# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_12yuj24 #TrackingRef '18278_web_deposit_cif_file_0_ChunhuaHu_1362518436.12yuj24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H20 Co N2 O3 P' _chemical_formula_weight 534.37 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' P P 0.1023 0.0942 '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 'I 2' 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' _cell_length_a 13.042(4) _cell_length_b 7.3431(13) _cell_length_c 13.093(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.215(2) _cell_angle_gamma 90.00 _cell_volume 1253.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1556 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 21.10 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9473 _exptl_absorpt_correction_T_max 0.9769 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8266 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.41 _reflns_number_total 2586 _reflns_number_gt 2270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0130P)^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 0.049(14) _refine_ls_number_reflns 2586 _refine_ls_number_parameters 166 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.5000 0.50082(6) 0.5000 0.01399(14) Uani 1 2 d S . . O1 O 0.68311(16) 0.7056(3) 0.44456(15) 0.0409(6) Uani 1 1 d . . . O2 O 0.5000 0.0997(4) 0.5000 0.0350(8) Uani 1 2 d S . . N1 N 0.43131(15) 0.5116(4) 0.27634(15) 0.0217(5) Uani 1 1 d . . . C1 C 0.45660(17) 0.5032(5) 0.36086(17) 0.0173(5) Uani 1 1 d . . . C2 C 0.6120(2) 0.6262(4) 0.4665(2) 0.0214(7) Uani 1 1 d . . . C3 C 0.5000 0.2555(6) 0.5000 0.0216(9) Uani 1 2 d S . . P1 P 0.0000 0.83159(12) 0.5000 0.0137(2) Uani 1 2 d S . . C4 C 0.0424(2) 0.6852(4) 0.39977(19) 0.0155(6) Uani 1 1 d . . . C5 C 0.1404(2) 0.6949(4) 0.36107(19) 0.0175(6) Uani 1 1 d . . . H5 H 0.1878 0.7820 0.3875 0.021 Uiso 1 1 calc R . . C6 C 0.1692(2) 0.5777(4) 0.2839(2) 0.0218(7) Uani 1 1 d . . . H6 H 0.2364 0.5843 0.2575 0.026 Uiso 1 1 calc R . . C7 C 0.0998(2) 0.4506(3) 0.2450(2) 0.0224(7) Uani 1 1 d . . . H7 H 0.1192 0.3712 0.1915 0.027 Uiso 1 1 calc R . . C8 C 0.0020(2) 0.4398(4) 0.2843(2) 0.0256(7) Uani 1 1 d . . . H8 H -0.0455 0.3533 0.2576 0.031 Uiso 1 1 calc R . . C9 C -0.0260(2) 0.5545(3) 0.36225(19) 0.0191(7) Uani 1 1 d . . . H9 H -0.0923 0.5444 0.3905 0.023 Uiso 1 1 calc R . . C10 C 0.10240(17) 0.9767(4) 0.54453(18) 0.0138(6) Uani 1 1 d . . . C11 C 0.13960(18) 0.9689(4) 0.64466(18) 0.0165(7) Uani 1 1 d . . . H11 H 0.1113 0.8851 0.6916 0.020 Uiso 1 1 calc R . . C12 C 0.2186(2) 1.0849(4) 0.6755(2) 0.0204(7) Uani 1 1 d . . . H12 H 0.2446 1.0804 0.7438 0.024 Uiso 1 1 calc R . . C13 C 0.2592(2) 1.2069(4) 0.6068(2) 0.0222(7) Uani 1 1 d . . . H13 H 0.3137 1.2850 0.6281 0.027 Uiso 1 1 calc R . . C14 C 0.2213(2) 1.2166(4) 0.5071(2) 0.0220(7) Uani 1 1 d . . . H14 H 0.2498 1.3005 0.4603 0.026 Uiso 1 1 calc R . . C15 C 0.1418(2) 1.1034(4) 0.4763(2) 0.0185(6) Uani 1 1 d . . . H15 H 0.1141 1.1119 0.4088 0.022 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 0.0139(3) 0.0151(3) 0.0131(3) 0.000 0.0012(2) 0.000 O1 0.0333(13) 0.0593(17) 0.0301(13) 0.0105(11) -0.0004(11) -0.0278(12) O2 0.043(2) 0.0183(18) 0.044(2) 0.000 -0.0010(16) 0.000 