 0.9800 . ? C4 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C5 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C6 H9 0.9800 . ? C7 C8 1.402(4) . ? C7 H10 0.9500 . ? C8 C13 1.383(4) . ? C8 C9 1.531(4) . ? C9 C12 1.493(6) . ? C9 C10 1.520(5) . ? C9 C11 1.531(6) . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 H17 0.9800 . ? C12 H18 0.9800 . ? C12 H19 0.9800 . ? C13 C14 1.393(4) . ? C13 H20 0.9500 . ? C14 C15 1.499(4) . ? C15 H21 0.9900 . ? C15 H22 0.9900 . ? C16 C17 1.512(4) . ? C16 H23 0.9900 . ? C16 H24 0.9900 . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 H27 0.9800 . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C19 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C20 C21 1.508(4) . ? C20 H33 0.9900 . ? C20 H34 0.9900 . ? C21 C22 1.402(4) . ? C21 C34 1.411(4) . ? C22 C23 1.383(5) . ? C22 H35 0.9500 . ? C23 C28 1.400(5) . ? C23 C24 1.538(4) . ? C24 C26 1.532(5) . ? C24 C25 1.533(5) . ? C24 C27 1.535(5) . ? C25 H36 0.9800 . ? C25 H37 0.9800 . ? C25 H38 0.9800 . ? C26 H39 0.9800 . ? C26 H40 0.9800 . ? C26 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C27 H44 0.9800 . ? C28 C29 1.394(4) . ? C28 H45 0.9500 . ? C29 C34 1.422(4) . ? C29 C30 1.538(4) . ? C30 C32 1.528(5) . ? C30 C33 1.531(5) . ? C30 C31 1.537(5) . ? C31 H46 0.9800 . ? C31 H47 0.9800 . ? C31 H48 0.9800 . ? C32 H49 0.9800 . ? C32 H50 0.9800 . ? C32 H51 0.9800 . ? C33 H52 0.9800 . ? C33 H53 0.9800 . ? C33 H54 0.9800 . ? C35 C36 1.508(4) . ? C36 H55 0.9800 . ? C36 H56 0.9800 . ? C36 H57 0.9800 . ? C37 H58 0.9800 . ? C37 H59 0.9800 . ? C37 H60 0.9800 . ? C38 H62 0.9800 . ? C38 H63 0.9800 . ? C38 H64 0.9800 . ? C38 H65 1.44(6) . ? C39 C40 1.497(7) . ? C39 H66 0.9800 . ? C39 H67 0.9800 . ? C39 H68 0.9800 . ? C40 C41 1.361(6) . ? C40 C45 1.393(7) . ? C41 C42 1.396(8) . ? C41 H69 0.9500 . ? C42 C43 1.375(8) . ? C42 H70 0.9500 . ? C43 C44 1.348(8) . ? C43 H71 0.9500 . ? C44 C45 1.372(8) . ? C44 H72 0.9500 . ? C45 H73 0.9500 . ? 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 133.91(9) . . ? O2 Co1 O3 94.39(9) . . ? O1 Co1 O3 94.51(9) . . ? O2 Co1 N2 114.17(10) . . ? O1 Co1 N2 110.60(10) . . ? O3 Co1 N2 91.96(9) . . ? O2 Co1 N1 88.23(9) . . ? O1 Co1 N1 88.53(9) . . ? O3 Co1 N1 172.71(9) . . ? N2 Co1 N1 80.77(9) . . ? O6 Co2 O6 180.0 3_566 . ? O6 Co2 O4 95.30(11) 3_566 3_566 ? O6 Co2 O4 84.70(11) . 3_566 ? O6 Co2 O4 84.70(11) 3_566 . ? O6 Co2 O4 95.30(11) . . ? O4 Co2 O4 179.996(1) 3_566 . ? O6 Co2 O5 90.59(18) 3_566 3_566 ? O6 Co2 O5 89.41(18) . 3_566 ? O4 Co2 O5 86.85(11) 3_566 3_566 ? O4 Co2 O5 93.15(11) . 3_566 ? O6 Co2 O5 89.41(18) 3_566 . ? O6 Co2 O5 90.58(18) . . ? O4 Co2 O5 93.15(11) 3_566 . ? O4 Co2 O5 86.85(11) . . ? O5 Co2 O5 180.00(14) 3_566 . ? C1 O1 Co1 121.08(18) . . ? C34 O2 Co1 123.48(18) . . ? C35 O3 Co1 112.42(19) . . ? C35 O4 Co2 171.5(2) . . ? C37 O5 Co2 128.9(3) . . ? C37 O5 H61 87(4) . . ? Co2 O5 H61 78(4) . . ? C38 O6 Co2 126.7(3) . . ? C38 O6 H65 75(4) . . ? Co2 O6 H65 82(4) . . ? C16 N1 C20 109.8(2) . . ? C16 N1 C15 111.1(2) . . ? C20 N1 C15 107.1(2) . . ? C16 N1 Co1 108.18(18) . . ? C20 N1 Co1 110.67(18) . . ? C15 N1 Co1 109.94(17) . . ? C18 N2 C19 108.2(3) . . ? C18 N2 C17 109.1(2) . . ? C19 N2 C17 110.4(2) . . ? C18 N2 Co1 111.0(2) . . ? C19 N2 Co1 109.70(19) . . ? C17 N2 Co1 108.39(18) . . ? O1 C1 C14 118.9(3) . . ? O1 C1 C2 122.3(3) . . ? C14 C1 C2 118.8(3) . . ? C7 C2 C1 117.0(3) . . ? C7 C2 C3 121.0(3) . . ? C1 C2 C3 121.9(3) . . ? C2 C3 C6 112.0(3) . . ? C2 C3 C5 110.4(3) . . ? C6 C3 C5 106.3(3) . . ? C2 C3 C4 110.6(3) . . ? C6 C3 C4 108.2(3) . . ? C5 C3 C4 109.3(3) . . ? C3 C4 H1 109.5 . . ? C3 C4 H2 109.5 . . ? H1 C4 H2 109.5 . . ? C3 C4 H3 109.5 . . ? H1 C4 H3 109.5 . . ? H2 C4 H3 109.5 . . ? C3 C5 H4 109.5 . . ? C3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C5 H6 109.5 . . ? H4 C5 H6 109.5 . . ? H5 C5 H6 109.5 . . ? C3 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C6 H9 109.5 . . ? H7 