# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\gift\struct~2\copyof~1\44co1m3 #TrackingRef '18975_web_deposit_cif_file_0_GiftMehlana_1364469091.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.50 H27.75 Co N2 O7.38' _chemical_formula_weight 551.19 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' 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 tetragonal _symmetry_space_group_name_H-M P4212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z' '-x, -y, z' 'y+1/2, -x+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 'y, x, -z' '-y, -x, -z' _cell_length_a 22.6591(11) _cell_length_b 22.6591(11) _cell_length_c 12.7035(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6522.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2294 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8857 _exptl_absorpt_correction_T_max 0.8953 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43343 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8130 _reflns_number_gt 6087 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1429P)^2^+6.5693P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 8130 _refine_ls_number_parameters 319 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2347 _refine_ls_wR_factor_gt 0.2142 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.25688(2) 0.26245(2) 0.24712(4) 0.02489(17) Uani 1 1 d . . . O15B O 0.28321(16) 0.31553(14) 0.1260(2) 0.0322(7) Uani 1 1 d . . . O14A O 0.20525(14) 0.24737(17) 0.3771(2) 0.0352(7) Uani 1 1 d . . . O15A O 0.16078(14) 0.29198(16) 0.2454(3) 0.0389(7) Uani 1 1 d . . . C13A C 0.1598(2) 0.2719(2) 0.3371(3) 0.0304(9) Uani 1 1 d . . . N1A N -0.16428(16) 0.26085(19) 0.6832(3) 0.0294(8) Uani 1 1 d . . . O14B O 0.27737(18) 0.36030(15) 0.2789(3) 0.0374(8) Uani 1 1 d . . . C10A C 0.1044(2) 0.2762(2) 0.4024(3) 0.0316(10) Uani 1 1 d . . . N1B N 0.26044(18) 0.68707(17) -0.1604(3) 0.0289(8) Uani 1 1 d . . . C10B C 0.2889(2) 0.4200(2) 0.1246(3) 0.0320(10) Uani 1 1 d . . . C7A C 0.0002(2) 0.2768(2) 0.5182(3) 0.0339(10) Uani 1 1 d . . . C9A C 0.1016(2) 0.2464(2) 0.4986(4) 0.0392(11) Uani 1 1 d . . . H9A H 0.1351 0.2259 0.5246 0.047 Uiso 1 1 calc R . . C13B C 0.2839(2) 0.3624(2) 0.1793(3) 0.0293(9) Uani 1 1 d . . . C7B C 0.2862(3) 0.5279(2) 0.0162(4) 0.0361(11) Uani 1 1 d . . . C4B C 0.2788(2) 0.5843(2) -0.0429(3) 0.0337(10) Uani 1 1 d . . . C3A C -0.0568(2) 0.2741(2) 0.5762(4) 0.0327(10) Uani 1 1 d . . . C4A C -0.1100(2) 0.2737(2) 0.5228(3) 0.0341(11) Uani 1 1 d . . . H4A H -0.1107 0.2780 0.4484 0.041 Uiso 1 1 calc R . . C5B C 0.2429(2) 0.6291(2) -0.0055(4) 0.0344(10) Uani 1 1 d . . . H5B H 0.2242 0.6255 0.0611 0.041 Uiso 1 1 calc R . . C8A C 0.0496(2) 0.2471(3) 0.5556(4) 0.0405(12) Uani 1 1 d . . . H8A H 0.0476 0.2271 0.6212 0.049 Uiso 1 1 calc R . . C8B C 0.2976(3) 0.4744(2) -0.0361(4) 0.0395(12) Uani 1 1 d . . . H8B H 0.3046 0.4748 -0.1098 0.047 Uiso 1 1 calc R . . C2B C 0.2959(2) 0.6443(2) -0.1952(3) 0.0347(11) Uani 1 1 d . . . H2B H 0.3144 0.6492 -0.2617 0.042 Uiso 1 1 calc R . . C6A C -0.1623(2) 0.2670(2) 0.5785(4) 0.0327(10) Uani 1 1 d . . . H6A H -0.1984 0.2668 0.5405 0.039 Uiso 1 1 calc R . . C11A C 0.0562(2) 0.3071(2) 0.3666(4) 0.0370(11) Uani 1 1 d . . . H11A H 0.0584 0.3281 0.3020 0.044 Uiso 1 1 calc R . . C6B C 0.2348(2) 0.6789(2) -0.0654(4) 0.0324(10) Uani 1 1 d . . . H6B H 0.2098 0.7091 -0.0388 0.039 Uiso 1 1 calc R . . C2A C -0.1127(2) 0.2638(3) 0.7354(4) 0.0428(12) Uani 1 1 d . . . H2A H -0.1134 0.2616 0.8100 0.051 Uiso 1 1 calc R . . C25 C -0.0590(2) 0.2698(3) 0.6859(4) 0.0455(14) Uani 1 1 d . . . H25 H -0.0237 0.2710 0.7261 0.055 Uiso 1 1 calc R . . C12A C 0.0045(2) 0.3077(3) 0.4245(4) 0.0390(11) Uani 1 1 d . . . H12A H -0.0285 0.3295 0.3997 0.047 Uiso 1 1 calc R . . C11B C 0.2803(3) 0.4730(2) 0.1787(4) 0.0409(12) Uani 1 1 d . . . H11B H 0.2754 0.4725 0.2530 0.049 Uiso 1 1 calc R . . C12B C 0.2787(3) 0.5262(2) 0.1255(4) 0.0426(13) Uani 1 1 d . . . H12B H 0.2725 0.5619 0.1633 0.051 Uiso 1 1 calc R . . C9B C 0.2987(2) 0.4218(2) 0.0167(4) 0.0368(11) Uani 1 1 d . . . H9B H 0.3062 0.3862 -0.0207 0.044 Uiso 1 1 calc R . . C3B C 0.3069(3) 0.5934(2) -0.1397(4) 0.0398(12) Uani 1 1 d . . . H3B H 0.3334 0.5646 -0.1668 0.048 Uiso 1 1 calc R . . OW1 O 0.3801(3) 0.3941(4) 0.3917(5) 0.0463(19) Uani 0.50 1 d P A -21 O1C O 0.1014(4) 0.0875(4) 0.3863(6) 0.121(3) Uiso 1 1 d . . . O1E O 0.8874(4) 0.0169(4) 0.2774(7) 0.136(3) Uiso 1 1 d D . . C2C C 0.0529(6) 0.1145(6) 0.3460(10) 0.119(4) Uiso 1 1 d . . . OW2 O 0.121(2) 0.409(2) 0.159(3) 0.079(12) Uiso 0.13 1 d P . . O1D O 0.1176(7) 0.5597(7) -0.1960(12) 0.113(5) Uiso 0.50 1 d P . . C2D C 0.1104(10) 0.5544(10) -0.0695(18) 0.105(7) Uiso 0.50 1 d P . . C3 C 0.9205(5) 0.0501(5) 0.2040(9) 0.111(4) Uiso 1 1 d D . . OW3 O 1.0000 0.0000 0.1608(15) 0.113(6) Uiso 0.50 2 d SP . . 