# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Co N2 O4' _chemical_formula_weight 511.42 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 12.8267(7) _cell_length_b 12.4005(7) _cell_length_c 14.4996(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.7840(10) _cell_angle_gamma 90.00 _cell_volume 2294.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060.0 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12582 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.14 _reflns_number_total 4572 _reflns_number_gt 3527 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.7376P] 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 4572 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.74303(2) 0.63330(2) 0.98438(2) 0.02162(10) Uani 1 1 d . . . N2 N 0.58293(13) 0.62657(14) 0.94900(12) 0.0205(4) Uani 1 1 d . . . O4 O 0.72948(11) 0.54743(13) 1.09726(11) 0.0283(4) Uani 1 1 d . . . O2 O 0.67990(13) 0.78006(13) 1.04665(13) 0.0361(4) Uani 1 1 d . . . C11 C 0.95809(19) 0.35523(18) 1.23705(17) 0.0297(6) Uani 1 1 d . . . H11 H 1.0079 0.3105 1.2685 0.036 Uiso 1 1 calc R . . O1 O 0.76748(12) 0.53218(14) 0.88406(12) 0.0332(4) Uani 1 1 d . . . O3 O 0.79412(12) 0.76262(13) 0.88951(12) 0.0325(4) Uani 1 1 d . . . N1 N 0.90117(14) 0.65614(14) 1.02383(13) 0.0222(4) Uani 1 1 d . . . C14 C 0.80399(17) 0.48918(18) 1.13982(15) 0.0234(5) Uani 1 1 d . . . C9 C 0.91324(17) 0.50188(18) 1.12852(15) 0.0218(5) Uani 1 1 d . . . C8 C 0.95452(17) 0.58486(18) 1.07417(15) 0.0235(5) Uani 1 1 d . . . H8 H 1.0271 0.5880 1.0750 0.028 Uiso 1 1 calc R . . C22 C 0.53779(17) 0.56158(17) 0.88757(16) 0.0253(5) Uani 1 1 d . . . H22 H 0.4650 0.5589 0.8828 0.030 Uiso 1 1 calc R . . C16 C 0.57358(19) 0.77582(19) 1.05276(17) 0.0290(5) Uani 1 1 d . . . C28 C 0.69941(18) 0.48404(18) 0.82540(16) 0.0255(5) Uani 1 1 d . . . C23 C 0.58854(18) 0.49344(18) 0.82628(16) 0.0247(5) Uani 1 1 d . . . C21 C 0.52070(17) 0.69234(18) 1.00201(16) 0.0232(5) Uani 1 1 d . . . C10 C 0.98689(18) 0.43263(18) 1.17749(16) 0.0260(5) Uani 1 1 d . . . H10 H 1.0574 0.4400 1.1689 0.031 Uiso 1 1 calc R . . C2 C 0.89457(17) 0.80001(18) 0.91239(16) 0.0245(5) Uani 1 1 d . . . C7 C 0.95295(17) 0.74149(18) 0.98217(16) 0.0235(5) Uani 1 1 d . . . C20 C 0.41409(18) 0.6812(2) 1.00774(17) 0.0300(6) Uani 1 1 d . . . H20 H 0.3780 0.6250 0.9764 0.036 Uiso 1 1 calc R . . C26 C 0.6684(2) 0.3629(2) 0.69334(18) 0.0397(7) Uani 1 1 d . . . H26 H 0.6952 0.3211 0.6480 0.048 Uiso 1 1 calc R . . C27 C 0.7353(2) 0.41842(19) 0.75557(17) 0.0325(6) Uani 1 1 d . . . H27 H 0.8070 0.4127 0.7518 0.039 Uiso 1 1 calc R . . C13 C 0.77844(18) 0.40903(19) 1.20236(16) 0.0287(5) Uani 1 1 d . . . H13 H 0.7084 0.3994 1.2119 0.034 Uiso 1 1 calc R . . C24 C 0.5221(2) 0.43231(19) 0.76268(18) 0.0357(6) Uani 1 1 d . . . H24 H 0.4501 0.4357 0.7655 0.043 Uiso 1 1 calc R . . C19 C 0.3605(2) 0.7522(2) 1.05920(19) 0.0410(7) Uani 1 1 d . . . H19 H 0.2889 0.7438 1.0623 0.049 Uiso 1 1 calc R . . C3 C 0.93636(19) 0.88770(19) 0.87115(17) 0.0302(6) Uani 1 1 d . . . H3 H 0.8963 0.9258 0.8250 0.036 Uiso 1 1 calc R . . C12 C 0.8519(2) 0.34484(19) 1.24955(18) 0.0329(6) Uani 1 1 d . . . H12 H 0.8310 0.2934 1.2906 0.039 Uiso 1 1 calc R . . C6 C 1.05471(19) 