C6 H9 109.5 . . ? H8 C6 H9 109.5 . . ? C2 C7 C8 124.6(3) . . ? C2 C7 H10 117.7 . . ? C8 C7 H10 117.7 . . ? C13 C8 C7 116.4(3) . . ? C13 C8 C9 123.3(3) . . ? C7 C8 C9 120.2(3) . . ? C12 C9 C10 109.2(4) . . ? C12 C9 C8 112.8(3) . . ? C10 C9 C8 110.8(3) . . ? C12 C9 C11 108.5(4) . . ? C10 C9 C11 107.1(4) . . ? C8 C9 C11 108.2(3) . . ? C9 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C9 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C9 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C9 C12 H17 109.5 . . ? C9 C12 H18 109.5 . . ? H17 C12 H18 109.5 . . ? C9 C12 H19 109.5 . . ? H17 C12 H19 109.5 . . ? H18 C12 H19 109.5 . . ? C8 C13 C14 121.4(3) . . ? C8 C13 H20 119.3 . . ? C14 C13 H20 119.3 . . ? C13 C14 C1 121.1(3) . . ? C13 C14 C15 121.0(3) . . ? C1 C14 C15 117.9(3) . . ? N1 C15 C14 114.5(2) . . ? N1 C15 H21 108.6 . . ? C14 C15 H21 108.6 . . ? N1 C15 H22 108.6 . . ? C14 C15 H22 108.6 . . ? H21 C15 H22 107.6 . . ? N1 C16 C17 111.7(2) . . ? N1 C16 H23 109.3 . . ? C17 C16 H23 109.3 . . ? N1 C16 H24 109.3 . . ? C17 C16 H24 109.3 . . ? H23 C16 H24 107.9 . . ? N2 C17 C16 110.8(2) . . ? N2 C17 H25 109.5 . . ? C16 C17 H25 109.5 . . ? N2 C17 H26 109.5 . . ? C16 C17 H26 109.5 . . ? H25 C17 H26 108.1 . . ? N2 C18 H27 109.5 . . ? N2 C18 H28 109.5 . . ? H27 C18 H28 109.5 . . ? N2 C18 H29 109.5 . . ? H27 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? N2 C19 H30 109.5 . . ? N2 C19 H31 109.5 . . ? H30 C19 H31 109.5 . . ? N2 C19 H32 109.5 . . ? H30 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? N1 C20 C21 114.2(2) . . ? N1 C20 H33 108.7 . . ? C21 C20 H33 108.7 . . ? N1 C20 H34 108.7 . . ? C21 C20 H34 108.7 . . ? H33 C20 H34 107.6 . . ? C22 C21 C34 120.9(3) . . ? C22 C21 C20 120.7(3) . . ? C34 C21 C20 118.4(3) . . ? C23 C22 C21 121.0(3) . . ? C23 C22 H35 119.5 . . ? C21 C22 H35 119.5 . . ? C22 C23 C28 117.2(3) . . ? C22 C23 C24 123.7(3) . . ? C28 C23 C24 119.2(3) . . ? C26 C24 C25 108.1(3) . . ? C26 C24 C27 108.9(3) . . ? C25 C24 C27 108.5(3) . . ? C26 C24 C23 109.5(3) . . ? C25 C24 C23 112.3(3) . . ? C27 C24 C23 109.4(3) . . ? C24 C25 H36 109.5 . . ? C24 C25 H37 109.5 . . ? H36 C25 H37 109.5 . . ? C24 C25 H38 109.5 . . ? H36 C25 H38 109.5 . . ? H37 C25 H38 109.5 . . ? C24 C26 H39 109.5 . . ? C24 C26 H40 109.5 . . ? H39 C26 H40 109.5 . . ? C24 C26 H41 109.5 . . ? H39 C26 H41 109.5 . . ? H40 C26 H41 109.5 . . ? C24 C27 H42 109.5 . . ? C24 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? C24 C27 H44 109.5 . . ? H42 C27 H44 109.5 . . ? H43 C27 H44 109.5 . . ? C29 C28 C23 124.5(3) . . ? C29 C28 H45 117.7 . . ? C23 C28 H45 117.7 . . ? C28 C29 C34 117.3(3) . . ? C28 C29 C30 120.8(3) . . ? C34 C29 C30 121.9(3) . . ? C32 C30 C33 109.4(3) . . ? C32 C30 C31 106.5(3) . . ? C33 C30 C31 107.8(3) . . ? C32 C30 C29 111.2(3) . . ? C33 C30 C29 109.8(3) . . ? C31 C30 C29 112.1(3) . . ? C30 C31 H46 109.5 . . ? C30 C31 H47 109.5 . . ? H46 C31 H47 109.5 . . ? C30 C31 H48 109.5 . . ? H46 C31 H48 109.5 . . ? H47 C31 H48 109.5 . . ? C30 C32 H49 109.5 . . ? C30 C32 H50 109.5 . . ? H49 C32 H50 109.5 . . ? C30 C32 H51 109.5 . . ? H49 C32 H51 109.5 . . ? H50 C32 H51 109.5 . . ? C30 C33 H52 109.5 . . ? C30 C33 H53 109.5 . . ? H52 C33 H53 109.5 . . ? C30 C33 H54 109.5 . . ? H52 C33 H54 109.5 . . ? H53 C33 H54 109.5 . . ? O2 C34 C21 118.9(3) . . ? O2 C34 C29 122.1(3) . . ? C21 C34 C29 119.0(3) . . ? O4 C35 O3 123.2(3) . . ? O4 C35 C36 119.9(3) . . ? O3 C35 C36 116.9(3) . . ? C35 C36 H55 109.5 . . ? C35 C36 H56 109.5 . . ? H55 C36 H56 109.5 . . ? C35 C36 H57 109.5 . . ? H55 C36 H57 109.5 . . ? H56 C36 H57 109.5 . . ? O5 C37 H58 109.5 . . ? O5 C37 H59 109.5 . . ? H58 C37 H59 109.5 . . ? O5 C37 H60 109.5 . . ? H58 C37 H60 109.5 . . ? H59 C37 H60 109.5 . . ? O6 C38 H62 109.5 . . ? O6 C38 H63 109.5 . . ? H62 C38 H63 109.5 . . ? O6 C38 H64 109.5 . . ? H62 C38 H64 109.5 . . ? H63 C38 H64 109.5 . . ? O6 C38 H65 37(2) . . ? H62 C38 H65 108.9 . . ? H63 C38 H65 