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 0.0250(3) 0.0280(3) 0.0216(3) -0.0003(2) 0.0002(2) -0.0015(2) O15B 0.0422(19) 0.0254(15) 0.0289(15) -0.0010(12) 0.0036(13) -0.0054(14) O14A 0.0259(16) 0.051(2) 0.0283(15) -0.0028(14) 0.0018(12) 0.0023(15) O15A 0.0324(17) 0.055(2) 0.0290(15) 0.0056(17) 0.0044(15) 0.0046(14) C13A 0.030(2) 0.034(2) 0.027(2) -0.0058(18) 0.0006(17) -0.0033(19) N1A 0.0247(18) 0.037(2) 0.0263(17) 0.0021(15) 0.0026(14) 0.0007(16) O14B 0.052(2) 0.0333(18) 0.0263(15) -0.0001(12) 0.0069(14) 0.0033(16) C10A 0.026(2) 0.039(3) 0.030(2) -0.0037(18) -0.0009(17) -0.0020(19) N1B 0.033(2) 0.0278(18) 0.0256(17) -0.0016(14) -0.0015(15) -0.0008(16) C10B 0.036(3) 0.032(2) 0.028(2) 0.0024(18) -0.0011(18) 0.0018(19) C7A 0.029(2) 0.042(3) 0.030(2) 0.0005(19) 0.0030(17) -0.002(2) C9A 0.032(2) 0.054(3) 0.032(2) 0.005(3) 0.004(2) 0.002(2) C13B 0.033(2) 0.029(2) 0.026(2) 0.0019(17) -0.0010(18) 0.0005(19) C7B 0.051(3) 0.028(2) 0.030(2) 0.0018(18) -0.002(2) 0.003(2) C4B 0.048(3) 0.026(2) 0.027(2) -0.0001(17) -0.001(2) 0.003(2) C3A 0.027(2) 0.042(3) 0.029(2) 0.0017(19) 0.0023(17) -0.003(2) C4A 0.029(2) 0.047(3) 0.026(2) 0.0007(18) 0.0001(16) 0.000(2) C5B 0.045(3) 0.032(2) 0.027(2) -0.0005(18) 0.005(2) 0.003(2) C8A 0.032(2) 0.061(4) 0.029(2) 0.009(2) 0.0013(18) 0.003(2) C8B 0.063(4) 0.032(3) 0.024(2) -0.0017(18) 0.005(2) 0.003(2) C2B 0.044(3) 0.034(2) 0.026(2) 0.0026(18) 0.005(2) 0.002(2) C6A 0.027(2) 0.044(3) 0.027(2) 0.0015(19) -0.0028(17) 0.000(2) C11A 0.033(3) 0.044(3) 0.035(2) 0.009(2) 0.003(2) 0.005(2) C6B 0.040(3) 0.029(2) 0.028(2) -0.0010(17) 0.0051(19) 0.003(2) C2A 0.031(2) 0.072(4) 0.026(2) 0.002(2) 0.0008(18) -0.004(2) C25 0.028(2) 0.081(4) 0.027(2) 0.002(2) -0.0021(18) -0.006(3) C12A 0.028(2) 0.051(3) 0.037(2) 0.009(2) 0.002(2) 0.005(2) C11B 0.069(4) 0.030(2) 0.024(2) 0.0006(17) 0.000(2) 0.000(2) C12B 0.068(4) 0.028(2) 0.031(2) -0.0039(19) 0.004(2) 0.002(2) C9B 0.053(3) 0.028(2) 0.029(2) -0.0028(17) 0.003(2) 0.004(2) C3B 0.054(3) 0.033(3) 0.033(2) 0.0021(19) 0.009(2) 0.013(2) OW1 0.039(4) 0.065(5) 0.036(3) 0.008(3) -0.013(3) -0.018(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 O15B 2.042(3) . ? Co1 O14A 2.052(3) . ? Co1 N1A 2.063(4) 5_556 ? Co1 N1B 2.070(4) 6_545 ? Co1 O15A 2.278(3) . ? Co1 O14B 2.301(4) . ? Co1 C13A 2.489(5) . ? Co1 C13B 2.499(5) . ? O15B C13B 1.259(6) . ? O14A C13A 1.276(6) . ? O15A C13A 1.252(6) . ? C13A C10A 1.507(6) . ? N1A C6A 1.338(6) . ? N1A C2A 1.345(6) . ? N1A Co1 2.063(4) 5_456 ? O14B C13B 1.275(5) . ? C10A C11A 1.374(7) . ? C10A C9A 1.398(7) . ? N1B C2B 1.335(6) . ? N1B C6B 1.353(6) . ? N1B Co1 2.070(4) 6 ? C10B C9B 1.389(6) . ? C10B C11B 1.399(7) . ? C10B C13B 1.483(6) . ? C7A C12A 1.384(7) . ? C7A C8A 1.390(7) . ? C7A C3A 1.488(6) . ? C9A C8A 1.383(7) . ? C7B C12B 1.400(6) . ? C7B C8B 1.406(7) . ? C7B C4B 1.493(6) . ? C4B C5B 1.384(7) . ? C4B C3B 1.400(7) . ? C3A C4A 1.382(7) . ? C3A C25 1.398(6) . ? C4A C6A 1.390(7) . ? C5B C6B 1.373(7) . ? C8B C9B 1.369(7) . ? C2B C3B 1.374(7) . ? C11A C12A 1.384(7) . ? C2A C25 1.377(7) . ? C11B C12B 1.382(7) . ? O1C C2C 1.358(14) . ? O1E C3 1.413(7) . ? O1D C2D 1.62(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O15B Co1 O14A 150.56(15) . . ? O15B Co1 N1A 102.79(15) . 5_556 ? O14A Co1 N1A 96.06(14) . 5_556 ? O15B Co1 N1B 98.06(13) . 6_545 ? O14A Co1 N1B 100.53(15) . 6_545 ? N1A Co1 N1B 100.46(16) 5_556 6_545 ? O15B Co1 O15A 95.67(13) . . ? O14A Co1 O15A 60.79(12) . . ? N1A Co1 O15A 155.13(14) 5_556 . ? N1B Co1 O15A 93.20(15) 6_545 . ? O15B Co1 O14B 60.37(12) . . ? O14A Co1 O14B 97.72(13) . . ? N1A Co1 O14B 89.81(15) 5_556 . ? N1B Co1 O14B 157.92(13) 6_545 . ? O15A Co1 O14B 84.93(14) . . ? O15B Co1 C13A 123.64(15) . . ? O14A Co1 C13A 30.76(14) . . ? N1A Co1 C13A 126.18(15) 5_556 . ? N1B Co1 C13A 98.49(15) 6_545 . ? O15A Co1 C13A 30.04(13) . . ? O14B Co1 C13A 90.87(14) . . ? O15B Co1 C13B 30.11(13) . . ? O14A Co1 C13B 124.60(15) . . ? N1A Co1 C13B 99.68(16) 5_556 . ? N1B Co1 C13B 127.63(15) 6_545 . ? O15A Co1 C13B 87.96(14) . . ? O14B Co1 C13B 30.44(13) . . ? C13A Co1 C13B 107.28(16) . . ? C13B O15B Co1 95.4(3) . . ? C13A O14A Co1 93.9(3) . . ? C13A O15A Co1 84.3(3) . . ? O15A C13A O14A 121.0(4) . . ? O15A C13A C10A 120.2(4) . . ? O14A C13A C10A 118.8(4) . . ? O15A C13A Co1 65.6(2) . . ? O14A C13A Co1 55.4(2) . . ? C10A C13A Co1 173.9(3) . . ? C6A N1A C2A 117.1(4) . . ? C6A N1A Co1 118.8(3) . 5_456 ? C2A N1A Co1 123.6(3) . 5_456 ? C13B O14B Co1 83.4(3) . . ? C11A C10A C9A 120.0(4) . . ? C11A C10A C13A 120.8(4) . . ? C9A C10A C13A 119.2(4) . . ? C2B N1B C6B 117.1(4) . . ? C2B N1B Co1 122.5(3) . 6 ? C6B N1B Co1 120.4(3) . 