0.7752(2) 1.00846(18) 0.0334(6) Uani 1 1 d . . . H6 H 1.0951 0.7380 1.0550 0.040 Uiso 1 1 calc R . . C25 C 0.5602(2) 0.3683(2) 0.69707(19) 0.0436(7) Uani 1 1 d . . . H25 H 0.5149 0.3291 0.6557 0.052 Uiso 1 1 calc R . . C4 C 1.03807(19) 0.9188(2) 0.89862(18) 0.0354(6) Uani 1 1 d . . . H4 H 1.0667 0.9779 0.8707 0.042 Uiso 1 1 calc R . . C17 C 0.5203(2) 0.8476(2) 1.10330(19) 0.0421(7) Uani 1 1 d . . . H17 H 0.5560 0.9036 1.1353 0.051 Uiso 1 1 calc R . . C5 C 1.0973(2) 0.8627(2) 0.96714(19) 0.0395(7) Uani 1 1 d . . . H5 H 1.1658 0.8838 0.9855 0.047 Uiso 1 1 calc R . . C15 C 0.7374(2) 0.8677(2) 1.0909(2) 0.0607(10) Uani 1 1 d . . . H15A H 0.7107 0.9346 1.0650 0.091 Uiso 1 1 calc R . . H15B H 0.8101 0.8609 1.0814 0.091 Uiso 1 1 calc R . . H15C H 0.7300 0.8665 1.1562 0.091 Uiso 1 1 calc R . . C18 C 0.4137(2) 0.8357(2) 1.1061(2) 0.0487(8) Uani 1 1 d . . . H18 H 0.3774 0.8844 1.1398 0.058 Uiso 1 1 calc R . . C1 C 0.7308(2) 0.8153(3) 0.8173(2) 0.0638(11) Uani 1 1 d . . . H1A H 0.7138 0.8865 0.8371 0.096 Uiso 1 1 calc R . . H1B H 0.6674 0.7750 0.8026 0.096 Uiso 1 1 calc R . . H1C H 0.7682 0.8201 0.7634 0.096 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 0.01811(16) 0.02380(17) 0.02270(18) -0.00118(14) 0.00086(12) -0.00183(13) N2 0.0192(9) 0.0208(9) 0.0216(10) 0.0016(8) 0.0022(7) -0.0009(8) O4 0.0188(8) 0.0369(9) 0.0293(9) 0.0069(8) 0.0032(7) 0.0005(7) O2 0.0266(9) 0.0322(10) 0.0503(12) -0.0178(9) 0.0075(8) -0.0051(8) C11 0.0315(13) 0.0257(13) 0.0308(14) 0.0033(11) -0.0028(10) 0.0041(11) O1 0.0218(8) 0.0414(10) 0.0370(10) -0.0146(8) 0.0055(7) -0.0065(8) O3 0.0219(9) 0.0364(9) 0.0373(10) 0.0135(8) -0.0065(7) -0.0040(7) N1 0.0207(10) 0.0250(10) 0.0208(10) 0.0007(8) 0.0022(8) -0.0031(8) C14 0.0221(12) 0.0266(12) 0.0214(12) -0.0030(10) 0.0015(9) -0.0016(10) C9 0.0234(12) 0.0234(11) 0.0186(12) -0.0021(9) 0.0017(9) -0.0006(9) C8 0.0170(11) 0.0302(12) 0.0234(12) -0.0025(10) 0.0024(9) -0.0007(10) C22 0.0179(11) 0.0255(12) 0.0315(14) 0.0028(10) -0.0031(10) -0.0014(10) C16 0.0287(13) 0.0285(13) 0.0310(14) 0.0000(11) 0.0082(10) 0.0038(10) C28 0.0323(13) 0.0218(12) 0.0233(13) 0.0000(10) 0.0074(10) -0.0030(10) C23 0.0291(13) 0.0205(11) 0.0234(13) 0.0014(10) -0.0026(10) -0.0004(10) C21 0.0234(12) 0.0243(12) 0.0223(12) 0.0064(10) 0.0037(9) 0.0052(10) C10 0.0236(12) 0.0273(12) 0.0271(13) -0.0039(10) 0.0018(10) 0.0007(10) C2 0.0213(12) 0.0252(12) 0.0272(13) 0.0001(10) 0.0034(9) -0.0017(10) C7 0.0225(12) 0.0246(12) 0.0236(12) -0.0008(10) 0.0034(9) -0.0045(10) C20 0.0248(13) 0.0373(14) 0.0284(14) 0.0104(11) 0.0049(10) 0.0027(11) C26 0.0619(19) 0.0281(14) 0.0293(15) -0.0073(12) 0.0061(13) 0.0021(13) C27 0.0409(15) 0.0285(13) 0.0294(14) -0.0020(11) 0.0104(11) -0.0007(11) C13 0.0242(12) 0.0366(13) 0.0254(13) 0.0038(11) 0.0029(10) -0.0072(11) C24 0.0373(15) 0.0277(13) 0.0392(16) -0.0052(12) -0.0112(12) -0.0019(11) C19 0.0282(14) 0.0552(18) 0.0420(17) 0.0140(14) 0.0143(12) 0.0127(13) C3 0.0287(13) 0.0289(13) 0.0330(14) 0.0065(11) 0.0035(11) 0.0000(11) C12 0.0384(14) 0.0310(13) 0.0291(14) 0.0074(11) 0.0023(11) -0.0070(11) C6 0.0273(13) 0.0374(14) 0.0341(15) 0.0091(12) -0.0044(11) -0.0075(11) C25 0.0584(19) 0.0300(14) 0.0381(16) -0.0093(13) -0.0165(14) -0.0001(14) C4 