# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jones, Leigh' _publ_contact_author_email leigh.jones@nuigalway.ie _publ_section_title ; Old Dog, New Tricks: 2,2'-Biphenol as a Bridging and Book-End Ligand in Discrete and Extended Co(II) Architectures. ; _publ_requested_coeditor_name A.Prescimone@ed.ac.uk loop_ _publ_author_name L.Jones N.Berg E.Brechin # Attachment '- Co2(1).cif' data_p-1 _database_code_depnum_ccdc_archive 'CCDC 852543' #TrackingRef '- Co2(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co2(biphen)2(py)4).2EtOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Co2 N4 O6' _chemical_formula_weight 894.76 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.416(2) _cell_length_b 11.022(2) _cell_length_c 11.536(2) _cell_angle_alpha 114.31(3) _cell_angle_beta 92.94(3) _cell_angle_gamma 115.71(3) _cell_volume 1043.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 466 _exptl_absorpt_coefficient_mu 0.850 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 3.3669 _cell_measurement_reflns_used 5662 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _exptl_absorpt_correction_T_min 0.97768 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 8127 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.3669 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0151918000 _diffrn_orient_matrix_UB_12 0.0226206000 _diffrn_orient_matrix_UB_13 -0.0493453000 _diffrn_orient_matrix_UB_21 0.0742284000 _diffrn_orient_matrix_UB_22 0.0165421000 _diffrn_orient_matrix_UB_23 0.0174568000 _diffrn_orient_matrix_UB_31 -0.0213864000 _diffrn_orient_matrix_UB_32 -0.0765715000 _diffrn_orient_matrix_UB_33 -0.0469000000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -2.00 87.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 64.0000 48.0000 89 #__ type_ start__ end____ width___ exp.time_ 2 omega 7.00 83.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 -180.0000 76 #__ type_ start__ end____ width___ exp.time_ 3 omega -44.00 50.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 -77.0000 -90.0000 94 #__ type_ start__ end____ width___ exp.time_ 4 omega -8.00 32.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 150.0000 40 #__ type_ start__ end____ width___ exp.time_ 5 omega 59.00 89.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 150.0000 30 #__ type_ start__ end____ width___ exp.time_ 6 omega 56.00 91.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 37.0000 -30.0000 35 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 3814 _reflns_number_gt 3510 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+1.2875P] 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 3814 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.92873(3) 0.57365(3) 0.60592(3) 0.01607(10) Uani 1 1 d . . . N1 N 0.7876(2) 0.6313(2) 0.53727(18) 0.0193(4) Uani 1 1 d . . . N2 N 1.0300(2) 0.7930(2) 0.78390(18) 0.0197(4) Uani 1 1 d . . . O1 O 0.82081(17) 0.44909(17) 0.68560(15) 0.0210(3) Uani 1 1 d . . . O2 O 0.87710(15) 0.38620(16) 0.42566(14) 0.0173(3) Uani 1 1 d . . . O3 O 0.70613(14) 0.54241(15) 0.88678(13) 0.0523(5) Uiso 1 1 d . . . H3A H 0.6697 0.5425 0.8201 0.063 Uiso 1 1 calc R . . C1 C 0.84435(14) 0.33325(15) 0.66829(13) 0.0196(4) Uani 1 1 d R . . C2 C 0.93257(14) 0.34911(15) 0.77575(13) 0.0260(5) Uani 1 1 d R . . H2 H 0.9749 0.4419 0.8576 0.031 Uiso 1 1 calc R . . C3 C 0.9593(3) 0.2330(3) 0.7652(3) 0.0315(6) Uani 1 1 d . . . H3 H 1.0200 0.2469 0.8391 0.038 Uiso 1 1 calc R . . C4 C 0.8981(3) 0.0972(3) 0.6477(3) 0.0332(6) Uani 1 1 d . . . H4 H 0.9152 0.0167 0.6401 0.040 Uiso 1 1 calc R . . C5 C 0.8111(3) 0.0797(3) 0.5408(2) 0.0272(5) Uani 1 1 d . . . H5 H 0.7691 -0.0142 0.4599 0.033 Uiso 1 1 calc R . . C6 C 0.7827(2) 0.1945(2) 0.5471(2) 0.0205(5) Uani 1 1 d . . . C7 C 0.6887(2) 0.1641(2) 0.4256(2) 0.0192(4) Uani 1 1 d . . . C8 C 0.5500(3) 0.0305(3) 0.3589(2) 0.0259(5) Uani 1 1 d . . . H8 H 0.5126 -0.0358 0.3964 0.031 Uiso 1 1 calc R . . C9 C 0.4657(3) -0.0078(3) 0.2399(2) 0.0301(6) Uani 1 1 d . . . H9 H 0.3705 -0.0976 0.1978 0.036 Uiso 1 1 calc R . . C10 C 0.5209(3) 0.0852(3) 0.1825(2) 0.0280(5) Uani 1 1 d . . . H10 H 0.4646 0.0582 0.0996 0.034 Uiso 1 1 calc R . . C11 C 0.6581(2) 0.2179(3) 0.2457(2) 0.0223(5) Uani 1 1 d . . . H11 H 0.6954 0.2817 0.2059 0.027 Uiso 1 1 calc R . . C12 C 0.7423(2) 0.2592(2) 0.3673(2) 0.0173(4) Uani 1 1 d . . . C13 C 0.7009(3) 0.6677(3) 0.6103(2) 0.0242(5) Uani 1 1 d . . . H13 H 0.7130 0.6751 0.6955 0.029 Uiso 1 1 calc R . . C14 C 0.5954(3) 0.6948(3) 0.5673(3) 0.0282(5) Uani 1 1 d . . . H14 H 0.5365 0.7208 0.6221 0.034 Uiso 1 1 calc R . . C15 C 0.5768(3) 0.6835(3) 0.4441(3) 0.0325(6) Uani 1 1 d . . . H15 H 0.5029 0.6990 0.4111 0.039 Uiso 1 1 calc R . . C16 C 0.6667(2) 0.6495(2) 0.36908(18) 0.0400(7) Uani 1 1 d . . . H16 H 0.6581 0.6445 0.2846 0.048 Uiso 1 1 calc R . . C17 C 0.7707(2) 0.6226(2) 0.41853(18) 0.0288(5) Uani 1 1 d R . . H17 H 0.8315 0.5972 0.3657 0.035 Uiso 1 1 calc R . . C18 C 1.0912(3) 0.9181(3) 0.7678(2) 0.0230(5) Uani 1 1 d . . . H18 H 1.0711 0.9049 0.6809 0.028 Uiso 1 1 calc R . . C19 C 1.1816(3) 1.0647(3) 0.8714(3) 0.0290(5) Uani 1 1 d . . . H19 H 1.2224 1.1502 0.8558 0.035 Uiso 1 1 calc R . . C20 C 1.2119(3) 1.0852(3) 0.9979(2) 0.0306(6) Uani 1 1 d . . . H20 H 1.2741 1.1850 1.0710 0.037 Uiso 1 1 calc R . . C21 C 1.1502(3) 0.9579(3) 1.0161(2) 0.0280(5) Uani 1 1 d . . . H21 H 1.1693 0.9685 1.1022 0.034 Uiso 1 1 calc R . . C22 C 1.0604(2) 0.8148(3) 0.9075(2) 0.0230(5) Uani 1 1 d . . . H22 H 1.0182 0.7277 0.9210 0.028 Uiso 1 1 calc R . . C50 C 0.6054(3) 0.4106(3) 0.8927(3) 0.0394(6) Uiso 1 1 d . . . H50A H 0.5797 0.3181 0.8081 0.047 Uiso 1 1 calc R . . H50B H 0.5131 0.4139 0.9033 0.047 Uiso 1 1 calc R . . C51 C 0.6667(4) 0.3979(4) 1.0042(3) 0.0473(7) Uiso 1 1 d . . . H51A H 0.7496 0.3795 0.9876 0.071 Uiso 1 1 calc R . . H51B H 0.5889 0.3121 1.0112 0.071 Uiso 1 1 calc R . . H51C H 0.7017 0.4936 1.0871 0.071 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 0.01529(16) 0.01744(16) 0.01625(16) 0.00790(12) 0.00515(11) 0.00890(12) N1 0.0188(9) 0.0185(9) 0.0196(9) 0.0073(8) 0.0045(7) 0.0104(8) N2 0.0182(9) 0.0207(9) 0.0194(9) 0.0074(8) 0.0055(7) 0.0113(8) O1 0.0256(8) 0.0198(8) 0.0198(8) 0.0105(6) 0.0095(6) 0.0120(7) O2 0.0149(7) 0.0162(7) 0.0169(7) 0.0059(6) 0.0044(6) 0.0065(6) C1 0.0175(11) 0.0221(11) 0.0229(11) 0.0147(9) 0.0088(9) 0.0088(9) C2 0.0231(12) 0.0301(12) 0.0240(12) 0.0157(10) 0.0063(10) 0.0102(10) C3 0.0275(13) 0.0442(15) 0.0362(14) 0.0301(13) 0.0099(11) 0.0183(12) C4 0.0359(14) 0.0354(14) 0.0469(16) 0.0297(13) 0.0161(12) 0.0227(12) C5 0.0291(13) 0.0227(12) 0.0321(13) 0.0157(10) 0.0105(10) 0.0122(10) C6 0.0188(11) 0.0205(11) 0.0241(11) 0.0128(9) 0.0086(9) 0.0092(9) C7 0.0176(11) 0.0176(10) 0.0181(11) 0.0047(9) 0.0060(9) 0.0089(9) C8 0.0213(12) 0.0196(11) 0.0273(12) 0.0069(10) 0.0092(10) 0.0065(10) C9 0.0167(11) 0.0251(12) 0.0259(12) -0.0003(10) 0.0022(10) 0.0051(10) C10 0.0204(12) 0.0360(13) 0.0170(11) 0.0035(10) 0.0013(9) 0.0149(11) C11 0.0211(11) 0.0282(12) 0.0189(11) 0.0095(9) 0.0069(9) 0.0152(10) C12 0.0133(10) 0.0170(10) 0.0187(10) 0.0046(9) 0.0054(8) 0.0090(9) C13 0.0233(12) 0.0245(11) 0.0214(11) 0.0074(10) 0.0073(9) 0.0126(10) C14 0.0246(12) 0.0241(12) 0.0357(14) 0.0100(11) 0.0111(10) 0.0160(10) C15 0.0304(14) 0.0313(13) 0.0406(15) 0.0161(12) 0.0039(11) 0.0210(12) C16 0.0581(19) 0.0551(18) 0.0307(14) 0.0254(13) 0.0142(13) 0.0425(16) C17 0.0365(14) 0.0387(14) 0.0269(12) 0.0188(11) 0.0148(11) 0.0277(12) C18 0.0238(12) 0.0251(11) 0.0241(12) 0.0116(10) 0.0079(9) 0.0154(10) C19 0.0267(13) 0.0202(11) 0.0365(14) 0.0110(11) 0.0077(11) 0.0115(10) C20 0.0227(12) 0.0242(12) 0.0272(13) 0.0010(10) 0.0016(10) 0.0091(10) C21 0.0227(12) 0.0343(13) 0.0195(11) 0.0079(10) 0.0031(9) 0.0133(11) C22 0.0210(11) 0.0266(12) 0.0233(11) 0.0121(10) 0.0078(9) 0.0133(10) _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 1.9492(16) . ? Co1 O2 1.9624(15) 2_766 ? Co1 O2 2.0653(18) . ? Co1 N1 2.0729(19) . ? Co1 N2 2.157(2) . ? N1 C17 1.330(3) . ? N1 C13 1.341(3) . ? N2 C18 1.342(3) . ? N2 C22 1.341(3) . ? O1 C1 1.340(2) . ? O2 C12 1.344(3) . ? O2 Co1 1.9624(15) 2_766 ? O3 C50 1.408(3) . ? O3 H3A 0.8400 . ? C1 C2 1.4061 . ? C1 C6 1.414(3) . ? C2 C3 1.384(3) . ? C2 H2 0.9500 . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 C7 1.491(3) . ? C7 C8 1.398(3) . ? C7 C12 1.405(3) . ? C8 C9 1.383(4) . ? C8 H8 0.9500 . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C13 C14 1.376(3) . ? C13 H13 0.9500 . ? C14 C15 1.371(4) . ? C14 H14 0.9500 . ? C15 C16 1.373(3) . ? C15 H15 0.9500 . ? C16 C17 1.3943 . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.378(3) . ? C18 H18 0.9500 . ? C19 C20 1.378(4) . ? C19 H19 0.9500 . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.380(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C50 C51 1.491(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 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 126.68(7) . 2_766 ? O1 Co1 O2 94.08(7) . . ? O2 Co1 O2 76.50(8) 2_766 . ? O1 Co1 N1 106.95(7) . . ? O2 Co1 N1 125.89(7) 2_766 . ? O2 Co1 N1 94.73(7) . . ? O1 Co1 N2 96.78(7) . . ? O2 Co1 N2 90.98(8) 2_766 . ? O2 Co1 N2 166.81(7) . . ? N1 Co1 N2 89.25(8) . . ? C17 N1 C13 117.96(18) . . ? C17 N1 Co1 122.63(14) . . ? C13 N1 Co1 119.21(15) . . ? C18 N2 C22 117.2(2) . . ? C18 N2 Co1 116.41(15) . . ? C22 N2 Co1 125.22(15) . . ? C1 O1 Co1 116.46(11) . . ? C12 O2 Co1 131.87(13) . 2_766 ? C12 O2 Co1 123.26(13) . . ? Co1 O2 Co1 103.50(8) 2_766 . ? C50 O3 H3A 109.5 . . ? O1 C1 C2 118.69(9) . . ? O1 C1 C6 122.97(15) . . ? C2 C1 C6 118.33(11) . . ? C3 C2 C1 121.64(13) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 122.5(2) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 118.3(2) . . ? C5 C6 C7 118.1(2) . . ? C1 C6 C7 123.55(18) . . ? C8 C7 C12 118.0(2) . . ? C8 C7 C6 120.3(2) . . ? C12 C7 C6 121.34(19) . . ? C9 C8 C7 121.8(2) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 119.6(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.0(2) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? O2 C12 C11 120.0(2) . . ? O2 C12 C7 120.12(19) . . ? C11 C12 C7 119.9(2) . . ? N1 C13 C14 123.0(2) . . ? N1 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C15 C14 C13 118.9(2) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 C14 118.9(2) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.15(13) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N1 C17 C16 122.08(11) . . ? N1 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? N2 C18 C19 123.1(2) . . ? N2 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C18 C19 C20 119.0(2) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 118.6(2) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 119.0(2) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N2 C22 C21 123.0(2) . . ? N2 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? O3 C50 C51 112.4(2) . . ? O3 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? O3 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.256 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.059 # Attachment '- Co2(2).cif' data_nb240j2 _database_code_depnum_ccdc_archive 'CCDC 852544' #TrackingRef '- Co2(2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ?[Co2(Biphen)2(3-pic)4].2(BiphenH2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 Co2 N4 O8' _chemical_formula_weight 1231.13 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.119(2) _cell_length_b 12.486(3) _cell_length_c 13.342(3) _cell_angle_alpha 111.49(3) _cell_angle_beta 113.74(3) _cell_angle_gamma 95.46(3) _cell_volume 1512.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 0.610 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.8831 _cell_measurement_reflns_used 5715 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _exptl_absorpt_correction_T_min 0.95165 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 12216 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.8831 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0572385000 _diffrn_orient_matrix_UB_12 -0.0404884000 _diffrn_orient_matrix_UB_13 -0.0566105000 _diffrn_orient_matrix_UB_21 0.0343060000 _diffrn_orient_matrix_UB_22 -0.0452570000 _diffrn_orient_matrix_UB_23 -0.0031788000 _diffrn_orient_matrix_UB_31 -0.0288506000 _diffrn_orient_matrix_UB_32 -0.0192054000 _diffrn_orient_matrix_UB_33 0.0314026000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -21.00 22.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - -18.3278 -101.0000 175.0000 43 #__ type_ start__ end____ width___ exp.time_ 2 omega -18.00 10.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - -18.3278 -101.0000 79.0000 28 #__ type_ start__ end____ width___ exp.time_ 3 omega -2.00 61.