6 ? C9B C10B C11B 118.9(4) . . ? C9B C10B C13B 120.0(4) . . ? C11B C10B C13B 121.0(4) . . ? C12A C7A C8A 118.8(5) . . ? C12A C7A C3A 120.5(5) . . ? C8A C7A C3A 120.6(4) . . ? C8A C9A C10A 119.4(5) . . ? O15B C13B O14B 120.1(4) . . ? O15B C13B C10B 119.4(4) . . ? O14B C13B C10B 120.4(4) . . ? O15B C13B Co1 54.4(2) . . ? O14B C13B Co1 66.2(3) . . ? C10B C13B Co1 168.0(3) . . ? C12B C7B C8B 117.9(4) . . ? C12B C7B C4B 120.5(4) . . ? C8B C7B C4B 121.5(4) . . ? C5B C4B C3B 117.5(4) . . ? C5B C4B C7B 121.5(4) . . ? C3B C4B C7B 121.1(4) . . ? C4A C3A C25 117.3(4) . . ? C4A C3A C7A 120.9(4) . . ? C25 C3A C7A 121.8(4) . . ? C3A C4A C6A 119.6(4) . . ? C6B C5B C4B 119.4(4) . . ? C9A C8A C7A 120.8(5) . . ? C9B C8B C7B 121.5(4) . . ? N1B C2B C3B 123.3(4) . . ? N1A C6A C4A 123.1(4) . . ? C10A C11A C12A 120.1(4) . . ? N1B C6B C5B 123.4(4) . . ? N1A C2A C25 123.2(4) . . ? C2A C25 C3A 119.6(5) . . ? C7A C12A C11A 120.8(5) . . ? C12B C11B C10B 120.8(4) . . ? C11B C12B C7B 120.4(5) . . ? C8B C9B C10B 120.4(4) . . ? C2B C3B C4B 119.4(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.063 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.147 _database_code_depnum_ccdc_archive 'CCDC 931535' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\gift\struct~2\co6cf7~1\44co1m #TrackingRef '18976_web_deposit_cif_file_1_GiftMehlana_1364469091.3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H57.90 Co2 N4 O16.35' _chemical_formula_weight 1154.41 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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 17.0218(5) _cell_length_b 10.5990(3) _cell_length_c 18.3064(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.0730(10) _cell_angle_gamma 90.00 _cell_volume 3173.63(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1201 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7788 _exptl_absorpt_correction_T_max 0.8938 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57343 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.29 _reflns_number_total 15725 _reflns_number_gt 12839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1258P)^2^+2.4973P] 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 0.00 _refine_ls_number_reflns 15725 _refine_ls_number_parameters 715 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.075 _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 0.88120(8) 0.46505(3) 0.39724(8) 0.01990(11) Uani 1 1 d . . . Co2 Co 1.13118(9) 0.49991(12) 1.14716(8) 0.01940(11) Uani 1 1 d . . . O1 O 0.8051(3) 0.3193(5) 0.4250(3) 0.0303(12) Uani 1 1 d . . . O2 O 0.9569(3) 0.3205(5) 0.3692(3) 0.0269(11) Uani 1 1 d . . . O15D O 0.8033(3) 0.4642(5) 0.2900(3) 0.0287(13) Uani 1 1 d . . . O4 O 1.0012(3) 0.5175(5) 1.1289(3) 0.0325(13) Uani 1 1 d . . . O15C O 0.9602(3) 0.4623(5) 0.5048(3) 0.0269(12) Uani 1 1 d . . . O6 O 1.2614(3) 0.4843(5) 1.1649(3) 0.0245(11) Uani 1 1 d . . . O15A O 1.1255(3) 0.3102(5) 1.1594(3) 0.0312(12) Uani 1 1 d . . . O15B O 1.1372(3) 0.6905(4) 1.1356(3) 0.0244(11) Uani 1 1 d . . . N1D N 0.6526(4) 0.4744(6) -0.2327(3) 0.0238(13) Uani 1 1 d . . . N1A N 0.9499(3) -0.3881(6) 1.3628(3) 0.0263(13) Uani 1 1 d . . . N1B N 1.3132(3) 1.3896(5) 0.9322(3) 0.0231(12) Uani 1 1 d . . . N1C N 1.1091(3) 0.4722(6) 1.0254(3) 0.0216(12) Uani 1 1 d . . . O14C O 1.0269(3) 0.2821(6) 0.5154(3) 0.0363(13) Uani 1 1 d . . . O14B O 1.0119(3) 0.7335(6) 1.0627(3) 0.0388(14) Uani 1 1 d . . . O14A O 1.2510(3) 0.2594(5) 1.2307(3) 0.0349(13) Uani 1 1 d . . . O14D O 0.7363(3) 0.2784(6) 0.2812(3) 0.0395(15) Uani 1 1 d . . . C9C C 1.0326(5) 0.5118(8) 0.6593(4) 0.0297(18) Uani 1 1 d . . . H9C H 1.0261 0.5843 0.6276 0.045 Uiso 1 1 calc R . . C8B C 1.1232(5) 1.0241(8) 0.9610(4) 0.0340(17) Uani 1 1 d . . . H8B H 1.0992 1.0548 0.9111 0.051 Uiso 1 1 calc R . . C3D C 0.6366(4) 0.5367(7) -0.1118(4) 0.0250(16) Uani 1 1 d . . . H3D H 0.6123 0.5938 -0.0844 0.038 Uiso 1 1 calc R . . C13B C 1.0869(4) 0.7565(7) 1.0881(4) 0.0247(15) Uani 1 1 d . . . C13A C 1.1756(4) 0.2387(7) 1.2062(4) 0.0250(15) Uani 1 1 d . . . C4C C 1.0766(4) 0.4369(7) 0.8675(4) 0.0242(14) Uani 1 1 d . . . C7A C 1.0671(4) -0.0770(7) 1.2860(4) 0.0264(15) Uani 1 1 d . . . C7B C 1.1956(5) 1.0777(7) 1.0066(4) 0.0279(16) Uani 1 1 d . . . C13C C 1.0017(4) 0.3755(8) 0.5416(4) 0.0283(16) Uani 1 1 d . . . C13D C 0.7572(4) 0.3774(7) 0.2516(4) 0.0240(14) Uani 1 1 d . . . C6C C 1.0645(4) 0.3776(7) 0.9901(4) 0.0255(15) Uani 1 1 d . . . H6C H 1.0439 0.3188 1.0195 0.038 Uiso 1 1 calc R . . C10C C 1.0256(4) 0.3928(7) 0.6275(4) 0.0244(15) Uani 1 1 d . . . C6D C 0.6999(4) 0.3751(8) -0.1961(4) 0.0305(17) Uani 1 1 d . . . H6D H 0.7220 0.3183 -0.2253 0.046 Uiso 1 1 calc R . . C10B C 1.1237(4) 0.8754(7) 1.0611(4) 0.0268(15) Uani 1 1 d . . . C10A C 1.1406(4) 0.1304(7) 1.2343(4) 0.0236(14) Uani 1 1 d . . . C2D C 0.6222(4) 0.5504(7) -0.1896(4) 0.0263(16) Uani 1 1 d . . . H2D H 0.5884 0.6183 -0.2137 0.039 Uiso 1 1 calc R . . C3C C 1.1252(5) 0.5404(8) 0.9048(4) 0.0306(18) Uani 1 1 d . . . H3C H 1.1472 0.5997 0.8768 0.046 Uiso 1 1 calc R . . C4D C 0.6846(4) 0.4430(8) -0.0747(4) 0.0279(16) Uani 1 1 d . . . C7C C 1.0614(4) 0.4204(9) 0.7844(4) 0.0301(17) Uani 1 1 d . . . C12B C 1.2308(5) 1.0257(7) 1.0802(4) 0.0285(16) Uani 1 1 d . . . H12B H 1.2791 1.0622 1.1124 0.043 Uiso 1 1 calc R . . C5C C 1.0456(4) 0.3591(8) 0.9109(4) 0.0290(16) Uani 1 1 d . . . H5C H 1.0109 0.2914 0.8880 0.043 Uiso 1 1 calc R . . C10D C 0.7341(4) 0.3921(8) 0.1670(4) 0.0271(16) Uani 1 1 d . . . C5D C 0.7160(5) 0.3553(8) -0.1201(4) 0.0331(17) Uani 1 1 d . . . H5D H 0.7475 0.2846 -0.0970 0.050 Uiso 1 1 calc R . . C9A C 1.0678(5) 0.0800(7) 1.1895(5) 0.0307(17) Uani 1 1 d . . . H9A H 1.0420 0.1160 1.1414 0.046 Uiso 1 1 calc R . . C4B C 1.2346(4) 1.1872(7) 0.9805(4) 0.0265(15) Uani 1 1 d . . . C8C C 1.0490(5) 