0.0327(14) 0.0335(14) 0.0409(16) 0.0082(12) 0.0082(12) -0.0102(11) C17 0.0471(17) 0.0393(16) 0.0417(17) -0.0086(13) 0.0135(13) 0.0071(13) C5 0.0258(13) 0.0450(16) 0.0467(17) 0.0090(14) -0.0020(12) -0.0159(12) C15 0.0500(19) 0.0506(19) 0.084(3) -0.0399(18) 0.0170(17) -0.0225(16) C18 0.0504(18) 0.0509(18) 0.0487(19) -0.0002(15) 0.0243(15) 0.0190(15) C1 0.0415(17) 0.072(2) 0.071(2) 0.040(2) -0.0256(16) -0.0153(16) _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 1.9693(16) . ? Co1 O4 1.9749(16) . ? Co1 N2 2.0677(17) . ? Co1 N1 2.0707(18) . ? Co1 O2 2.2204(16) . ? Co1 O3 2.2528(16) . ? N2 C22 1.294(3) . ? N2 C21 1.420(3) . ? O4 C14 1.303(3) . ? O2 C16 1.377(3) . ? O2 C15 1.429(3) . ? C11 C10 1.367(3) . ? C11 C12 1.399(3) . ? O1 C28 1.301(3) . ? O3 C2 1.378(3) . ? O3 C1 1.418(3) . ? N1 C8 1.297(3) . ? N1 C7 1.417(3) . ? C14 C13 1.406(3) . ? C14 C9 1.436(3) . ? C9 C10 1.414(3) . ? C9 C8 1.430(3) . ? C22 C23 1.430(3) . ? C16 C17 1.377(3) . ? C16 C21 1.405(3) . ? C28 C27 1.412(3) . ? C28 C23 1.428(3) . ? C23 C24 1.412(3) . ? C21 C20 1.385(3) . ? C2 C3 1.375(3) . ? C2 C7 1.399(3) . ? C7 C6 1.387(3) . ? C20 C19 1.381(4) . ? C26 C27 1.367(3) . ? C26 C25 1.395(4) . ? C13 C12 1.363(3) . ? C24 C25 1.367(4) . ? C19 C18 1.381(4) . ? C3 C4 1.380(3) . ? C6 C5 1.379(3) . ? C4 C5 1.377(3) . ? C17 C18 1.380(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O4 107.62(7) . . ? O1 Co1 N2 91.10(7) . . ? O4 Co1 N2 90.90(7) . . ? O1 Co1 N1 93.82(7) . . ? O4 Co1 N1 90.60(7) . . ? N2 Co1 N1 174.17(7) . . ? O1 Co1 O2 156.05(7) . . ? O4 Co1 O2 92.22(7) . . ? N2 Co1 O2 74.94(6) . . ? N1 Co1 O2 99.37(6) . . ? O1 Co1 O3 85.67(7) . . ? O4 Co1 O3 160.94(6) . . ? N2 Co1 O3 102.71(6) . . ? N1 Co1 O3 74.59(6) . . ? O2 Co1 O3 78.77(7) . . ? C22 N2 C21 119.56(19) . . ? C22 N2 Co1 124.07(16) . . ? C21 N2 Co1 116.16(14) . . ? C14 O4 Co1 124.74(15) . . ? C16 O2 C15 118.0(2) . . ? C16 O2 Co1 113.52(14) . . ? C15 O2 Co1 127.83(16) . . ? C10 C11 C12 118.4(2) . . ? C28 O1 Co1 128.96(15) . . ? C2 O3 C1 118.4(2) . . ? C2 O3 Co1 114.51(13) . . ? C1 O3 Co1 126.75(16) . . ? C8 N1 C7 120.38(19) . . ? C8 N1 Co1 120.59(15) . . ? C7 N1 Co1 118.21(14) . . ? O4 C14 C13 119.3(2) . . ? O4 C14 C9 124.3(2) . . ? C13 C14 C9 116.4(2) . . ? C10 C9 C8 116.6(2) . . ? C10 C9 C14 119.1(2) . . ? C8 C9 C14 124.2(2) . . ? N1 C8 C9 126.7(2) . . ? N2 C22 C23 126.6(2) . . ? O2 C16 C17 123.9(2) . . ? O2 C16 C21 115.1(2) . . ? C17 C16 C21 121.1(2) . . ? O1 C28 C27 119.2(2) . . ? O1 C28 C23 124.1(2) . . ? C27 C28 C23 116.7(2) . . ? C24 C23 C22 116.2(2) . . ? C24 C23 C28 119.1(2) . . ? C22 C23 C28 124.7(2) . . ? C20 C21 C16 118.0(2) . . ? C20 C21 N2 126.0(2) . . ? C16 C21 N2 116.0(2) . . ? C11 C10 C9 122.3(2) . . ? C3 C2 O3 123.9(2) . . ? C3 C2 C7 121.4(2) . . ? O3 C2 C7 114.8(2) . . ? C6 C7 C2 117.6(2) . . ? C6 C7 N1 125.2(2) . . ? C2 C7 N1 117.13(19) . . ? C19 C20 C21 121.1(2) . . ? C27 C26 C25 120.7(3) . . ? C26 C27 C28 122.4(3) . . ? C12 C13 C14 122.8(2) . . ? C25 C24 C23 122.1(3) . . ? C20 C19 C18 119.7(3) . . ? C2 C3 C4 119.6(2) . . ? C13 C12 C11 120.9(2) . . ? C5 C6 C7 121.4(2) . . ? C24 C25 C26 118.8(2) . . ? C3 C4 C5 120.2(2) . . ? C16 C17 C18 119.5(3) . . ? C6 C5 C4 119.8(2) . . ? C17 