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - 18.6403 -101.0000 -4.0000 63 #__ type_ start__ end____ width___ exp.time_ 4 omega 39.00 86.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - 18.6403 179.0000 150.0000 47 #__ type_ start__ end____ width___ exp.time_ 5 omega -4.00 86.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - 18.6403 37.0000 -60.0000 90 #__ type_ start__ end____ width___ exp.time_ 6 omega 65.00 90.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - 18.6403 37.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 7 omega -51.00 35.00 1.0000 39.0300 omega____ theta____ kappa____ phi______ frames - 18.6403 -37.0000 120.0000 86 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 5527 _reflns_number_gt 4451 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^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_number_reflns 5527 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.34877(3) 0.42237(2) 0.39714(3) 0.01807(9) Uani 1 1 d . . . N1 N 0.24129(17) 0.38651(14) 0.20890(16) 0.0203(4) Uani 1 1 d . . . N2 N 0.20340(16) 0.50337(14) 0.42535(15) 0.0198(4) Uani 1 1 d . . . O1 O 0.48404(13) 0.48087(11) 0.58030(12) 0.0187(3) Uani 1 1 d . . . O2 O 0.30785(14) 0.25581(11) 0.37195(13) 0.0219(3) Uani 1 1 d . . . O3 O 0.06157(15) 0.14721(13) 0.22307(14) 0.0263(4) Uani 1 1 d . . . H3H H 0.1465 0.1661 0.2683 0.032 Uiso 1 1 calc R . . O4 O -0.11233(17) 0.05373(15) -0.01033(14) 0.0377(4) Uani 1 1 d . . . H4H H -0.0389 0.0726 0.0536 0.045 Uiso 1 1 calc R . . C1 C 0.4577(2) 0.44138(17) 0.65305(18) 0.0184(4) Uani 1 1 d . . . C2 C 0.4387(2) 0.51914(18) 0.74765(19) 0.0237(5) Uani 1 1 d . . . H2 H 0.4402 0.5988 0.7581 0.028 Uiso 1 1 calc R . . C3 C 0.4175(2) 0.4823(2) 0.8268(2) 0.0288(5) Uani 1 1 d . . . H3 H 0.4056 0.5367 0.8914 0.035 Uiso 1 1 calc R . . C4 C 0.4138(2) 0.36637(19) 0.8116(2) 0.0279(5) Uani 1 1 d . . . H4 H 0.3989 0.3402 0.8653 0.033 Uiso 1 1 calc R . . C5 C 0.4321(2) 0.28842(19) 0.7171(2) 0.0237(5) Uani 1 1 d . . . H5 H 0.4299 0.2088 0.7073 0.028 Uiso 1 1 calc R . . C6 C 0.4537(2) 0.32268(17) 0.63631(19) 0.0190(4) Uani 1 1 d . . . C7 C 0.4825(2) 0.23834(17) 0.54149(19) 0.0188(5) Uani 1 1 d . . . C8 C 0.5850(2) 0.18292(18) 0.5788(2) 0.0242(5) Uani 1 1 d . . . H8 H 0.6347 0.2021 0.6629 0.029 Uiso 1 1 calc R . . C9 C 0.6158(2) 0.10115(18) 0.4963(2) 0.0293(5) Uani 1 1 d . . . H9 H 0.6866 0.0657 0.5238 0.035 Uiso 1 1 calc R . . C10 C 0.5428(2) 0.07177(19) 0.3742(2) 0.0305(6) Uani 1 1 d . . . H10 H 0.5624 0.0150 0.3169 0.037 Uiso 1 1 calc R . . C11 C 0.4410(2) 0.12430(17) 0.3343(2) 0.0259(5) Uani 1 1 d . . . H11 H 0.3913 0.1028 0.2496 0.031 Uiso 1 1 calc R . . C12 C 0.4098(2) 0.20856(17) 0.41638(19) 0.0191(5) Uani 1 1 d . . . C13 C 0.2240(2) 0.48252(19) 0.1877(2) 0.0248(5) Uani 1 1 d . . . H13 H 0.2495 0.5578 0.2556 0.030 Uiso 1 1 calc R . . C14 C 0.1715(2) 0.4777(2) 0.0735(2) 0.0292(5) Uani 1 1 d . . . H14 H 0.1639 0.5490 0.0641 0.035 Uiso 1 1 calc R . . C15 C 0.1296(2) 0.3696(2) -0.0280(2) 0.0311(5) Uani 1 1 d . . . C16 C 0.0688(3) 0.3606(3) -0.1557(2) 0.0513(7) Uani 1 1 d . . . H16A H 0.1287 0.3349 -0.1915 0.077 Uiso 1 1 calc R . . H16B H 0.0604 0.4393 -0.1519 0.077 Uiso 1 1 calc R . . H16C H -0.0220 0.3019 -0.2062 0.077 Uiso 1 1 calc R . . C17 C 0.1458(2) 0.2697(2) -0.0070(2) 0.0325(6) Uani 1 1 d . . . H17 H 0.1184 0.1930 -0.0737 0.039 Uiso 1 1 calc R . . C18 C 0.2018(2) 0.28185(18) 0.1105(2) 0.0246(5) Uani 1 1 d . . . H18 H 0.2131 0.2123 0.1225 0.030 Uiso 1 1 calc R . . C19 C 0.0674(2) 0.45016(18) 0.35422(19) 0.0216(5) Uani 1 1 d . . . H19 H 0.0371 0.3685 0.2956 0.026 Uiso 1 1 calc R . . C20 C -0.0290(2) 0.50854(18) 0.36263(19) 0.0220(5) Uani 1 1 d . . . H20 H -0.1236 0.4666 0.3117 0.026 Uiso 1 1 calc R . . C21 C 0.0109(2) 0.62869(18) 0.44519(19) 0.0203(5) Uani 1 1 d . . . C22 C -0.0898(2) 0.6969(2) 0.4559(2) 0.0288(5) Uani 1 1 d . . . H22A H -0.1263 0.6784 0.5053 0.043 Uiso 1 1 calc R . . H22B H -0.1651 0.6740 0.3743 0.043 Uiso 1 1 calc R . . H22C H -0.0443 0.7832 0.4952 0.043 Uiso 1 1 calc R . . C23 C 0.1510(2) 0.68305(18) 0.5186(2) 0.0249(5) Uani 1 1 d . . . H23 H 0.1837 0.7648 0.5773 0.030 Uiso 1 1 calc R . . C24 C 0.2423(2) 0.61916(18) 0.50684(19) 0.0248(5) Uani 1 1 d . . . H24 H 0.3375 0.6585 0.5587 0.030 Uiso 1 1 calc R . . C25 C -0.0043(2) 0.07225(17) 0.24889(19) 0.0207(5) Uani 1 1 d . . . C26 C 0.0678(2) 0.02439(18) 0.3256(2) 0.0244(5) Uani 1 1 d . . . H26 H 0.1644 0.0406 0.3577 0.029 Uiso 1 1 calc R . . C27 C -0.0012(2) -0.04693(19) 0.3555(2) 0.0307(6) Uani 1 1 d . . . H27 H 0.0483 -0.0782 0.4095 0.037 Uiso 1 1 calc R . . C28 C -0.1418(2) -0.0726(2) 0.3069(2) 0.0353(6) Uani 1 1 d . . . H28 H -0.1892 -0.1208 0.3280 0.042 Uiso 1 1 calc R . . C29 C -0.2131(2) -0.0282(2) 0.2275(2) 0.0318(6) Uani 1 1 d . . . H29 H -0.3101 -0.0482 0.1930 0.038 Uiso 1 1 calc R . . C30 C -0.1473(2) 0.04568(18) 0.19588(19) 0.0233(5) Uani 1 1 d . . . C31 C -0.2277(2) 0.09636(19) 0.1146(2) 0.0288(5) Uani 1 1 d . . . C32 C -0.3337(2) 0.1389(2) 0.1303(2) 0.0428(7) Uani 1 1 d . . . H32 H -0.3506 0.1363 0.1938 0.051 Uiso 1 1 calc R . . C33 C -0.4149(2) 0.18480(16) 0.0559(2) 0.0588(9) Uani 1 1 d . . . H33 H -0.4871 0.2125 0.0677 0.071 Uiso 1 1 calc R . . C34 C -0.3894(2) 0.18958(16) -0.0351(2) 0.0619(9) Uani 1 1 d R . . H34 H -0.4438 0.2216 -0.0861 0.074 Uiso 1 1 calc R . . C35 C -0.2854(3) 0.1484(2) -0.0534(2) 0.0490(7) Uani 1 1 d . . . H35 H -0.2686 0.1527 -0.1165 0.059 Uiso 1 1 calc R . . C36 C -0.2054(2) 0.10082(19) 0.0198(2) 0.0323(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01653(16) 0.01676(16) 0.01894(17) 0.00860(12) 0.00606(12) 0.00452(11) N1 0.0182(9) 0.0208(9) 0.0214(10) 0.0104(8) 0.0079(8) 0.0052(7) N2 0.0178(9) 0.0206(9) 0.0186(10) 0.0097(8) 0.0057(8) 0.0047(7) O1 0.0193(8) 0.0188(7) 0.0169(8) 0.0098(6) 0.0064(6) 0.0032(6) O2 0.0188(8) 0.0171(7) 0.0215(9) 0.0089(6) 0.0025(7) 0.0024(6) O3 0.0192(8) 0.0270(8) 0.0248(9) 0.0145(7) 0.0020(7) 0.0003(6) O4 0.0346(10) 0.0487(10) 0.0239(10) 0.0158(8) 0.0085(8) 0.0123(8) C1 0.0122(10) 0.0211(11) 0.0171(11) 0.0085(9) 0.0031(9) 0.0036(8) C2 0.0241(12) 0.0205(11) 0.0228(12) 0.0091(9) 0.0083(10) 0.0061(9) C3 0.0291(13) 0.0366(14) 0.0217(13) 0.0115(10) 0.0139(11) 0.0101(10) C4 0.0279(13) 0.0372(13) 0.0245(13) 0.0191(11) 0.0128(11) 0.0098(10) C5 0.0217(12) 0.0263(12) 0.0274(13) 0.0179(10) 0.0096(10) 0.0089(9) C6 0.0142(10) 0.0218(11) 0.0194(12) 0.0105(9) 0.0054(9) 0.0048(8) C7 0.0153(11) 0.0170(10) 0.0229(12) 0.0100(9) 0.0075(9) 0.0021(8) C8 0.0212(12) 0.0235(12) 0.0272(13) 0.0142(10) 0.0080(10) 0.0062(9) C9 0.0240(12) 0.0251(12) 0.0469(17) 0.0200(11) 0.0189(12) 0.0139(10) C10 0.0353(14) 0.0209(12) 0.0417(16) 0.0127(11) 0.0247(13) 0.0094(10) C11 0.0319(13) 0.0184(11) 0.0247(13) 0.0073(9) 0.0137(11) 0.0035(9) C12 0.0173(11) 0.0136(10) 0.0266(13) 0.0105(9) 0.0095(10) 0.0024(8) C13 0.0215(12) 0.0227(12) 0.0237(13) 0.0096(10) 0.0056(10) 0.0045(9) C14 0.0310(13) 0.0326(13) 0.0331(15) 0.0220(11) 0.0151(11) 0.0153(10) C15 0.0337(14) 0.0438(14) 0.0262(14) 0.0202(11) 0.0178(12) 0.0180(11) C16 0.077(2) 0.0630(18) 0.0319(17) 0.0298(14) 0.0298(16) 0.0397(16) C17 0.0408(15) 0.0315(13) 0.0215(13) 0.0078(10) 0.0147(12) 0.0110(11) C18 0.0275(12) 0.0230(12) 0.0253(13) 0.0112(10) 0.0138(11) 0.0073(9) C19 0.0221(12) 0.0201(11) 0.0206(12) 0.0107(9) 0.0072(10) 0.0038(9) C20 0.0162(11) 0.0273(12) 0.0212(12) 0.0130(9) 0.0060(10) 0.0037(9) C21 0.0229(11) 0.0259(12) 0.0203(12) 0.0160(9) 0.0117(10) 0.0101(9) C22 0.0266(13) 0.0334(13) 0.0297(14) 0.0161(10) 0.0135(11) 0.0130(10) C23 0.0268(12) 0.0207(11) 0.0227(13) 0.0069(9) 0.0104(10) 0.0059(9) C24 0.0187(11) 0.0259(12) 0.0227(13) 0.0084(10) 0.0062(10) 0.0032(9) C25 0.0214(11) 0.0170(11) 0.0199(12) 0.0058(9) 0.0086(10) 0.0046(9) C26 0.0210(12) 0.0245(12) 0.0244(13) 0.0105(9) 0.0081(10) 0.0066(9) C27 0.0352(14) 0.0294(12) 0.0283(14) 0.0158(10) 0.0135(12) 0.0076(10) C28 0.0343(14) 0.0369(14) 0.0375(16) 0.0178(12) 0.0198(13) 0.0032(11) C29 0.0223(12) 0.0358(13) 0.0302(14) 0.0075(11) 0.0132(11) 0.0051(10) C30 0.0204(11) 0.0213(11) 0.0193(12) 0.0030(9) 0.0068(10) 0.0070(9) C31 0.0235(12) 0.0232(12) 0.0222(13) 0.0030(10) 0.0014(10) 0.0066(9) C32 0.0337(15) 0.0413(15) 0.0273(15) 0.0006(11) 0.0022(12) 0.0206(12) C33 0.0497(18) 0.0549(18) 0.0303(17) -0.0036(14) -0.0026(14) 0.0357(14) C34 0.069(2) 0.0399(16) 0.0365(19) 0.0077(13) -0.0064(16) 0.0333(15) C35 0.0593(19) 0.0365(15) 0.0257(16) 0.0104(12) 0.0001(14) 0.0146(13) C36 0.0311(14) 0.0228(12) 0.0229(14) 0.0048(10) -0.0004(11) 0.0074(10) _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 1.9570(14) . ? Co1 O1 1.9649(14) 2_666 ? Co1 O1 2.0716(17) . ? Co1 N2 2.0735(18) . ? Co1 N1 2.1433(19) . ? N1 C18 1.340(3) . ? N1 C13 1.342(3) . ? N2 C24 1.345(3) . ? N2 C19 1.349(3) . ? O1 C1 1.350(2) . ? O1 Co1 1.9649(14) 2_666 ? O2 C12 1.351(2) . ? O3 C25 1.356(2) . ? O3 H3H 0.8400 . ? O4 C36 1.362(3) . ? O4 H4H 0.8400 . ? C1 C2 1.392(3) . ? C1 C6 1.409(3) . ? C2 C3 1.385(3) . ? C2 H2 0.9500 . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.492(3) . ? C7 C8 1.404(3) . ? C7 C12 1.407(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.374(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C13 C14 1.371(3) . ? C13 H13 0.9500 . ? C14 C15 1.380(3) . ? C14 H14 0.9500 . ? C15 C17 1.388(3) . ? C15 C16 1.513(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.375(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.370(3) . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 H20 0.9500 . ? C21 C23 1.389(3) . ? C21 C22 1.491(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.372(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.388(3) . ? C25 C30 1.400(3) . ? C26 C27 1.384(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.377(3) . ? C28 H28 0.9500 . ? C29 C30 1.403(3) . ? C29 H29 0.9500 . ? C30 C31 1.486(3) . ? C31 C32 1.396(3) . ? C31 C36 1.402(3) . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.3734 . ? C33 H33 0.9500 . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 C36 1.387(3) . ? C35 H35 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 127.76(6) . 2_666 ? O2 Co1 O1 91.31(7) . . ? O1 Co1 O1 76.67(7) 2_666 . ? O2 Co1 N2 111.83(6) . . ? O1 Co1 N2 119.83(6) 2_666 . ? O1 Co1 N2 95.99(7) . . ? O2 Co1 N1 97.22(7) . . ? O1 Co1 N1 91.59(7) 2_666 . ? O1 Co1 N1 168.16(5) . . ? N2 Co1 N1 88.47(7) . . ? C18 N1 C13 116.24(19) . . ? C18 N1 Co1 127.50(15) . . ? C13 N1 Co1 115.89(14) . . ? C24 N2 C19 116.74(19) . . ? C24 N2 Co1 119.95(14) . . ? C19 N2 Co1 122.74(14) . . ? C1 O1 Co1 132.51(12) . 2_666 ? C1 O1 Co1 123.52(11) . . ? Co1 O1 Co1 103.33(7) 2_666 . ? C12 O2 Co1 120.73(11) . . ? C25 O3 H3H 109.5 . . ? C36 O4 H4H 109.5 . . ? O1 C1 C2 120.01(18) . . ? O1 C1 C6 120.37(17) . . ? C2 C1 C6 119.59(18) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 119.8(2) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 122.3(2) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 117.95(19) . . ? C5 C6 C7 120.26(18) . . ? C1 C6 C7 121.61(17) . . ? C8 C7 C12 118.23(19) . . ? C8 C7 C6 118.1(2) . . ? C12 C7 C6 123.61(19) . . ? C9 C8 C7 121.9(2) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 121.2(2) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? O2 C12 C11 118.7(2) . . ? O2 C12 C7 122.33(18) . . ? C11 C12 C7 119.0(2) . . ? N1 C13 C14 123.5(2) . . ? N1 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 120.2(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C17 116.7(2) . . ? C14 C15 C16 121.6(2) . . ? C17 C15 C16 121.7(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C15 119.8(2) . . ? C18 C17 H17 120.1 . . ? C15 C17 H17 120.1 . . ? N1 C18 C17 123.5(2) . . ? N1 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? N2 C19 C20 122.98(19) . . ? N2 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C19 C20 C21 120.41(19) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C23 C21 C20 116.4(2) . . ? C23 C21 C22 121.08(19) . . ? C20 C21 C22 122.48(19) . . ? 