75.4 . . ? H64 C38 H65 136.5 . . ? C40 C39 H66 109.5 . . ? C40 C39 H67 109.5 . . ? H66 C39 H67 109.5 . . ? C40 C39 H68 109.5 . . ? H66 C39 H68 109.5 . . ? H67 C39 H68 109.5 . . ? C41 C40 C45 116.8(5) . . ? C41 C40 C39 120.6(5) . . ? C45 C40 C39 122.5(5) . . ? C40 C41 C42 121.5(5) . . ? C40 C41 H69 119.2 . . ? C42 C41 H69 119.2 . . ? C43 C42 C41 120.2(5) . . ? C43 C42 H70 119.9 . . ? C41 C42 H70 119.9 . . ? C44 C43 C42 118.6(5) . . ? C44 C43 H71 120.7 . . ? C42 C43 H71 120.7 . . ? C43 C44 C45 121.4(5) . . ? C43 C44 H72 119.3 . . ? C45 C44 H72 119.3 . . ? C44 C45 C40 121.3(5) . . ? C44 C45 H73 119.4 . . ? C40 C45 H73 119.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.170 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.094 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 766027' #TrackingRef 'Kozak_Compiled_CIF.cif' # start Validation Reply Form _vrf_PLAT220_6 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.82 Ratio RESPONSE: This atom is part of a tertiary terminal group that exhibited some disorder that was not modelled. The atom was refined anisotropically. This should not be taken as an indication for an incorrectly identified atomic species. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C40 H66 N2 O2) Co]2 [(C H3 C O2)2 (C H3 O H)4 Co]' _chemical_formula_sum 'C88 H154 Co3 N4 O12' _chemical_formula_weight 1637.00 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.862(2) _cell_length_b 22.109(3) _cell_length_c 18.557(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.714(3) _cell_angle_gamma 90.00 _cell_volume 4583.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 17525 _cell_measurement_theta_min 2.2341 _cell_measurement_theta_max 30.7573 _exptl_crystal_description Prism _exptl_crystal_colour 'Light Purple' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1774 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9758 _exptl_absorpt_correction_T_min 0.9430 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 40123 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 26.50 _reflns_number_total 9487 _reflns_number_gt 8768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0727P)^2^+5.4526P] 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 9487 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.22147(3) 0.373373(17) 0.44496(2) 0.02414(12) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 0.5000 0.02536(15) Uani 1 2 d S . . O1 O 0.37953(18) 0.34482(9) 0.53549(12) 0.0266(4) Uani 1 1 d . . . O2 O 0.17531(17) 0.43293(9) 0.35299(12) 0.0261(4) Uani 1 1 d . . . O3 O 0.20418(18) 0.43788(9) 0.51694(13) 0.0296(5) Uani 1 1 d . . . O4 O 0.36468(19) 0.48153(10) 0.52573(14) 0.0349(5) Uani 1 1 d . . . O5 O 0.3637(2) 0.49562(10) 0.37705(13) 0.0333(5) Uani 1 1 d . . . H73 H 0.2986 0.4718 0.3734 0.040 Uiso 1 1 d . . . O6 O 0.4783(2) 0.59397(10) 0.49999(14) 0.0341(5) Uani 1 1 d . . . H77 H 0.4623 0.5765 0.4500 0.041 Uiso 1 1 d . . . N1 N 0.2324(2) 0.30349(11) 0.36136(14) 0.0248(5) Uani 1 1 d . . . N2 N 0.0800(2) 0.31151(11) 0.43455(16) 0.0280(5) Uani 1 1 d . . . C1 C 0.4018(2) 0.28544(13) 0.55310(17) 0.0251(6) Uani 1 1 d . . . C2 C 0.4434(2) 0.26267(13) 0.63428(18) 0.0259(6) Uani 1 1 d . . . C3 C 0.4795(3) 0.30490(13) 0.70914(18) 0.0286(6) Uani 1 1 d . . . C4 C 0.3687(3) 0.34092(15) 0.69688(19) 0.0327(7) Uani 1 1 d . . . H1 H 0.3305 0.3597 0.6412 0.039 Uiso 1 1 calc R . . H2 H 0.3105 0.3120 0.6977 0.039 Uiso 1 1 calc R . . C5 C 0.3928(4) 0.39047(18) 0.7609(2) 0.0485(9) Uani 1 1 d . . . H3 H 0.3171 0.4095 0.7488 0.058 Uiso 1 1 calc R . . H4 H 0.4460 0.4210 0.7582 0.058 Uiso 1 1 calc R . . H5 H 0.4309 0.3727 0.8165 0.058 Uiso 1 1 calc R . . C6 C 0.5792(3) 0.34713(15) 0.7162(2) 0.0345(7) Uani 1 1 d . . . H6 H 0.5462 0.3751 0.6690 0.041 Uiso 1 1 calc R . . H7 H 0.6431 0.3230 0.7162 0.041 Uiso 1 1 calc R . . H8 H 0.6118 0.3702 0.7680 0.041 Uiso 1 1 calc R . . C7 C 0.5303(3) 0.26907(15) 0.79076(19) 0.0349(7) Uani 