C18 C19 120.5(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.14 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.270 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 950121' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 Co N4 O2' _chemical_formula_weight 777.88 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 15.7846(9) _cell_length_b 16.9833(10) _cell_length_c 19.7804(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.2680(10) _cell_angle_gamma 90.00 _cell_volume 4907.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652.0 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 147(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26479 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.95 _reflns_number_total 9507 _reflns_number_gt 6797 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+3.5221P] 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 9507 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.09659(3) 0.80581(3) 0.27791(2) 0.02170(14) Uani 1 1 d . . . N2 N -0.00832(18) 0.74339(16) 0.27236(14) 0.0238(6) Uani 1 1 d . . . N1 N 0.08387(17) 0.85307(16) 0.36041(14) 0.0235(6) Uani 1 1 d . . . N4 N 0.02008(18) 0.88271(16) 0.21103(15) 0.0250(6) Uani 1 1 d . . . N3 N 0.10363(17) 0.75750(15) 0.19377(14) 0.0230(6) Uani 1 1 d . . . O1 O 0.17628(15) 0.73554(13) 0.34347(11) 0.0267(5) Uani 1 1 d . . . O2 O 0.19634(15) 0.86636(13) 0.28089(12) 0.0267(5) Uani 1 1 d . . . C1 C -0.0178(2) 0.9466(2) 0.22566(19) 0.0294(8) Uani 1 1 d . . . H1 H -0.0121 0.9565 0.2745 0.035 Uiso 1 1 calc R . . C2 C -0.0662(3) 0.9999(2) 0.1707(2) 0.0371(9) Uani 1 1 d . . . H2 H -0.0942 1.0448 0.1821 0.045 Uiso 1 1 calc R . . C3 C -0.0732(2) 0.9876(2) 0.1007(2) 0.0357(8) Uani 1 1 d . . . H3 H -0.1058 1.0236 0.0631 0.043 Uiso 1 1 calc R . . C4 C -0.0316(2) 0.9212(2) 0.0850(2) 0.0320(8) Uani 1 1 d . . . C5 C -0.0310(2) 0.9037(2) 0.01405(19) 0.0336(8) Uani 1 1 d . . . H5 H -0.0625 0.9371 -0.0262 0.040 Uiso 1 1 calc R . . C6 C 0.0139(2) 0.8404(2) 0.00466(18) 0.0317(8) Uani 1 1 d . . . H6 H 0.0143 0.8302 -0.0424 0.038 Uiso 1 1 calc R . . C7 C 0.0604(2) 0.7885(2) 0.06219(19) 0.0324(8) Uani 1 1 d . . . H7 H 0.0919 0.7442 0.0539 0.039 Uiso 1 1 calc R . . C8 C 0.0599(2) 0.80240(19) 0.12998(16) 0.0230(7) Uani 1 1 d . . . C9 C 0.0149(2) 0.86956(19) 0.14062(17) 0.0247(7) Uani 1 1 d . . . C10 C 0.1436(2) 0.69114(19) 0.19369(17) 0.0233(7) Uani 1 1 d . . . H10 H 0.1391 0.6710 0.1476 0.028 Uiso 1 1 calc R . . C11 C 0.1935(2) 0.64573(19) 0.25626(18) 0.0251(7) Uani 1 1 d . . . C12 C 0.2121(2) 0.67270(19) 0.32835(16) 0.0222(7) Uani 1 1 d . . . C13 C 0.2742(2) 0.6275(2) 0.38704(18) 0.0268(7) Uani 1 1 d . . . C14 C 0.3041(2) 0.5570(2) 0.37066(19) 0.0298(8) Uani 1 1 d . . . H14 H 0.3426 0.5259 0.4104 0.036 Uiso 1 1 calc R . . C15 C 0.2280(2) 0.5729(2) 0.2442(2) 0.0313(8) Uani 1 1 d . . . H15 H 0.2124 0.5553 0.1954 0.038 Uiso 1 1 calc R . . C16 C 0.2826(2) 0.5266(2) 0.29961(19) 0.0303(8) Uani 1 1 d . . . C17 C 0.3091(2) 0.6605(2) 0.46554(18) 0.0346(8) Uani 1 1 d . . . C18 C 0.2310(3) 0.6748(2) 0.4920(2) 0.0392(9) Uani 1 1 d . . . H18A H 0.1986 0.6253 0.4906 0.059 Uiso 1 1 calc R . . H18B H 0.1883 0.7135 0.4602 0.059 Uiso 1 1 calc R . . H18C H 0.2560 0.6949 0.5422 0.059 Uiso 1 1 calc R . . C19 C 0.3594(3) 0.7383(3) 0.4662(2) 0.0477(11) Uani 1 1 d . . . H19A H 0.3868 0.7582 0.5164 0.072 Uiso 1 1 calc R . . H19B H 0.3159 0.7771 0.4354 0.072 Uiso 1 1 calc R . . H19C H 0.4077 0.7291 0.4473 0.072 Uiso 1 1 calc R . . C20 C -0.0415(2) 0.76541(19) 0.32465(17) 0.0232(7) Uani 1 1 d . . . C21 C 0.0069(2) 0.82522(19) 0.37285(17) 0.0240(7) Uani 1 1 d . . . C22 C -0.0243(2) 0.8509(2) 0.42506(19) 0.0300(8) Uani 1 1 d . . . H22 H 0.0080 0.8907 0.4588 0.036 Uiso 1 1 calc R . . C23 C -0.1208(2) 0.7320(2) 0.32848(18) 0.0285(7) Uani 1 1 d . . . C24 C -0.1046(3) 0.8179(2) 0.4282(2) 0.0350(8) Uani 1 1 d . . . H24 H -0.1258 0.8360 0.4644 0.042 Uiso 1 1 calc R . . C25 C -0.1521(2) 0.7614(2) 0.3816(2) 0.0321(8) Uani 1 1 d . . . H25 H -0.2068 0.7413 0.3844 0.039 Uiso 1 1 calc R . . C26 C -0.1286(2) 0.6491(2) 0.2279(2) 0.0347(8) Uani 1 1 d . . . H26 H -0.1562 0.6075 0.1947 0.042 Uiso 1 1 calc R . . C27 C -0.1643(2) 0.6723(2) 0.2773(2) 0.0340(8) Uani 1 1 d . . . H27 H -0.2186 0.6483 0.2775 0.041 Uiso 1 1 calc R . . C28 C -0.0509(2) 0.6872(2) 0.22634(19) 0.0311(8) Uani 1 1 d . . . H28 H -0.0277 0.6717 0.1905 0.037 Uiso 1 1 calc R . . C30 C 0.1399(2) 0.9044(2) 0.40156(17) 0.0265(7) Uani 1 1 d . . . H30 H 0.1324 0.9183 0.4455 0.032 Uiso 1 1 calc R . . C31 C 0.2113(2) 0.94198(19) 0.38763(18) 0.0244(7) Uani 1 1 d . . . C32 C 0.2341(2) 0.92410(19) 0.32634(18) 0.0248(7) Uani 1 1 d . . . C33 C 0.3021(2) 0.97008(19) 0.31431(18) 0.0261(7) Uani 1 1 d . . . C34 C 0.3425(2) 1.0302(2) 0.36238(19) 0.0299(8) Uani 1 1 d . . . H34 H 0.3880 1.0606 0.3539 0.036 Uiso 1 1 calc R . . C35 C 0.3212(2) 1.0498(2) 0.42335(19) 0.0298(8) Uani 1 1 d . . . C36 C 0.2568(2) 1.0040(2) 0.43441(18) 0.0294(8) Uani 1 1 d . . . H36 H 0.2419 1.0144 0.4758 0.035 Uiso 1 1 calc R . . C37 C 0.3683(3) 1.1199(2) 0.4719(2) 0.0433(10) Uani 1 1 d . . . C38 C 0.3697(4) 1.1907(3) 0.4276(3) 0.0766(17) Uani 1 1 d . . . H38A H 0.3070 1.2041 0.3954 0.115 Uiso 1 1 calc R . . H38B H 0.4061 1.1793 0.3981 0.115 Uiso 1 1 calc R . . H38C H 0.3971 1.2350 0.4603 0.115 Uiso 1 1 calc R . . C39 C 0.4665(4) 1.1000(4) 0.5141(4) 0.120(3) Uani 1 1 d . . . H39A H 0.4980 1.0930 0.4803 0.180 Uiso 1 1 calc R . . H39B H 0.4703 1.0511 0.5414 0.180 Uiso 1 1 calc R . . H39C H 0.4957 1.1428 0.5482 0.180 Uiso 1 1 calc R . . C40 C 0.3211(5) 1.1416(4) 0.5218(4) 0.126(3) Uani 1 1 d . . . H40A H 0.3473 1.1905 0.5475 0.189 Uiso 1 1 calc R . . H40B H 0.3293 1.0993 0.5575 0.189 Uiso 1 1 calc R . . H40C H 0.2556 1.1491 0.4933 0.189 Uiso 1 1 calc R . . C41 C 0.3290(3) 0.9518(2) 0.2490(2) 0.0368(9) Uani 1 1 d . . . C42 C 0.4034(3) 1.0071(3) 0.2453(3) 0.0590(13) Uani 1 1 d . . . H42A H 0.3837 1.0618 0.2454 0.089 Uiso 1 1 calc R . . H42B H 0.4142 0.9969 0.2005 0.089 Uiso 1 1 calc R . . H42C H 0.4601 0.9982 0.2878 0.089 Uiso 1 1 calc R . . C43 C 0.2460(3) 0.9606(3) 0.1763(2) 0.0446(10) Uani 1 1 d . . . H43A H 0.1961 0.9266 0.1769 0.067 Uiso 1 1 calc R . . H43B H 0.2636 0.9453 0.1357 0.067 Uiso 1 1 calc R . . H43C H 0.2254 1.0155 0.1701 0.067 Uiso 1 1 calc R . . C44 C 0.3671(3) 0.8674(3) 0.2552(3) 0.0513(11) Uani 1 1 d . . . H44A H 0.4240 0.8635 0.2984 0.077 Uiso 1 1 calc R . . H44B