N1 0.0244(12) 0.0217(13) 0.0188(11) -0.0029(14) -0.0006(9) -0.0031(15) C1 0.0158(12) 0.0143(13) 0.0220(14) 0.0001(17) 0.0030(10) 0.0005(16) C2 0.0261(18) 0.0259(18) 0.0121(15) 0.0008(12) -0.0044(13) -0.0028(14) C3 0.021(2) 0.026(3) 0.018(2) 0.000 0.0050(17) 0.000 P1 0.0132(5) 0.0148(7) 0.0132(5) 0.000 -0.0008(4) 0.000 C4 0.0173(15) 0.0164(15) 0.0127(14) 0.0028(11) -0.0016(11) 0.0026(12) C5 0.0155(15) 0.0186(16) 0.0183(15) 0.0000(12) -0.0023(12) 0.0012(12) C6 0.0207(16) 0.0247(17) 0.0200(16) 0.0027(13) 0.0037(13) 0.0050(13) C7 0.0273(16) 0.019(2) 0.0210(15) -0.0056(11) 0.0045(13) 0.0025(12) C8 0.0256(16) 0.0216(19) 0.0294(18) -0.0057(12) -0.0018(14) -0.0038(12) C9 0.0166(14) 0.0200(19) 0.0209(15) -0.0025(11) 0.0024(12) -0.0036(11) C10 0.0102(12) 0.0151(17) 0.0160(13) -0.0028(13) 0.0000(10) 0.0033(13) C11 0.0155(13) 0.0186(19) 0.0154(13) -0.0023(12) 0.0009(10) 0.0013(12) C12 0.0150(15) 0.0329(18) 0.0132(15) -0.0036(13) -0.0026(12) 0.0009(13) C13 0.0165(15) 0.0274(18) 0.0228(16) -0.0060(14) -0.0005(13) -0.0049(13) C14 0.0224(17) 0.0232(18) 0.0206(16) -0.0001(13) 0.0039(13) -0.0066(13) C15 0.0210(16) 0.0197(16) 0.0149(15) -0.0005(12) -0.0024(12) -0.0002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C2 1.789(3) . ? Co1 C2 1.789(3) 2_656 ? Co1 C3 1.801(4) . ? Co1 C1 1.896(2) . ? Co1 C1 1.896(2) 2_656 ? O1 C2 1.138(3) . ? O2 C3 1.145(4) . ? N1 C1 1.150(3) . ? P1 C4 1.793(3) 2_556 ? P1 C4 1.793(3) . ? P1 C10 1.796(3) . ? P1 C10 1.796(3) 2_556 ? C4 C5 1.386(3) . ? C4 C9 1.393(3) . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.389(3) . ? C6 H6 0.9500 . ? C7 C8 1.387(4) . ? C7 H7 0.9500 . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.389(3) . ? C10 C15 1.396(4) . ? C11 C12 1.390(3) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 H15 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 C2 Co1 C2 118.05(19) . 2_656 ? C2 Co1 C3 120.97(10) . . ? C2 Co1 C3 120.97(10) 2_656 . ? C2 Co1 C1 89.35(12) . . ? C2 Co1 C1 90.10(12) 2_656 . ? C3 Co1 C1 90.53(11) . . ? C2 Co1 C1 90.10(12) . 2_656 ? C2 Co1 C1 89.35(12) 2_656 2_656 ? C3 Co1 C1 90.53(11) . 2_656 ? C1 Co1 C1 178.9(2) . 2_656 ? N1 C1 Co1 177.4(3) . . ? O1 C2 Co1 179.5(3) . . ? O2 C3 Co1 180.000(1) . . ? C4 P1 C4 106.33(17) 2_556 . ? C4 P1 C10 110.92(12) 2_556 . ? C4 P1 C10 110.76(11) . . ? C4 P1 C10 110.76(11) 2_556 2_556 ? C4 P1 C10 110.92(12) . 2_556 ? C10 P1 C10 107.20(18) . 2_556 ? C5 C4 C9 119.7(2) . . ? C5 C4 P1 122.5(2) . . ? C9 C4 P1 117.8(2) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 119.9(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.0(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 120.2(2) . . ? C8 C9 H9 119.9 . . ? C4 C9 H9 119.9 . . ? C11 C10 C15 120.4(3) . . ? C11 C10 P1 121.6(2) . . ? C15 C10 P1 117.99(18) . . ? C10 C11 C12 119.4(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C10 119.9(2) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.351 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 927721' ####################################################################### # # 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_12yuj30new _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H42 Co N3 O3 P2' _chemical_formula_weight 