1 1 d . . . H9 H 0.5534 0.2972 0.8371 0.042 Uiso 1 1 calc R . . H10 H 0.6007 0.2461 0.7993 0.042 Uiso 1 1 calc R . . H11 H 0.4692 0.2411 0.7879 0.042 Uiso 1 1 calc R . . C8 C 0.4551(3) 0.20030(14) 0.64427(18) 0.0295(6) Uani 1 1 d . . . H12 H 0.4807 0.1844 0.6980 0.035 Uiso 1 1 calc R . . C9 C 0.4319(3) 0.15932(13) 0.58044(18) 0.0287(6) Uani 1 1 d . . . C10 C 0.4436(3) 0.09150(14) 0.5988(2) 0.0333(7) Uani 1 1 d . . . C11 C 0.3556(4) 0.07245(16) 0.6283(2) 0.0441(8) Uani 1 1 d . . . H13 H 0.3650 0.0285 0.6400 0.053 Uiso 1 1 calc R . . H14 H 0.3784 0.0935 0.6812 0.053 Uiso 1 1 calc R . . C12 C 0.2251(4) 0.0852(2) 0.5687(3) 0.0587(11) Uani 1 1 d . . . H15 H 0.1777 0.0756 0.5954 0.070 Uiso 1 1 calc R . . H16 H 0.1979 0.0602 0.5189 0.070 Uiso 1 1 calc R . . H17 H 0.2149 0.1280 0.5531 0.070 Uiso 1 1 calc R . . C13 C 0.5726(3) 0.07687(16) 0.6682(3) 0.0533(10) Uani 1 1 d . . . H18 H 0.6295 0.0894 0.6504 0.064 Uiso 1 1 calc R . . H19 H 0.5802 0.0333 0.6791 0.064 Uiso 1 1 calc R . . H20 H 0.5898 0.0987 0.7189 0.064 Uiso 1 1 calc R . . C14 C 0.4200(3) 0.05425(14) 0.5232(2) 0.0383(7) Uani 1 1 d . . . H21 H 0.4296 0.0112 0.5376 0.046 Uiso 1 1 calc R . . H22 H 0.4769 0.0659 0.5051 0.046 Uiso 1 1 calc R . . H23 H 0.3382 0.0617 0.4782 0.046 Uiso 1 1 calc R . . C15 C 0.3969(3) 0.18342(13) 0.50248(18) 0.0288(6) Uani 1 1 d . . . H24 H 0.3826 0.1572 0.4580 0.035 Uiso 1 1 calc R . . C16 C 0.3825(3) 0.24578(13) 0.48880(17) 0.0264(6) Uani 1 1 d . . . C17 C 0.3505(3) 0.27162(13) 0.40542(17) 0.0272(6) Uani 1 1 d . . . H25 H 0.4140 0.3004 0.4128 0.033 Uiso 1 1 calc R . . H26 H 0.3501 0.2383 0.3696 0.033 Uiso 1 1 calc R . . C18 C 0.1320(3) 0.26069(14) 0.33656(19) 0.0304(6) Uani 1 1 d . . . H27 H 0.1540 0.2210 0.3233 0.036 Uiso 1 1 calc R . . H28 H 0.0609 0.2759 0.2859 0.036 Uiso 1 1 calc R . . C19 C 0.1011(3) 0.25280(13) 0.40508(18) 0.0285(6) Uani 1 1 d . . . H29 H 0.0284 0.2275 0.3843 0.034 Uiso 1 1 calc R . . H30 H 0.1674 0.2313 0.4523 0.034 Uiso 1 1 calc R . . C20 C 0.0816(3) 0.29796(15) 0.5141(2) 0.0340(7) Uani 1 1 d . . . H31 H 0.1640 0.2861 0.5560 0.041 Uiso 1 1 calc R . . H32 H 0.0292 0.2626 0.5050 0.041 Uiso 1 1 calc R . . C21 C 0.0422(4) 0.34885(17) 0.5499(3) 0.0464(9) Uani 1 1 d . . . H33 H 0.0626 0.3387 0.6068 0.056 Uiso 1 1 calc R . . H34 H -0.0446 0.3544 0.5159 0.056 Uiso 1 1 calc R . . H35 H 0.0830 0.3863 0.5501 0.056 Uiso 1 1 calc R . . C22 C -0.0353(3) 0.33957(15) 0.3718(2) 0.0354(7) Uani 1 1 d . . . H36 H -0.0301 0.3480 0.3213 0.042 Uiso 1 1 calc R . . H37 H -0.0433 0.3790 0.3940 0.042 Uiso 1 1 calc R . . C23 C -0.1496(3) 0.30352(19) 0.3460(3) 0.0497(9) Uani 1 1 d . . . H38 H -0.1503 0.2677 0.3147 0.060 Uiso 1 1 calc R . . H39 H -0.2193 0.3288 0.3111 0.060 Uiso 1 1 calc R . . H40 H -0.1525 0.2909 0.3956 0.060 Uiso 1 1 calc R . . C24 C 0.2255(3) 0.33225(13) 0.28639(17) 0.0269(6) Uani 1 1 d . . . H41 H 0.2295 0.3002 0.2506 0.032 Uiso 1 1 calc R . . H42 H 0.2960 0.3588 0.3041 0.032 Uiso 1 1 calc R . . C25 C 0.1137(3) 0.36892(13) 0.23629(18) 0.0252(6) Uani 1 1 d . . . C26 C 0.0304(3) 0.35232(14) 0.15620(18) 0.0282(6) Uani 1 1 d . . . H43 H 0.0447 0.3173 0.1327 0.034 Uiso 1 1 calc R . . C27 C -0.0733(3) 0.38541(14) 0.10930(18) 0.0303(6) Uani 1 1 d . . . C28 C -0.1694(3) 0.36305(17) 0.0233(2) 0.0436(9) Uani 1 1 d . . . C29 C -0.2000(5) 0.2957(2) 0.0326(3) 0.0791(16) Uani 1 1 d . . . H44 H -0.1266 0.2708 0.0543 0.095 Uiso 1 1 calc R . . H45 H -0.2591 0.2797 -0.0225 0.095 Uiso 1 1 calc R . . C30 C -0.2529(5) 0.2908(3) 0.0935(4) 0.0830(17) Uani 1 1 d . . . H46 H -0.3365 0.3042 0.0647 0.100 Uiso 1 1 calc R . . H47 H -0.2062 0.3164 0.1422 0.100 Uiso 1 1 calc R . . H48 H -0.2487 0.2487 0.1112 0.100 Uiso 1 1 calc R . . C31 C -0.2772(5) 0.4002(3) -0.0144(3) 0.120(3) Uani 1 1 d . . . H49 H -0.3341 0.3847 0.0018 0.144 Uiso 1 1 calc R . . H50 H -0.3138 0.3987 -0.0750 0.144 Uiso 1 1 calc R . . H51 H -0.2563 0.4421 0.0045 0.144 Uiso 1 1 calc R . . C32 C -0.1179(5) 