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 . . ? C24 C23 C21 120.3(2) . . ? C24 C23 H23 119.8 . . ? C21 C23 H23 119.8 . . ? N2 C24 C23 123.1(2) . . ? N2 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? O3 C25 C26 121.09(19) . . ? O3 C25 C30 117.53(19) . . ? C26 C25 C30 121.38(19) . . ? C27 C26 C25 119.9(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 119.7(2) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 122.2(2) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C25 C30 C29 116.7(2) . . ? C25 C30 C31 122.90(18) . . ? C29 C30 C31 120.4(2) . . ? C32 C31 C36 117.8(2) . . ? C32 C31 C30 118.9(2) . . ? C36 C31 C30 123.3(2) . . ? C33 C32 C31 122.0(3) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C34 C33 C32 118.90(16) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C33 C34 C35 120.78(15) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? O4 C36 C35 116.6(2) . . ? O4 C36 C31 123.1(2) . . ? C35 C36 C31 120.2(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.283 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.055 # Attachment '- Co8(3).cif' data_nb257L1 _database_code_depnum_ccdc_archive 'CCDC 852545' #TrackingRef '- Co8(3).cif' _audit_creation_date 11-10-07 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 'NB257L-1 in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _chemical_compound_source 'Leigh F. Jones' _exptl_crystal_recrystallization_method ; Slow evaporation of the mother liquor ; _publ_section_exptl_refinement ; The H atoms were all positioned geometrically. U~iso~(H) (in the range 1.2 times U~eq~ of the parent atom), the positions were refined with riding constraints. one of the ligands is disordered over two orientations and had to be refined isotropically with rigid body restraints on the aromatic rings. see the bottom part of the file for the full list of the applied restraints. #-------------------------------------------------------------- CHECKCIF OUTPUT: #-------------------------------------------------------------- 093_ALERT_1_B No su's on H-atoms, but refinement reported as . mixed H atoms on the aromatic rings treated as rigid bodies do not have su associated with them. 301_ALERT_3_B Note: Main Residue Disorder ................... 18.00 Perc. one ligand is disordered over two different orientations. 432_ALERT_2_B Short Inter X...Y Contact C43 .. C61 .. 2.76 Ang. 432_ALERT_2_B Short Inter X...Y Contact C61 .. C65 .. 2.84 Ang. 411_ALERT_2_G Short Inter H...H Contact H411 .. H671 .. 2.00 Ang. 432_ALERT_2_G Short Inter X...Y Contact C57 .. C61 .. 3.15 Ang. these alerts are caused by disordered atoms with no full occupancy. 912_ALERT_4_B Missing # of FCF Reflections Above STh/L= 0.600 1917 029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.95 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 14 the completeness is 100% up to 0.82 angstrom. INTENSITY STATISTICS FOR DATASET # 1 nb257l1.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.11 584 602 97.0 3.72 401.1 46.43 0.0234 0.0161 2.11 - 1.67 588 588 100.0 2.85 225.4 23.61 0.0292 0.0284 1.67 - 1.45 614 614 100.0 2.59 219.7 20.44 0.0380 0.0327 1.45 - 1.32 590 590 100.0 2.51 134.5 14.70 0.0468 0.0488 1.32 - 1.22 635 635 100.0 2.28 94.4 10.39 0.0592 0.0687 1.22 - 1.14 677 677 100.0 2.13 66.4 7.59 0.0672 0.0958 1.14 - 1.08 629 629 100.0 2.05 56.7 6.55 0.0765 0.1135 1.08 - 1.03 672 672 100.0 1.94 57.3 5.99 0.0792 0.1201 1.03 - 0.99 634 634 100.0 1.88 56.1 5.63 0.0846 0.1317 0.99 - 0.95 753 753 100.0 1.80 51.3 4.91 0.1061 0.1503 0.95 - 0.92 625 625 100.0 1.72 41.0 3.96 0.1280 0.1860 0.92 - 0.89 735 735 100.0 1.66 32.1 3.18 0.1564 0.2345 0.89 - 0.86 834 834 100.0 1.60 24.4 2.52 0.1948 0.3050 0.86 - 0.84 638 638 100.0 1.53 19.3 2.11 0.2094 0.3864 0.84 - 0.82 691 691 100.0 1.49 17.0 1.90 0.2479 0.4399 0.82 - 0.80 728 773 94.2 1.35 18.5 1.86 0.2392 0.4234 0.80 - 0.77 684 1288 53.1 0.67 15.3 1.58 0.2853 0.5171 0.77 - 0.73 285 1595 17.9 0.20 11.3 1.22 0.3267 0.6827 #----------------------------------------------------------------------------- 0.82 - 0.73 2055 4014 51.2 0.68 16.1 1.67 0.2589 0.4834 Inf - 0.73 11596 13573 85.4 1.68 82.4 8.77 0.0474 0.0871 Merged [A], lowest resolution = 6.94 Angstroms, 374 outliers downweighted 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.64 Ratio 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.67 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O68 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C52 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C44 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C45 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C46 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C47 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C49 222_ALERT_3_G Large Non-Solvent H Uiso(max)/Uso(min) ... 4.09 Ratio 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C2 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C3 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C4 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C59 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C62 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C65 241_ALERT_2_G Check High Ueq as Compared to Neighbors for C74 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for Co4 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for O43 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C30 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C48 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C60 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C63 242_ALERT_2_G Check Low Ueq as Compared to Neighbors for C66 The vast majority of these alerts are caused by atoms belonging to the disordered ligand... therefore they are not unexpected. 795_ALERT_4_B C-Atom in CIF Coordinate List out of Sequence .. C1 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 1 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O3 Noted, but no action taken. ; #end of refcif _cell_length_a 12.7876(5) _cell_length_b 19.4297(7) _cell_length_c 20.1892(8) _cell_angle_alpha 90 _cell_angle_beta 103.649(4) _cell_angle_gamma 90 _cell_volume 4874.5(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C102 H64 Co8 N8 O19 # Dc = 1.48 Fooo = 2268.00 Mu = 13.98 M = 1088.57 # Found Formula = C104 H87 Co8 N9 O18 # Dc = 1.51 FOOO = 2268.00 Mu = 13.99 M = 1111.17 _chemical_formula_sum 'C104 H87 Co8 N9 O18' _chemical_formula_moiety 'C104 H87 Co8 N9 O18' _chemical_formula_weight 2222.35 _cell_measurement_temperature 149.9 _cell_measurement_reflns_used 6353 _cell_measurement_theta_min 2.9276 _cell_measurement_theta_max 29.1198 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 1.399 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_T_min 0.89329 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 149.9 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_measurement_method '\w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_theta 26.32 _reflns_odcompleteness_iscentric 1 _reflns_number_total 11257 _diffrn_reflns_number 22869 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.1319 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 11257 # Theoretical number of reflections is about 26152 _diffrn_reflns_theta_min 2.994 _diffrn_reflns_theta_max 29.184 _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 25.098 _diffrn_measured_fraction_theta_full 0.951 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.27 _refine_diff_density_max 1.10 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 6831 _refine_ls_number_restraints 475 _refine_ls_number_parameters 557 _oxford_refine_ls_R_factor_ref 0.0698 _refine_ls_wR_factor_ref 0.0232 _refine_ls_goodness_of_fit_ref 1.1163 _refine_ls_shift/su_max 0.0034579 _refine_ls_shift/su_mean 0.0001970 # The values computed from all data _oxford_reflns_number_all 11224 _refine_ls_R_factor_all 0.1285 _refine_ls_wR_factor_all 0.0331 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6831 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_gt 0.0232 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 8.33 -33.1 -4.97 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Co1 Co -0.03677(3) 0.43562(2) 0.45293(2) 0.0209 1.0000 Uani . . . . . . Co3 Co -0.00732(4) 0.44189(3) 0.29958(2) 0.0275 1.0000 Uani . . . . . . Co2 Co 0.03451(4) 0.57742(2) 0.38813(2) 0.0223 1.0000 Uani . . . . . . Co4 Co 0.15295(4) 0.69491(2) 0.49067(2) 0.0269 1.0000 Uani . . . . . . N8 N -0.1558(3) 0.48139(17) 0.25996(16) 0.0328 1.0000 Uani . U . . . . N15 N 0.0088(3) 0.74330(17) 0.46898(16) 0.0346 1.0000 Uani . U . . . . N59 N -0.0469(3) 0.63800(15) 0.30267(17) 0.0324 1.0000 Uani . U . . . . N62 N 0.0239(3) 0.3759(2) 0.22961(18) 0.0442 1.0000 Uani . U . . . . O2 O -0.02036(19) 0.61616(13) 0.61979(11) 0.0266 1.0000 Uani . U . . . . O4 O 0.09690(19) 0.51772(13) 0.31919(13) 0.0279 1.0000 Uani . U . . . . O6 O -0.09629(19) 0.50794(12) 0.36992(11) 0.0242 1.0000 Uani . U . . . . O13 O -0.02919(19) 0.62973(13) 0.45985(12) 0.0281 1.0000 Uani . U . . . . O17 O 0.16542(19) 0.64230(12) 0.40779(12) 0.0257 1.0000 Uani . U . . . . O30 O 0.16692(19) 0.62987(12) 0.56634(12) 0.0243 1.0000 Uani . U . . . . O57 O 0.08455(17) 0.50994(11) 0.47113(11) 0.0208 1.0000 Uani . U . . . . C7 C -0.1756(3) 0.51237(17) 0.31512(17) 0.0252 1.0000 Uani . U . . . . C9 C -0.2280(4) 0.4840(2) 0.1997(2) 0.0439 1.0000 Uani . U . . . . C10 C -0.3216(4) 0.5195(3) 0.1926(2) 0.0502 1.0000 Uani . U . . . . C11 C -0.3452(3) 0.5515(2) 0.2499(2) 0.0413 1.0000 Uani . U . . . . C12 C -0.2715(3) 0.54878(18) 0.3116(2) 0.0318 1.0000 Uani . U . . . . C14 C -0.0648(3) 0.69292(19) 0.45311(15) 0.0278 1.0000 Uani . U . . . . C18 C 0.1799(3) 0.6772(2) 0.35220(18) 0.0294 1.0000 Uani . U . . . . C19 C 0.2214(3) 0.6411(2) 0.30253(19) 0.0332 1.0000 Uani . U . . . . C20 C 0.2641(3) 0.5693(2) 0.3120(2) 0.0362 1.0000 Uani . U . . . . C21 C 0.2018(3) 0.51154(19) 0.32099(18) 0.0300 1.0000 Uani . U . . . . C22 C 0.2513(3) 0.44679(19) 0.32939(19) 0.0331 1.0000 Uani . U . . . . C23 C 0.3565(4) 0.4380(2) 0.3293(3) 0.0461 1.0000 Uani . U . . . . C24 C 0.4191(4) 0.4943(3) 0.3204(3) 0.0594 1.0000 Uani . U . . . . C25 C 0.3709(4) 0.5592(3) 0.3122(3) 0.0548 1.0000 Uani . U . . . . C26 C 0.2338(4) 0.6768(2) 0.2451(2) 0.0455 1.0000 Uani . U . . . . C27 C 0.2047(4) 0.7467(2) 0.2355(2) 0.0482 1.0000 Uani . U . . . . C28 C 0.1675(3) 0.7813(2) 0.2848(2) 0.0408 1.0000 Uani . U . . . . C29 C 0.1567(3) 0.7472(2) 0.3428(2) 0.0391 1.0000 Uani . U . . . . C31 C 0.2226(3) 0.64423(18) 0.63047(17) 0.0278 1.0000 Uani . U . . . . C32 C 0.3259(3) 0.61712(19) 0.65351(18) 0.0295 1.0000 Uani . U . . . . C33 C 0.3855(3) 0.6311(2) 0.7196(2) 0.0397 1.0000 Uani . U . . . . C34 C 0.3451(4) 0.6731(3) 0.7616(2) 0.0485 1.0000 Uani . U . . . . C35 C 0.2425(4) 0.7008(2) 0.7391(2) 0.0479 1.0000 Uani . U . . . . C36 C 0.1803(3) 0.68851(18) 0.67327(19) 0.0321 1.0000 Uani . U . . . . C37 C 0.0736(3) 0.7229(2) 0.6507(2) 0.0375 1.0000 Uani . U . . . . C38 C -0.0208(3) 0.68499(18) 0.62349(17) 0.0294 1.0000 Uani . U . . . . C39 C -0.1196(3) 0.7211(2) 0.6041(2) 0.0360 1.0000 Uani . U . . . . C40 C -0.1232(4) 0.7911(2) 0.6116(2) 0.0453 1.0000 Uani . U . . . . C41 C -0.0292(4) 0.8275(3) 0.6378(3) 0.0558 1.0000 Uani . U . . . . C42 C 0.0661(4) 0.7936(2) 0.6555(3) 0.0540 1.0000 Uani . U . . . . C53 C -0.0231(4) 0.8096(2) 0.4661(2) 0.0482 1.0000 Uani . U . . . . C54 C -0.1318(5) 0.8288(3) 0.4433(3) 0.0601 1.0000 Uani . U . . . . C55 C -0.2072(4) 0.7754(3) 0.4271(3) 0.0554 1.0000 Uani . U . . . . C56 C -0.1746(4) 0.7091(3) 0.4316(2) 0.0446 1.0000 Uani . U . . . . C58 C 0.1946(3) 0.48468(19) 0.48896(19) 0.0285 1.0000 Uani . U . . . . C60 C -0.0709(4) 0.6551(2) 0.2483(2) 0.0419 1.0000 Uani . U . . . . C61 C -0.0982(7) 0.6758(4) 0.1769(3) 0.0898 1.0000 Uani . U . . . . C63 C 0.0321(4) 0.3281(3) 0.1967(2) 0.0501 1.0000 Uani . U . . . . C64 C 0.0435(6) 0.2677(4) 0.1580(4) 0.0906 1.0000 Uani . U . . . . N65 N 0.5912(8) 0.6241(5) 0.4262(5) 0.0649(17) 0.5000 Uiso . U . . 1 . C1 C 0.5279(10) 0.5971(7) 0.4455(6) 0.0653(18) 0.5000 Uiso D U . . 1 . C30 C 0.4460(10) 0.5677(6) 0.4760(7) 0.0672(19) 0.5000 Uiso D U . . 1 . C65 C 0.4723(8) 0.8454(5) 0.5550(6) 0.1143(18) 0.5000 Uiso G U . . 2 . C43 C 0.5521(8) 0.8709(6) 0.6090(6) 0.116(2) 0.5000 Uiso G U . . 2 . C57 C 0.5458(8) 0.9384(6) 0.6315(5) 0.117(2) 0.5000 Uiso G U . . 2 . C76 C 0.4597(10) 0.9805(5) 0.5999(6) 0.117(2) 0.5000 Uiso G U . . 2 . C100 C 0.3799(8) 0.9550(4) 0.5458(6) 0.116(2) 0.5000 Uiso G U . . 2 . C59 C 0.3862(7) 0.8875(4) 0.5234(4) 0.1157(19) 0.5000 Uiso G U . . 2 . O3 O 0.2958(8) 0.8708(6) 0.4665(5) 0.118(2) 0.5000 Uiso G U . . 2 . O68 O 0.2743(10) 0.7595(7) 0.5128(7) 0.104(2) 0.5000 Uiso . U . . 2 . C2 C 0.3844(8) 0.7287(6) 0.5113(7) 0.1071(19) 0.5000 Uiso G U . . 2 . C62 C 0.4016(8) 0.6615(6) 0.4921(7) 0.107(2) 0.5000 Uiso G U . . 2 . C3 C 0.5049(10) 0.6401(5) 0.4906(7) 0.108(2) 0.5000 Uiso G U . . 2 . C74 C 0.5909(7) 0.6857(6) 0.5083(7) 0.109(2) 0.5000 Uiso G U . . 2 . C4 C 0.5736(9) 0.7528(6) 0.5274(7) 0.109(2) 0.5000 Uiso G U . . 2 . C52 C 0.4704(10) 0.7743(5) 0.5289(7) 0.1098(18) 0.5000 Uiso G U . . 2 . O43 O 0.2453(5) 0.7754(3) 0.5134(3) 0.0384(12) 0.5000 Uiso . U . . 1 . C44 C 0.3477(4) 0.7855(3) 0.5111(3) 0.0465(11) 0.5000 Uiso G U . . 