0.5258(8) 0.7372(5) 0.0304(17) Uani 1 1 d . . . H8C H 1.0519 0.6079 0.7587 0.046 Uiso 1 1 calc R . . C4A C 1.0272(4) -0.1839(7) 1.3138(4) 0.0264(15) Uani 1 1 d . . . C12D C 0.7077(5) 0.3017(8) 0.0419(4) 0.0339(18) Uani 1 1 d . . . H12D H 0.6996 0.2289 0.0104 0.051 Uiso 1 1 calc R . . C7D C 0.7023(4) 0.4241(7) 0.0092(4) 0.0251(15) Uani 1 1 d . . . C11B C 1.1967(4) 0.9262(7) 1.1044(4) 0.0262(15) Uani 1 1 d . . . H11B H 1.2231 0.8897 1.1524 0.039 Uiso 1 1 calc R . . C8D C 0.7111(5) 0.5281(8) 0.0572(4) 0.0308(18) Uani 1 1 d . . . H8D H 0.7028 0.6106 0.0361 0.046 Uiso 1 1 calc R . . C8A C 1.0316(5) -0.0265(7) 1.2161(4) 0.0285(17) Uani 1 1 d . . . H8A H 0.9826 -0.0621 1.1848 0.043 Uiso 1 1 calc R . . C12C C 1.0569(6) 0.3038(8) 0.7538(4) 0.042(2) Uani 1 1 d . . . H12C H 1.0644 0.2322 0.7862 0.063 Uiso 1 1 calc R . . C2A C 0.9515(4) -0.3823(7) 1.2900(4) 0.0275(15) Uani 1 1 d . . . H2A H 0.9256 -0.4464 1.2553 0.041 Uiso 1 1 calc R . . C2C C 1.1398(4) 0.5525(8) 0.9836(4) 0.0257(16) Uani 1 1 d . . . H2C H 1.1730 0.6204 1.0086 0.039 Uiso 1 1 calc R . . C5A C 1.0274(5) -0.1969(7) 1.3892(4) 0.0302(17) Uani 1 1 d . . . H5A H 1.0553 -0.1376 1.4263 0.045 Uiso 1 1 calc R . . C3B C 1.2733(5) 1.2794(7) 1.0303(5) 0.0287(16) Uani 1 1 d . . . H3B H 1.2745 1.2754 1.0824 0.043 Uiso 1 1 calc R . . C9D C 0.7320(5) 0.5126(8) 0.1361(4) 0.0284(17) Uani 1 1 d . . . H9D H 0.7447 0.5840 0.1686 0.043 Uiso 1 1 calc R . . C9B C 1.0861(5) 0.9226(7) 0.9909(5) 0.0327(18) Uani 1 1 d . . . H9B H 1.0355 0.8883 0.9619 0.049 Uiso 1 1 calc R . . C6A C 0.9850(5) -0.3007(8) 1.4102(4) 0.0312(17) Uani 1 1 d . . . H6A H 0.9823 -0.3061 1.4613 0.047 Uiso 1 1 calc R . . C3A C 0.9912(5) -0.2821(8) 1.2648(5) 0.0320(18) Uani 1 1 d . . . H3A H 0.9936 -0.2808 1.2136 0.048 Uiso 1 1 calc R . . C5B C 1.2381(5) 1.1962(8) 0.9045(4) 0.0320(17) Uani 1 1 d . . . H5B H 1.2153 1.1314 0.8691 0.048 Uiso 1 1 calc R . . C11D C 0.7251(5) 0.2893(9) 0.1209(5) 0.040(2) Uani 1 1 d . . . H11D H 0.7307 0.2074 0.1428 0.060 Uiso 1 1 calc R . . C11C C 1.0414(5) 0.2860(8) 0.6756(4) 0.0321(17) Uani 1 1 d . . . H11C H 1.0415 0.2037 0.6550 0.048 Uiso 1 1 calc R . . C62 C 1.3260(3) 0.5710(4) 1.1908(3) 0.0269(9) Uani 1 1 d . . . H62A H 1.3067 0.6562 1.1743 0.040 Uiso 1 1 calc R . . H62B H 1.3712 0.5486 1.1698 0.040 Uiso 1 1 calc R . . H62C H 1.3450 0.5683 1.2465 0.040 Uiso 1 1 calc R . . C11A C 1.1766(5) 0.0707(9) 1.3056(5) 0.041(2) Uani 1 1 d . . . H11A H 1.2266 0.1026 1.3373 0.061 Uiso 1 1 calc R . . C6B C 1.2736(4) 1.2958(7) 0.8828(4) 0.0292(16) Uani 1 1 d . . . H6B H 1.2716 1.3031 0.8306 0.044 Uiso 1 1 calc R . . C12A C 1.1419(6) -0.0287(9) 1.3288(5) 0.046(2) Uani 1 1 d . . . H12A H 1.1688 -0.0675 1.3759 0.069 Uiso 1 1 calc R . . C66 C 0.9420(5) 0.2197(9) 0.3173(5) 0.049(2) Uani 1 1 d . . . H66A H 0.8957 0.1699 0.3233 0.074 Uiso 1 1 calc R . . H66B H 0.9907 0.1660 0.3270 0.074 Uiso 1 1 calc R . . H66C H 0.9293 0.2529 0.2653 0.074 Uiso 1 1 calc R . . C67 C 0.8221(6) 0.2169(8) 0.4774(5) 0.043(2) Uani 1 1 d . . . H67A H 0.8450 0.1464 0.4554 0.064 Uiso 1 1 calc R . . H67B H 0.7714 0.1899 0.4883 0.064 Uiso 1 1 calc R . . H67C H 0.8616 0.2441 0.5247 0.064 Uiso 1 1 calc R . . C69 C 0.9297(9) 0.407(2) 1.0961(9) 0.229(13) Uani 1 1 d . . . H69A H 0.9009 0.4246 1.0429 0.344 Uiso 1 1 calc R . . H69B H 0.8906 0.4070 1.1266 0.344 Uiso 1 1 calc R . . H69C H 0.9558 0.3237 1.0997 0.344 Uiso 1 1 calc R . . O1E O 1.0351(6) -0.1267(14) 1.5734(7) 0.080(5) Uani 0.50 1 d PD . . H1E H 1.0658 -0.1062 1.6161 0.119 Uiso 0.50 1 calc PR . . C2E C 0.9568(6) -0.0775(15) 1.5649(14) 0.089(9) Uani 0.50 1 d PD . . H2E1 H 0.9511 -0.0526 1.6148 0.134 Uiso 0.50 1 calc PR . . H2E2 H 0.9158 -0.1418 1.5426 0.134 Uiso 0.50 1 calc PR . . H2E3 H 0.9485 -0.0036 1.5314 0.134 Uiso 0.50 1 calc PR . . O1G O 1.3313(4) -0.0653(9) 1.4476(4) 0.054(2) Uani 0.50 1 d PD . . H1G H 1.3443 0.0104 1.4438 0.080 Uiso 0.50 1 calc PR . . C2B C 1.3099(5) 1.3770(7) 1.0036(4) 0.0302(16) Uani 1 1 d . . . H2B H 1.3349 1.4408 1.0388 0.045 Uiso 1 1 calc R . . C2G C 1.3955(6) -0.1277(15) 1.4976(9) 0.079(5) Uani 0.50 1 d PD . . H2G1 H 1.4187 -0.0740 1.5419 0.118 Uiso 0.50 1 calc PR . . H2G2 H 1.4377 -0.1469 1.4721 0.118 Uiso 0.50 1 calc PR . . H2G3 H 1.3755 -0.2064 1.5141 0.118 Uiso 0.50 1 calc PR . . C1K C 0.5940(6) 0.1691(10) 0.2198(6) 0.063(2) Uiso 0.70 1 d P . . O3 O 0.9001(13) 0.1274(19) 0.8289(12) 0.058(4) Uiso 0.25 1 d P A -21 O5 O 1.3890(10) 0.0905(16) 0.5389(9) 0.052(4) Uiso 0.25 1 d P . . O7 O 0.8593(10) 0.6488(17) 0.9073(10) 0.058(4) Uiso 0.25 1 d P B 21 O8 O 0.8900(11) -0.2069(17) 0.8422(10) 0.100(5) Uiso 0.40 1 d P . . O9 O 1.1406(5) 0.0900(9) 0.5640(5) 0.119(3) Uiso 1 1 d . . . O10 O 1.2219(9) 0.1095(16) 0.7140(9) 0.084(5) Uiso 0.50 1 d P . . C11 C 1.3060(11) 0.064(2) 0.7308(11) 0.063(5) Uiso 0.50 1 d P . . O12 O 0.6494(6) 0.0433(10) 0.2657(6) 0.092(3) Uiso 0.70 1 d P . . C5 C 1.3324(15) 0.158(3) 0.5161(15) 0.236(10) 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 0.02560(19) 0.02165(19) 0.01202(17) 0.0001(5) 0.00451(13) 0.0000(5) Co2 0.02371(19) 0.02020(19) 0.01397(17) 