0.3595(3) -0.0336(3) 0.0861(18) Uani 1 1 d . . . H52 H -0.1304 0.3981 -0.0627 0.103 Uiso 1 1 calc R . . H53 H -0.1577 0.3271 -0.0742 0.103 Uiso 1 1 calc R . . H54 H -0.0319 0.3510 -0.0011 0.103 Uiso 1 1 calc R . . C33 C -0.0866(3) 0.43824(14) 0.14491(19) 0.0309(6) Uani 1 1 d . . . H55 H -0.1556 0.4623 0.1127 0.037 Uiso 1 1 calc R . . C34 C -0.0049(3) 0.45818(13) 0.22517(17) 0.0257(6) Uani 1 1 d . . . C35 C -0.0278(3) 0.51711(13) 0.25926(18) 0.0285(6) Uani 1 1 d . . . C36 C 0.0792(3) 0.56058(15) 0.2887(2) 0.0395(8) Uani 1 1 d . . . H56 H 0.0623 0.5973 0.3116 0.047 Uiso 1 1 calc R . . H57 H 0.1506 0.5409 0.3344 0.047 Uiso 1 1 calc R . . C37 C 0.1090(4) 0.57966(19) 0.2227(3) 0.0579(11) Uani 1 1 d . . . H58 H 0.1841 0.6026 0.2484 0.069 Uiso 1 1 calc R . . H59 H 0.0444 0.6051 0.1815 0.069 Uiso 1 1 calc R . . H60 H 0.1178 0.5437 0.1953 0.069 Uiso 1 1 calc R . . C38 C -0.1401(3) 0.55021(15) 0.1944(2) 0.0366(7) Uani 1 1 d . . . H61 H -0.1497 0.5880 0.2181 0.044 Uiso 1 1 calc R . . H62 H -0.2105 0.5245 0.1778 0.044 Uiso 1 1 calc R . . H63 H -0.1320 0.5594 0.1457 0.044 Uiso 1 1 calc R . . C39 C -0.0471(3) 0.50238(15) 0.3328(2) 0.0392(8) Uani 1 1 d . . . H64 H -0.0650 0.5397 0.3530 0.047 Uiso 1 1 calc R . . H65 H 0.0257 0.4839 0.3775 0.047 Uiso 1 1 calc R . . H66 H -0.1141 0.4741 0.3147 0.047 Uiso 1 1 calc R . . C40 C 0.0961(2) 0.42095(13) 0.27306(17) 0.0249(6) Uani 1 1 d . . . C41 C 0.2808(3) 0.47986(13) 0.54109(18) 0.0277(6) Uani 1 1 d . . . C42 C 0.2679(4) 0.52913(17) 0.5918(2) 0.0464(9) Uani 1 1 d . . . H67 H 0.1878 0.5469 0.5608 0.056 Uiso 1 1 calc R . . H68 H 0.3283 0.5604 0.6038 0.056 Uiso 1 1 calc R . . H69 H 0.2793 0.5122 0.6440 0.056 Uiso 1 1 calc R . . C43 C 0.3857(3) 0.48104(17) 0.3114(2) 0.0386(7) Uani 1 1 d . . . H70 H 0.4319 0.5136 0.3047 0.046 Uiso 1 1 calc R . . H71 H 0.3093 0.4763 0.2598 0.046 Uiso 1 1 calc R . . H72 H 0.4311 0.4432 0.3242 0.046 Uiso 1 1 calc R . . C44 C 0.3676(3) 0.62497(15) 0.4680(2) 0.0391(8) Uani 1 1 d . . . H74 H 0.3786 0.6616 0.5007 0.047 Uiso 1 1 calc R . . H75 H 0.3087 0.5986 0.4711 0.047 Uiso 1 1 calc R . . H76 H 0.3391 0.6361 0.4100 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0238(2) 0.0226(2) 0.0243(2) -0.00052(14) 0.01062(17) -0.00144(14) Co2 0.0256(3) 0.0239(3) 0.0263(3) -0.0023(2) 0.0126(2) -0.0026(2) O1 0.0285(10) 0.0208(10) 0.0263(10) 0.0009(8) 0.0104(8) 0.0000(8) O2 0.0271(10) 0.0231(10) 0.0230(10) -0.0018(8) 0.0085(8) -0.0018(8) O3 0.0299(11) 0.0268(11) 0.0312(11) -0.0038(8) 0.0145(9) -0.0035(9) O4 0.0315(11) 0.0383(12) 0.0386(12) 0.0034(10) 0.0200(10) -0.0015(10) O5 0.0322(11) 0.0391(12) 0.0276(11) -0.0024(9) 0.0140(9) -0.0071(9) O6 0.0343(11) 0.0246(11) 0.0444(13) -0.0022(9) 0.0204(10) 0.0009(9) N1 0.0251(12) 0.0248(12) 0.0235(12) 0.0011(9) 0.0113(10) -0.0007(10) N2 0.0292(13) 0.0233(12) 0.0312(13) -0.0005(10) 0.0146(11) -0.0016(10) C1 0.0225(13) 0.0248(14) 0.0262(14) 0.0009(11) 0.0107(11) -0.0003(11) C2 0.0239(13) 0.0271(14) 0.0257(14) -0.0005(11) 0.0116(11) -0.0015(11) C3 0.0268(14) 0.0274(15) 0.0272(15) -0.0016(11) 0.0101(12) -0.0022(12) C4 0.0324(16) 0.0374(17) 0.0273(15) -0.0024(13) 0.0139(13) 0.0029(13) C5 0.049(2) 0.049(2) 0.046(2) -0.0124(17) 0.0228(18) 0.0084(18) C6 0.0322(16) 0.0373(17) 0.0296(16) -0.0059(13) 0.0120(13) -0.0081(13) C7 0.0405(17) 0.0364(17) 0.0246(15) -0.0010(12) 0.0137(14) -0.0008(14) C8 0.0317(15) 0.0299(15) 0.0252(15) 0.0037(12) 0.0128(12) 0.0009(12) C9 0.0307(15) 0.0207(14) 0.0305(15) 0.0001(11) 0.0120(12) 0.0009(11) C10 0.0386(17) 0.0231(15) 0.0343(16) 0.0024(12) 0.0152(14) 0.0022(12) C11 0.062(2) 0.0307(17) 0.047(2) -0.0002(15) 0.0322(19) -0.0028(16) C12 0.059(3) 0.053(2) 0.086(3) 0.004(2) 0.052(3) -0.001(2) C13 0.049(2) 0.0298(18) 0.055(2) 0.0106(16) 0.0051(18) 0.0061(16) C14 0.0476(19) 0.0255(15) 0.047(2) -0.0049(14) 0.0277(17) -0.0009(14) C15 0.0302(15) 0.0268(15) 0.0275(15) -0.0001(11) 0.0127(12) 0.0035(12) C16 0.0283(14) 0.0255(14) 0.0246(14) 