H 0.3793 0.8549 0.2113 0.077 Uiso 1 1 calc R . . H44C H 0.3221 0.8302 0.2597 0.077 Uiso 1 1 calc R . . C45 C 0.3145(2) 0.4450(2) 0.2880(2) 0.0389(9) Uani 1 1 d . . . C46 C 0.4079(3) 0.4257(3) 0.3454(3) 0.0652(15) Uani 1 1 d . . . H46A H 0.4043 0.4256 0.3938 0.098 Uiso 1 1 calc R . . H46B H 0.4523 0.4654 0.3441 0.098 Uiso 1 1 calc R . . H46C H 0.4273 0.3736 0.3354 0.098 Uiso 1 1 calc R . . C47 C 0.3218(4) 0.4397(4) 0.2127(3) 0.0850(19) Uani 1 1 d . . . H47A H 0.3502 0.3896 0.2086 0.128 Uiso 1 1 calc R . . H47B H 0.3593 0.4833 0.2072 0.128 Uiso 1 1 calc R . . H47C H 0.2604 0.4430 0.1743 0.128 Uiso 1 1 calc R . . C48 C 0.2473(4) 0.3843(3) 0.2934(4) 0.091(2) Uani 1 1 d . . . H48A H 0.2496 0.3826 0.3436 0.137 Uiso 1 1 calc R . . H48B H 0.2633 0.3324 0.2801 0.137 Uiso 1 1 calc R . . H48C H 0.1853 0.3985 0.2601 0.137 Uiso 1 1 calc R . . C49 C 0.3777(3) 0.6057(3) 0.5198(2) 0.0572(13) Uani 1 1 d . . . H49A H 0.4039 0.6315 0.5676 0.086 Uiso 1 1 calc R . . H49B H 0.4266 0.5930 0.5026 0.086 Uiso 1 1 calc R . . H49C H 0.3467 0.5571 0.5243 0.086 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 0.0249(2) 0.0198(2) 0.0215(2) -0.00173(18) 0.01008(17) -0.00024(18) N2 0.0278(14) 0.0219(14) 0.0193(13) 0.0005(11) 0.0064(11) 0.0002(11) N1 0.0259(14) 0.0234(14) 0.0247(14) -0.0003(11) 0.0136(11) 0.0013(11) N4 0.0270(14) 0.0221(14) 0.0287(15) -0.0002(11) 0.0139(12) 0.0008(11) N3 0.0251(13) 0.0211(14) 0.0211(14) -0.0035(11) 0.0069(11) -0.0021(11) O1 0.0315(12) 0.0250(12) 0.0223(12) -0.0041(9) 0.0085(10) 0.0014(10) O2 0.0281(12) 0.0276(13) 0.0278(12) -0.0081(10) 0.0146(10) -0.0058(10) C1 0.0278(17) 0.0313(19) 0.0317(19) -0.0014(15) 0.0142(15) 0.0024(14) C2 0.043(2) 0.031(2) 0.046(2) 0.0096(17) 0.0273(18) 0.0122(16) C3 0.037(2) 0.028(2) 0.043(2) 0.0094(16) 0.0172(17) 0.0076(15) C4 0.0306(18) 0.0306(19) 0.0344(19) 0.0066(15) 0.0119(15) 0.0015(15) C5 0.039(2) 0.037(2) 0.0248(18) 0.0077(15) 0.0115(15) -0.0001(16) C6 0.0394(19) 0.034(2) 0.0192(17) -0.0008(14) 0.0088(14) -0.0017(16) C7 0.042(2) 0.029(2) 0.0287(19) -0.0007(14) 0.0155(16) 0.0056(15) C8 0.0223(15) 0.0263(17) 0.0199(15) -0.0013(13) 0.0073(12) -0.0032(13) C9 0.0233(16) 0.0261(18) 0.0241(17) -0.0039(14) 0.0084(13) -0.0037(13) C10 0.0257(16) 0.0239(17) 0.0187(15) -0.0054(13) 0.0068(12) -0.0003(13) C11 0.0227(16) 0.0261(18) 0.0264(17) 0.0005(14) 0.0093(13) 0.0016(13) C12 0.0215(15) 0.0239(17) 0.0207(16) -0.0015(13) 0.0073(13) -0.0018(12) C13 0.0201(15) 0.0292(18) 0.0299(18) -0.0007(14) 0.0080(13) 0.0008(13) C14 0.0272(17) 0.0296(19) 0.0264(18) 0.0028(14) 0.0029(14) 0.0009(14) C15 0.0335(19) 0.0272(19) 0.0307(19) -0.0066(15) 0.0095(15) 0.0007(15) C16 0.0254(17) 0.0307(19) 0.0309(19) -0.0020(15) 0.0061(14) 0.0045(14) C17 0.0356(19) 0.039(2) 0.0219(17) -0.0022(15) 0.0032(15) 0.0028(16) C18 0.043(2) 0.050(2) 0.0268(19) -0.0036(17) 0.0153(16) -0.0071(18) C19 0.043(2) 0.056(3) 0.041(2) -0.020(2) 0.0119(18) -0.021(2) C20 0.0238(15) 0.0213(16) 0.0248(17) 0.0041(13) 0.0097(13) 0.0025(13) C21 0.0288(16) 0.0208(17) 0.0225(16) 0.0037(13) 0.0096(13) 0.0007(13) C22 0.0339(18) 0.0262(18) 0.0346(19) -0.0065(15) 0.0182(15) -0.0046(14) C23 0.0314(17) 0.0254(18) 0.0311(19) 0.0010(14) 0.0145(15) 0.0006(14) C24 0.044(2) 