889.77 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' P P 0.1023 0.0942 '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 9.7538(3) _cell_length_b 11.1003(3) _cell_length_c 21.8916(6) _cell_angle_alpha 96.4350(10) _cell_angle_beta 95.4790(10) _cell_angle_gamma 108.4320(10) _cell_volume 2212.79(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.71 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8921 _exptl_absorpt_correction_T_max 0.9509 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40694 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.71 _reflns_number_total 8418 _reflns_number_gt 7212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0268P)^2^+1.4080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8418 _refine_ls_number_parameters 565 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.15130(2) -0.01212(2) 0.248763(10) 0.01398(7) Uani 1 1 d . . . O1 O -0.14971(14) -0.12415(13) 0.27234(7) 0.0325(3) Uani 1 1 d . . . O2 O 0.31506(15) -0.16081(13) 0.19089(6) 0.0278(3) Uani 1 1 d . . . N1 N 0.30071(17) 0.28132(14) 0.28965(7) 0.0211(3) Uani 1 1 d . . . N2 N 0.05160(18) 0.02123(15) 0.11725(7) 0.0254(4) Uani 1 1 d . . . N3 N 0.26659(17) -0.06709(14) 0.37385(7) 0.0222(3) Uani 1 1 d . . . C1 C 0.24266(18) 0.17251(16) 0.27448(8) 0.0156(4) Uani 1 1 d . . . C2 C 0.08796(19) 0.01184(16) 0.16804(9) 0.0180(4) Uani 1 1 d . . . C3 C 0.22269(18) -0.04410(15) 0.32690(8) 0.0163(4) Uani 1 1 d . . . C4 C -0.0318(2) -0.07670(17) 0.26363(8) 0.0199(4) Uani 1 1 d . . . C5 C 0.25413(19) -0.09869(16) 0.21421(8) 0.0172(4) Uani 1 1 d . . . P1 P 0.58770(5) 0.33269(4) 0.09745(2) 0.01383(10) Uani 1 1 d . . . C6 C 0.44280(19) 0.39344(16) 0.11400(8) 0.0159(4) Uani 1 1 d . . . C7 C 0.30974(19) 0.31012(17) 0.12554(8) 0.0203(4) Uani 1 1 d . . . H7 H 0.2961 0.2215 0.1254 0.024 Uiso 1 1 calc R . . C8 C 0.1983(2) 0.35771(19) 0.13710(9) 0.0247(4) Uani 1 1 d . . . H8 H 0.1086 0.3019 0.1458 0.030 Uiso 1 1 calc R . . C9 C 0.2168(2) 0.48657(19) 0.13601(8) 0.0250(4) Uani 1 1 d . . . H9 H 0.1397 0.5185 0.1440 0.030 Uiso 1 1 calc R . . C10 C 0.3471(2) 0.56883(18) 0.12336(8) 0.0231(4) Uani 1 1 d . . . H10 H 0.3587 0.6567 0.1221 0.028 Uiso 1 1 calc R . . C11 C 0.4607(2) 0.52292(17) 0.11246(8) 0.0189(4) Uani 1 1 d . . . H11 H 0.5504 0.5794 0.1040 0.023 Uiso 1 1 calc R . . C12 C 0.74565(18) 0.46637(16) 0.09231(8) 0.0159(4) Uani 1 1 d . . . C13 C 0.78855(19) 0.49516(17) 0.03550(8) 0.0192(4) Uani 1 1 d . . . H13 H 0.7387 0.4398 -0.0018 0.023 Uiso 1 1 calc R . . C14 C 0.9049(2) 0.60546(17) 0.03354(9) 0.0232(4) Uani 1 1 d . . . H14 H 0.9352 0.6255 -0.0051 0.028 Uiso 1 1 calc R . . C15 C 0.9763(2) 0.68593(17) 0.08788(9) 0.0229(4) Uani 1 1 d . . . H15 H 1.0554 0.7616 0.0864 0.027 Uiso 1 1 calc R . . C16 C 0.9334(2) 0.65716(17) 0.14470(9) 0.0225(4) Uani 1 1 d . . . H16 H 0.9830 0.7131 0.1818 0.027 Uiso 1 1 calc R . . C17 C 0.81890(19) 0.54735(17) 0.14720(8) 0.0207(4) Uani 1 1 d . . . H17 H 0.7900 0.5269 0.1860 0.025 Uiso 1 1 calc R . . C18 C 0.53192(19) 0.22854(15) 0.02390(8) 0.0166(4) Uani 1 1 d . . . C19 C 0.6279(2) 0.17021(16) 0.00070(8) 0.0188(4) Uani 1 1 d . . . H19 H 0.7181 0.1803 0.0249 0.023 Uiso 1 1 calc R . . C20 C 0.5904(2) 0.09762(17) -0.05786(8) 0.0226(4) Uani 