# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Leigh Jones' _publ_contact_author_email leigh.jones@nuigalway.ie _publ_author_name L.Jones data_pk2a-3 _database_code_depnum_ccdc_archive 'CCDC 843603' #TrackingRef '- (1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co7(OH)6(L)6)(NO3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 Co7 N8 O24' _chemical_formula_weight 1623.66 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 Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 14.110(2) _cell_length_b 14.110(2) _cell_length_c 22.770(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3926.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1654 _exptl_absorpt_coefficient_mu 1.511 _cell_measurement_theta_max 25.33 _cell_measurement_theta_min 3.0209 _cell_measurement_reflns_used 3440 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.78955 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) 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 9071 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.0209 _diffrn_reflns_theta_max 25.33 _diffrn_orient_matrix_UB_11 -0.0331254991 _diffrn_orient_matrix_UB_12 -0.0175410019 _diffrn_orient_matrix_UB_13 -0.0256281654 _diffrn_orient_matrix_UB_21 -0.0337550607 _diffrn_orient_matrix_UB_22 0.0192699568 _diffrn_orient_matrix_UB_23 0.0120226927 _diffrn_orient_matrix_UB_31 0.0338461552 _diffrn_orient_matrix_UB_32 0.0519512887 _diffrn_orient_matrix_UB_33 -0.0131052487 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 68.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 0.0000 30.0000 117 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 123(2) _reflns_number_total 2353 _reflns_number_gt 1767 _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^)+(0.1604P)^2^+11.2858P] 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 2353 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2796 _refine_ls_wR_factor_gt 0.2671 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _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 0.0000 1.0000 0.5000 0.0274(7) Uani 1 6 d S . . Co2 Co 0.14493(9) 0.89020(9) 0.51236(5) 0.0302(5) Uani 1 1 d . . . N1 N 0.1940(6) 0.8169(6) 0.5762(4) 0.0402(19) Uani 1 1 d . . . N2 N 0.6667 1.3333 0.7952(7) 0.052(4) Uani 1 3 d S . . O1 O 0.0037(4) 0.8724(4) 0.5457(2) 0.0311(13) Uani 1 1 d . . . H1 H -0.0091 0.8649 0.5891 0.037 Uiso 1 1 calc R . . O2 O 0.3996(4) 1.2395(5) 0.5532(3) 0.0371(15) Uani 1 1 d . . . O3 O 0.2757(5) 1.0322(4) 0.5344(3) 0.0313(13) Uani 1 1 d . . . O4 O 0.6546(8) 1.2395(8) 0.7912(5) 0.098(3) Uani 1 1 d . . . C1 C 0.1263(9) 0.6942(7) 0.5806(6) 0.060(3) Uani 1 1 d . . . H1A H 0.1524 0.6688 0.6136 0.090 Uiso 1 1 calc R . . H1B H 0.1328 0.6612 0.5441 0.090 Uiso 1 1 calc R . . H1C H 0.0494 0.6728 0.5871 0.090 Uiso 1 1 calc R . . C2 C 0.2728(8) 0.8627(7) 0.6127(4) 0.040(2) Uani 1 1 d . . . H2 H 0.2853 0.8169 0.6383 0.048 Uiso 1 1 calc R . . C3 C 0.3458(7) 0.9821(7) 