1 . C45 C 0.4257(5) 0.7358(2) 0.5358(3) 0.0484(12) 0.5000 Uiso G U . . 1 . C46 C 0.5333(4) 0.7496(3) 0.5383(4) 0.0531(13) 0.5000 Uiso G U . . 1 . C47 C 0.5628(4) 0.8131(3) 0.5161(4) 0.0573(14) 0.5000 Uiso G U . . 1 . C48 C 0.4848(5) 0.8629(3) 0.4913(4) 0.0579(13) 0.5000 Uiso G U . . 1 . C49 C 0.3772(4) 0.8491(3) 0.4888(4) 0.0562(11) 0.5000 Uiso G U . . 1 . O52 O 0.1983(6) 0.8943(4) 0.5477(3) 0.0709(15) 0.5000 Uiso G U . . 1 . C50 C 0.2060(4) 0.9241(3) 0.4854(2) 0.0735(13) 0.5000 Uiso G U . . 1 . C51 C 0.1183(5) 0.9723(4) 0.4419(3) 0.0784(16) 0.5000 Uiso G U . . 1 . C67 C 0.1289(6) 0.9978(5) 0.3699(3) 0.0819(17) 0.5000 Uiso G U . . 1 . C68 C 0.2271(7) 0.9751(5) 0.3414(3) 0.0815(17) 0.5000 Uiso G U . . 1 . C69 C 0.3148(6) 0.9268(5) 0.3849(4) 0.0766(15) 0.5000 Uiso G U . . 1 . C66 C 0.3043(5) 0.9013(4) 0.4570(3) 0.0692(13) 0.5000 Uiso G U . . 1 . H91 H -0.2134 0.4607 0.1615 0.0530 1.0000 Uiso R . . . . . H101 H -0.3707 0.5226 0.1493 0.0604 1.0000 Uiso R . . . . . H111 H -0.4116 0.5749 0.2459 0.0492 1.0000 Uiso R . . . . . H121 H -0.2853 0.5708 0.3506 0.0382 1.0000 Uiso R . . . . . H221 H 0.2099 0.4077 0.3355 0.0400 1.0000 Uiso R . . . . . H231 H 0.3877 0.3934 0.3353 0.0554 1.0000 Uiso R . . . . . H241 H 0.4927 0.4887 0.3199 0.0711 1.0000 Uiso R . . . . . H251 H 0.4134 0.5980 0.3067 0.0657 1.0000 Uiso R . . . . . H261 H 0.2622 0.6537 0.2117 0.0546 1.0000 Uiso R . . . . . H271 H 0.2109 0.7700 0.1952 0.0577 1.0000 Uiso R . . . . . H281 H 0.1493 0.8287 0.2790 0.0491 1.0000 Uiso R . . . . . H291 H 0.1328 0.7720 0.3770 0.0470 1.0000 Uiso R . . . . . H321 H 0.3559 0.5891 0.6241 0.0355 1.0000 Uiso R . . . . . H331 H 0.4547 0.6110 0.7354 0.0480 1.0000 Uiso R . . . . . H341 H 0.3868 0.6834 0.8060 0.0582 1.0000 Uiso R . . . . . H351 H 0.2140 0.7288 0.7692 0.0573 1.0000 Uiso R . . . . . H391 H -0.1840 0.6965 0.5855 0.0431 1.0000 Uiso R . . . . . H401 H -0.1901 0.8146 0.5990 0.0545 1.0000 Uiso R . . . . . H411 H -0.0315 0.8760 0.6432 0.0669 1.0000 Uiso R . . . . . H421 H 0.1300 0.8194 0.6719 0.0646 1.0000 Uiso R . . . . . H531 H 0.0296 0.8445 0.4801 0.0576 1.0000 Uiso R . . . . . H541 H -0.1531 0.8758 0.4391 0.0722 1.0000 Uiso R . . . . . H551 H -0.2817 0.7860 0.4128 0.0663 1.0000 Uiso R . . . . . H561 H -0.2262 0.6733 0.4201 0.0537 1.0000 Uiso R . . . . . H611 H -0.1641 0.7006 0.1674 0.1066 1.0000 Uiso R . . . . . H612 H -0.0427 0.7042 0.1679 0.1066 1.0000 Uiso R . . . . . H613 H -0.1057 0.6360 0.1488 0.1066 1.0000 Uiso R . . . . . H641 H 0.0238 0.2782 0.1107 0.1093 1.0000 Uiso R . . . . . H642 H 0.1162 0.2526 0.1700 0.1093 1.0000 Uiso R . . . . . H643 H -0.0019 0.2323 0.1678 0.1093 1.0000 Uiso R . . . . . H581 H 0.2038 0.4550 0.5273 0.0346 1.0000 Uiso R . . . . . H582 H 0.2427 0.5225 0.4998 0.0346 1.0000 Uiso R . . . . . H583 H 0.2092 0.4601 0.4515 0.0346 1.0000 Uiso R . . . . . H301 H 0.4159 0.5282 0.4509 0.0807 0.5000 Uiso R . . . 1 . H302 H 0.4777 0.5550 0.5217 0.0807 0.5000 Uiso R . . . 1 . H303 H 0.3910 0.6008 0.4753 0.0807 0.5000 Uiso R . . . 1 . H431 H 0.6103 0.8422 0.6306 0.1391 0.5000 Uiso . . . . 2 . H571 H 0.6001 0.9558 0.6681 0.1404 0.5000 Uiso . . . . 2 . H761 H 0.4555 1.0264 0.6151 0.1402 0.5000 Uiso . . . . 2 . H1001 H 0.3210 0.9834 0.5245 0.1394 0.5000 Uiso . . . . 2 . H621 H 0.3428 0.6305 0.4795 0.1276 0.5000 Uiso . . . . 2 . H31 H 0.5166 0.5942 0.4775 0.1294 0.5000 Uiso . . . . 2 . H741 H 0.6615 0.6707 0.5076 0.1300 0.5000 Uiso . . . . 2 . H41 H 0.6326 0.7837 0.5398 0.1307 0.5000 Uiso . . . . 2 . H451 H 0.4053 0.6926 0.5508 0.0581 0.5000 Uiso . . . . 1 . H461 H 0.5865 0.7158 0.5550 0.0638 0.5000 Uiso . . . . 1 . H471 H 0.6364 0.8225 0.5177 0.0688 0.5000 Uiso . . . . 1 . H481 H 0.5052 0.9061 0.4762 0.0695 0.5000 Uiso . . . . 1 . H511 H 0.0583 0.9860 0.4592 0.0940 0.5000 Uiso . . . . 1 . H671 H 0.0749 1.0270 0.3438 0.0984 0.5000 Uiso . . . . 1 . H681 H 0.2329 0.9904 0.2979 0.0980 0.5000 Uiso . . . . 1 . H691 H 0.3742 0.9128 0.3677 0.0919 0.5000 Uiso . . . . 1 . H520 H 0.1930 0.8505 0.5508 0.0852 0.5000 Uiso . . . . 1 . H30 H 0.2400 0.8461 0.4673 0.1414 0.5000 Uiso . . . . 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 0.0219(2) 0.0240(2) 0.0175(2) -0.00234(16) 0.00625(16) -0.00380(17) Co3 0.0287(2) 0.0341(3) 0.0213(2) -0.00503(19) 0.00907(18) -0.00239(19) Co2 0.0250(2) 0.0258(2) 0.0178(2) 0.00002(16) 0.00818(16) -0.00388(17) Co4 0.0277(2) 0.0286(2) 0.0248(2) -0.0013(2) 0.00701(18) -0.0051(2) N8 0.0351(16) 0.0372(17) 0.0254(13) -0.0001(12) 0.0058(10) -0.0007(13) N15 0.0386(15) 0.0334(14) 0.0327(16) 0.0102(13) 0.0101(13) 0.0023(11) N59 0.0415(17) 0.0259(15) 0.0311(14) 0.0045(12) 0.0109(13) -0.0009(13) N62 0.045(2) 0.056(2) 0.0310(18) -0.0094(14) 0.0086(15) 0.0047(17) O2 0.0333(12) 0.0313(11) 0.0190(11) -0.0083(9) 0.0137(9) -0.0019(10) O4 0.0248(11) 0.0327(13) 0.0275(13) -0.0061(9) 0.0089(9) -0.0024(9) O6 0.0268(11) 0.0255(12) 0.0189(11) -0.0025(9) 0.0031(8) -0.0050(9) O13 0.0352(13) 0.0299(11) 0.0206(11) 0.0006(9) 0.0096(10) -0.0020(10) O17 0.0276(12) 0.0264(11) 0.0239(12) 0.0006(9) 0.0078(9) -0.0019(9) O30 0.0287(12) 0.0210(11) 0.0211(11) -0.0028(8) 0.0016(8) -0.0047(9) O57 0.0178(10) 0.0219(11) 0.0234(11) -0.0034(9) 0.0064(8) -0.0030(8) C7 0.0264(14) 0.0269(17) 0.0225(14) 0.0049(12) 0.0065(10) -0.0067(11) C9 0.043(2) 0.058(3) 0.0269(17) -0.0060(18) 0.0011(14) -0.0076(17) C10 0.047(2) 0.060(3) 0.036(2) 0.0070(17) -0.0052(17) 0.0006(18) C11 0.0296(18) 0.044(2) 0.0468(18) 0.0141(16) 0.0023(13) 0.0060(16) C12 0.0293(15) 0.0265(17) 0.0394(17) 0.0053(14) 0.0077(12) -0.0045(12) C14 0.0326(15) 0.0349(14) 0.0164(15) -0.0006(13) 0.0069(12) 0.0039(11) C18 0.0251(17) 0.0365(15) 0.0282(16) 0.0025(12) 0.0097(13) -0.0009(13) C19 0.0332(18) 0.0359(15) 0.0347(18) 0.0016(13) 0.0161(15) -0.0026(14) C20 0.0401(17) 0.0356(14) 0.040(2) 0.0000(15) 0.0238(16) 0.0019(13) C21 0.0302(14) 0.0387(15) 0.0253(18) -0.0004(14) 0.0148(14) 0.0020(12) C22 0.0365(15) 0.0335(16) 0.0306(18) -0.0125(14) 0.0107(14) -0.0043(13) C23 0.0406(17) 0.0350(18) 0.065(3) -0.0047(19) 0.0164(19) 0.0062(15) C24 0.034(2) 0.047(2) 0.105(4) -0.017(3) 0.032(2) -0.0012(14) C25 0.0375(18) 0.045(2) 0.090(4) -0.004(2) 0.031(2) -0.0020(16) C26 0.062(3) 0.0472(19) 0.0350(19) 0.0011(15) 0.027(2) -0.001(2) C27 0.055(3) 0.050(2) 0.044(2) 0.0153(18) 0.022(2) 0.000(2) C28 0.038(2) 0.0350(18) 0.050(2) 0.0129(14) 0.0113(16) 0.0041(16) C29 0.040(2) 0.0353(16) 0.045(2) 0.0052(15) 0.0174(17) -0.0018(16) C31 0.0288(15) 0.0321(18) 0.0204(14) -0.0015(12) 0.0013(11) -0.0027(12) C32 0.0288(15) 0.0293(17) 0.0291(15) -0.0023(13) 0.0044(12) -0.0029(12) C33 0.0308(18) 0.048(2) 0.0353(17) -0.0048(15) -0.0021(13) -0.0033(16) C34 0.045(2) 0.059(3) 0.033(2) -0.0135(17) -0.0087(15) -0.0004(18) C35 0.049(2) 0.046(2) 0.041(2) -0.0243(19) -0.0026(16) 0.0053(18) C36 0.0386(17) 0.0256(17) 0.0313(15) -0.0080(13) 0.0065(12) -0.0040(13) C37 0.0383(16) 0.0385(16) 0.034(2) -0.0128(16) 0.0048(15) -0.0004(12) C38 0.0343(15) 0.0316(14) 0.0228(16) -0.0059(14) 0.0077(12) 0.0024(12) C39 0.0287(16) 0.0507(17) 0.0314(19) -0.0121(16) 0.0126(14) 0.0032(14) C40 0.0375(19) 0.0516(19) 0.046(2) -0.0093(19) 0.0091(17) 0.0166(15) C41 0.057(2) 0.044(2) 0.064(3) -0.023(2) 0.008(2) 0.0068(15) C42 0.045(2) 0.0371(17) 0.073(3) -0.017(2) 0.001(2) -0.0040(16) C53 0.065(2) 0.0312(16) 0.054(3) -0.0011(18) 0.026(2) 0.0017(18) C54 0.081(3) 0.052(2) 0.047(3) 0.013(2) 0.016(2) 0.0301(18) C55 0.050(2) 0.074(2) 0.042(2) -0.003(2) 0.0104(19) 0.0333(17) C56 0.0368(17) 0.061(2) 0.0335(19) -0.0056(18) 0.0039(16) 0.0129(17) C58 0.0190(14) 0.039(2) 0.0292(18) 0.0027(14) 0.0085(12) 0.0031(13) C60 0.050(2) 0.038(2) 0.0336(17) 0.0052(16) 0.0031(18) -0.0035(18) C61 0.127(6) 0.087(4) 0.043(2) 0.028(3) -0.004(3) -0.001(4) C63 0.046(2) 0.055(2) 0.045(2) -0.0125(18) 0.0023(19) 0.010(2) C64 0.089(4) 0.089(4) 0.083(5) -0.049(4) -0.001(4) 0.022(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.060(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . O13 2_566 2.173(2) yes Co1 . O57 2_566 2.070(2) yes Co1 . O30 2_566 2.058(2) yes Co1 . O2 2_566 2.051(2) yes Co1 . O6 . 2.182(2) yes Co1 . O57 . 2.088(2) yes Co3 . O2 2_566 1.943(2) yes Co3 . N8 . 2.029(3) yes Co3 . N62 . 2.016(4) yes Co3 . O4 . 1.963(2) yes Co3 . O6 . 2.392(2) yes Co2 . N59 . 2.144(3) yes Co2 . O4 . 2.108(2) yes Co2 . O6 . 2.113(2) yes Co2 . O13 . 2.086(2) yes Co2 . O17 . 2.058(2) yes Co2 . O57 . 2.105(2) yes Co4 . N15 . 2.023(3) yes Co4 . O13 . 2.595(2) yes Co4 . O17 . 1.999(2) yes Co4 . O30 . 1.958(2) yes Co4 . O43 . 1.948(6) yes N8 . C7 . 1.342(5) yes N8 . C9 . 1.344(5) yes N15 . C14 . 1.343(5) yes N15 . C53 . 1.348(6) yes N59 . C60 . 1.118(5) yes N62 . C63 . 1.161(6) yes O2 . C38 . 1.339(4) yes O4 . C21 . 1.338(4) yes O6 . C7 . 1.316(4) yes O13 . C14 . 1.305(5) yes O17 . C18 . 1.360(4) yes O30 . C31 . 1.352(4) yes O57 . C58 . 1.453(4) yes C7 . C12 . 1.403(5) yes C9 . C10 . 1.360(7) yes C9 . H91 . 0.950 no C10 . C11 . 1.407(7) yes C10 . H101 . 0.950 no C11 . C12 . 1.374(6) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 no C14 . C56 . 1.404(6) yes C18 . C19 . 1.426(5) yes C18 . C29 . 1.395(6) yes C19 . C20 . 1.493(5) yes C19 . C26 . 1.392(6) yes C20 . C21 . 1.413(5) yes C20 . C25 . 1.379(6) yes C21 . C22 . 1.401(5) yes C22 . C23 . 1.357(6) yes C22 . H221 . 0.950 no C23 . C24 . 1.391(7) yes C23 . H231 . 0.950 no C24 . C25 . 1.397(7) yes C24 . H241 . 0.950 no C25 . H251 . 0.950 no C26 . C27 . 1.410(7) yes C26 . H261 . 0.950 no C27 . C28 . 1.375(7) yes C27 . H271 . 0.950 no C28 . C29 . 1.381(6) yes C28 . H281 . 0.950 no C29 . H291 . 0.950 no C31 . C32 . 1.396(5) yes C31 . C36 . 1.414(5) yes C32 . C33 . 1.398(5) yes C32 . H321 . 0.950 no C33 . C34 . 1.364(6) yes C33 . H331 . 0.950 no C34 . C35 . 1.391(6) yes C34 . H341 . 0.950 no C35 . C36 . 1.399(5) yes C35 . H351 . 0.950 no C36 . C37 . 1.491(6) yes C37 . C38 . 1.410(5) yes C37 . C42 . 1.383(6) yes C38 . C39 . 1.417(5) yes C39 . C40 . 1.371(6) yes C39 . H391 . 0.950 no C40 . C41 . 1.388(7) yes C40 . H401 . 0.950 no C41 . C42 . 1.355(7) yes C41 . H411 . 0.950 no C42 . H421 . 0.950 no C53 . C54 . 1.408(7) yes C53 . H531 . 0.950 no C54 . C55 . 1.402(8) yes C54 . H541 . 0.950 no C55 . C56 . 1.350(7) yes C55 . H551 . 0.950 no C56 . H561 . 0.950 no C58 . H581 . 0.950 no C58 . H582 . 0.950 no C58 . H583 . 0.950 no C60 . C61 . 1.458(7) yes C61 . H611 . 0.950 no C61 . H612 . 0.950 no C61 . H613 . 0.950 no C63 . C64 . 1.436(7) yes C64 . H641 . 0.950 no C64 . H642 . 0.950 no C64 . H643 . 0.950 no N65 . C1 . 1.110(14) yes C1 . C30 . 1.451(16) yes C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C65 . C43 . 1.39713(7) yes C65 . C59 . 1.399 yes C65 . C52 . 1.477(12) yes C43 . C57 . 1.39701(6) yes C43 . H431 . 0.950 no C57 . C76 . 1.399 yes C57 . H571 . 0.948 no C76 . C100 . 1.39712(7) yes C76 . H761 . 0.949 no C100 . C59 . 1.39701(6) yes C100 . H1001 . 0.950 no C59 . O3 . 1.46074(8) yes O3 . H30 . 0.863 no O68 . C2 . 1.536(15) yes C2 . C62 . 1.392 yes C2 . C52 . 1.39210(6) yes C62 . C3 . 1.39199(7) yes C62 . H621 . 0.950 no C3 . C74 . 1.39210(6) yes C3 . H31 . 0.952 no C74 . C4 . 1.392 yes C74 . H741 . 0.952 no C4 . C52 . 1.39198(7) yes C4 . H41 . 0.950 no O43 . C44 . 1.335(8) yes C44 . C45 . 1.394 yes C44 . C49 . 1.396 yes C45 . C46 . 1.39103(5) yes C45 . H451 . 0.949 no C46 . C47 . 1.396 yes C46 . H461 . 0.950 no C47 . C48 . 1.394 yes C47 . H471 . 0.951 no C48 . C49 . 1.39103(5) yes C48 . H481 . 0.951 no C49 . C66 . 1.426(7) yes O52 . C50 . 1.408 yes O52 . H520 . 0.857 no C50 . C51 . 1.56341(6) yes C50 . C66 . 1.56393(6) yes C51 . C67 . 1.57154(6) yes C51 . H511 . 0.953 no C67 . C68 . 1.56392(6) yes C67 . H671 . 0.950 no C68 . C69 . 1.56340(6) yes C68 . H681 . 0.947 no C69 . C66 . 1.57154(6) yes C69 . H691 . 0.947 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O13 2_566 Co1 . O57 2_566 79.89(9) yes O13 2_566 Co1 . O30 2_566 86.21(9) yes O57 2_566 Co1 . O30 2_566 95.12(9) yes O13 2_566 Co1 . O2 2_566 99.07(10) yes O57 2_566 Co1 . O2 2_566 176.35(9) yes O30 2_566 Co1 . O2 2_566 88.29(10) yes O13 2_566 Co1 . O6 . 175.52(9) yes O57 2_566 Co1 . O6 . 97.43(9) yes O30 2_566 Co1 . O6 . 97.65(9) yes O2 2_566 Co1 . O6 . 83.38(9) yes O13 2_566 Co1 . O57 . 97.54(9) yes O57 2_566 Co1 . O57 . 81.56(9) yes O30 2_566 Co1 . O57 . 174.43(9) yes O2 2_566 Co1 . O57 . 95.15(9) yes O6 . Co1 . O57 . 78.45(9) yes O2 2_566 Co3 . N8 . 121.23(12) yes O2 2_566 Co3 . N62 . 101.00(13) yes N8 . Co3 . N62 . 106.60(14) yes O2 2_566 Co3 . O4 . 106.61(10) yes N8 . Co3 . O4 . 108.85(12) yes N62 . Co3 . O4 . 112.41(13) yes O2 2_566 Co3 . O6 . 80.34(9) yes N8 . Co3 . O6 . 59.95(11) yes N62 . Co3 . O6 . 163.29(12) yes O4 . Co3 . O6 . 