1 1 d . . . H20 H 0.6557 0.0586 -0.0741 0.027 Uiso 1 1 calc R . . C21 C 0.4579(2) 0.08177(17) -0.09284(9) 0.0243(4) Uani 1 1 d . . . H21 H 0.4334 0.0327 -0.1332 0.029 Uiso 1 1 calc R . . C22 C 0.3616(2) 0.13660(18) -0.06955(9) 0.0253(4) Uani 1 1 d . . . H22 H 0.2700 0.1233 -0.0934 0.030 Uiso 1 1 calc R . . C23 C 0.3979(2) 0.21137(17) -0.01119(8) 0.0213(4) Uani 1 1 d . . . H23 H 0.3322 0.2504 0.0046 0.026 Uiso 1 1 calc R . . C24 C 0.64005(18) 0.25522(15) 0.15939(8) 0.0156(4) Uani 1 1 d . . . C25 C 0.77132(19) 0.22850(17) 0.15983(8) 0.0199(4) Uani 1 1 d . . . H25 H 0.8301 0.2513 0.1280 0.024 Uiso 1 1 calc R . . C26 C 0.8152(2) 0.16913(18) 0.20648(9) 0.0237(4) Uani 1 1 d . . . H26 H 0.9041 0.1509 0.2067 0.028 Uiso 1 1 calc R . . C27 C 0.7292(2) 0.13608(17) 0.25311(9) 0.0231(4) Uani 1 1 d . . . H27 H 0.7593 0.0949 0.2851 0.028 Uiso 1 1 calc R . . C28 C 0.6003(2) 0.16275(18) 0.25314(9) 0.0227(4) Uani 1 1 d . . . H28 H 0.5421 0.1397 0.2851 0.027 Uiso 1 1 calc R . . C29 C 0.55508(19) 0.22307(17) 0.20668(8) 0.0191(4) Uani 1 1 d . . . H29 H 0.4669 0.2423 0.2071 0.023 Uiso 1 1 calc R . . P2 P 0.79511(5) 0.58659(4) 0.41864(2) 0.01460(10) Uani 1 1 d . . . C30 C 0.67750(19) 0.64805(18) 0.37305(8) 0.0214(4) Uani 1 1 d . . . C31 C 0.6511(2) 0.7593(2) 0.39655(10) 0.0280(4) Uani 1 1 d . . . H31 H 0.6979 0.8048 0.4364 0.034 Uiso 1 1 calc R . . C32 C 0.5558(2) 0.8031(3) 0.36124(12) 0.0423(6) Uani 1 1 d . . . H32 H 0.5374 0.8791 0.3768 0.051 Uiso 1 1 calc R . . C33 C 0.4881(3) 0.7363(3) 0.30374(12) 0.0530(8) Uani 1 1 d . . . H33 H 0.4228 0.7664 0.2798 0.064 Uiso 1 1 calc R . . C34 C 0.5140(2) 0.6263(3) 0.28057(11) 0.0501(7) Uani 1 1 d . . . H34 H 0.4658 0.5809 0.2409 0.060 Uiso 1 1 calc R . . C35 C 0.6094(2) 0.5813(2) 0.31442(9) 0.0345(5) Uani 1 1 d . . . H35 H 0.6284 0.5061 0.2981 0.041 Uiso 1 1 calc R . . C36 C 0.69228(18) 0.44609(16) 0.44820(8) 0.0173(4) Uani 1 1 d . . . C37 C 0.7422(2) 0.41777(17) 0.50515(9) 0.0212(4) Uani 1 1 d . . . H37 H 0.8250 0.4779 0.5308 0.025 Uiso 1 1 calc R . . C38 C 0.6704(2) 0.30156(19) 0.52401(10) 0.0273(4) Uani 1 1 d . . . H38 H 0.7020 0.2831 0.5632 0.033 Uiso 1 1 calc R . . C39 C 0.5529(2) 0.21280(18) 0.48555(10) 0.0286(5) Uani 1 1 d . . . H39 H 0.5063 0.1320 0.4978 0.034 Uiso 1 1 calc R . . C40 C 0.5025(2) 0.24048(18) 0.42943(10) 0.0284(5) Uani 1 1 d . . . H40 H 0.4210 0.1789 0.4036 0.034 Uiso 1 1 calc R . . C41 C 0.5700(2) 0.35742(18) 0.41066(9) 0.0237(4) Uani 1 1 d . . . H41 H 0.5336 0.3772 0.3726 0.028 Uiso 1 1 calc R . . C42 C 0.89935(19) 0.71113(16) 0.48084(8) 0.0153(4) Uani 1 1 d . . . C43 C 1.03595(19) 0.79375(16) 0.47344(8) 0.0185(4) Uani 1 1 d . . . H43 H 1.0777 0.7798 0.4369 0.022 Uiso 1 1 calc R . . C44 C 1.1105(2) 0.89608(18) 0.51945(9) 0.0243(4) Uani 1 1 d . . . H44 H 1.2043 0.9516 0.5147 0.029 Uiso 1 1 calc R . . C45 C 1.0492(2) 0.91789(17) 0.57236(9) 0.0248(4) Uani 1 1 d . . . H45 H 1.1009 0.9884 0.6037 0.030 Uiso 1 1 calc R . . C46 C 0.9128(2) 0.83726(17) 0.57970(8) 0.0232(4) Uani 1 1 d . . . H46 H 0.8709 0.8530 0.6159 0.028 Uiso 1 1 calc R . . C47 C 0.8373(2) 0.73370(17) 0.53436(8) 0.0198(4) Uani 1 1 d . . . H47 H 0.7439 0.6782 0.5395 0.024 Uiso 1 1 calc R . . C48 C 0.91366(18) 0.54221(16) 0.36920(8) 