0.0008(11) 0.0125(12) 0.0030(11) C17 0.0287(14) 0.0258(14) 0.0251(14) -0.0005(11) 0.0119(12) 0.0054(11) C18 0.0322(15) 0.0251(14) 0.0288(15) -0.0057(12) 0.0113(13) -0.0033(12) C19 0.0299(15) 0.0223(14) 0.0310(15) -0.0022(11) 0.0135(12) -0.0057(12) C20 0.0347(16) 0.0346(17) 0.0367(17) -0.0043(13) 0.0207(14) -0.0080(13) C21 0.058(2) 0.0393(19) 0.058(2) -0.0115(17) 0.041(2) -0.0139(17) C22 0.0271(15) 0.0338(17) 0.0436(18) 0.0062(14) 0.0163(14) 0.0013(13) C23 0.0287(17) 0.054(2) 0.058(2) 0.0146(18) 0.0150(17) -0.0017(16) C24 0.0293(14) 0.0285(15) 0.0223(14) 0.0009(11) 0.0124(12) 0.0042(12) C25 0.0245(14) 0.0246(14) 0.0243(14) 0.0014(11) 0.0104(12) 0.0003(11) C26 0.0299(15) 0.0286(15) 0.0258(14) -0.0028(12) 0.0135(12) 0.0012(12) C27 0.0273(15) 0.0337(16) 0.0224(14) -0.0025(12) 0.0066(12) 0.0018(12) C28 0.0369(18) 0.046(2) 0.0291(17) -0.0104(15) 0.0019(14) 0.0056(15) C29 0.069(3) 0.060(3) 0.065(3) -0.024(2) 0.000(2) 0.001(2) C30 0.070(3) 0.092(4) 0.088(4) -0.024(3) 0.040(3) -0.044(3) C31 0.069(3) 0.122(5) 0.075(4) -0.064(4) -0.036(3) 0.050(3) C32 0.079(3) 0.120(5) 0.038(2) -0.017(3) 0.013(2) 0.033(3) C33 0.0283(15) 0.0308(16) 0.0280(15) -0.0004(12) 0.0097(12) 0.0035(12) C34 0.0279(14) 0.0244(14) 0.0238(14) 0.0001(11) 0.0121(12) -0.0010(11) C35 0.0283(15) 0.0259(14) 0.0289(15) -0.0012(12) 0.0123(12) 0.0023(12) C36 0.0356(17) 0.0253(16) 0.047(2) -0.0027(14) 0.0127(15) 0.0001(13) C37 0.055(2) 0.046(2) 0.076(3) 0.009(2) 0.035(2) -0.0086(19) C38 0.0343(16) 0.0300(16) 0.0395(18) -0.0021(13) 0.0137(14) 0.0061(13) C39 0.049(2) 0.0339(17) 0.0391(19) -0.0024(14) 0.0250(16) 0.0083(15) C40 0.0242(13) 0.0262(14) 0.0218(13) 0.0010(11) 0.0096(11) -0.0008(11) C41 0.0300(15) 0.0261(15) 0.0264(14) 0.0019(11) 0.0135(12) 0.0001(12) C42 0.055(2) 0.0392(19) 0.056(2) -0.0172(17) 0.0355(19) -0.0106(17) C43 0.0412(18) 0.047(2) 0.0310(17) -0.0046(14) 0.0202(15) -0.0054(15) C44 0.0353(17) 0.0329(17) 0.052(2) 0.0048(15) 0.0235(16) 0.0067(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 O1 1.992(2) . ? Co1 O2 1.999(2) . ? Co1 O3 2.040(2) . ? Co1 N2 2.207(2) . ? Co1 N1 2.242(2) . ? Co2 O4 2.061(2) 3_666 ? Co2 O4 2.061(2) . ? Co2 O5 2.079(2) . ? Co2 O5 2.079(2) 3_666 ? Co2 O6 2.096(2) 3_666 ? Co2 O6 2.096(2) . ? Co2 H77 1.8732 . ? O1 C1 1.349(3) . ? O2 C40 1.345(3) . ? O3 C41 1.263(4) . ? O4 C41 1.246(4) . ? O5 C43 1.418(4) . ? O5 H73 0.9630 . ? O6 C44 1.418(4) . ? O6 H77 0.9299 . ? N1 C18 1.478(4) . ? N1 C24 1.492(4) . ? N1 C17 1.498(4) . ? N2 C19 1.485(4) . ? N2 C22 1.493(4) . ? N2 C20 1.497(4) . ? C1 C16 1.400(4) . ? C1 C2 1.418(4) . ? C2 C8 1.390(4) . ? C2 C3 1.542(4) . ? C3 C6 1.538(4) . ? C3 C7 1.539(4) . ? C3 C4 1.548(4) . ? C4 C5 1.530(5) . ? C4 H1 0.9900 . ? C4 H2 0.9900 . ? C5 H3 0.9800 . ? C5 H4 0.9800 . ? C5 H5 0.9800 . ? C6 H6 0.9800 . ? C6 H7 0.9800 . ? C6 H8 0.9800 . ? C7 H9 0.9800 . ? C7 H10 0.9800 . ? C7 H11 0.9800 . ? C8 C9 1.401(4) . ? C8 H12 0.9500 . ? C9 C15 1.391(4) . ? C9 C10 1.529(4) . ? C10 C14 1.522(4) . ? C10 C11 1.539(5) . ? C10 C13 1.548(5) . ? C11 C12 1.510(6) . ? C11 H13 0.9900 . ? C11 H14 0.9900 . ? C12 H15 0.9800 . ? C12 H16 0.9800 . ? C12 H17 0.9800 . ? C13 H18 0.9800 . ? C13 H19 0.9800 . ? C13 H20 0.9800 . ? C14 H21 0.9800 . ? C14 H22 0.9800 . ? C14 H23 0.9800 . ? C15 C16 1.397(4) . ? C15 H24 0.9500 . ? C16 C17 1.503(4) . ? C17 H25 0.9900 . ? C17 H26 0.9900 . ? C18 C19 1.519(4) . ? C18 H27 0.9900 . ? C18 H28 0.9900 . ? C19 H29 0.9900 . ? C19 H30 0.9900 . ? C20 C21 1.516(5) . ? C20 H31 0.9900 . ? C20 H32 0.9900 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C21 H35 0.9800 . ? C22 C23 1.525(5) . ? C22 H36 0.9900 . ? C22 H37 0.9900 . ? C23 H38 0.9800 . ? C23 H39 0.9800 . ? C23 H40 0.9800 . ? C24 C25 1.505(4) . ? C24 H41 0.9900 . ? C24 H42 0.9900 . ? C25 C26 1.383(4) . ? C25 C40 1.412(4) . ? C26 C27 1.386(4) . ? C26 H43 0.9500 . ? C27 C33 1.394(4) . ? C27 C28 1.538(4) . ? C28 C31 1.458(6) . ? C28 C32 1.502(6) . ? C28 C29 1.571(6) . ? C29 