82.71(9) yes N59 . Co2 . O4 . 87.61(11) yes N59 . Co2 . O6 . 89.81(10) yes O4 . Co2 . O6 . 86.62(9) yes N59 . Co2 . O13 . 95.51(11) yes O4 . Co2 . O13 . 175.77(10) yes O6 . Co2 . O13 . 90.54(9) yes N59 . Co2 . O17 . 92.14(11) yes O4 . Co2 . O17 . 92.69(10) yes O6 . Co2 . O17 . 177.91(10) yes O13 . Co2 . O17 . 90.04(10) yes N59 . Co2 . O57 . 168.85(11) yes O4 . Co2 . O57 . 95.26(10) yes O6 . Co2 . O57 . 79.63(9) yes O13 . Co2 . O57 . 81.15(9) yes O17 . Co2 . O57 . 98.47(9) yes N15 . Co4 . O13 . 56.93(11) yes N15 . Co4 . O17 . 107.76(12) yes O13 . Co4 . O17 . 78.12(8) yes N15 . Co4 . O30 . 112.30(12) yes O13 . Co4 . O30 . 77.50(9) yes O17 . Co4 . O30 . 108.21(10) yes N15 . Co4 . O43 . 98.6(2) yes O13 . Co4 . O43 . 155.29(19) yes O17 . Co4 . O43 . 116.3(2) yes O30 . Co4 . O43 . 113.3(2) yes Co3 . N8 . C7 . 100.7(2) yes Co3 . N8 . C9 . 138.6(3) yes C7 . N8 . C9 . 120.7(3) yes Co4 . N15 . C14 . 105.3(2) yes Co4 . N15 . C53 . 134.8(3) yes C14 . N15 . C53 . 119.9(4) yes Co2 . N59 . C60 . 157.1(3) yes Co3 . N62 . C63 . 165.7(4) yes Co1 2_566 O2 . Co3 2_566 106.84(12) yes Co1 2_566 O2 . C38 . 122.4(2) yes Co3 2_566 O2 . C38 . 122.36(19) yes Co2 . O4 . Co3 . 101.62(11) yes Co2 . O4 . C21 . 124.4(2) yes Co3 . O4 . C21 . 124.5(2) yes Co1 . O6 . Co2 . 99.17(9) yes Co1 . O6 . Co3 . 88.96(9) yes Co2 . O6 . Co3 . 88.75(9) yes Co1 . O6 . C7 . 138.4(2) yes Co2 . O6 . C7 . 121.8(2) yes Co3 . O6 . C7 . 85.2(2) yes Co1 2_566 O13 . Co2 . 97.89(10) yes Co1 2_566 O13 . Co4 . 86.33(8) yes Co2 . O13 . Co4 . 85.92(8) yes Co1 2_566 O13 . C14 . 133.9(2) yes Co2 . O13 . C14 . 124.7(2) yes Co4 . O13 . C14 . 80.6(2) yes Co2 . O17 . Co4 . 104.64(10) yes Co2 . O17 . C18 . 114.1(2) yes Co4 . O17 . C18 . 119.3(2) yes Co1 2_566 O30 . Co4 . 109.32(11) yes Co1 2_566 O30 . C31 . 121.9(2) yes Co4 . O30 . C31 . 123.0(2) yes Co2 . O57 . Co1 . 102.53(9) yes Co2 . O57 . Co1 2_566 100.60(9) yes Co1 . O57 . Co1 2_566 98.44(9) yes Co2 . O57 . C58 . 120.2(2) yes Co1 . O57 . C58 . 116.49(19) yes Co1 2_566 O57 . C58 . 115.3(2) yes N8 . C7 . O6 . 114.2(3) yes N8 . C7 . C12 . 121.2(3) yes O6 . C7 . C12 . 124.6(3) yes N8 . C9 . C10 . 120.9(4) yes N8 . C9 . H91 . 119.5 no C10 . C9 . H91 . 119.6 no C9 . C10 . C11 . 119.5(4) yes C9 . C10 . H101 . 120.2 no C11 . C10 . H101 . 120.3 no C10 . C11 . C12 . 119.6(4) yes C10 . C11 . H111 . 120.2 no C12 . C11 . H111 . 120.3 no C7 . C12 . C11 . 118.0(4) yes C7 . C12 . H121 . 121.0 no C11 . C12 . H121 . 120.9 no N15 . C14 . O13 . 116.9(3) yes N15 . C14 . C56 . 120.2(4) yes O13 . C14 . C56 . 122.8(4) yes O17 . C18 . C19 . 118.7(3) yes O17 . C18 . C29 . 122.1(3) yes C19 . C18 . C29 . 119.1(3) yes C18 . C19 . C20 . 123.7(3) yes C18 . C19 . C26 . 118.3(4) yes C20 . C19 . C26 . 117.6(3) yes C19 . C20 . C21 . 123.9(3) yes C19 . C20 . C25 . 117.7(4) yes C21 . C20 . C25 . 118.3(4) yes C20 . C21 . O4 . 121.1(3) yes C20 . C21 . C22 . 118.5(3) yes O4 . C21 . C22 . 120.4(3) yes C21 . C22 . C23 . 122.2(4) yes C21 . C22 . H221 . 118.9 no C23 . C22 . H221 . 118.9 no C22 . C23 . C24 . 120.2(4) yes C22 . C23 . H231 . 120.0 no C24 . C23 . H231 . 119.8 no C23 . C24 . C25 . 118.3(4) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 120.8 no C24 . C25 . C20 . 122.5(4) yes C24 . C25 . H251 . 118.7 no C20 . C25 . H251 . 118.7 no C19 . C26 . C27 . 121.1(4) yes C19 . C26 . H261 . 119.5 no C27 . C26 . H261 . 119.3 no C26 . C27 . C28 . 119.7(4) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.0 no C27 . C28 . C29 . 120.0(4) yes C27 . C28 . H281 . 120.0 no C29 . C28 . H281 . 120.0 no C18 . C29 . C28 . 121.5(4) yes C18 . C29 . H291 . 119.3 no C28 . C29 . H291 . 119.2 no O30 . C31 . C32 . 119.0(3) yes O30 . C31 . C36 . 121.3(3) yes C32 . C31 . C36 . 119.6(3) yes C31 . C32 . C33 . 120.3(4) yes C31 . C32 . H321 . 119.9 no C33 . C32 . H321 . 119.8 no C32 . C33 . C34 . 120.5(4) yes C32 . C33 . H331 . 119.8 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 119.7(4) yes C33 . C34 . H341 . 120.2 no C35 . C34 . H341 . 120.2 no C34 . C35 . C36 . 121.7(4) yes C34 . C35 . H351 . 119.2 no C36 . C35 . H351 . 119.1 no C31 . C36 . C35 . 118.1(4) yes C31 . C36 . C37 . 122.7(3) yes C35 . C36 . C37 . 119.2(3) yes C36 . C37 . C38 . 121.5(3) yes C36 . C37 . C42 . 119.9(4) yes C38 . C37 . C42 . 118.6(4) yes C37 . C38 . O2 . 121.9(3) yes C37 . C38 . C39 . 118.4(3) yes O2 . C38 . C39 . 119.6(3) yes C38 . C39 . C40 . 120.8(4) yes C38 . C39 . H391 . 119.6 no C40 . C39 . H391 . 119.6 no C39 . C40 . C41 . 119.9(4) yes C39 . C40 . H401 . 120.0 no C41 . C40 . H401 . 120.1 no C40 . C41 . C42 . 119.8(4) yes C40 . C41 . H411 . 120.1 no C42 . C41 . H411 . 120.1 no C37 . C42 . C41 . 122.5(4) yes C37 . C42 . H421 . 118.7 no C41 . C42 . H421 . 118.8 no N15 . C53 . C54 . 122.2(5) yes N15 . C53 . H531 . 118.9 no C54 . C53 . H531 . 118.9 no C53 . C54 . C55 . 116.8(4) yes C53 . C54 . H541 . 121.6 no C55 . C54 . H541 . 121.6 no C54 . C55 . C56 . 120.4(5) yes C54 . C55 . H551 . 119.7 no C56 . C55 . H551 . 119.9 no C14 . C56 . C55 . 120.3(5) yes C14 . C56 . H561 . 119.9 no C55 . C56 . H561 . 119.8 no O57 . C58 . H581 . 109.5 no O57 . C58 . H582 . 109.4 no H581 . C58 . H582 . 109.5 no O57 . C58 . H583 . 109.5 no H581 . C58 . H583 . 109.5 no H582 . C58 . H583 . 109.5 no N59 . C60 . C61 . 177.6(6) yes C60 . C61 . H611 . 109.5 no C60 . C61 . H612 . 109.4 no H611 . C61 . H612 . 109.5 no C60 . C61 . H613 . 109.5 no H611 . C61 . H613 . 109.5 no H612 . C61 . H613 . 109.5 no N62 . C63 . C64 . 178.1(6) yes C63 . C64 . H641 . 109.5 no C63 . C64 . H642 . 109.4 no H641 . C64 . H642 . 109.5 no C63 . C64 . H643 . 109.4 no H641 . C64 . H643 . 109.5 no H642 . C64 . H643 . 109.5 no N65 . C1 . C30 . 173.8(14) yes C1 . C30 . H301 . 109.5 no C1 . C30 . H302 . 109.3 no H301 . C30 . H302 . 109.5 no C1 . C30 . H303 . 109.6 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no C43 . C65 . C59 . 120.043(3) yes C43 . C65 . C52 . 123.9(7) yes C59 . C65 . C52 . 116.1(7) yes C65 . C43 . C57 . 119.922 yes C65 . C43 . H431 . 119.9 no C57 . C43 . H431 . 120.2 no C43 . C57 . C76 . 120.035 yes C43 . C57 . H571 . 119.9 no C76 . C57 . H571 . 120.0 no C57 . C76 . C100 . 120.042(4) yes C57 . C76 . H761 . 120.0 no C100 . C76 . H761 . 119.9 no C76 . C100 . C59 . 119.923 yes C76 . C100 . H1001 . 120.1 no C59 . C100 . H1001 . 119.9 no C65 . C59 . C100 . 120.035(4) yes C65 . C59 . O3 . 128.393(3) yes C100 . C59 . O3 . 111.572 yes C59 . O3 . H30 . 127.7 no Co4 . O68 . C2 . 115.1(9) yes O68 . C2 . C62 . 125.2(10) yes O68 . C2 . C52 . 114.7(10) yes C62 . C2 . C52 . 120.013 yes C2 . C62 . C3 . 120.005 yes C2 . C62 . H621 . 120.0 no C3 . C62 . H621 . 120.0 no C62 . C3 . C74 . 119.981(3) yes C62 . C3 . H31 . 119.9 no C74 . C3 . H31 . 120.1 no C3 . C74 . C4 . 120.013(4) yes C3 . C74 . H741 . 119.8 no C4 . C74 . H741 . 120.2 no C74 . C4 . C52 . 120.005 yes C74 . C4 . H41 . 119.8 no C52 . C4 . H41 . 120.2 no C65 . C52 . C2 . 129.3(9) yes C65 . C52 . C4 . 110.6(9) yes C2 . C52 . C4 . 119.982(4) yes Co4 . O43 . C44 . 131.0(5) yes O43 . C44 . C45 . 120.6(5) yes O43 . C44 . C49 . 119.0(5) yes C45 . C44 . C49 . 120.174(3) yes C44 . C45 . C46 . 119.846(3) yes C44 . C45 . H451 . 120.0 no C46 . C45 . H451 . 120.1 no C45 . C46 . C47 . 119.980 yes C45 . C46 . H461 . 120.0 no C47 . C46 . H461 . 120.0 no C46 . C47 . C48 . 120.174 yes C46 . C47 . H471 . 119.9 no C48 . C47 . H471 . 120.0 no C47 . C48 . C49 . 119.845(3) yes C47 . C48 . H481 . 120.0 no C49 . C48 . H481 . 120.2 no C44 . C49 . C48 . 119.981 yes C44 . C49 . C66 . 125.3(5) yes C48 . C49 . C66 . 114.5(5) yes C50 . O52 . H520 . 119.7 no O52 . C50 . C51 . 123.755(3) yes O52 . C50 . C66 . 116.363(3) yes C51 . C50 . C66 . 119.666 yes C50 . C51 . C67 . 120.150 yes C50 . C51 . H511 . 119.6 no C67 . C51 . H511 . 120.3 no C51 . C67 . C68 . 120.183(3) yes C51 . C67 . H671 . 119.4 no C68 . C67 . H671 . 120.4 no C67 . C68 . C69 . 119.666(3) yes C67 . C68 . H681 . 119.8 no C69 . C68 . H681 . 120.5 no C68 . C69 . C66 . 120.151 yes C68 . C69 . H691 . 119.8 no C66 . C69 . H691 . 120.1 no C50 . C66 . C69 . 120.183(3) yes C50 . C66 . C49 . 122.2(4) yes C69 . C66 . C49 . 116.9(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 07/10/11 at 15:35:30 # #LIST 12 BLOCK SCALE X'S CONT CO(1, U'S) UNTIL CO(4) CONT N(8,U'S) UNTIL C(64) CONT N(65,U[ISO]) UNTIL C(66) GROUP C(44) C(45) C(46) C(47) C(48) C(49) GROUP C(50) C(51) C(67) C(68) C(69) C(66) O(52) GROUP C(2) C(62) C(3) C(74) C(4) C(52) GROUP C(65) C(43) C(57) C(76) C(100) C(59) O(3) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) H ( 613,X'S) RIDE C ( 64,X'S) H ( 641,X'S) H ( 642,X'S) H ( 643,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 58,X'S) H ( 581,X'S) H ( 582,X'S) H ( 583,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 07/10/11 at 15:35:30 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 1.450000 , 0.040000 = C(1) TO C(30) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = N(8) TO C(7) VIBR .0, 0.00200 = N(8) TO C(9) VIBR .0, 0.00500 = C(9) TO C(7) VIBR .0, 0.00200 = N(15) TO C(14) VIBR .0, 0.00200 = N(15) TO C(53) VIBR .0, 0.00500 = C(53) TO C(14) VIBR .0, 0.00200 = N(59) TO C(60) VIBR .0, 0.00200 = N(62) TO C(63) VIBR .0, 0.00200 = O(2) TO C(38) VIBR .0, 0.00200 = O(4) TO C(21) VIBR .0, 0.00200 = O(6) TO C(7) VIBR .0, 0.00200 = O(13) TO C(14) VIBR .0, 0.00200 = O(17) TO C(18) VIBR .0, 0.00200 = O(30) TO C(31) VIBR .0, 0.00200 = O(57) TO C(58) VIBR .0, 0.00200 = C(7) TO C(12) VIBR .0, 0.00500 = O(6) TO N(8) VIBR .0, 0.00500 = C(12) TO N(8) VIBR .0, 0.00500 = C(12) TO O(6) VIBR .0, 0.00200 = C(9) TO C(10) VIBR .0, 0.00500 = C(10) TO N(8) VIBR .0, 0.00200 = C(10) TO C(11) VIBR .0, 0.00500 = C(11) TO C(9) VIBR .0, 0.00200 = C(11) TO C(12) VIBR .0, 0.00500 = C(12) TO C(10) VIBR .0, 0.00500 = C(11) TO C(7) VIBR .0, 0.00200 = C(14) TO C(56) VIBR .0, 0.00500 = O(13) TO N(15) VIBR .0, 0.00500 = C(56) TO N(15) VIBR .0, 0.00500 = C(56) TO O(13) VIBR .0, 0.00200 = C(18) TO C(19) VIBR .0, 0.00200 = C(18) TO C(29) VIBR .0, 0.00500 = C(19) TO O(17) VIBR .0, 0.00500 = C(29) TO O(17) VIBR .0, 0.00500 = C(29) TO C(19) VIBR .0, 0.00200 = C(19) TO C(20) VIBR .0, 0.00200 = C(19) TO C(26) VIBR .0, 0.00500 = C(20) TO C(18) VIBR .0, 0.00500 = C(26) TO C(18) VIBR .0, 0.00500 = C(26) TO C(20) VIBR .0, 0.00200 = C(20) TO C(21) VIBR .0, 0.00200 = C(20) TO C(25) VIBR .0, 0.00500 = C(21) TO C(19) VIBR .0, 0.00500 = C(25) TO C(19) VIBR .0, 0.00500 = C(25) TO C(21) VIBR .0, 0.00200 = C(21) TO C(22) VIBR .0, 0.00500 = O(4) TO C(20) VIBR .0, 0.00500 = C(22) TO C(20) VIBR .0, 0.00500 = C(22) TO O(4) VIBR .0, 0.00200 = C(22) TO C(23) VIBR .0, 0.00500 = C(23) TO C(21) VIBR .0, 0.00200 = C(23) TO C(24) VIBR .0, 0.00500 = C(24) TO C(22) VIBR .0, 0.00200 = C(24) TO C(25) VIBR .0, 0.00500 = C(25) TO C(23) VIBR .0, 0.00500 = C(20) TO C(24) VIBR .0, 0.00200 = C(26) TO C(27) VIBR .0, 0.00500 = C(27) TO C(19) VIBR .0, 0.00200 = C(27) TO C(28) VIBR .0, 0.00500 = C(28) TO C(26) VIBR .0, 0.00200 = C(28) TO C(29) VIBR .0, 0.00500 = C(29) TO C(27) VIBR .0, 0.00500 = C(28) TO C(18) VIBR .0, 0.00200 = C(31) TO C(32) VIBR .0, 0.00200 = C(31) TO C(36) VIBR .0, 0.00500 = C(32) TO O(30) VIBR .0, 0.00500 = C(36) TO O(30) VIBR .0, 0.00500 = C(36) TO C(32) VIBR .0, 0.00200 = C(32) TO C(33) VIBR .0, 0.00500 = C(33) TO C(31) VIBR .0, 0.00200 = C(33) TO C(34) VIBR .0, 0.00500 = C(34) TO C(32) VIBR .0, 0.00200 = C(34) TO C(35) VIBR .0, 0.00500 = C(35) TO C(33) VIBR .0, 0.00200 = C(35) TO C(36) VIBR .0, 0.00500 = C(36) TO C(34) VIBR .0, 0.00200 = C(36) TO C(37) VIBR .0, 0.00500 = C(31) TO C(35) VIBR .0, 0.00500 = C(37) TO C(35) VIBR .0, 0.00500 = C(37) TO C(31) VIBR .0, 0.00200 = C(37) TO C(38) VIBR .0, 0.00200 = C(37) TO C(42) VIBR .0, 0.00500 = C(38) TO C(36) VIBR .0, 0.00500 = C(42) TO C(36) VIBR .0, 0.00500 = C(42) TO C(38) VIBR .0, 0.00200 = C(38) TO C(39) VIBR .0, 0.00500 = O(2) TO C(37) VIBR .0, 0.00500 = C(39) TO C(37) VIBR .0, 0.00500 = C(39) TO O(2) VIBR .0, 0.00200 = C(39) TO C(40) VIBR .0, 0.00500 = C(40) TO C(38) VIBR .0, 0.00200 = C(40) TO C(41) VIBR .0, 0.00500 = C(41) TO C(39) VIBR .0, 0.00200 = C(41) TO C(42) VIBR .0, 0.00500 = C(42) TO C(40) VIBR .0, 0.00500 = C(41) TO C(37) VIBR .0, 0.00200 = C(53) TO C(54) VIBR .0, 0.00500 = C(54) TO N(15) VIBR .0, 0.00200 = C(54) TO C(55) VIBR .0, 0.00500 = C(55) TO C(53) VIBR .0, 0.00200 = C(55) TO C(56) VIBR .0, 0.00500 = C(56) TO C(54) VIBR .0, 0.00500 = C(55) TO C(14) VIBR .0, 0.00200 = C(60) TO C(61) VIBR .0, 0.00500 = C(61) TO N(59) VIBR .0, 0.00200 = C(63) TO C(64) VIBR .0, 0.00500 = C(64) TO N(62) VIBR .0, 0.00200 = N(65) TO C(1) VIBR .0, 0.00200 = C(1) TO C(30) VIBR .0, 0.00500 = C(30) TO N(65) VIBR .0, 0.00200 = C(65) TO C(43) VIBR .0, 0.00200 = C(65) TO C(59) VIBR .0, 0.00200 = C(65) TO C(52) VIBR .0, 0.00500 = C(59) TO C(43) VIBR .0, 0.00500 = C(52) TO C(43) VIBR .0, 0.00500 = C(52) TO C(59) VIBR .0, 0.00200 = C(43) TO C(57) VIBR .0, 0.00500 = C(57) TO C(65) VIBR .0, 0.00200 = C(57) TO C(76) VIBR .0, 0.00500 = C(76) TO C(43) VIBR .0, 0.00200 = C(76) TO C(100) VIBR .0, 0.00500 = C(100) TO C(57) VIBR .0, 0.00200 = C(100) TO C(59) VIBR .0, 0.00500 = C(59) TO C(76) VIBR .0, 0.00200 = C(59) TO O(3) VIBR .0, 0.00500 = C(100) TO C(65) VIBR .0, 0.00500 = O(3) TO C(65) VIBR .0, 0.00500 = O(3) TO C(100) VIBR .0, 0.00200 = O(68) TO C(2) VIBR .0, 0.00200 = C(2) TO C(62) VIBR .0, 0.00200 = C(2) TO C(52) VIBR .0, 0.00500 = C(62) TO O(68) VIBR .0, 0.00500 = C(52) TO O(68) VIBR .0, 0.00500 = C(52) TO C(62) VIBR .0, 0.00200 = C(62) TO C(3) VIBR .0, 0.00500 = C(3) TO C(2) VIBR .0, 0.00200 = C(3) TO C(74) VIBR .0, 0.00500 = C(74) TO C(62) VIBR .0, 0.00200 = C(74) TO C(4) VIBR .0, 0.00500 = C(4) TO C(3) VIBR .0, 0.00200 = C(4) TO C(52) VIBR .0, 0.00500 = C(52) TO C(74) VIBR .0, 0.00500 = C(2) TO C(65) VIBR .0, 0.00500 = C(4) TO C(65) VIBR .0, 0.00500 = C(4) TO C(2) VIBR .0, 0.00200 = O(43) TO C(44) VIBR .0, 0.00200 = C(44) TO C(45) VIBR .0, 0.00200 = C(44) TO C(49) VIBR .0, 0.00500 = C(45) TO O(43) VIBR .0, 0.00500 = C(49) TO O(43) VIBR .0, 0.00500 = C(49) TO C(45) VIBR .0, 0.00200 = C(45) TO C(46) VIBR .0, 0.00500 = C(46) TO C(44) VIBR .0, 0.00200 = C(46) TO C(47) VIBR .0, 0.00500 = C(47) TO C(45) VIBR .0, 0.00200 = C(47) TO C(48) VIBR .0, 0.00500 = C(48) TO C(46) VIBR .0, 0.00200 = C(48) TO C(49) VIBR .0, 0.00500 = C(49) TO C(47) VIBR .0, 0.00200 = C(49) TO C(66) VIBR .0, 0.00500 = C(48) TO C(44) VIBR .0, 0.00500 = C(66) TO C(44) VIBR .0, 0.00500 = C(66) TO C(48) VIBR .0, 0.00200 = O(52) TO C(50) VIBR .0, 0.00200 = C(50) TO C(51) VIBR .0, 0.00200 = C(50) TO C(66) VIBR .0, 0.00500 = C(51) TO O(52) VIBR .0, 0.00500 = C(66) TO O(52) VIBR .0, 0.00500 = C(66) TO C(51) VIBR .0, 0.00200 = C(51) TO C(67) VIBR .0, 0.00500 = C(67) TO C(50) VIBR .0, 0.00200 = C(67) TO C(68) VIBR .0, 0.00500 = C(68) TO C(51) VIBR .0, 0.00200 = C(68) TO C(69) VIBR .0, 0.00500 = C(69) TO C(67) VIBR .0, 0.00200 = C(69) TO C(66) VIBR .0, 0.00500 = C(66) TO C(68) VIBR .0, 0.00500 = C(69) TO C(50) VIBR .0, 0.00500 = C(49) TO C(50) VIBR .0, 0.00500 = C(49) TO C(69) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = N(8) TO C(7) U(IJ) .0, 0.04000 = N(8) TO C(9) U(IJ) .0, 0.04000 = N(15) TO C(14) U(IJ) .0, 0.04000 = N(15) TO C(53) U(IJ) .0, 0.08000 = N(59) TO C(60) U(IJ) .0, 0.08000 = N(62) TO C(63) U(IJ) .0, 0.08000 = O(2) TO C(38) U(IJ) .0, 0.08000 = O(4) TO C(21) U(IJ) .0, 0.08000 = O(6) TO C(7) U(IJ) .0, 0.08000 = O(13) TO C(14) U(IJ) .0, 0.08000 = O(17) TO C(18) U(IJ) .0, 0.08000 = O(30) TO C(31) U(IJ) .0, 0.08000 = O(57) TO C(58) U(IJ) .0, 0.04000 = C(7) TO C(12) U(IJ) .0, 0.04000 = C(9) TO C(10) U(IJ) .0, 0.04000 = C(10) TO C(11) U(IJ) .0, 0.04000 = C(11) TO C(12) U(IJ) .0, 0.04000 = C(14) TO C(56) U(IJ) .0, 0.04000 = C(18) TO C(19) U(IJ) .0, 0.04000 = C(18) TO C(29) U(IJ) .0, 0.04000 = C(19) TO C(20) U(IJ) .0, 0.04000 = C(19) TO C(26) U(IJ) .0, 0.04000 = C(20) TO C(21) U(IJ) .0, 0.04000 = C(20) TO C(25) U(IJ) .0, 0.04000 = C(21) TO C(22) U(IJ) .0, 0.04000 = C(22) TO C(23) U(IJ) .0, 0.04000 = C(23) TO C(24) U(IJ) .0, 0.04000 = C(24) TO C(25) U(IJ) .0, 0.04000 = C(26) TO C(27) U(IJ) .0, 0.04000 = C(27) TO C(28) U(IJ) .0, 0.04000 = C(28) TO C(29) U(IJ) .0, 0.04000 = C(31) TO C(32) U(IJ) .0, 0.04000 = C(31) TO C(36) U(IJ) .0, 0.04000 = C(32) TO C(33) U(IJ) .0, 0.04000 = C(33) TO C(34) U(IJ) .0, 0.04000 = C(34) TO C(35) U(IJ) .0, 0.04000 = C(35) TO C(36) U(IJ) .0, 0.04000 = C(36) TO C(37) U(IJ) .0, 0.04000 = C(37) TO C(38) U(IJ) .0, 0.04000 = C(37) TO C(42) U(IJ) .0, 0.04000 = C(38) TO C(39) U(IJ) .0, 0.04000 = C(39) TO C(40) U(IJ) .0, 0.04000 = C(40) TO C(41) U(IJ) .0, 0.04000 = C(41) TO C(42) U(IJ) .0, 0.04000 = C(53) TO C(54) U(IJ) .0, 0.04000 = C(54) TO C(55) U(IJ) .0, 0.04000 = C(55) TO C(56) U(IJ) .0, 0.08000 = C(60) TO C(61) U(IJ) .0, 0.08000 = C(63) TO C(64) U(IJ) .0, 0.08000 = N(65) TO C(1) U(IJ) .0, 0.08000 = C(1) TO C(30) U(IJ) .0, 0.04000 = C(65) TO C(43) U(IJ) .0, 0.04000 = C(65) TO C(59) U(IJ) .0, 0.04000 = C(65) TO C(52) U(IJ) .0, 0.04000 = C(43) TO C(57) U(IJ) .0, 0.04000 = C(57) TO C(76) U(IJ) .0, 0.04000 = C(76) TO C(100) U(IJ) .0, 0.04000 = C(100) TO C(59) U(IJ) .0, 0.08000 = C(59) TO O(3) U(IJ) .0, 0.08000 = O(68) TO C(2) U(IJ) .0, 0.04000 = C(2) TO C(62) U(IJ) .0, 0.04000 = C(2) TO C(52) U(IJ) .0, 0.04000 = C(62) TO C(3) U(IJ) .0, 0.04000 = C(3) TO C(74) U(IJ) .0, 0.04000 = C(74) TO C(4) U(IJ) .0, 0.04000 = C(4) TO C(52) U(IJ) .0, 0.08000 = O(43) TO C(44) U(IJ) .0, 0.04000 = C(44) TO C(45) U(IJ) .0, 0.04000 = C(44) TO C(49) U(IJ) .0, 0.04000 = C(45) TO C(46) U(IJ) .0, 0.04000 = C(46) TO C(47) U(IJ) .0, 0.04000 = C(47) TO C(48) U(IJ) .0, 0.04000 = C(48) TO C(49) U(IJ) .0, 0.04000 = C(49) TO C(66) U(IJ) .0, 0.08000 = O(52) TO C(50) U(IJ) .0, 0.04000 = C(50) TO C(51) U(IJ) .0, 0.04000 = C(50) TO C(66) U(IJ) .0, 0.04000 = C(51) TO C(67) U(IJ) .0, 0.04000 = C(67) TO C(68) U(IJ) .0, 0.04000 = C(68) TO C(69) U(IJ) .0, 0.04000 = C(69) TO C(66) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -2 10 9 x . 2 0 4 x . -3 5 2 x . 3 1 4 x . 1 4 3 x . 0 5 1 x . 0 4 0 x . # Attachment '- Cochain(4).cif' data_nb242d2 _database_code_depnum_ccdc_archive 'CCDC 852546' #TrackingRef '- Cochain(4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co(L1H)(L2)2(NO3)).(L1H2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H47 Co N5 O7' _chemical_formula_weight 888.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 10.572(2) _cell_length_b 13.755(3) _cell_length_c 15.127(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.03(3) _cell_angle_gamma 90.00 _cell_volume 2194.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 930 _exptl_absorpt_coefficient_mu 0.450 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9559 _cell_measurement_reflns_used 1620 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _exptl_absorpt_correction_T_min 0.94121 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 9904 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.9559 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0176813000 _diffrn_orient_matrix_UB_12 0.0435389000 _diffrn_orient_matrix_UB_13 0.0227707000 _diffrn_orient_matrix_UB_21 0.0593842000 _diffrn_orient_matrix_UB_22 -0.0008329000 _diffrn_orient_matrix_UB_23 -0.0190245000 _diffrn_orient_matrix_UB_31 -0.0260208000 _diffrn_orient_matrix_UB_32 0.0276036000 _diffrn_orient_matrix_UB_33 -0.0365211000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -40.00 51.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ frames - -18.3278 52.0000 -67.0000 91 #__ type_ start__ end____ width___ exp.time_ 2 omega -89.00 7.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ frames - -18.3278 -37.0000 120.0000 96 #__ type_ start__ end____ width___ exp.time_ 3 omega -4.00 25.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ frames - 18.7966 -37.0000 -60.0000 29 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 5134 _reflns_number_gt 3308 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^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 0.00(3) _refine_ls_number_reflns 5134 _refine_ls_number_parameters 571 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1213 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.027 _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 0.86464(13) 1.00422(8) 0.58740(10) 0.0246(3) Uani 1 1 d . . . N1 N 0.9814(8) 1.0938(5) 0.5109(5) 0.0240(19) Uani 1 1 d . . . N2 N 0.8430(8) 0.8908(5) 0.4933(5) 0.030(2) Uani 1 1 d . . . N3 N 0.6848(9) 1.1316(6) 0.5935(6) 0.037(2) Uani 1 1 d . . . N4 N 1.7515(8) 1.0794(5) 0.1738(5) 0.026(2) Uani 1 1 d . . . N5 N 0.5666(9) 0.4805(6) 0.0347(5) 0.041(2) Uani 1 1 d . . . O1 O 1.0149(6) 0.9699(5) 0.6671(4) 0.0342(17) Uani 1 1 d . . . O2 O 1.1382(7) 0.8152(4) 0.6756(4) 0.0365(17) Uani 1 1 d . . . H2H H 1.0822 0.8584 0.6768 0.044 Uiso 1 1 calc R . . O3 O 0.7816(7) 1.1351(5) 0.6473(4) 0.0357(18) Uani 1 1 d . . . O4 O 0.6812(6) 1.0671(5) 0.5348(5) 0.0365(18) Uani 1 1 d . . . O5 O 0.5958(7) 1.1896(5) 0.6006(5) 0.051(2) Uani 1 1 d . . . O6 O 0.3438(7) 0.4832(5) -0.0493(4) 0.0400(18) Uani 1 1 d . . . H6 H 0.4007 0.4485 -0.0237 0.048 Uiso 1 1 calc R . . O7 O 0.1060(7) 0.4473(5) -0.0341(5) 0.0389(18) Uani 1 1 d . . . H7 H 0.1833 0.4372 -0.0400 0.047 Uiso 1 1 calc R . . C1 C 1.0233(10) 1.1814(6) 0.5450(6) 0.031(2) Uani 1 1 d . . . H1 H 0.9746 1.2141 0.5864 0.037 Uiso 1 1 calc R . . C2 C 1.1329(9) 1.2228(7) 0.5211(7) 0.033(3) Uani 1 1 d . . . H2 H 1.1617 1.2811 0.5496 0.040 Uiso 1 1 calc R . . C3 C 1.0476(10) 1.0563(7) 0.4476(6) 0.031(2) Uani 1 1 d . . . H3 H 1.0181 0.9974 0.4206 0.038 Uiso 1 1 calc R . . C4 C 1.1557(9) 1.0970(6) 0.4188(6) 0.025(2) Uani 1 1 d . . . H4 H 1.1982 1.0667 0.3728 0.030 Uiso 1 1 calc R . . C5 C 1.2032(9) 1.1834(6) 0.4573(6) 0.025(2) Uani 1 1 d . . . C6 C 1.3260(9) 1.2290(6) 0.4358(6) 0.031(2) Uani 1 1 d . . . H6A H 1.3815 1.2331 0.4912 0.037 Uiso 1 1 calc R . . H6B H 1.3083 1.2964 0.4155 0.037 Uiso 1 1 calc R . . C7 C 1.3992(9) 1.1782(6) 0.3663(6) 0.031(2) Uani 1 1 d . . . H7A H 1.4190 1.1108 0.3857 0.037 Uiso 1 1 calc R . . H7B H 1.3463 1.1750 0.3097 0.037 Uiso 1 1 calc R . . C8 C 1.5209(9) 1.2317(6) 0.3522(6) 0.031(2) Uani 1 1 d . . . H8A H 1.4999 1.2972 0.3283 0.038 Uiso 1 1 calc R . . H8B H 1.5693 1.2402 0.4101 0.038 Uiso 1 1 calc R . . C9 C 1.6025(10) 1.1803(6) 0.2901(6) 0.030(2) Uani 1 1 d . . . C10 C 1.5680(9) 1.1734(7) 0.1991(6) 0.030(2) Uani 1 1 d . . . H10 H 1.4920 1.2028 0.1751 0.036 Uiso 1 1 calc R . . C11 C 1.6448(10) 1.1238(6) 0.1446(7) 0.033(2) Uani 1 1 d . . . H11 H 1.6203 1.1211 0.0830 0.040 Uiso 1 1 calc R . . C12 C 1.7864(9) 1.0856(6) 0.2615(6) 0.028(2) Uani 1 1 d . . . H12 H 1.8637 1.0561 0.2833 0.034 Uiso 1 1 calc R . . C13 C 1.7132(9) 1.1334(6) 0.3206(6) 0.028(2) Uani 1 1 d . . . H13 H 1.7390 1.1341 0.3820 0.034 Uiso 1 1 calc R . . C14 C 0.7600(10) 0.8940(7) 0.4222(6) 0.035(3) Uani 1 1 d . . . H14 H 0.7138 0.9522 0.4097 0.042 Uiso 1 1 calc R . . C15 C 0.7399(10) 0.8152(7) 0.3667(6) 0.037(3) Uani 1 1 d . . . H15 H 0.6783 0.8199 0.3180 0.044 Uiso 1 1 calc R . . C16 C 0.8060(10) 0.7305(6) 0.3796(6) 0.028(2) Uani 1 1 d . . . C17 C 0.8932(10) 0.7273(7) 0.4528(7) 0.045(3) Uani 1 1 d . . . H17 H 0.9427 0.6707 0.4655 0.054 Uiso 1 1 calc R . . C18 C 0.9060(10) 0.8081(7) 0.5066(7) 0.039(3) Uani 1 1 d . . . H18 H 0.9644 0.8043 0.5571 0.047 Uiso 1 1 calc R . . C19 C 0.7937(10) 0.6451(7) 0.3170(7) 0.037(3) Uani 1 1 d . . . H19A H 0.7110 0.6485 0.2822 0.045 Uiso 1 1 calc R . . H19B H 0.7959 0.5840 0.3517 0.045 Uiso 1 1 calc R . . C20 C 0.9009(10) 0.6438(6) 0.2536(6) 0.033(3) Uani 1 1 d . . . H20A H 0.8907 0.6997 0.2124 0.039 Uiso 1 1 calc R . . H20B H 0.9835 0.6508 0.2881 0.039 Uiso 1 1 calc R . . C21 C 0.9002(11) 0.5498(6) 0.2006(7) 0.044(3) Uani 1 1 d . . . H21A H 0.9723 0.5520 0.1624 0.053 Uiso 1 1 calc R . . H21B H 0.9165 0.4955 0.2429 0.053 Uiso 1 1 calc R . . C22 C 0.7828(10) 0.5253(6) 0.1428(6) 0.031(2) Uani 1 1 d . . . C23 C 0.7344(12) 0.4333(7) 0.1371(7) 0.048(3) Uani 1 1 d . . . H23 H 0.7743 0.3828 0.1717 0.058 Uiso 1 1 calc R . . C24 C 0.6303(12) 0.4130(7) 0.0829(7) 0.055(4) Uani 1 1 d . . . H24 H 0.6013 0.3477 0.0791 0.066 Uiso 1 1 calc R . . C25 C 0.6100(10) 0.5713(7) 0.0408(6) 0.036(3) Uani 1 1 d . . . H25 H 0.5651 0.6212 0.0084 0.043 Uiso 1 1 calc R . . C26 C 0.7171(10) 0.5952(7) 0.0921(7) 0.037(3) Uani 1 1 d . . . H26 H 0.7468 0.6603 0.0930 0.044 Uiso 1 1 calc R . . C27 C 1.1115(10) 1.0308(7) 0.6933(6) 0.032(2) Uani 1 1 d . . . C28 C 1.0890(11) 1.1100(7) 0.7494(6) 0.042(3) Uani 1 1 d . . . H28 H 1.0065 1.1199 0.7690 0.050 Uiso 1 1 calc R . . C29 C 1.1845(12) 1.1722(8) 0.7759(7) 0.052(3) Uani 1 1 d . . . H29 H 1.1674 1.2261 0.8125 0.062 Uiso 1 1 calc R . . C30 C 1.3060(11) 1.1578(8) 0.7500(8) 0.053(3) Uani 1 1 d . . . H30 H 1.3726 1.2013 0.7683 0.063 Uiso 1 1 calc R . . C31 C 1.3286(11) 1.0777(7) 0.6963(7) 0.041(3) Uani 1 1 d . . . H31 H 1.4120 1.0667 0.6790 0.049 Uiso 1 1 calc R . . C32 C 1.2331(9) 1.0140(7) 0.6677(6) 0.029(2) Uani 1 1 d . . . C33 C 1.2638(10) 0.9321(7) 0.6070(6) 0.032(2) Uani 1 1 d . . . C34 C 1.3523(10) 0.9502(8) 0.5414(7) 0.042(3) Uani 1 1 d . . . H34 H 1.3856 1.0138 0.5351 0.050 Uiso 1 1 calc R . . C35 C 1.3895(11) 0.8771(8) 0.4878(7) 0.044(3) Uani 1 1 d . . . H35 H 1.4475 0.8906 0.4442 0.052 Uiso 1 1 calc R . . C36 C 1.3437(12) 0.7842(8) 0.4964(7) 0.048(3) Uani 1 1 d . . . H36 H 1.3706 0.7338 0.4591 0.058 