0.0152(4) Uani 1 1 d . . . C49 C 0.98315(19) 0.62832(17) 0.33087(8) 0.0193(4) Uani 1 1 d . . . H49 H 0.9617 0.7056 0.3288 0.023 Uiso 1 1 calc R . . C50 C 1.0833(2) 0.60044(17) 0.29601(8) 0.0216(4) Uani 1 1 d . . . H50 H 1.1324 0.6596 0.2707 0.026 Uiso 1 1 calc R . . C51 C 1.1123(2) 0.48609(17) 0.29797(8) 0.0210(4) Uani 1 1 d . . . H51 H 1.1814 0.4674 0.2741 0.025 Uiso 1 1 calc R . . C52 C 1.0408(2) 0.39958(17) 0.33458(8) 0.0205(4) Uani 1 1 d . . . H52 H 1.0597 0.3208 0.3351 0.025 Uiso 1 1 calc R . . C53 C 0.94175(19) 0.42679(16) 0.37058(8) 0.0178(4) Uani 1 1 d . . . H53 H 0.8934 0.3673 0.3960 0.021 Uiso 1 1 calc R . . O3 O -0.06276(18) 0.12562(15) 0.01620(7) 0.0380(4) Uani 1 1 d D . . H1 H -0.061(3) 0.078(2) -0.0169(8) 0.057 Uiso 1 1 d D . . H2 H -0.027(3) 0.092(2) 0.0446(9) 0.057 Uiso 1 1 d 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 0.01473(12) 0.01311(12) 0.01444(12) 0.00192(9) 0.00297(9) 0.00486(9) O1 0.0191(7) 0.0349(8) 0.0469(9) 0.0150(7) 0.0123(6) 0.0082(6) O2 0.0383(8) 0.0331(8) 0.0221(7) 0.0044(6) 0.0094(6) 0.0243(7) N1 0.0238(8) 0.0170(8) 0.0226(8) 0.0012(6) 0.0060(7) 0.0066(7) N2 0.0281(9) 0.0237(8) 0.0223(9) 0.0055(7) -0.0007(7) 0.0063(7) N3 0.0259(9) 0.0203(8) 0.0205(8) 0.0028(6) 0.0048(7) 0.0075(7) C1 0.0170(9) 0.0202(9) 0.0131(8) 0.0036(7) 0.0055(7) 0.0097(7) C2 0.0167(9) 0.0135(8) 0.0237(10) 0.0025(7) 0.0038(7) 0.0046(7) C3 0.0171(9) 0.0122(8) 0.0191(9) -0.0001(7) 0.0052(7) 0.0043(7) C4 0.0238(10) 0.0181(9) 0.0205(10) 0.0045(7) 0.0031(8) 0.0100(8) C5 0.0200(9) 0.0176(9) 0.0132(9) 0.0049(7) 0.0011(7) 0.0047(7) P1 0.0138(2) 0.0126(2) 0.0144(2) 0.00061(17) 0.00263(17) 0.00370(17) C6 0.0180(9) 0.0174(8) 0.0130(8) 0.0005(7) 0.0014(7) 0.0078(7) C7 0.0206(9) 0.0207(9) 0.0209(9) 0.0054(7) 0.0033(7) 0.0078(8) C8 0.0188(10) 0.0368(11) 0.0213(10) 0.0071(8) 0.0043(8) 0.0118(8) C9 0.0292(11) 0.0398(11) 0.0150(9) 0.0013(8) 0.0024(8) 0.0251(9) C10 0.0362(11) 0.0225(9) 0.0143(9) -0.0015(7) -0.0004(8) 0.0173(8) C11 0.0241(10) 0.0202(9) 0.0124(9) 0.0000(7) 0.0013(7) 0.0088(8) C12 0.0140(8) 0.0140(8) 0.0193(9) 0.0014(7) 0.0033(7) 0.0039(7) C13 0.0212(9) 0.0182(9) 0.0156(9) 0.0003(7) 0.0011(7) 0.0039(7) C14 0.0242(10) 0.0226(9) 0.0208(10) 0.0069(8) 0.0050(8) 0.0032(8) C15 0.0202(9) 0.0176(9) 0.0270(10) 0.0048(8) 0.0017(8) 0.0011(7) C16 0.0212(10) 0.0186(9) 0.0230(10) -0.0032(7) -0.0003(8) 0.0032(8) C17 0.0215(9) 0.0222(9) 0.0158(9) -0.0003(7) 0.0038(7) 0.0042(8) C18 0.0198(9) 0.0113(8) 0.0157(9) 0.0013(7) 0.0036(7) 0.0010(7) C19 0.0210(9) 0.0157(8) 0.0193(9) 0.0039(7) 0.0047(7) 0.0045(7) C20 0.0317(11) 0.0142(8) 0.0215(10) 0.0022(7) 0.0110(8) 0.0048(8) C21 0.0333(11) 0.0153(9) 0.0163(9) -0.0013(7) 0.0042(8) -0.0023(8) C22 0.0242(10) 0.0229(10) 0.0218(10) 0.0012(8) -0.0015(8) 0.0002(8) C23 0.0211(9) 0.0194(9) 0.0213(10) 0.0012(7) 0.0019(8) 0.0047(7) C24 0.0163(9) 0.0128(8) 0.0160(9) -0.0001(7) 0.0015(7) 0.0035(7) C25 0.0179(9) 0.0220(9) 0.0196(9) 0.0013(7) 0.0040(7) 0.0064(7) C26 0.0203(10) 0.0266(10) 0.0272(10) 0.0031(8) 0.0015(8) 0.0126(8) C27 0.0274(10) 0.0219(9) 0.0202(10) 0.0030(8) -0.0011(8) 0.0100(8) C28 0.0259(10) 0.0257(10) 0.0192(10) 0.0053(8) 0.0061(8) 0.0108(8) C29 0.0172(9) 0.0220(9) 0.0202(9) 0.0026(7) 0.0047(7) 0.0089(7) P2 0.0136(2) 