C30 1.585(8) . ? C29 H44 0.9900 . ? C29 H45 0.9900 . ? C30 H46 0.9800 . ? C30 H47 0.9800 . ? C30 H48 0.9800 . ? C31 H49 0.9800 . ? C31 H50 0.9800 . ? C31 H51 0.9800 . ? C32 H52 0.9800 . ? C32 H53 0.9800 . ? C32 H54 0.9800 . ? C33 C34 1.402(4) . ? C33 H55 0.9500 . ? C34 C40 1.418(4) . ? C34 C35 1.540(4) . ? C35 C38 1.532(4) . ? C35 C39 1.537(4) . ? C35 C36 1.540(4) . ? C36 C37 1.514(5) . ? C36 H56 0.9900 . ? C36 H57 0.9900 . ? C37 H58 0.9800 . ? C37 H59 0.9800 . ? C37 H60 0.9800 . ? C38 H61 0.9800 . ? C38 H62 0.9800 . ? C38 H63 0.9800 . ? C39 H64 0.9800 . ? C39 H65 0.9800 . ? C39 H66 0.9800 . ? C41 C42 1.502(4) . ? C42 H67 0.9800 . ? C42 H68 0.9800 . ? C42 H69 0.9800 . ? C43 H70 0.9800 . ? C43 H71 0.9800 . ? C43 H72 0.9800 . ? C44 H74 0.9800 . ? C44 H75 0.9800 . ? C44 H76 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 132.53(8) . . ? O1 Co1 O3 93.80(8) . . ? O2 Co1 O3 90.91(8) . . ? O1 Co1 N2 109.27(9) . . ? O2 Co1 N2 116.77(9) . . ? O3 Co1 N2 97.91(9) . . ? O1 Co1 N1 88.71(8) . . ? O2 Co1 N1 87.55(8) . . ? O3 Co1 N1 177.48(9) . . ? N2 Co1 N1 81.03(9) . . ? O4 Co2 O4 179.999(1) 3_666 . ? O4 Co2 O5 96.00(9) 3_666 . ? O4 Co2 O5 84.00(9) . . ? O4 Co2 O5 84.00(9) 3_666 3_666 ? O4 Co2 O5 96.00(9) . 3_666 ? O5 Co2 O5 180.00(10) . 3_666 ? O4 Co2 O6 93.95(9) 3_666 3_666 ? O4 Co2 O6 86.05(9) . 3_666 ? O5 Co2 O6 89.64(9) . 3_666 ? O5 Co2 O6 90.36(9) 3_666 3_666 ? O4 Co2 O6 86.05(9) 3_666 . ? O4 Co2 O6 93.95(9) . . ? O5 Co2 O6 90.36(9) . . ? O5 Co2 O6 89.64(9) 3_666 . ? O6 Co2 O6 180.0 3_666 . ? O4 Co2 H77 75.4 3_666 . ? O4 Co2 H77 104.6 . . ? O5 Co2 H77 68.1 . . ? O5 Co2 H77 111.9 3_666 . ? O6 Co2 H77 153.7 3_666 . ? O6 Co2 H77 26.3 . . ? C1 O1 Co1 121.22(17) . . ? C40 O2 Co1 123.63(17) . . ? C41 O3 Co1 115.28(19) . . ? C41 O4 Co2 170.3(2) . . ? C43 O5 Co2 122.3(2) . . ? C43 O5 H73 110.7 . . ? Co2 O5 H73 109.4 . . ? C44 O6 Co2 125.80(19) . . ? C44 O6 H77 95.9 . . ? Co2 O6 H77 63.3 . . ? C18 N1 C24 110.1(2) . . ? C18 N1 C17 111.2(2) . . ? C24 N1 C17 106.5(2) . . ? C18 N1 Co1 108.19(17) . . ? C24 N1 Co1 110.87(17) . . ? C17 N1 Co1 109.93(17) . . ? C19 N2 C22 111.6(2) . . ? C19 N2 C20 105.8(2) . . ? C22 N2 C20 112.0(2) . . ? C19 N2 Co1 106.29(17) . . ? C22 N2 Co1 105.56(17) . . ? C20 N2 Co1 115.47(18) . . ? O1 C1 C16 118.5(2) . . ? O1 C1 C2 121.7(3) . . ? C16 C1 C2 119.8(3) . . ? C8 C2 C1 116.9(3) . . ? C8 C2 C3 121.1(3) . . ? C1 C2 C3 121.9(3) . . ? C6 C3 C7 107.4(2) . . ? C6 C3 C2 108.1(2) . . ? C7 C3 C2 111.5(2) . . ? C6 C3 C4 111.6(3) . . ? C7 C3 C4 108.7(3) . . ? C2 C3 C4 109.5(2) . . ? C5 C4 C3 115.9(3) . . ? C5 C4 H1 108.3 . . ? C3 C4 H1 108.3 . . ? C5 C4 H2 108.3 . . ? C3 C4 H2 108.3 . . ? H1 C4 H2 107.4 . . ? C4 C5 H3 109.5 . . ? C4 C5 H4 109.5 . . ? H3 C5 H4 109.5 . . ? C4 C5 H5 109.5 . . ? H3 C5 H5 109.5 . . ? H4 C5 H5 109.5 . . ? C3 C6 H6 109.5 . . ? C3 C6 H7 109.5 . . ? H6 C6 H7 109.5 . . ? C3 C6 H8 109.5 . . ? H6 C6 H8 109.5 . . ? H7 C6 H8 109.5 . . ? C3 C7 H9 109.5 . . ? C3 C7 H10 109.5 . . ? H9 C7 H10 109.5 . . ? C3 C7 H11 109.5 . . ? H9 C7 H11 109.5 . . ? H10 C7 H11 109.5 . . ? C2 C8 C9 124.4(3) . . ? C2 C8 H12 117.8 . . ? C9 C8 H12 117.8 . . ? C15 C9 C8 117.1(3) . . ? C15 C9 C10 123.6(3) . . ? C8 C9 C10 119.3(3) . . ? C14 C10 C9 111.8(3) . . ? C14 C10 C11 109.5(3) . . ? C9 C10 C11 109.9(3) . . ? C14 C10 C13 107.1(3) . . ? C9 C10 C13 109.7(3) . . ? C11 C10 C13 108.8(3) . . ? C12 C11 C10 115.8(3) . . ? C12 C11 H13 108.3 . . ? C10 C11 H13 108.3 . . ? C12 C11 H14 108.3 . . ? C10 C11 H14 108.3 . . ? H13 C11 H14 107.4 . . ? C11 C12 H15 109.5 . . ? C11 C12 H16 109.5 . . ? H15 C12 H16 109.5 . . ? C11 C12 H17 109.5 . . ? H15 C12 H17 109.5 . . ? H16 C12 H17 109.5 . . ? C10 C13 H18 109.5 . . ? C10 C13 H19 109.5 . . ? H18 C13 H19 109.5 . . ? C10 C13 H20 109.5 . . ? H18 C13 H20 109.5 . . ? H19 C13 H20 109.5 . . ? C10 C14 H21 109.5 . . ? C10 C14 H22 109.5 . . ? H21 C14 H22 109.5 . . ? C10 C14 H23 109.5 . . ? H21 C14 H23 109.5 . . ? H22 