Uiso 1 1 calc R . . C37 C 1.2575(12) 0.7641(8) 0.5602(8) 0.050(3) Uani 1 1 d . . . H37 H 1.2257 0.7001 0.5667 0.060 Uiso 1 1 calc R . . C38 C 1.2196(10) 0.8382(8) 0.6130(6) 0.034(3) Uani 1 1 d . . . C39 C 0.3448(11) 0.4712(7) -0.1390(6) 0.042(3) Uani 1 1 d . . . C40 C 0.4384(11) 0.4259(8) -0.1764(8) 0.055(3) Uani 1 1 d . . . H40 H 0.5070 0.3998 -0.1400 0.066 Uiso 1 1 calc R . . C41 C 0.4377(12) 0.4159(10) -0.2687(8) 0.071(4) Uani 1 1 d . . . H41 H 0.5077 0.3860 -0.2940 0.085 Uiso 1 1 calc R . . C42 C 0.3375(12) 0.4487(10) -0.3229(9) 0.069(4) Uani 1 1 d . . . H42 H 0.3337 0.4379 -0.3850 0.082 Uiso 1 1 calc R . . C43 C 0.2430(11) 0.4977(8) -0.2845(7) 0.047(3) Uani 1 1 d . . . H43 H 0.1764 0.5251 -0.3219 0.056 Uiso 1 1 calc R . . C44 C 0.2392(10) 0.5098(7) -0.1908(7) 0.036(3) Uani 1 1 d . . . C45 C 0.1308(10) 0.5597(7) -0.1561(6) 0.032(2) Uani 1 1 d . . . C46 C 0.0801(11) 0.6432(7) -0.1978(7) 0.044(3) Uani 1 1 d . . . H46 H 0.1253 0.6719 -0.2432 0.053 Uiso 1 1 calc R . . C47 C -0.0281(12) 0.6850(8) -0.1773(8) 0.046(3) Uani 1 1 d . . . H47 H -0.0582 0.7406 -0.2096 0.055 Uiso 1 1 calc R . . C48 C -0.0987(11) 0.6485(7) -0.1088(8) 0.043(3) Uani 1 1 d . . . H48 H -0.1763 0.6773 -0.0945 0.051 Uiso 1 1 calc R . . C49 C -0.0476(11) 0.5675(7) -0.0632(7) 0.041(3) Uani 1 1 d . . . H49 H -0.0913 0.5401 -0.0164 0.050 Uiso 1 1 calc R . . C50 C 0.0656(11) 0.5266(6) -0.0852(7) 0.037(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0239(6) 0.0318(6) 0.0183(6) -0.0006(6) 0.0027(5) -0.0008(7) N1 0.029(5) 0.027(4) 0.017(4) 0.012(4) 0.010(4) -0.001(4) N2 0.037(6) 0.026(4) 0.027(5) 0.001(4) 0.006(4) -0.005(4) N3 0.030(6) 0.041(5) 0.039(6) 0.013(5) 0.006(5) -0.001(4) N4 0.028(5) 0.028(4) 0.023(5) -0.002(4) -0.002(4) 0.003(4) N5 0.043(6) 0.047(6) 0.032(5) 0.002(4) -0.006(4) 0.004(5) O1 0.021(4) 0.044(4) 0.037(4) 0.012(3) -0.003(3) -0.008(3) O2 0.044(5) 0.034(4) 0.031(4) 0.012(3) 0.000(4) -0.004(3) O3 0.030(5) 0.053(4) 0.024(4) -0.004(3) -0.002(3) 0.000(4) O4 0.024(4) 0.049(4) 0.035(4) 0.001(4) -0.004(3) 0.000(3) O5 0.028(5) 0.046(4) 0.080(6) 0.002(4) 0.001(4) 0.010(4) O6 0.028(5) 0.059(5) 0.031(4) 0.006(4) -0.009(3) -0.001(4) O7 0.042(5) 0.042(4) 0.033(4) 0.013(3) 0.007(4) -0.001(4) C1 0.035(7) 0.018(5) 0.040(7) -0.004(5) 0.007(5) 0.008(5) C2 0.028(6) 0.037(6) 0.035(7) 0.001(5) 0.007(5) 0.000(5) C3 0.038(7) 0.034(6) 0.023(6) -0.002(5) 0.002(5) -0.007(5) C4 0.018(5) 0.032(5) 0.024(5) 0.004(4) 0.002(4) 0.003(4) C5 0.024(6) 0.026(5) 0.027(6) 0.005(4) 0.007(4) 0.001(4) C6 0.019(6) 0.037(5) 0.035(6) -0.003(5) 0.004(5) 0.002(4) C7 0.038(7) 0.031(5) 0.024(6) 0.004(4) 0.009(5) -0.011(5) C8 0.023(6) 0.037(6) 0.035(6) -0.004(5) 0.005(5) -0.002(5) C9 0.035(6) 0.020(5) 0.037(6) 0.005(5) 0.004(5) -0.010(5) C10 0.022(6) 0.041(6) 0.027(6) -0.005(5) -0.002(5) 0.001(5) C11 0.038(7) 0.034(6) 0.027(6) -0.001(5) 0.002(5) 0.003(5) C12 0.032(6) 0.041(6) 0.012(5) 0.002(4) 0.002(4) 0.003(5) C13 0.033(6) 0.035(5) 0.017(5) -0.002(4) -0.001(4) 0.004(5) C14 0.045(7) 0.038(6) 0.021(6) -0.006(5) -0.001(5) 0.002(5) C15 0.040(7) 0.045(6) 0.025(6) 0.007(5) 0.004(5) -0.005(5) C16 0.041(7) 0.028(5) 0.016(5) -0.008(4) 0.002(5) -0.002(5) C17 0.045(8) 0.036(6) 0.052(8) -0.014(5) -0.004(6) 0.011(5) C18 0.031(7) 0.041(6) 0.043(7) -0.001(5) -0.011(5) 0.000(5) C19 0.040(8) 0.035(6) 0.037(7) -0.006(5) 0.008(6) -0.002(5) C20 0.040(7) 0.030(5) 0.028(6) -0.005(5) -0.001(5) 0.002(5) C21 0.042(8) 0.039(6) 0.050(8) -0.007(5) -0.014(6) -0.006(5) C22 0.034(6) 0.029(5) 0.028(6) -0.008(4) 0.000(5) 0.010(5) C23 0.067(9) 0.032(6) 0.043(7) 0.009(5) -0.022(6) 0.001(6) C24 0.075(10) 0.022(5) 0.063(9) 0.002(5) -0.026(7) -0.004(6) C25 0.043(7) 0.035(6) 0.029(6) 0.018(5) -0.001(5) 0.005(5) C26 0.033(7) 0.037(6) 0.041(7) 0.005(5) 0.005(5) 0.005(5) C27 0.029(6) 0.043(6) 0.023(6) 0.009(5) 0.004(5) 0.005(5) C28 0.054(8) 0.046(6) 0.026(6) -0.002(5) 0.002(5) 0.013(6) C29 0.056(9) 0.048(7) 0.049(8) -0.016(6) -0.015(7) 0.000(7) C30 0.038(8) 0.046(7) 0.071(9) -0.007(6) -0.016(7) -0.014(6) C31 0.033(7) 0.031(6) 0.056(8) 0.009(5) -0.009(6) 0.000(5) C32 0.028(6) 0.039(6) 0.020(5) 0.007(5) 0.003(4) -0.003(5) C33 0.038(7) 0.035(6) 0.022(6) 0.002(5) 0.004(5) 0.011(5) C34 0.029(7) 0.059(7) 0.035(7) 0.003(5) -0.007(5) 0.008(5) C35 0.044(8) 0.056(7) 0.030(7) 0.005(6) -0.001(6) 0.007(6) C36 0.046(8) 0.060(8) 0.039(7) -0.016(6) 0.002(6) 0.028(7) C37 0.055(9) 0.048(7) 0.045(7) -0.010(6) -0.013(6) -0.004(6) C38 0.034(7) 0.048(7) 0.017(6) 0.018(5) -0.008(5) 0.001(5) C39 0.038(7) 0.067(8) 0.018(6) 0.014(5) -0.005(5) -0.001(6) C40 0.032(8) 0.094(10) 0.037(7) 0.016(7) -0.003(6) 0.003(7) C41 0.035(8) 0.146(13) 0.033(8) 0.004(8) 0.013(6) 0.009(8) C42 0.037(8) 0.134(12) 0.036(8) 0.007(7) 0.013(6) -0.006(8) C43 0.034(7) 0.070(8) 0.036(7) 0.006(6) 0.003(5) -0.003(6) C44 0.036(7) 0.050(6) 0.022(6) 0.008(5) -0.003(5) -0.007(5) C45 0.033(7) 0.037(6) 0.025(6) -0.002(5) -0.005(5) -0.006(5) C46 0.043(8) 0.045(7) 0.041(7) 0.004(5) -0.013(6) -0.012(6) C47 0.055(9) 0.040(6) 0.042(7) 0.001(6) -0.004(6) 0.000(6) C48 0.046(8) 0.029(6) 0.052(8) -0.017(5) -0.005(6) 0.014(5) C49 0.042(8) 0.046(7) 0.036(7) -0.008(5) 0.007(6) 0.000(6) C50 0.047(8) 0.030(6) 0.033(7) -0.005(5) -0.004(5) -0.003(5) _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 1.983(6) . ? Co1 N2 2.113(7) . ? Co1 N1 2.140(8) . ? Co1 N4 2.164(8) 2_475 ? Co1 O4 2.219(7) . ? Co1 O3 2.223(7) . ? N1 C3 1.330(12) . ? N1 C1 1.372(11) . ? N2 C18 1.325(11) . ? N2 C14 1.340(11) . ? N3 O5 1.244(10) . ? N3 O4 1.254(10) . ? N3 O3 1.262(10) . ? N4 C11 1.330(11) . ? N4 C12 1.354(10) . ? N4 Co1 2.164(8) 2_674 ? N5 C25 1.332(12) . ? N5 C24 1.333(11) . ? O1 C27 1.358(11) . ? O2 C38 1.360(11) . ? O2 H2H 0.8400 . ? O6 C39 1.369(11) . ? O6 H6 0.8400 . ? O7 C50 1.387(11) . ? O7 H7 0.8400 . ? C1 C2 1.363(13) . ? C1 H1 0.9500 . ? C2 C5 1.371(13) . ? C2 H2 0.9500 . ? C3 C4 1.370(13) . ? C3 H3 0.9500 . ? C4 C5 1.401(12) . ? C4 H4 0.9500 . ? C5 C6 1.498(12) . ? C6 C7 1.519(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.510(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.498(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C13 1.387(12) . ? C9 C10 1.402(12) . ? C10 C11 1.377(13) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.390(12) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.378(12) . ? C14 H14 0.9500 . ? C15 C16 1.365(12) . ? C15 H15 0.9500 . ? C16 C17 1.390(13) . ? C16 C19 1.508(12) . ? C17 C18 1.379(13) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.536(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.522(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.505(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.365(12) . ? C22 C26 1.386(12) . ? C23 C24 1.355(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.367(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.387(13) . ? C27 C28 1.411(13) . ? C28 C29 1.362(14) . ? C28 H28 0.9500 . ? C29 C30 1.383(15) . ? C29 H29 0.9500 . ? C30 C31 1.399(15) . ? C30 H30 0.9500 . ? C31 C32 1.383(13) . ? C31 H31 0.9500 . ? C32 C33 1.503(13) . ? C33 C38 1.379(13) . ? C33 C34 1.432(14) . ? C34 C35 1.366(14) . ? C34 H34 0.9500 . ? C35 C36 1.375(14) . ? C35 H35 0.9500 . ? C36 C37 1.400(16) . ? C36 H36 0.9500 . ? C37 C38 1.373(14) . ? C37 H37 0.9500 . ? C39 C40 1.329(15) . ? C39 C44 1.421(14) . ? C40 C41 1.402(15) . ? C40 H40 0.9500 . ? C41 C42 1.370(16) . ? C41 H41 0.9500 . ? C42 C43 1.368(16) . ? C42 H42 0.9500 . ? C43 C44 1.430(13) . ? C43 H43 0.9500 . ? C44 C45 1.463(14) . ? C45 C50 1.392(14) . ? C45 C46 1.399(13) . ? C46 C47 1.336(15) . ? C46 H46 0.9500 . ? C47 C48 1.411(15) . ? C47 H47 0.9500 . ? C48 C49 1.399(13) . ? C48 H48 0.9500 . ? C49 C50 1.384(14) . ? C49 H49 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 O1 Co1 N2 106.1(3) . . ? O1 Co1 N1 89.9(3) . . ? N2 Co1 N1 95.8(3) . . ? O1 Co1 N4 87.7(3) . 2_475 ? N2 Co1 N4 88.6(3) . 2_475 ? N1 Co1 N4 175.4(3) . 2_475 ? O1 Co1 O4 162.4(3) . . ? N2 Co1 O4 89.8(3) . . ? N1 Co1 O4 96.0(3) . . ? N4 Co1 O4 85.3(3) 2_475 . ? O1 Co1 O3 105.5(3) . . ? N2 Co1 O3 147.7(3) . . ? N1 Co1 O3 90.8(3) . . ? N4 Co1 O3 86.2(3) 2_475 . ? O4 Co1 O3 58.0(2) . . ? C3 N1 C1 116.1(8) . . ? C3 N1 Co1 121.2(6) . . ? C1 N1 Co1 119.1(6) . . ? C18 N2 C14 116.3(8) . . ? C18 N2 Co1 120.1(7) . . ? C14 N2 Co1 123.4(6) . . ? O5 N3 O4 122.0(9) . . ? O5 N3 O3 120.2(9) . . ? O4 N3 O3 117.8(8) . . ? C11 N4 C12 117.6(9) . . ? C11 N4 Co1 122.4(7) . 2_674 ? C12 N4 Co1 120.0(6) . 2_674 ? C25 N5 C24 117.2(9) . . ? C27 O1 Co1 125.7(6) . . ? C38 O2 H2H 109.5 . . ? N3 O3 Co1 91.8(6) . . ? N3 O4 Co1 92.3(6) . . ? C39 O6 H6 109.5 . . ? C50 O7 H7 109.5 . . ? C2 C1 N1 121.7(9) . . ? C2 C1 H1 119.2 . . ? N1 C1 H1 119.2 . . ? C1 C2 C5 122.3(9) . . ? C1 C2 H2 118.8 . . ? C5 C2 H2 118.8 . . ? N1 C3 C4 124.3(9) . . ? N1 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? C3 C4 C5 119.8(9) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C2 C5 C4 115.6(9) . . ? C2 C5 C6 120.5(8) . . ? C4 C5 C6 123.8(9) . . ? C5 C6 C7 116.6(8) . . ? C5 C6 H6A 108.1 . . ? C7 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? C7 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 C6 110.7(7) . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C7 113.1(7) . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C13 C9 C10 116.8(9) . . ? C13 C9 C8 121.4(9) . . ? C10 C9 C8 121.8(9) . . ? C11 C10 C9 119.8(10) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N4 C11 C10 123.4(9) . . ? N4 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? N4 C12 C13 122.3(9) . . ? N4 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C9 C13 C12 120.1(9) . . ? C9 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? N2 C14 C15 121.8(9) . . ? N2 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 121.9(10) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 116.4(8) . . ? C15 C16 C19 123.6(9) . . ? C17 C16 C19 119.9(9) . . ? C18 C17 C16 118.4(9) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N2 C18 C17 125.1(10) . . ? N2 C18 H18 117.5 . . ? C17 C18 H18 117.5 . . ? C16 C19 C20 111.5(8) . . ? C16 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C16 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 111.2(9) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 118.0(9) . . ? C22 C21 H21A 107.8 . . ? C20 C21 H21A 107.8 . . ? C22 C21 H21B 107.8 . . ? C20 C21 H21B 107.8 . . ? H21A C21 H21B 107.1 . . ? C23 C22 C26 115.9(9) . . ? C23 C22 C21 122.3(8) . . ? C26 C22 C21 121.8(8) . . ? C24 C23 C22 120.9(9) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? N5 C24 C23 123.1(9) . . ? N5 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? N5 C25 C26 122.1(9) . . ? N5 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C22 120.7(9) . . ? C25 C26 H26 119.6 . . ? C22 C26 H26 119.6 . . ? O1 C27 C32 120.5(9) . . ? O1 C27 C28 119.7(10) . . ? C32 C27 C28 119.7(10) . . ? C29 C28 C27 120.6(12) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.7(11) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C31 118.5(11) . . ? C29 C30 H30 120.8 . . ? C31 C30 H30 120.8 . . ? C32 C31 C30 122.0(11) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C31 C32 C27 118.5(10) . . ? C31 C32 C33 118.8(10) . . ? C27 C32 C33 122.7(9) . . ? C38 C33 C34 116.7(9) . . ? C38 C33 C32 125.0(10) . . ? C34 C33 C32 118.2(9) . . ? C35 C34 C33 120.8(11) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.6(11) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C37 119.9(11) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 119.0(11) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? O2 C38 C37 117.2(10) . . ? O2 C38 C33 119.8(9) . . ? C37 C38 C33 122.9(10) . . ? C40 C39 O6 122.4(10) . . ? C40 C39 C44 121.4(10) . . ? O6 C39 C44 116.2(10) . . ? C39 C40 C41 121.1(11) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 120.9(12) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C43 C42 C41 117.7(12) . . ? C43 C42 H42 121.1 . . ? C41 C42 H42 121.1 . . ? C42 C43 C44 123.4(11) . . ? C42 C43 H43 118.3 . . ? C44 C43 H43 118.3 . . ? C39 C44 C43 115.3(10) . . ? C39 C44 C45 125.6(10) . . ? C43 C44 C45 119.1(9) . . ? C50 C45 C46 114.9(10) . . ? C50 C45 C44 124.4(9) . . ? C46 C45 C44 120.6(10) . . ? C47 C46 C45 123.8(11) . . ? C47 C46 H46 118.1 . . ? C45 C46 H46 118.1 . . ? C46 C47 C48 121.5(11) . . ? C46 C47 H47 119.2 . . ? C48 C47 H47 119.2 . . ? C49 C48 C47 116.1(11) . . ? C49 C48 H48 122.0 . . ? C47 C48 H48 122.0 . . ? C50 C49 C48 121.1(11) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 O7 115.0(10) . . ? C49 C50 C45 122.4(9) . . ? O7 C50 C45 122.5(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.981 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.088 # Attachment '- Co-2DNet(5).cif' data_nb286b2 _database_code_depnum_ccdc_archive 'CCDC 863199' #TrackingRef '- Co-2DNet(5).