0.0177(2) 0.0127(2) 0.00144(17) 0.00166(17) 0.00581(18) C30 0.0145(9) 0.0335(10) 0.0197(9) 0.0115(8) 0.0047(7) 0.0099(8) C31 0.0238(10) 0.0384(12) 0.0314(11) 0.0172(9) 0.0114(9) 0.0174(9) C32 0.0320(12) 0.0621(16) 0.0542(16) 0.0378(13) 0.0208(11) 0.0315(12) C33 0.0262(12) 0.101(2) 0.0515(16) 0.0536(16) 0.0125(11) 0.0320(14) C34 0.0253(12) 0.094(2) 0.0282(12) 0.0247(13) -0.0039(10) 0.0125(13) C35 0.0239(11) 0.0550(14) 0.0219(11) 0.0091(10) -0.0006(8) 0.0094(10) C36 0.0153(9) 0.0197(9) 0.0172(9) 0.0011(7) 0.0064(7) 0.0057(7) C37 0.0170(9) 0.0238(9) 0.0231(10) 0.0038(8) 0.0031(8) 0.0068(8) C38 0.0266(11) 0.0301(11) 0.0321(11) 0.0139(9) 0.0116(9) 0.0139(9) C39 0.0268(11) 0.0196(9) 0.0437(13) 0.0073(9) 0.0201(9) 0.0083(8) C40 0.0214(10) 0.0246(10) 0.0329(12) -0.0070(9) 0.0114(9) 0.0007(8) C41 0.0190(9) 0.0284(10) 0.0197(10) -0.0029(8) 0.0057(8) 0.0037(8) C42 0.0190(9) 0.0153(8) 0.0139(8) 0.0013(7) 0.0002(7) 0.0098(7) C43 0.0199(9) 0.0208(9) 0.0165(9) 0.0013(7) 0.0039(7) 0.0089(7) C44 0.0244(10) 0.0205(9) 0.0257(10) 0.0002(8) 0.0024(8) 0.0056(8) C45 0.0361(11) 0.0181(9) 0.0189(10) -0.0020(7) -0.0012(8) 0.0103(8) C46 0.0379(11) 0.0207(9) 0.0165(9) 0.0031(7) 0.0081(8) 0.0161(9) C47 0.0232(10) 0.0208(9) 0.0195(9) 0.0056(7) 0.0071(8) 0.0110(8) C48 0.0145(8) 0.0176(8) 0.0112(8) -0.0022(7) -0.0003(7) 0.0043(7) C49 0.0229(9) 0.0184(9) 0.0170(9) 0.0024(7) 0.0030(7) 0.0075(7) C50 0.0243(10) 0.0227(9) 0.0190(9) 0.0063(7) 0.0079(8) 0.0069(8) C51 0.0213(9) 0.0273(10) 0.0154(9) -0.0004(7) 0.0043(7) 0.0099(8) C52 0.0255(10) 0.0204(9) 0.0172(9) 0.0003(7) 0.0020(8) 0.0110(8) C53 0.0197(9) 0.0177(9) 0.0145(9) 0.0026(7) 0.0016(7) 0.0043(7) O3 0.0461(10) 0.0428(9) 0.0348(9) 0.0152(7) 0.0062(8) 0.0250(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C5 1.7586(18) . ? Co1 C4 1.7781(19) . ? Co1 C2 1.8912(19) . ? Co1 C3 1.8978(18) . ? Co1 C1 1.9499(17) . ? O1 C4 1.148(2) . ? O2 C5 1.152(2) . ? N1 C1 1.154(2) . ? N2 C2 1.161(2) . ? N3 C3 1.161(2) . ? P1 C12 1.7925(17) . ? P1 C6 1.7970(17) . ? P1 C18 1.8008(17) . ? P1 C24 1.8016(18) . ? C6 C11 1.397(2) . ? C6 C7 1.400(2) . ? C7 C8 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.389(2) . ? C12 C17 1.396(2) . ? C13 C14 1.389(2) . ? C13 H13 0.9500 . ? C14 C15 1.382(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.379(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.398(3) . ? C18 C19 1.398(2) . ? C19 C20 1.385(2) . ? C19 H19 0.9500 . ? C20 C21 1.388(3) . ? C20 H20 0.9500 . ? C21 C22 1.377(3) . ? C21 H21 0.9500 . ? C22 C23 1.392(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.395(2) . ? C24 C25 1.402(2) . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.390(3) . ? C26 H26 0.9500 . ? C27 C28 1.380(3) . ? C27 H27 0.9500 . ? C28 C29 1.390(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? P2 C30 1.7907(18) . ? P2 C36 1.7938(18) . ? P2 C42 1.7955(17) . ? P2 C48 1.7974(17) . ? C30 C31 1.392(3) . ? C30 C35 1.396(3) . ? C31 C32 1.390(3) . ? C31 H31 0.9500 . ? C32 C33 1.376(4) . ? C32 H32 0.9500 . ? C33 C34 1.375(4) . ? C33 H33 0.9500 . ? C34 C35 1.383(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.399(2) . ? C36 C37 1.400(3) . ? C37 C38 1.389(3) . ? C37 H37 0.9500 . ? C38 C39 1.382(3) . ? C38 H38 