0.00178(12) 0.00466(13) -0.00247(12) O1 0.041(3) 0.027(3) 0.022(3) 0.001(2) 0.008(2) -0.007(2) O2 0.028(2) 0.030(3) 0.024(3) -0.006(2) 0.009(2) 0.000(2) O15D 0.036(3) 0.028(3) 0.018(3) 0.002(2) 0.001(2) 0.002(2) O4 0.023(3) 0.041(3) 0.036(3) -0.008(3) 0.011(2) -0.006(2) O15C 0.033(3) 0.031(3) 0.013(2) 0.003(2) 0.000(2) 0.005(2) O6 0.025(3) 0.025(2) 0.022(2) 0.004(2) 0.003(2) -0.0019(19) O15A 0.036(3) 0.027(3) 0.025(3) 0.009(2) 0.000(2) 0.002(2) O15B 0.038(3) 0.017(2) 0.018(2) -0.0029(19) 0.0070(19) -0.009(2) N1D 0.030(3) 0.027(3) 0.012(3) 0.002(2) 0.002(2) 0.000(2) N1A 0.026(3) 0.033(3) 0.023(3) 0.009(3) 0.012(2) 0.000(3) N1B 0.032(3) 0.017(3) 0.019(3) -0.004(2) 0.004(2) 0.002(2) N1C 0.021(3) 0.028(3) 0.018(3) 0.003(3) 0.008(2) -0.001(2) O14C 0.046(3) 0.035(3) 0.025(3) -0.001(2) 0.006(2) 0.005(2) O14B 0.035(3) 0.034(3) 0.045(3) 0.017(3) 0.006(2) 0.001(2) O14A 0.028(3) 0.030(3) 0.044(3) 0.009(2) 0.005(2) -0.003(2) O14D 0.047(3) 0.052(3) 0.015(2) 0.002(2) 0.001(2) -0.026(3) C9C 0.037(4) 0.030(4) 0.021(4) 0.000(3) 0.008(3) -0.005(3) C8B 0.038(4) 0.032(4) 0.029(4) 0.008(3) 0.005(3) -0.011(3) C3D 0.026(4) 0.032(4) 0.018(3) -0.005(3) 0.008(3) 0.007(3) C13B 0.034(4) 0.018(3) 0.023(4) 0.002(3) 0.010(3) -0.003(3) C13A 0.030(4) 0.024(3) 0.021(3) -0.001(3) 0.007(3) 0.001(3) C4C 0.025(3) 0.026(3) 0.018(3) -0.001(3) 0.000(3) 0.000(3) C7A 0.031(4) 0.023(4) 0.026(4) 0.002(3) 0.010(3) -0.004(3) C7B 0.034(4) 0.024(4) 0.027(4) 0.005(3) 0.011(3) 0.008(3) C13C 0.025(3) 0.047(4) 0.013(3) -0.007(3) 0.005(3) -0.005(3) C13D 0.025(3) 0.025(3) 0.020(3) -0.007(3) 0.002(3) 0.000(3) C6C 0.028(3) 0.029(4) 0.021(3) 0.005(3) 0.008(3) 0.000(3) C10C 0.022(3) 0.033(4) 0.017(3) 0.004(3) 0.003(2) 0.004(3) C6D 0.040(4) 0.032(4) 0.017(3) 0.001(3) 0.004(3) 0.013(3) C10B 0.034(4) 0.021(3) 0.027(4) 0.004(3) 0.010(3) -0.001(3) C10A 0.027(3) 0.021(3) 0.024(3) 0.002(3) 0.009(3) 0.004(3) C2D 0.034(4) 0.027(4) 0.019(3) 0.002(3) 0.008(3) 0.012(3) C3C 0.034(4) 0.040(5) 0.018(3) 0.001(3) 0.008(3) -0.003(3) C4D 0.030(4) 0.042(4) 0.012(3) -0.001(3) 0.006(3) -0.002(3) C7C 0.025(3) 0.048(5) 0.017(3) 0.006(3) 0.005(3) -0.002(3) C12B 0.032(4) 0.029(4) 0.023(4) 0.000(3) 0.006(3) 0.005(3) C5C 0.033(4) 0.032(4) 0.018(3) -0.008(3) 0.002(3) -0.007(3) C10D 0.026(3) 0.039(4) 0.016(3) 0.003(3) 0.003(3) 0.002(3) C5D 0.041(4) 0.036(4) 0.019(3) -0.006(3) 0.003(3) 0.012(3) C9A 0.040(4) 0.023(3) 0.026(4) 0.004(3) 0.005(3) -0.002(3) C4B 0.031(4) 0.030(4) 0.021(3) 0.007(3) 0.013(3) 0.002(3) C8C 0.028(4) 0.035(4) 0.026(4) -0.004(3) 0.005(3) -0.003(3) C4A 0.028(3) 0.018(3) 0.031(4) 0.002(3) 0.005(3) 0.000(3) C12D 0.047(4) 0.031(4) 0.019(3) 0.001(3) 0.001(3) 0.009(3) C7D 0.028(3) 0.028(3) 0.017(3) 0.005(3) 0.001(3) 0.002(3) C11B 0.036(4) 0.026(3) 0.016(3) 0.001(3) 0.007(3) -0.002(3) C8D 0.046(5) 0.032(4) 0.014(3) -0.001(3) 0.007(3) 0.001(3) C8A 0.038(4) 0.025(3) 0.023(4) 0.001(3) 0.008(3) -0.011(3) C12C 0.070(6) 0.037(4) 0.017(4) 0.010(3) 0.007(4) 0.014(4) C2A 0.037(4) 0.029(3) 0.018(3) 0.005(3) 0.009(3) 0.003(3) C2C 0.023(3) 0.034(4) 0.020(3) 0.000(3) 0.006(3) 0.000(3) C5A 0.038(4) 0.023(3) 0.024(4) 0.000(3) 0.001(3) -0.009(3) C3B 0.042(4) 0.024(4) 0.027(4) 0.000(3) 0.021(3) 0.000(3) C9D 0.030(4) 0.037(4) 0.015(3) -0.005(3) 0.001(3) -0.002(3) C9B 0.030(3) 0.025(3) 0.039(4) 0.017(3) 0.003(3) -0.004(3) C6A 0.040(4) 0.031(4) 0.025(4) 0.003(3) 0.013(3) -0.008(3) C3A 0.048(5) 0.028(4) 0.023(4) -0.001(3) 0.015(3) -0.003(3) C5B 0.037(4) 0.038(4) 0.022(4) 0.001(3) 0.008(3) -0.007(3) C11D 0.056(5) 0.040(5) 0.022(4) 0.001(3) 0.008(3) -0.005(4) C11C 0.043(4) 0.030(4) 0.016(3) 0.000(3) -0.005(3) 0.003(3) C62 0.0178(19) 0.0270(19) 0.034(2) -0.0109(17) 0.0044(16) -0.0165(16) C11A 0.036(4) 0.047(5) 0.031(4) 0.012(4) -0.003(3) -0.008(4) C6B 0.034(3) 0.032(4) 0.016(3) -0.001(3) -0.002(3) -0.003(3) C12A 0.040(4) 0.045(5) 0.041(4) 0.027(4) -0.008(3) 0.001(4) C66 0.039(4) 0.054(5) 0.048(5) -0.031(4) 0.003(4) 0.005(4) C67 0.058(5) 0.033(4) 0.037(4) 0.008(4) 0.015(4) -0.008(4) C69 0.124(11) 0.47(4) 0.124(11) 0.092(16) 0.076(9) 0.187(18) O1E 0.048(5) 0.099(9) 0.064(6) -0.017(6) -0.032(4) 0.054(6) C2E 0.026(5) 0.036(7) 0.168(19) -0.034(8) -0.035(7) 0.021(5) O1G 0.028(3) 0.081(6) 0.039(4) -0.006(4) -0.013(3) 0.013(4) C2B 0.046(4) 0.022(3) 0.028(4) -0.012(3) 0.020(3) -0.009(3) C2G 0.025(5) 0.100(11) 0.095(10) 0.074(9) -0.011(6) -0.009(6) _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 O15D 2.043(5) . ? Co1 O15C 2.054(5) . ? Co1 N1B 2.128(6) 2_474 ? Co1 N1A 2.143(6) 1_564 ? Co1 O2 2.153(5) . ? Co1 O1 2.165(5) . ? Co2 O15A 2.029(5) . ? Co2 O15B 2.037(5) . ? Co2 N1D 2.145(6) 2_566 ? Co2 O4 2.153(5) . ? Co2 O6 2.156(5) . ? Co2 N1C 2.174(6) . ? O1 C67 1.424(9) . ? O2 C66 1.406(9) . ? O15D C13D 1.284(8) . ? O4 C69 1.68(2) . ? O15C C13C 1.240(9) . ? O6 C62 1.411(6) . ? O15A C13A 1.276(8) . ? O15B C13B 1.252(8) . ? N1D C2D 1.328(10) . ? N1D C6D 1.380(9) . ? N1D Co2 2.145(6) 2_463 ? N1A C6A 1.296(10) . ? N1A C2A 1.343(9) . ? N1A Co1 2.143(6) 1_546 ? N1B C2B 1.332(10) . ? N1B C6B 1.388(9) . ? N1B Co1 2.128(6) 2_575 ? N1C C6C 1.314(9) . ? N1C