0.031(2) 0.044(2) -0.0048(16) 0.0319(18) -0.0039(16) C25 0.0279(17) 0.032(2) 0.040(2) 0.0036(16) 0.0179(15) -0.0005(15) C26 0.0362(19) 0.032(2) 0.0311(19) -0.0042(16) 0.0079(15) -0.0088(16) C27 0.0299(18) 0.030(2) 0.039(2) 0.0014(16) 0.0105(16) -0.0069(15) C28 0.0316(18) 0.033(2) 0.0294(18) -0.0078(15) 0.0123(15) -0.0050(15) C30 0.0313(17) 0.0316(19) 0.0189(16) -0.0024(14) 0.0120(14) 0.0021(14) C31 0.0251(16) 0.0222(17) 0.0261(17) -0.0031(13) 0.0100(13) 0.0009(13) C32 0.0236(16) 0.0222(17) 0.0282(18) -0.0024(14) 0.0094(14) -0.0021(13) C33 0.0268(16) 0.0235(17) 0.0322(18) 0.0002(14) 0.0160(14) 0.0017(13) C34 0.0224(16) 0.0293(19) 0.042(2) -0.0017(16) 0.0173(15) -0.0047(14) C35 0.0289(17) 0.0300(19) 0.0308(19) -0.0032(15) 0.0118(15) -0.0018(14) C36 0.0293(17) 0.0335(19) 0.0259(18) -0.0097(14) 0.0110(14) -0.0005(14) C37 0.045(2) 0.041(2) 0.047(2) -0.0176(19) 0.0206(19) -0.0173(18) C38 0.114(5) 0.047(3) 0.066(3) -0.012(3) 0.030(3) -0.023(3) C39 0.086(4) 0.069(4) 0.135(6) -0.034(4) -0.037(4) -0.011(3) C40 0.150(6) 0.117(6) 0.167(7) -0.114(5) 0.125(6) -0.104(5) C41 0.037(2) 0.039(2) 0.044(2) -0.0133(17) 0.0263(17) -0.0062(16) C42 0.065(3) 0.067(3) 0.068(3) -0.020(2) 0.051(3) -0.029(2) C43 0.055(2) 0.051(3) 0.033(2) -0.0048(18) 0.0212(19) -0.006(2) C44 0.046(2) 0.053(3) 0.067(3) -0.012(2) 0.034(2) 0.001(2) C45 0.0322(19) 0.029(2) 0.048(2) -0.0084(17) 0.0071(17) 0.0088(15) C46 0.046(3) 0.052(3) 0.075(3) -0.019(2) -0.003(2) 0.020(2) C47 0.110(5) 0.078(4) 0.064(4) -0.010(3) 0.029(3) 0.048(4) C48 0.066(3) 0.041(3) 0.167(7) -0.026(3) 0.045(4) 0.001(3) C49 0.050(2) 0.071(3) 0.035(2) 0.001(2) -0.0021(19) 0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.858(2) . ? Co1 O2 1.863(2) . ? Co1 N1 1.896(3) . ? Co1 N3 1.896(3) . ? Co1 N4 1.924(3) . ? Co1 N2 1.934(3) . ? N2 C28 1.314(4) . ? N2 C20 1.376(4) . ? N1 C30 1.288(4) . ? N1 C21 1.410(4) . ? N4 C1 1.323(4) . ? N4 C9 1.382(4) . ? N3 C10 1.292(4) . ? N3 C8 1.411(4) . ? O1 C12 1.295(4) . ? O2 C32 1.311(4) . ? C1 C2 1.399(5) . ? C2 C3 1.363(5) . ? C3 C4 1.397(5) . ? C4 C9 1.380(5) . ? C4 C5 1.439(5) . ? C5 C6 1.339(5) . ? C6 C7 1.406(5) . ? C7 C8 1.365(5) . ? C8 C9 1.401(5) . ? C10 C11 1.417(4) . ? C11 C15 1.408(5) . ? C11 C12 1.419(4) . ? C12 C13 1.427(4) . ? C13 C14 1.370(5) . ? C13 C17 1.543(5) . ? C14 C16 1.413(5) . ? C15 C16 1.359(5) . ? C16 C45 1.521(5) . ? C17 C49 1.521(5) . ? C17 C18 1.530(5) . ? C17 C19 1.539(6) . ? C20 C23 1.402(5) . ? C20 C21 1.404(5) . ? C21 C22 1.373(5) . ? C22 C24 1.410(5) . ? C23 C25 1.412(5) . ? C23 C27 1.413(5) . ? C24 C25 1.344(5) . ? C26 C27 1.358(5) . ? C26 C28 1.397(5) . ? C30 C31 1.410(5) . ? C31 C36 1.406(5) . ? C31 C32 1.422(5) . ? C32 C33 1.419(4) . ? C33 C34 1.376(5) . ? C33 C41 1.538(5) . ? C34 C35 1.409(5) . ? C35 C36 1.362(5) . ? C35 C37 1.533(5) . ? C37 C40 1.492(7) . ? C37 C38 1.492(7) . ? C37 C39 1.495(7) . ? C41 C42 1.527(5) . ? C41 C44 1.541(6) . ? C41 C43 1.543(5) . ? C45 C48 1.513(7) . ? C45 C46 1.517(5) . ? C45 C47 1.540(7) . ? 