C14 H23 109.5 . . ? C9 C15 C16 120.8(3) . . ? C9 C15 H24 119.6 . . ? C16 C15 H24 119.6 . . ? C15 C16 C1 120.8(3) . . ? C15 C16 C17 120.4(3) . . ? C1 C16 C17 118.8(3) . . ? N1 C17 C16 115.3(2) . . ? N1 C17 H25 108.5 . . ? C16 C17 H25 108.5 . . ? N1 C17 H26 108.5 . . ? C16 C17 H26 108.5 . . ? H25 C17 H26 107.5 . . ? N1 C18 C19 111.3(2) . . ? N1 C18 H27 109.4 . . ? C19 C18 H27 109.4 . . ? N1 C18 H28 109.4 . . ? C19 C18 H28 109.4 . . ? H27 C18 H28 108.0 . . ? N2 C19 C18 112.3(2) . . ? N2 C19 H29 109.1 . . ? C18 C19 H29 109.1 . . ? N2 C19 H30 109.1 . . ? C18 C19 H30 109.1 . . ? H29 C19 H30 107.9 . . ? N2 C20 C21 116.1(3) . . ? N2 C20 H31 108.3 . . ? C21 C20 H31 108.3 . . ? N2 C20 H32 108.3 . . ? C21 C20 H32 108.3 . . ? H31 C20 H32 107.4 . . ? C20 C21 H33 109.5 . . ? C20 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? C20 C21 H35 109.5 . . ? H33 C21 H35 109.5 . . ? H34 C21 H35 109.5 . . ? N2 C22 C23 117.3(3) . . ? N2 C22 H36 108.0 . . ? C23 C22 H36 108.0 . . ? N2 C22 H37 108.0 . . ? C23 C22 H37 108.0 . . ? H36 C22 H37 107.2 . . ? C22 C23 H38 109.5 . . ? C22 C23 H39 109.5 . . ? H38 C23 H39 109.5 . . ? C22 C23 H40 109.5 . . ? H38 C23 H40 109.5 . . ? H39 C23 H40 109.5 . . ? N1 C24 C25 113.7(2) . . ? N1 C24 H41 108.8 . . ? C25 C24 H41 108.8 . . ? N1 C24 H42 108.8 . . ? C25 C24 H42 108.8 . . ? H41 C24 H42 107.7 . . ? C26 C25 C40 120.8(3) . . ? C26 C25 C24 121.0(3) . . ? C40 C25 C24 118.3(2) . . ? C25 C26 C27 121.7(3) . . ? C25 C26 H43 119.1 . . ? C27 C26 H43 119.1 . . ? C26 C27 C33 116.8(3) . . ? C26 C27 C28 120.7(3) . . ? C33 C27 C28 122.5(3) . . ? C31 C28 C32 109.8(4) . . ? C31 C28 C27 113.7(3) . . ? C32 C28 C27 109.8(3) . . ? C31 C28 C29 110.8(4) . . ? C32 C28 C29 104.5(4) . . ? C27 C28 C29 107.9(3) . . ? C28 C29 C30 111.3(4) . . ? C28 C29 H44 109.4 . . ? C30 C29 H44 109.4 . . ? C28 C29 H45 109.4 . . ? C30 C29 H45 109.4 . . ? H44 C29 H45 108.0 . . ? C29 C30 H46 109.5 . . ? C29 C30 H47 109.5 . . ? H46 C30 H47 109.5 . . ? C29 C30 H48 109.5 . . ? H46 C30 H48 109.5 . . ? H47 C30 H48 109.5 . . ? C28 C31 H49 109.5 . . ? C28 C31 H50 109.5 . . ? H49 C31 H50 109.5 . . ? C28 C31 H51 109.5 . . ? H49 C31 H51 109.5 . . ? H50 C31 H51 109.5 . . ? C28 C32 H52 109.5 . . ? C28 C32 H53 109.5 . . ? H52 C32 H53 109.5 . . ? C28 C32 H54 109.5 . . ? H52 C32 H54 109.5 . . ? H53 C32 H54 109.5 . . ? C27 C33 C34 124.3(3) . . ? C27 C33 H55 117.8 . . ? C34 C33 H55 117.8 . . ? C33 C34 C40 117.1(3) . . ? C33 C34 C35 120.5(3) . . ? C40 C34 C35 122.4(2) . . ? C38 C35 C39 107.2(3) . . ? C38 C35 C34 112.3(2) . . ? C39 C35 C34 109.5(2) . . ? C38 C35 C36 108.0(3) . . ? C39 C35 C36 109.1(3) . . ? C34 C35 C36 110.7(2) . . ? C37 C36 C35 115.3(3) . . ? C37 C36 H56 108.4 . . ? C35 C36 H56 108.4 . . ? C37 C36 H57 108.4 . . ? C35 C36 H57 108.4 . . ? H56 C36 H57 107.5 . . ? C36 C37 H58 109.5 . . ? C36 C37 H59 109.5 . . ? H58 C37 H59 109.5 . . ? C36 C37 H60 109.5 . . ? H58 C37 H60 109.5 . . ? H59 C37 H60 109.5 . . ? C35 C38 H61 109.5 . . ? C35 C38 H62 109.5 . . ? H61 C38 H62 109.5 . . ? C35 C38 H63 109.5 . . ? H61 C38 H63 109.5 . . ? H62 C38 H63 109.5 . . ? C35 C39 H64 109.5 . . ? C35 C39 H65 109.5 . . ? H64 C39 H65 109.5 . . ? C35 C39 H66 109.5 . . ? H64 C39 H66 109.5 . . ? H65 C39 H66 109.5 . . ? O2 C40 C25 118.5(2) . . ? O2 C40 C34 122.3(3) . . ? C25 C40 C34 119.1(3) . . ? O4 C41 O3 123.5(3) . . ? O4 C41 C42 119.9(3) . . ? O3 C41 C42 116.5(3) . . ? C41 C42 H67 109.5 . . ? C41 C42 H68 109.5 . . ? H67 C42 H68 109.5 . . ? C41 C42 H69 109.5 . . ? H67 C42 H69 109.5 . . ? H68 C42 H69 109.5 . . ? O5 C43 H70 109.5 . . ? O5 C43 H71 109.5 . . ? H70 C43 H71 109.5 . . ? O5 C43 H72 109.5 . . ? H70 C43 H72 109.5 . . ? H71 C43 H72 109.5 . . ? O6 C44 H74 109.5 . . ? O6 C44 H75 109.5 . . ? H74 C44 H75 109.5 . . ? O6 C44 H76 109.5 . . ? H74 C44 H76 109.5 . . ? H75 C44 H76 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.243 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.074 #===END