0.9500 . ? C39 C40 1.382(3) . ? C39 H39 0.9500 . ? C40 C41 1.385(3) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.394(2) . ? C42 C47 1.402(2) . ? C43 C44 1.384(3) . ? C43 H43 0.9500 . ? C44 C45 1.386(3) . ? C44 H44 0.9500 . ? C45 C46 1.384(3) . ? C45 H45 0.9500 . ? C46 C47 1.385(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C53 1.395(2) . ? C48 C49 1.398(2) . ? C49 C50 1.384(2) . ? C49 H49 0.9500 . ? C50 C51 1.389(3) . ? C50 H50 0.9500 . ? C51 C52 1.381(3) . ? C51 H51 0.9500 . ? C52 C53 1.387(2) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? O3 H1 0.853(10) . ? O3 H2 0.861(10) . ? 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 C5 Co1 C4 126.25(8) . . ? C5 Co1 C2 87.48(8) . . ? C4 Co1 C2 91.47(8) . . ? C5 Co1 C3 88.10(7) . . ? C4 Co1 C3 90.92(8) . . ? C2 Co1 C3 175.58(7) . . ? C5 Co1 C1 118.49(7) . . ? C4 Co1 C1 115.25(7) . . ? C2 Co1 C1 91.59(7) . . ? C3 Co1 C1 90.75(7) . . ? N1 C1 Co1 177.97(15) . . ? N2 C2 Co1 176.33(16) . . ? N3 C3 Co1 177.96(15) . . ? O1 C4 Co1 176.73(16) . . ? O2 C5 Co1 176.48(16) . . ? C12 P1 C6 108.15(8) . . ? C12 P1 C18 109.36(8) . . ? C6 P1 C18 108.46(8) . . ? C12 P1 C24 106.05(8) . . ? C6 P1 C24 111.87(8) . . ? C18 P1 C24 112.82(8) . . ? C11 C6 C7 119.96(16) . . ? C11 C6 P1 119.83(13) . . ? C7 C6 P1 120.14(13) . . ? C8 C7 C6 119.54(17) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.36(18) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.35(17) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.01(17) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 119.76(17) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? C13 C12 C17 120.37(16) . . ? C13 C12 P1 121.63(13) . . ? C17 C12 P1 117.83(13) . . ? C12 C13 C14 119.54(16) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 119.94(17) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.52(17) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.00(17) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C12 119.62(17) . . ? C16 C17 H17 120.2 . . ? C12 C17 H17 120.2 . . ? C23 C18 C19 120.20(16) . . ? C23 C18 P1 120.65(14) . . ? C19 C18 P1 119.06(13) . . ? C20 C19 C18 119.44(17) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.21(18) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.50(17) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.24(18) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 119.37(17) . . ? C22 C23 H23 120.3 . . ? C18 C23 H23 120.3 . . ? C29 C24 C25 119.72(16) . . ? C29 C24 P1 121.97(13) . . ? C25 C24 P1 118.31(13) . . ? C26 C25 C24 120.07(17) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 119.90(17) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.31(17) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.45(17) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 119.53(16) . . ? C28 C29 H29 120.2 . . ? C24 C29 H29 120.2 . . ? C30 P2 C36 111.11(8) . . ? C30 P2 C42 108.18(8) . . ? C36 P2 C42 110.92(8) . . ? C30 P2 C48 107.93(8) . . ? C36 P2 C48 108.19(8) . . ? C42 P2 C48 110.47(8) . . ? C31 C30 C35 120.40(18) . . ? C31 C30 P2 120.30(15) . . ? C35 C30 P2 119.27(16) . . ? C32 C31 C30 119.4(2) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C33 C32 C31 119.9(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 