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 89.53(10) . . ? O1 Co1 N1 86.31(10) . . ? O2 Co1 N1 95.91(10) . . ? O1 Co1 N3 94.90(10) . . ? O2 Co1 N3 86.37(10) . . ? N1 Co1 N3 177.44(11) . . ? O1 Co1 N4 176.61(11) . . ? O2 Co1 N4 87.12(11) . . ? N1 Co1 N4 93.48(11) . . ? N3 Co1 N4 85.45(11) . . ? O1 Co1 N2 91.51(11) . . ? O2 Co1 N2 178.65(10) . . ? N1 Co1 N2 85.02(11) . . ? N3 Co1 N2 92.68(11) . . ? N4 Co1 N2 91.84(11) . . ? C28 N2 C20 118.5(3) . . ? C28 N2 Co1 129.7(2) . . ? C20 N2 Co1 111.7(2) . . ? C30 N1 C21 123.2(3) . . ? C30 N1 Co1 124.0(2) . . ? C21 N1 Co1 112.8(2) . . ? C1 N4 C9 119.6(3) . . ? C1 N4 Co1 128.6(2) . . ? C9 N4 Co1 111.4(2) . . ? C10 N3 C8 123.0(3) . . ? C10 N3 Co1 124.7(2) . . ? C8 N3 Co1 112.3(2) . . ? C12 O1 Co1 127.4(2) . . ? C32 O2 Co1 126.4(2) . . ? N4 C1 C2 121.3(3) . . ? C3 C2 C1 120.1(3) . . ? C2 C3 C4 119.0(3) . . ? C9 C4 C3 119.3(3) . . ? C9 C4 C5 116.6(3) . . ? C3 C4 C5 124.0(3) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C7 122.2(3) . . ? C8 C7 C6 119.4(3) . . ? C7 C8 C9 118.7(3) . . ? C7 C8 N3 127.0(3) . . ? C9 C8 N3 114.2(3) . . ? C4 C9 N4 120.7(3) . . ? C4 C9 C8 123.0(3) . . ? N4 C9 C8 116.3(3) . . ? N3 C10 C11 125.7(3) . . ? C15 C11 C10 117.0(3) . . ? C15 C11 C12 120.5(3) . . ? C10 C11 C12 122.5(3) . . ? O1 C12 C11 123.8(3) . . ? O1 C12 C13 118.8(3) . . ? C11 C12 C13 117.4(3) . . ? C14 C13 C12 118.0(3) . . ? C14 C13 C17 122.2(3) . . ? C12 C13 C17 119.7(3) . . ? C13 C14 C16 125.5(3) . . ? C16 C15 C11 122.7(3) . . ? C15 C16 C14 115.5(3) . . ? C15 C16 C45 123.4(3) . . ? C14 C16 C45 121.0(3) . . ? C49 C17 C18 107.8(3) . . ? C49 C17 C19 107.0(3) . . ? C18 C17 C19 110.0(3) . . ? C49 C17 C13 112.0(3) . . ? C18 C17 C13 112.1(3) . . ? C19 C17 C13 107.9(3) . . ? N2 C20 C23 122.2(3) . . ? N2 C20 C21 116.3(3) . . ? C23 C20 C21 121.5(3) . . ? C22 C21 C20 118.9(3) . . ? C22 C21 N1 127.1(3) . . ? C20 C21 N1 114.0(3) . . ? C21 C22 C24 119.4(3) . . ? C20 C23 C25 117.9(3) . . ? C20 C23 C27 116.9(3) . . ? C25 C23 C27 125.1(3) . . ? C25 C24 C22 122.1(3) . . ? C24 C25 C23 120.1(3) . . ? C27 C26 C28 119.2(3) . . ? C26 C27 C23 120.1(3) . . ? N2 C28 C26 122.9(3) . . ? N1 C30 C31 126.2(3) . . ? C36 C31 C30 117.2(3) . . ? C36 C31 C32 119.3(3) . . ? C30 C31 C32 123.3(3) . . ? O2 C32 C33 118.2(3) . . ? O2 C32 C31 123.3(3) . . ? C33 C32 C31 118.5(3) . . ? C34 C33 C32 118.3(3) . . ? C34 C33 C41 121.8(3) . . ? C32 C33 C41 119.8(3) . . ? C33 C34 C35 124.6(3) . . ? C36 C35 C34 115.9(3) . . ? C36 C35 C37 123.9(3) . . ? C34 C35 C37 120.2(3) . . ? C35 C36 C31 123.3(3) . . ? C40 C37 C38 108.2(5) . . ? C40 C37 C39 111.0(6) . . ? C38 C37 C39 105.5(5) . . ? C40 C37 C35 111.2(3) . . ? C38 C37 C35 111.7(4) . . ? C39 C37 C35 109.1(4) . . ? C42 C41 C33 112.2(3) . . ? C42 C41 C44 107.0(3) . . ? C33 C41 C44 110.2(3) . . ? C42 C41 C43 107.1(4) . . ? C33 C41 C43 110.8(3) . . ? C44 C41 C43 109.4(3) . . ? C48 C45 C46 107.9(4) . . ? C48 C45 C16 109.2(3) . . ? C46 C45 C16 111.6(3) . . ? C48 C45 C47 109.9(5) . . ? C46 C45 C47 107.8(4) . . ? C16 C45 C47 110.5(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.628 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.094 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 92 5 ' ' 2 0.000 0.500 1.000 92 5 ' ' 3 0.460 0.341 0.690 253 16 ' ' 4 0.460 0.159 1.190 254 16 ' ' 5 0.540 0.659 0.310 254 16 ' ' 6 0.540 0.841 0.810 254 16 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 950122'