C2C 1.344(9) . ? O14C C13C 1.229(9) . ? O14B C13B 1.256(9) . ? O14A C13A 1.257(9) . ? O14D C13D 1.276(9) . ? C9C C10C 1.381(11) . ? C9C C8C 1.383(11) . ? C8B C7B 1.403(11) . ? C8B C9B 1.431(10) . ? C3D C4D 1.344(10) . ? C3D C2D 1.386(10) . ? C13B C10B 1.548(10) . ? C13A C10A 1.450(10) . ? C4C C5C 1.350(11) . ? C4C C3C 1.429(10) . ? C4C C7C 1.481(10) . ? C7A C8A 1.366(10) . ? C7A C12A 1.394(12) . ? C7A C4A 1.482(10) . ? C7B C12B 1.425(10) . ? C7B C4B 1.480(10) . ? C13C C10C 1.522(10) . ? C13D C10D 1.497(10) . ? C6C C5C 1.409(9) . ? C10C C11C 1.413(11) . ? C6D C5D 1.359(10) . ? C10B C9B 1.362(10) . ? C10B C11B 1.385(10) . ? C10A C9A 1.390(10) . ? C10A C11A 1.427(10) . ? C3C C2C 1.400(10) . ? C4D C5D 1.445(11) . ? C4D C7D 1.493(9) . ? C7C C12C 1.351(12) . ? C7C C8C 1.393(11) . ? C12B C11B 1.338(11) . ? C10D C11D 1.360(12) . ? C10D C9D 1.393(11) . ? C9A C8A 1.432(10) . ? C4B C3B 1.373(11) . ? C4B C5B 1.413(10) . ? C4A C5A 1.388(11) . ? C4A C3A 1.399(10) . ? C12D C11D 1.401(11) . ? C12D C7D 1.421(11) . ? C7D C8D 1.392(11) . ? C8D C9D 1.399(10) . ? C12C C11C 1.394(11) . ? C2A C3A 1.404(11) . ? C5A C6A 1.426(10) . ? C3B C2B 1.365(10) . ? C5B C6B 1.330(11) . ? C11A C12A 1.334(13) . ? O1E C2E 1.400(5) . ? O1G C2G 1.384(5) . ? C1K O12 1.713(14) . ? O5 C5 1.18(3) . ? O10 C11 1.46(2) . ? 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 O15D Co1 O15C 178.87(14) . . ? O15D Co1 N1B 91.7(2) . 2_474 ? O15C Co1 N1B 89.3(2) . 2_474 ? O15D Co1 N1A 89.0(2) . 1_564 ? O15C Co1 N1A 91.5(2) . 1_564 ? N1B Co1 N1A 87.05(10) 2_474 1_564 ? O15D Co1 O2 92.3(2) . . ? O15C Co1 O2 86.7(2) . . ? N1B Co1 O2 175.9(2) 2_474 . ? N1A Co1 O2 92.1(2) 1_564 . ? O15D Co1 O1 87.2(2) . . ? O15C Co1 O1 92.3(2) . . ? N1B Co1 O1 92.0(2) 2_474 . ? N1A Co1 O1 176.0(2) 1_564 . ? O2 Co1 O1 89.13(9) . . ? O15A Co2 O15B 179.6(3) . . ? O15A Co2 N1D 90.7(2) . 2_566 ? O15B Co2 N1D 88.9(2) . 2_566 ? O15A Co2 O4 91.4(2) . . ? O15B Co2 O4 88.7(2) . . ? N1D Co2 O4 91.4(2) 2_566 . ? O15A Co2 O6 89.2(2) . . ? O15B Co2 O6 90.74(19) . . ? N1D Co2 O6 88.8(2) 2_566 . ? O4 Co2 O6 179.4(3) . . ? O15A Co2 N1C 88.8(2) . . ? O15B Co2 N1C 91.6(2) . . ? N1D Co2 N1C 179.5(3) 2_566 . ? O4 Co2 N1C 88.5(2) . . ? O6 Co2 N1C 91.3(2) . . ? C67 O1 Co1 132.7(5) . . ? C66 O2 Co1 134.0(5) . . ? C13D O15D Co1 131.6(5) . . ? C69 O4 Co2 127.4(6) . . ? C13C O15C Co1 131.0(5) . . ? C62 O6 Co2 132.3(4) . . ? C13A O15A Co2 128.3(5) . . ? C13B O15B Co2 125.6(5) . . ? C2D N1D C6D 116.4(6) . . ? C2D N1D Co2 123.2(5) . 2_463 ? C6D N1D Co2 120.4(5) . 2_463 ? C6A N1A C2A 120.0(7) . . ? C6A N1A Co1 120.7(5) . 1_546 ? C2A N1A Co1 119.2(5) . 1_546 ? C2B N1B C6B 115.0(6) . . ? C2B N1B Co1 122.9(5) . 2_575 ? C6B N1B Co1 122.0(5) . 2_575 ? C6C N1C C2C 117.8(6) . . ? C6C N1C Co2 121.3(5) . . ? C2C N1C Co2 120.9(5) . . ? C10C C9C C8C 120.1(8) . . ? C7B C8B C9B 119.0(7) . . ? C4D C3D C2D 120.5(7) . . ? O15B C13B O14B 125.3(7) . . ? O15B C13B C10B 114.7(6) . . ? O14B C13B C10B 120.0(6) . . ? O14A C13A O15A 124.1(7) . . ? O14A C13A C10A 119.4(6) . . ? O15A C13A C10A 116.4(6) . . ? C5C C4C C3C 117.1(7) . . ? C5C C4C C7C 123.2(7) . . ? C3C C4C C7C 119.7(7) . . ? C8A C7A C12A 118.8(7) . . ? C8A C7A C4A 119.7(7) . . ? C12A C7A C4A 121.5(7) . . ? C8B C7B C12B 118.4(7) . . ? C8B C7B C4B 121.6(7) . . ? C12B C7B C4B 120.0(7) . . ? O14C C13C O15C 126.4(6) . . ? O14C C13C C10C 118.6(7) . . ? O15C C13C C10C 115.0(7) . . ? O14D C13D O15D 123.8(6) . . ? O14D C13D C10D 120.1(6) . . ? O15D C13D C10D 115.9(7) . . ? N1C C6C C5C 123.2(7) . . ? C9C C10C C11C 119.4(7) . . ? C9C C10C C13C 120.8(7) . . ? C11C C10C C13C 119.8(7) . . ? C5D C6D N1D 122.7(7) . . ? C9B C10B C11B 120.7(7) . . ? C9B C10B C13B 118.3(6) . . ? C11B C10B C13B 120.8(7) . . ? C9A C10A C11A 117.1(7) . . ? C9A C10A C13A 118.8(6) . . ? C11A C10A C13A 124.1(7) . . ? N1D C2D C3D 124.1(7) . . ? C2C C3C C4C 118.5(7) . . ? C3D C4D C5D 117.0(6) . . ? C3D C4D C7D 122.7(7) . . ? C5D C4D C7D 120.2(7) . . ? C12C C7C C8C 119.7(7) . . ? C12C C7C C4C 120.6(7) . . ? C8C C7C C4C 119.7(8) . . ? C11B C12B C7B 120.7(7) . . ? C4C C5C C6C 120.4(7) . . ? C11D C10D C9D 119.8(7) . . ? C11D C10D C13D 120.7(7) . . ? C9D C10D C13D 119.0(7) . . ? C6D C5D C4D 119.2(7) . . ? C10A C9A C8A 120.0(7) . . ? C3B C4B C5B 117.6(7) . . ? C3B C4B C7B 121.3(7) . . ? C5B C4B C7B 121.0(7) . . ? C9C C8C C7C 120.4(8) . . ? C5A C4A C3A 116.4(7) . . ? C5A C4A C7A 122.8(7) . . ? C3A C4A C7A 120.7(7) . . ? C11D C12D C7D 119.4(8) . . ? C8D C7D C12D 118.3(7) . . ? C8D C7D C4D 119.8(7) . . ? C12D C7D C4D 121.8(7) . . ? C12B C11B C10B 121.3(7) . . ? C7D C8D C9D 120.7(8) . . ? C7A C8A C9A 120.5(7) . . ? C7C C12C C11C 121.5(8) . . ? N1A C2A C3A 120.3(7) . . ? N1C C2C C3C 122.9(7) . . ? C4A C5A C6A 118.9(7) . . ? C2B C3B C4B 118.9(7) . . ? C10D C9D C8D 119.9(7) . . ? C10B C9B C8B 119.7(7) . . ? N1A C6A C5A 123.0(7) . . ? C4A C3A C2A 121.2(8) . . ? C6B C5B C4B 119.6(8) . . ? C10D C11D C12D 121.4(8) . . ? C12C C11C C10C 118.7(7) . . ? C12A C11A C10A 121.8(8) . . ? C5B C6B N1B 123.6(7) . . ? C11A C12A C7A 121.8(7) . . ? N1B C2B C3B 