120.6(2) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C30 119.0(2) . . ? C34 C35 H35 120.5 . . ? C30 C35 H35 120.5 . . ? C41 C36 C37 119.85(17) . . ? C41 C36 P2 119.15(14) . . ? C37 C36 P2 120.62(13) . . ? C38 C37 C36 119.85(17) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C39 C38 C37 119.78(19) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 120.63(18) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 120.39(18) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C36 119.43(18) . . ? C40 C41 H41 120.3 . . ? C36 C41 H41 120.3 . . ? C43 C42 C47 119.75(16) . . ? C43 C42 P2 120.02(13) . . ? C47 C42 P2 119.92(13) . . ? C44 C43 C42 119.79(17) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.31(18) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C46 C45 C44 120.25(17) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 120.15(17) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 C42 119.74(17) . . ? C46 C47 H47 120.1 . . ? C42 C47 H47 120.1 . . ? C53 C48 C49 120.02(16) . . ? C53 C48 P2 121.15(13) . . ? C49 C48 P2 118.76(13) . . ? C50 C49 C48 119.69(16) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 120.16(17) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C52 C51 C50 120.11(17) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 120.54(17) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C52 C53 C48 119.44(16) . . ? C52 C53 H53 120.3 . . ? C48 C53 H53 120.3 . . ? H1 O3 H2 102(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.441 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.048 _vrf_PLAT230_12yuj30new ; PROBLEM: Hirshfeld Test Diff for O1 -- C4 .. 6.2 su Hirshfeld Test Diff for O2 -- C5 .. 6.3 su RESPONSE: The Hirshfeld-test alerts were caused by the anomalies of the C-atom mean-square displacement amplitude values on Co-C=O and Co-C=N. According to the study by Braga and Koetzle (Acta Cryst. 1988, B44, 151-155), such anomalies 'may be considered to reflect the deviation of the electron density distribution around the C-atom nuclei from the ideal spherical atom model, arising from the bonding interaction established by the CO (and also CN in our cases) molecule in these systems'. ; _vrf_PLAT232_12yuj30new ; PROBLEM: Hirshfeld Test Diff (M-X) Co1 -- C1 .. 8.3 su Hirshfeld Test Diff (M-X) Co1 -- C2 .. 9.3 su Hirshfeld Test Diff (M-X) Co1 -- C3 .. 8.0 su Hirshfeld Test Diff (M-X) Co1 -- C4 .. 9.8 su Hirshfeld Test Diff (M-X) Co1 -- C5 .. 10.2 su RESPONSE: The Hirshfeld-test alerts were caused by the anomalies of the C-atom mean-square displacement amplitude values on Co-C=O and Co-C=N. According to the study by Braga and Koetzle (Acta Cryst. 1988, B44, 151-155), such anomalies 'may be considered to reflect the deviation of the electron density distribution around the C-atom nuclei from the ideal spherical atom model, arising from the bonding interaction established by the CO (and also CN in our cases) molecule in these systems'. ; _vrf_PLAT860_12yuj30new ; PROBLEM: Note: Number of Least-Squares Restraints ....... 2 RESPONSE: Two distance restraints (DFIX) were applied to two O-H distances on the water molecule. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 927722'