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co(biphenH)(t-bpe)1.5(NO3)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H42 Co2 N8 O10' _chemical_formula_weight 1152.88 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 P21/c 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 10.1508(6) _cell_length_b 14.8829(7) _cell_length_c 18.3001(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.469(5) _cell_angle_gamma 90.00 _cell_volume 2709.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.680 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.8718 _cell_measurement_reflns_used 2482 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _exptl_absorpt_correction_T_min 0.97470 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 12414 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.8718 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0191759000 _diffrn_orient_matrix_UB_12 -0.0291898000 _diffrn_orient_matrix_UB_13 0.0267152000 _diffrn_orient_matrix_UB_21 -0.0319150000 _diffrn_orient_matrix_UB_22 -0.0288067000 _diffrn_orient_matrix_UB_23 -0.0290730000 _diffrn_orient_matrix_UB_31 0.0607783000 _diffrn_orient_matrix_UB_32 -0.0242969000 _diffrn_orient_matrix_UB_33 0.0023899000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -91.00 -63.00 1.0000 67.0000 omega____ theta____ kappa____ phi______ frames - -14.4216 179.0000 150.0000 28 #__ type_ start__ end____ width___ exp.time_ 2 omega -64.00 -11.00 1.0000 67.0000 omega____ theta____ kappa____ phi______ frames - -14.4216 126.0000 85.0000 53 #__ type_ start__ end____ width___ exp.time_ 3 omega -49.00 89.00 1.0000 67.0000 omega____ theta____ kappa____ phi______ frames - 22.7028 0.0000 -180.0000 138 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 4954 _reflns_number_gt 3145 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+2.8681P] 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 4954 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.32769(7) 0.23833(4) 0.77300(4) 0.0386(3) Uani 1 1 d . . . N1 N 0.4203(4) 0.3286(3) 0.7023(2) 0.0391(10) Uani 1 1 d . . . N2 N 0.3246(5) 0.1406(3) 0.6878(2) 0.0419(11) Uani 1 1 d . . . N3 N 0.2320(4) 0.1516(3) 0.8394(2) 0.0406(11) Uani 1 1 d . . . N4 N 0.5372(6) 0.2430(5) 0.8791(3) 0.0728(18) Uani 1 1 d . . . O1 O 0.1694(4) 0.3190(3) 0.7515(2) 0.0557(11) Uani 1 1 d . . . O2 O 0.0268(6) 0.3116(3) 0.6253(3) 0.0783(15) Uani 1 1 d . . . H2H H 0.0843 0.3213 0.6643 0.094 Uiso 1 1 calc R . . O3 O 0.4399(5) 0.2990(3) 0.8742(2) 0.0648(13) Uani 1 1 d . . . O4 O 0.5301(4) 0.1878(3) 0.8264(2) 0.0628(12) Uani 1 1 d . . . O5 O 0.6312(6) 0.2418(5) 0.9332(3) 0.119(3) Uani 1 1 d . . . C1 C 0.0787(6) 0.3376(4) 0.7915(3) 0.0527(15) Uani 1 1 d . . . C2 C 0.1105(7) 0.3925(6) 0.8535(4) 0.086(2) Uani 1 1 d . . . H2 H 0.1985 0.4168 0.8672 0.103 Uiso 1 1 calc R . . C3 C 0.0147(8) 0.4124(7) 0.8961(4) 0.098(3) Uani 1 1 d . . . H3 H 0.0398 0.4487 0.9394 0.118 Uiso 1 1 calc R . . C4 C -0.1106(8) 0.3823(7) 0.8778(4) 0.091(3) Uani 1 1 d . . . H4 H -0.1758 0.3993 0.9059 0.109 Uiso 1 1 calc R . . C5 C -0.1443(7) 0.3258(6) 0.8172(4) 0.076(2) Uani 1 1 d . . . H5 H -0.2332 0.3026 0.8049 0.091 Uiso 1 1 calc R . . C6 C -0.0499(6) 0.3011(4) 0.7724(3) 0.0547(15) Uani 1 1 d . . . C7 C -0.0944(6) 0.2375(4) 0.7093(4) 0.0630(18) Uani 1 1 d . . . C8 C -0.1792(7) 0.1655(6) 0.7188(6) 0.100(3) Uani 1 1 d . . . H8 H -0.2005 0.1526 0.7660 0.119 Uiso 1 1 calc R . . C9 C -0.2320(9) 0.1124(7) 0.6545(8) 0.134(5) Uani 1 1 d . . . H9 H -0.2954 0.0667 0.6584 0.161 Uiso 1 1 calc R . . C10 C -0.1944(11) 0.1251(10) 0.5874(8) 0.155(6) Uani 1 1 d . . . H10 H -0.2279 0.0865 0.5467 0.186 Uiso 1 1 calc R . . C11 C -0.1101(9) 0.1924(7) 0.5794(5) 0.100(3) Uani 1 1 d . . . H11 H -0.0855 0.2018 0.5325 0.120 Uiso 1 1 calc R . . C12 C -0.0590(7) 0.2478(5) 0.6385(4) 0.0667(18) Uani 1 1 d . . . C13 C 0.3630(5) 0.4069(4) 0.6774(3) 0.0431(13) Uani 1 1 d . . . H13 H 0.2945 0.4301 0.7007 0.052 Uiso 1 1 calc R . . C14 C 0.3978(6) 0.4557(4) 0.6200(3) 0.0502(15) Uani 1 1 d . . . H14 H 0.3541 0.5110 0.6048 0.060 Uiso 1 1 calc R . . C15 C 0.4980(6) 0.4233(4) 0.5841(3) 0.0483(14) Uani 1 1 d . . . C16 C 0.5343(6) 0.4658(4) 0.5185(3) 0.0581(17) Uani 1 1 d . . . C17 C 0.5614(6) 0.3448(4) 0.6130(3) 0.0528(16) Uani 1 1 d . . . H17 H 0.6337 0.3214 0.5930 0.063 Uiso 1 1 calc R . . C18 C 0.5202(6) 0.3006(4) 0.6707(3) 0.0498(15) Uani 1 1 d . . . H18 H 0.5658 0.2469 0.6890 0.060 Uiso 1 1 calc R . . C19 C 0.2292(7) 0.1710(4) 0.9104(3) 0.0607(18) Uani 1 1 d . . . H19 H 0.2802 0.2209 0.9326 0.073 Uiso 1 1 calc R . . C20 C 0.1574(6) 0.1235(4) 0.9530(3) 0.0575(18) Uani 1 1 d . . . H20 H 0.1574 0.1418 1.0027 0.069 Uiso 1 1 calc R . . C21 C 0.0848(6) 0.0488(4) 0.9238(3) 0.0507(16) Uani 1 1 d . . . C22 C 0.0082(7) -0.0084(4) 0.9658(3) 0.0633(19) Uani 1 1 d . . . C23 C 0.0891(7) 0.0282(4) 0.8509(3) 0.070(2) Uani 1 1 d . . . H23 H 0.0426 -0.0232 0.8282 0.084 Uiso 1 1 calc R . . C24 C 0.1601(6) 0.0811(4) 0.8104(3) 0.0541(16) Uani 1 1 d . . . H24 H 0.1574 0.0664 0.7596 0.065 Uiso 1 1 calc R . . C25 C 0.2871(7) 0.1606(4) 0.6152(3) 0.0542(16) Uani 1 1 d . . . H25 H 0.2275 0.2096 0.6008 0.065 Uiso 1 1 calc R . . C26 C 0.3326(7) 0.1119(4) 0.5603(3) 0.0621(19) Uani 1 1 d . . . H26 H 0.3064 0.1290 0.5095 0.075 Uiso 1 1 calc R . . C27 C 0.4162(7) 0.0383(5) 0.5795(4) 0.0648(19) Uani 1 1 d . . . C28 C 0.4832(8) -0.0155(5) 0.5277(4) 0.082(2) Uani 1 1 d . . . C29 C 0.4425(6) 0.0125(5) 0.6536(3) 0.0602(17) Uani 1 1 d . . . H29 H 0.4906 -0.0413 0.6688 0.072 Uiso 1 1 calc R . . C30 C 0.3981(6) 0.0656(4) 0.7043(3) 0.0520(15) Uani 1 1 d . . . H30 H 0.4209 0.0482 0.7552 0.062 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 0.0579(5) 0.0395(4) 0.0252(4) -0.0008(3) 0.0243(3) -0.0153(4) N1 0.048(3) 0.045(3) 0.029(2) 0.005(2) 0.0193(19) -0.010(2) N2 0.064(3) 0.043(3) 0.026(2) -0.001(2) 0.026(2) -0.007(2) N3 0.065(3) 0.038(2) 0.027(2) -0.0023(19) 0.029(2) -0.012(2) N4 0.069(4) 0.107(5) 0.045(3) 0.009(4) 0.017(3) -0.039(4) O1 0.063(3) 0.060(3) 0.053(2) 0.004(2) 0.034(2) -0.007(2) O2 0.124(4) 0.062(3) 0.049(3) 0.012(2) 0.018(3) 0.016(3) O3 0.090(4) 0.069(3) 0.042(2) -0.011(2) 0.029(2) -0.043(3) O4 0.069(3) 0.079(3) 0.044(3) 0.004(2) 0.018(2) -0.017(2) O5 0.082(4) 0.212(8) 0.054(3) 0.003(4) -0.008(3) -0.058(4) C1 0.059(4) 0.056(4) 0.051(4) 0.002(3) 0.028(3) -0.011(3) C2 0.071(5) 0.119(7) 0.072(5) -0.042(5) 0.025(4) -0.015(5) C3 0.084(6) 0.152(8) 0.062(5) -0.048(5) 0.021(4) 0.008(6) C4 0.065(5) 0.149(8) 0.065(5) -0.015(5) 0.027(4) 0.034(5) C5 0.055(4) 0.111(6) 0.068(5) 0.014(5) 0.026(3) 0.012(4) C6 0.058(4) 0.060(4) 0.048(4) 0.003(3) 0.015(3) 0.005(3) C7 0.048(4) 0.061(4) 0.081(5) 0.004(4) 0.013(3) 0.012(3) C8 0.056(5) 0.093(6) 0.153(9) -0.028(6) 0.029(5) -0.012(5) C9 0.064(5) 0.117(8) 0.231(14) -0.086(9) 0.053(7) -0.037(5) C10 0.088(7) 0.203(13) 0.181(13) -0.122(11) 0.046(8) -0.036(8) C11 0.082(6) 0.114(7) 0.092(7) -0.043(6) -0.009(5) 0.017(6) C12 0.066(4) 0.066(5) 0.065(5) -0.009(4) 0.004(4) 0.006(4) C13 0.053(3) 0.046(3) 0.036(3) 0.006(3) 0.021(3) -0.007(3) C14 0.062(4) 0.053(3) 0.042(3) 0.021(3) 0.024(3) -0.001(3) C15 0.055(3) 0.059(4) 0.036(3) 0.013(3) 0.020(3) -0.014(3) C16 0.066(4) 0.071(4) 0.041(4) 0.021(3) 0.021(3) -0.017(3) C17 0.050(3) 0.071(4) 0.043(3) 0.018(3) 0.023(3) -0.008(3) C18 0.056(3) 0.058(4) 0.041(3) 0.016(3) 0.023(3) -0.003(3) C19 0.103(5) 0.053(3) 0.036(3) -0.015(3) 0.037(3) -0.042(4) C20 0.098(5) 0.052(3) 0.034(3) -0.010(3) 0.042(3) -0.033(3) C21 0.084(4) 0.037(3) 0.042(3) -0.008(3) 0.038(3) -0.022(3) C22 0.108(5) 0.049(3) 0.048(4) -0.012(3) 0.052(4) -0.033(4) C23 0.123(6) 0.052(4) 0.052(4) -0.025(3) 0.061(4) -0.053(4) C24 0.090(4) 0.050(3) 0.033(3) -0.015(3) 0.040(3) -0.029(3) C25 0.092(5) 0.045(3) 0.030(3) 0.002(3) 0.024(3) -0.002(3) C26 0.106(5) 0.062(4) 0.023(3) -0.001(3) 0.024(3) -0.033(4) C27 0.082(5) 0.061(4) 0.060(4) -0.026(4) 0.036(4) -0.026(4) C28 0.107(6) 0.086(5) 0.060(5) -0.027(4) 0.030(4) -0.045(5) C29 0.064(4) 0.069(4) 0.050(4) -0.018(3) 0.018(3) 0.000(3) C30 0.071(4) 0.051(4) 0.038(3) -0.005(3) 0.021(3) -0.005(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 1.982(4) . ? Co1 N2 2.128(4) . ? Co1 N3 2.134(4) . ? Co1 O3 2.169(4) . ? Co1 N1 2.201(4) . ? Co1 O4 2.223(5) . ? N1 C18 1.330(7) . ? N1 C13 1.341(7) . ? N2 C25 1.341(7) . ? N2 C30 1.344(7) . ? N3 C24 1.328(7) . ? N3 C19 1.337(6) . ? N4 O5 1.231(7) . ? N4 O4 1.258(7) . ? N4 O3 1.282(8) . ? O1 C1 1.315(6) . ? O2 C12 1.343(8) . ? O2 H2H 0.8400 . ? C1 C2 1.384(9) . ? C1 C6 1.392(8) . ? C2 C3 1.393(9) . ? C2 H2 0.9500 . ? C3 C4 1.327(11) . ? C3 H3 0.9500 . ? C4 C5 1.380(10) . ? C4 H4 0.9500 . ? C5 C6 1.428(8) . ? C5 H5 0.9500 . ? C6 C7 1.492(9) . ? C7 C8 1.408(10) . ? C7 C12 1.420(10) . ? C8 C9 1.430(13) . ? C8 H8 0.9500 . ? C9 C10 1.368(16) . ? C9 H9 0.9500 . ? C10 C11 1.345(14) . ? C10 H10 0.9500 . ? C11 C12 1.377(10) . ? C11 H11 0.9500 . ? C13 C14 1.380(7) . ? C13 H13 0.9500 . ? C14 C15 1.401(8) . ? C14 H14 0.9500 . ? C15 C17 1.387(8) . ? C15 C16 1.467(7) . ? C16 C16 1.340(12) 3_666 ? C17 C18 1.377(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.365(7) . ? C19 H19 0.9500 . ? C20 C21 1.381(8) . ? C20 H20 0.9500 . ? C21 C23 1.378(7) . ? C21 C22 1.468(7) . ? C22 C22 1.320(11) 3_557 ? C23 C24 1.378(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.390(8) . ? C25 H25 0.9500 . ? C26 C27 1.386(9) . ? C26 H26 0.9500 . ? C27 C29 1.383(9) . ? C27 C28 1.503(9) . ? C28 C28 1.222(13) 3_656 ? C29 C30 1.361(8) . ? C29 H29 0.9500 . ? C30 H30 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 O1 Co1 N2 112.03(18) . . ? O1 Co1 N3 92.11(16) . . ? N2 Co1 N3 93.55(16) . . ? O1 Co1 O3 100.7(2) . . ? N2 Co1 O3 147.0(2) . . ? N3 Co1 O3 89.24(16) . . ? O1 Co1 N1 86.43(16) . . ? N2 Co1 N1 86.11(15) . . ? N3 Co1 N1 178.24(18) . . ? O3 Co1 N1 91.98(15) . . ? O1 Co1 O4 159.11(18) . . ? N2 Co1 O4 88.20(18) . . ? N3 Co1 O4 91.76(16) . . ? O3 Co1 O4 58.87(19) . . ? N1 Co1 O4 89.95(16) . . ? C18 N1 C13 116.1(4) . . ? C18 N1 Co1 121.1(4) . . ? C13 N1 Co1 121.5(3) . . ? C25 N2 C30 116.2(5) . . ? C25 N2 Co1 122.3(4) . . ? C30 N2 Co1 118.5(4) . . ? C24 N3 C19 116.2(4) . . ? C24 N3 Co1 121.8(3) . . ? C19 N3 Co1 121.6(3) . . ? O5 N4 O4 121.7(8) . . ? O5 N4 O3 121.9(7) . . ? O4 N4 O3 116.4(6) . . ? C1 O1 Co1 130.3(4) . . ? C12 O2 H2H 109.5 . . ? N4 O3 Co1 93.2(4) . . ? N4 O4 Co1 91.3(4) . . ? O1 C1 C2 120.4(6) . . ? O1 C1 C6 120.2(6) . . ? C2 C1 C6 119.4(6) . . ? C1 C2 C3 120.6(7) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 121.8(7) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 118.7(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 122.1(7) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 117.3(6) . . ? C1 C6 C7 124.5(5) . . ? C5 C6 C7 118.3(6) . . ? C8 C7 C12 117.9(7) . . ? C8 C7 C6 119.1(7) . . ? C12 C7 C6 123.0(6) . . ? C7 C8 C9 117.1(9) . . ? C7 C8 H8 121.4 . . ? C9 C8 H8 121.4 . . ? C10 C9 C8 122.5(10) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C11 C10 C9 119.9(10) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.5(10) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? O2 C12 C11 116.0(8) . . ? O2 C12 C7 122.1(6) . . ? C11 C12 C7 121.9(8) . . ? N1 C13 C14 123.9(5) . . ? N1 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C13 C14 C15 119.7(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C17 C15 C14 115.8(5) . . ? C17 C15 C16 120.1(5) . . ? C14 C15 C16 124.0(5) . . ? C16 C16 C15 123.5(7) 3_666 . ? C18 C17 C15 120.4(5) . . ? C18 C17 H17 119.8 . . ? C15 C17 H17 119.8 . . ? N1 C18 C17 123.9(6) . . ? N1 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? N3 C19 C20 124.1(5) . . ? N3 C19 H19 118.0 . . ? C20 C19 H19 118.0 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C23 C21 C20 115.9(5) . . ? C23 C21 C22 120.0(5) . . ? C20 C21 C22 124.1(5) . . ? C22 C22 C21 124.6(7) 3_557 . ? C21 C23 C24 120.9(5) . . ? C21 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? N3 C24 C23 122.8(5) . . ? N3 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? N2 C25 C26 122.0(6) . . ? N2 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C27 C26 C25 120.2(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C29 C27 C26 117.2(6) . . ? C29 C27 C28 116.5(7) . . ? C26 C27 C28 126.3(7) . . ? C28 C28 C27 123.9(11) 3_656 . ? C30 C29 C27 118.7(6) . . ? C30 C29 H29 120.6 . . ? C27 C29 H29 120.6 . . ? N2 C30 C29 125.0(6) . . ? N2 C30 H30 117.5 . . ? C29 C30 H30 117.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.805 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.087