125.1(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.396 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.132 _database_code_depnum_ccdc_archive 'CCDC 931536' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c:\gift\struct~2\copy(2~1\44co1mdy #TrackingRef '18977_web_deposit_cif_file_2_GiftMehlana_1364469091.4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.40 H24.20 Co N2 O7.10' _chemical_formula_weight 542.01 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 10.7022(4) _cell_length_b 10.7022(4) _cell_length_c 22.8742(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2268.9(2) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark pink' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 841 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9219 _exptl_absorpt_correction_T_max 0.9513 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9657 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 24.77 _reflns_number_total 2578 _reflns_number_gt 1836 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 2578 _refine_ls_number_parameters 320 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.3235 _refine_ls_wR_factor_gt 0.2944 _refine_ls_goodness_of_fit_ref 1.298 _refine_ls_restrained_S_all 1.297 _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 0.3553(2) 0.6450(2) 0.3225(2) 0.0529(6) Uani 1 1 d . . . N1A N 0.2118(15) 0.6643(18) 0.2627(5) 0.061(4) Uani 1 1 d . . . C2A C 0.2512(18) 0.733(2) 0.2120(8) 0.078(5) Uani 1 1 d . . . H2A H 0.3493 0.7699 0.2013 0.118 Uiso 1 1 calc R . . C3A C 0.1728(17) 0.755(2) 0.1752(7) 0.082(6) Uani 1 1 d D . . H3A H 0.2151 0.8119 0.1412 0.123 Uiso 1 1 calc R . . C4A C 0.0264(18) 0.6959(16) 0.1859(6) 0.068(5) Uani 1 1 d D . . C5A C -0.020(3) 0.614(3) 0.2332(10) 0.148(15) Uani 1 1 d D . . H5A H -0.1211 0.5579 0.2400 0.223 Uiso 1 1 calc R . . C6A C 0.073(3) 0.608(4) 0.2726(13) 0.146(14) Uani 1 1 d . . . H6A H 0.0352 0.5610 0.3089 0.219 Uiso 1 1 calc R . . C7A C -0.0666(16) 0.724(2) 0.1466(6) 0.064(4) Uani 1 1 d D . . C8A C -0.007(4) 0.850(4) 0.1136(13) 0.140(10) Uiso 1 1 d . . . H8A H 0.0913 0.9211 0.1178 0.210 Uiso 1 1 calc R . . C9A C -0.096(3) 0.870(3) 0.0737(14) 0.132(9) Uiso 1 1 d . . . H9A H -0.0537 0.9506 0.0481 0.198 Uiso 1 1 calc R . . C10A C -0.2467(18) 0.773(2) 0.0706(7) 0.073(5) Uani 1 1 d . . . C11A C -0.298(2) 0.668(3) 0.1083(11) 0.105(9) Uani 1 1 d . . . H11A H -0.4000 0.6111 0.1111 0.157 Uiso 1 1 calc R . . C12A C -0.2175(9) 0.6333(9) 0.1445(4) 0.092(6) Uiso 1 1 d . . . H12A H -0.2632 0.5487 0.1679 0.137 Uiso 1 1 calc R . . C13A C -0.3421(9) 0.8058(9) 0.0310(4) 0.078(5) Uani 1 1 d R . . O14A O -0.2782(9) 0.9157(9) -0.0025(4) 0.133(8) Uani 1 1 d R . . N1B N 0.3422(9) 0.7893(9) 0.3831(4) 0.059(4) Uani 1 1 d R . . C2B C 0.403(2) 0.932(2) 0.3742(9) 0.075(5) Uani 1 1 d . . . H2B H 0.4638 0.9724 0.3410 0.113 Uiso 1 1 calc R . . C3B C 0.383(2) 1.022(2) 0.4101(8) 0.083(6) Uani 1 1 d D . . H3B H 0.4278 1.1213 0.4003 0.125 Uiso 1 1 calc R . . C4B C 0.3011(13) 0.9745(17) 0.4596(5) 0.063(4) Uani 1 1 d D . . C5B C 0.246(2) 0.8317(19) 0.4689(7) 0.081(5) Uani 1 1 d D . . H5B H 0.1926 0.7907 0.5037 0.121 Uiso 1 1 calc R . . C6B C 0.263(2) 0.7437(19) 0.4310(8) 0.082(6) Uani 1 1 d . . . H6B H 0.2160 0.6434 0.4395 0.123 Uiso 1 1 calc R . . C7B C 0.274(2) 1.0659(18) 0.4989(7) 0.068(4) Uani 1 1 d D . . C8B C 0.361(3) 1.210(2) 0.4987(10) 0.106(9) Uani 1 1 d . . . H8B H 0.4401 1.2525 0.4723 0.159 Uiso 1 1 calc R . . C9B C 0.337(3) 1.297(2) 0.5369(9) 0.095(7) Uani 1 1 d . . . H9B H 0.4031 1.3981 0.5370 0.142 Uiso 1 1 calc R . . C10B C 0.224(2) 1.2454(19) 0.5734(8) 0.071(5) Uani 1 1 d . . . C11B C 0.130(3) 1.096(3) 0.5734(12) 0.110(7) Uani 1 1 d . . . H11B H 0.0478 1.0543 0.5981 0.165 Uiso 1 1 calc R . . C12B C 0.157(3) 1.008(3) 0.5378(9) 0.091(6) Uani 1 1 d . . . H12B H 0.0946 0.9069 0.5395 0.137 Uiso 1 1 calc R . . C13B C 0.198(2) 1.339(2) 0.6144(8) 0.078(5) Uani 1 1 d . . . O14B O 0.2893(14) 1.4727(13) 0.6141(5) 0.064(3) Uani 1 1 d . . . O15B O 0.087(2) 1.2778(15) 0.6470(9) 0.130(7) Uani 1 1 d . . . C1C C 0.497(4) 0.510(3) 0.4072(14) 0.142(11) Uani 1 1 d . . . H1C1 H 0.3951 0.4427 0.4159 0.212 Uiso 1 1 calc R . . H1C2 H 0.5522 0.5389 0.4437 0.212 Uiso 1 1 calc R . . H1C3 H 0.5344 0.4636 0.3815 0.212 Uiso 1 1 calc R . . O2C O 0.5097(16) 0.6368(15) 0.3786(5) 0.068(3) Uani 1 1 d . . . C1D C 0.486(4) 0.510(4) 0.2400(15) 0.151(12) Uiso 1 1 d . . . H1D1 H 0.4851 0.5298 0.1982 0.226 Uiso 1 1 calc R . . H1D2 H 0.4917 0.4220 0.2450 0.226 Uiso 1 1 calc R . . H1D3 H 0.5705 0.5914 0.2584 0.226 Uiso 1 1 calc R . . O2D O 0.3650(13) 0.4928(16) 0.2653(5) 0.069(3) Uani 1 1 d . . . O15A O -0.4731(12) 0.7132(13) 0.0313(5) 0.060(3) Uani 1 1 d . . . C1 C -0.145(9) 0.847(8) 0.660(3) 0.07(2) Uiso 0.20 1 d PD . . O2 O -0.176(7) 1.057(4) 0.6997(19) 0.139(19) Uani 0.40 1 d P . . O3 O -0.247(7) 0.268(7) 0.322(3) 0.080(16) Uiso 0.20 1 d PD . . C10 C -0.319(8) 0.340(8) 0.303(4) 0.06(2) Uiso 0.20 1 d PD . . O1 O -0.169(5) 0.764(5) 0.6094(18) 0.057(12) Uiso 0.20 1 d PD . . O5 O -0.275(7) 1.174(7) 0.779(3) 0.123(18) Uiso 0.30 1 d P . . 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 0.0571(14) 0.0563(13) 0.0382(8) 0.0056(8) 0.0057(8) 0.0230(9) N1A 0.045(7) 0.083(9) 0.042(7) 0.013(6) 0.011(5) 0.021(7) C2A 0.044(9) 0.095(13) 0.076(11) 0.007(10) -0.005(8) 0.019(9) C3A 0.043(9) 0.116(15) 0.062(9) 0.035(10) 0.006(7) 0.022(10) C4A 0.053(10) 0.087(12) 0.065(10) 0.013(9) 0.013(8) 0.035(9) C5A 0.076(15) 0.23(4) 0.113(18) 0.11(2) 0.030(14) 0.061(19) C6A 0.076(16) 0.20(3) 0.14(2) 0.13(2) 0.038(14) 0.048(17) C7A 0.038(8) 0.101(12) 0.046(7) 0.009(8) 0.000(6) 0.029(8) C10A 0.042(8) 0.098(13) 0.061(9) 0.023(9) 0.002(7) 0.022(9) C11A 0.037(10) 0.123(19) 0.14(2) 0.037(16) -0.014(11) 0.027(11) C13A 0.067(12) 0.107(15) 0.074(11) 0.027(10) 0.013(9) 0.054(12) O14A 0.060(8) 0.149(15) 0.155(14) 0.091(13) 0.000(8) 0.026(9) N1B 0.074(9) 0.047(7) 0.046(7) 0.013(6) 0.004(6) 0.024(7) C2B 0.075(12) 0.075(13) 0.075(11) 0.000(9) 0.000(9) 0.038(10) C3B 0.083(13) 0.083(14) 0.083(13) 0.000(11) 0.000(10) 0.042(11) C4B 0.079(11) 0.055(10) 0.041(8) 0.011(6) 0.011(7) 0.024(8) C5B 0.096(13) 0.067(11) 0.058(9) 0.010(8) 0.024(9) 0.025(10) C6B 0.120(16) 0.054(9) 0.058(9) 0.003(8) 0.029(10) 0.034(11) C7B 0.084(12) 0.048(9) 0.063(9) 0.011(7) 0.010(8) 0.026(9) C8B 0.14(2) 0.056(11) 0.099(16) 0.009(10) 0.054(15) 0.031(12) C9B 0.131(19) 0.061(12) 0.071(12) -0.001(9) 0.038(12) 0.033(12) C10B 0.082(12) 0.058(10) 0.070(10) -0.003(8) 0.021(9) 0.033(9) C11B 0.110(19) 0.110(19) 0.110(17) 0.000(14) 0.000(14) 0.055(16) C12B 0.091(14) 0.091(14) 0.091(13) 0.000(11) 0.000(11) 0.046(12) C13B 0.101(15) 0.074(13) 0.067(11) 0.005(9) 0.022(10) 0.049(12) O14B 0.084(8) 0.060(8) 0.046(6) -0.002(5) 0.005(5) 0.033(7) O15B 0.160(16) 0.053(7) 0.157(13) 0.018(8) 0.095(13) 0.038(9) C1C 0.14(2) 0.103(19) 0.17(3) 0.008(18) -0.06(2) 0.052(18) O2C 0.098(9) 0.069(8) 0.048(6) 0.004(5) -0.006(6) 0.050(7) O2D 0.059(7) 0.098(9) 0.051(6) -0.018(6) 0.005(5) 0.041(7) O15A 0.046(7) 0.073(7) 0.052(6) 0.011(5) 0.001(5) 0.023(6) O2 0.21(5) 0.06(2) 0.12(3) 0.02(2) 0.02(3) 0.04(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 O15A 2.064(12) 3_455 ? Co1 O14B 2.072(12) 2_774 ? Co1 O2C 2.128(13) . ? Co1 N1B 2.131(9) . ? Co1 O2D 2.132(12) . ? Co1 N1A 2.142(14) . ? N1A C6A 1.32(3) . ? N1A C2A 1.32(2) . ? C2A C3A 1.29(2) . ? C3A C4A 1.39(2) . ? C4A C5A 1.32(3) . ? C4A C7A 1.48(2) . ? C5A C6A 1.37(4) . ? C7A C8A 1.39(4) . ? C7A C12A 1.409(17) . ? C8A C9A 1.41(4) . ? C9A C10A 1.42(3) . ? C10A C11A 1.30(3) . ? C10A C13A 1.530(19) . ? C11A C12A 1.38(2) . ? C13A O15A 1.248(14) . ? C13A O14A 1.2773 . ? N1B C6B 1.318(18) . ? N1B C2B 1.34(2) . ? C2B C3B 1.36(3) . ? C3B C4B 1.37(2) . ? C4B C5B 1.35(2) . ? C4B C7B 1.46(2) . ? C5B C6B 1.36(3) . ? C7B C8B 1.34(3) . ? C7B C12B 1.40(3) . ? C8B C9B 1.40(3) . ? C9B C10B 1.34(3) . ? C10B C11B 1.40(3) . ? C10B C13B 1.50(2) . ? C11B C12B 1.37(3) . ? C13B O14B 1.27(2) . ? C13B O15B 1.27(2) . ? O14B Co1 2.072(12) 3_575 ? C1C O2C 1.45(3) . ? C1D O2D 1.35(4) . ? O15A Co1 2.064(12) 2_564 ? C1 O1 1.396(11) . ? O3 C10 1.406(11) . ? 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 O15A Co1 O14B 179.1(5) 3_455 2_774 ? O15A Co1 O2C 92.0(5) 3_455 . ? O14B Co1 O2C 87.2(5) 2_774 . ? O15A Co1 N1B 89.8(4) 3_455 . ? O14B Co1 N1B 90.5(4) 2_774 . ? O2C Co1 N1B 88.3(4) . . ? O15A Co1 O2D 87.8(5) 3_455 . ? O14B Co1 O2D 91.9(5) 2_774 . ? O2C Co1 O2D 90.2(5) . . ? N1B Co1 O2D 177.1(5) . . ? O15A Co1 N1A 91.9(5) 3_455 . ? O14B Co1 N1A 89.0(5) 2_774 . ? O2C Co1 N1A 176.2(6) . . ? N1B Co1 N1A 92.0(4) . . ? O2D Co1 N1A 89.6(5) . . ? C6A N1A C2A 112.2(16) . . ? C6A N1A Co1 123.2(13) . . ? C2A N1A Co1 124.5(11) . . ? C3A C2A N1A 128.1(17) . . ? C2A C3A C4A 119.3(15) . . ? C5A C4A C3A 114.4(19) . . ? C5A C4A C7A 124.2(18) . . ? C3A C4A C7A 121.4(15) . . ? C4A C5A C6A 122(2) . . ? N1A C6A C5A 123.2(19) . . ? C8A C7A C12A 117.2(19) . . ? C8A C7A C4A 120(2) . . ? C12A C7A C4A 122.5(14) . . ? C7A C8A C9A 119(3) . . ? C8A C9A C10A 122(3) . . ? C11A C10A C9A 116(2) . . ? C11A C10A C13A 123.2(15) . . ? C9A C10A C13A 120.5(19) . . ? C10A C11A C12A 125.7(18) . . ? C11A C12A C7A 119.5(13) . . ? O15A C13A O14A 127.3(6) . . ? O15A C13A C10A 115.4(10) . . ? O14A C13A C10A 116.9(7) . . ? C6B N1B C2B 113.8(13) . . ? C6B N1B Co1 122.3(9) . . ? C2B N1B Co1 123.7(10) . . ? N1B C2B C3B 123.6(17) . . ? C2B C3B C4B 122(2) . . ? C5B C4B C3B 112.7(17) . . ? C5B C4B C7B 122.7(14) . . ? C3B C4B C7B 124.6(16) . . ? C4B C5B C6B 123.3(15) . . ? N1B C6B C5B 123.9(15) . . ? C8B C7B C12B 117.4(19) . . ? C8B C7B C4B 120.6(16) . . ? C12B C7B C4B 122.0(16) . . ? C7B C8B C9B 121(2) . . ? C10B C9B C8B 123(2) . . ? C9B C10B C11B 117.2(19) . . ? C9B C10B C13B 123.0(18) . . ? C11B C10B C13B 119.8(18) . . ? C12B C11B C10B 120(2) . . ? C11B C12B C7B 122(2) . . ? O14B C13B O15B 125.5(17) . . ? O14B C13B C10B 117.0(16) . . ? O15B C13B C10B 117.5(18) . . ? C13B O14B Co1 131.1(12) . 3_575 ? C1C O2C Co1 126.8(15) . . ? C1D O2D Co1 124.7(18) . . ? C13A O15A Co1 130.4(8) . 2_564 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.674 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 931537'