0.6179(4) 0.0345(19) Uani 1 1 d . . . C4 C 0.4182(8) 1.0179(8) 0.6655(4) 0.045(2) Uani 1 1 d . . . H4 H 0.4208 0.9657 0.6908 0.054 Uiso 1 1 calc R . . C5 C 0.4865(8) 1.1290(8) 0.6763(4) 0.046(2) Uani 1 1 d . . . H5 H 0.5351 1.1528 0.7089 0.055 Uiso 1 1 calc R . . C6 C 0.4825(7) 1.2048(7) 0.6388(4) 0.038(2) Uani 1 1 d . . . H6 H 0.5289 1.2809 0.6457 0.045 Uiso 1 1 calc R . . C7 C 0.4116(7) 1.1699(7) 0.5920(4) 0.034(2) Uani 1 1 d . . . C8 C 0.3417(6) 1.0587(7) 0.5799(3) 0.0279(17) Uani 1 1 d . . . C9 C 0.4909(7) 1.3454(7) 0.5435(5) 0.047(2) Uani 1 1 d . . . H9A H 0.5089 1.3879 0.5799 0.070 Uiso 1 1 calc R . . H9B H 0.4730 1.3826 0.5128 0.070 Uiso 1 1 calc R . . H9C H 0.5539 1.3388 0.5310 0.070 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 0.0233(8) 0.0233(8) 0.0354(15) 0.000 0.000 0.0117(4) Co2 0.0278(7) 0.0234(6) 0.0391(8) -0.0038(5) -0.0080(5) 0.0126(5) N1 0.038(4) 0.032(4) 0.052(5) 0.002(4) -0.014(4) 0.018(3) N2 0.048(5) 0.048(5) 0.060(10) 0.000 0.000 0.024(3) O1 0.032(3) 0.026(3) 0.035(3) 0.003(2) -0.001(2) 0.015(2) O2 0.026(3) 0.025(3) 0.054(4) 0.007(3) -0.001(3) 0.008(2) O3 0.028(3) 0.022(3) 0.041(3) 0.006(2) -0.003(3) 0.011(2) O4 0.089(7) 0.076(6) 0.126(8) -0.008(6) -0.043(7) 0.039(6) C1 0.062(7) 0.026(5) 0.086(8) 0.003(5) -0.030(6) 0.017(5) C2 0.050(6) 0.035(5) 0.037(5) 0.004(4) -0.009(4) 0.022(4) C3 0.031(4) 0.031(4) 0.036(5) 0.000(4) -0.003(4) 0.011(4) C4 0.042(5) 0.043(5) 0.036(5) 0.010(4) -0.006(4) 0.010(5) C5 0.036(5) 0.053(6) 0.040(5) -0.005(5) -0.010(4) 0.017(5) C6 0.030(4) 0.031(5) 0.041(5) -0.002(4) 0.001(4) 0.007(4) C7 0.029(4) 0.036(5) 0.038(5) -0.005(4) 0.001(4) 0.016(4) C8 0.023(4) 0.028(4) 0.031(4) -0.002(3) 0.001(3) 0.011(3) C9 0.025(4) 0.030(5) 0.080(7) 0.006(5) 0.010(5) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.103(5) 8_456 ? Co1 O1 2.103(5) 2_675 ? Co1 O1 2.103(5) . ? Co1 O1 2.103(5) 7_576 ? Co1 O1 2.103(5) 9_666 ? Co1 O1 2.103(5) 3_465 ? Co2 O3 1.993(6) . ? Co2 O1 2.027(6) . ? Co2 O3 2.055(5) 8_456 ? Co2 N1 2.092(7) . ? Co2 O1 2.158(6) 9_666 ? Co2 O2 2.336(6) 8_456 ? N1 C2 1.276(11) . ? N1 C1 1.505(11) . ? N2 O4 1.252(11) . ? N2 O4 1.252(11) 2_775 ? N2 O4 1.252(11) 3_575 ? O1 Co2 2.158(6) 8_456 ? O1 H1 1.0000 . ? O2 C7 1.392(11) . ? O2 C9 1.420(10) . ? O2 Co2 2.336(6) 9_666 ? O3 C8 1.316(10) . ? O3 Co2 2.055(5) 9_666 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.476(12) . ? C2 H2 0.9500 . ? C3 C4 1.398(13) . ? C3 C8 1.409(12) . ? C4 C5 1.391(13) . ? C4 H4 0.9500 . ? C5 C6 1.391(13) . ? C5 H5 0.9500 . ? C6 C7 1.375(12) . ? C6 H6 0.9500 . ? C7 C8 1.401(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 O1 180.000(1) 8_456 2_675 ? O1 Co1 O1 82.4(2) 8_456 . ? O1 Co1 O1 97.6(2) 2_675 . ? O1 Co1 O1 97.6(2) 8_456 7_576 ? O1 Co1 O1 82.4(2) 2_675 7_576 ? O1 Co1 O1 180.0(3) . 7_576 ? O1 Co1 O1 97.6(2) 8_456 9_666 ? O1 Co1 O1 82.4(2) 2_675 9_666 ? O1 Co1 O1 82.4(2) . 9_666 ? O1 Co1 O1 97.6(2) 7_576 9_666 ? O1 Co1 O1 82.4(2) 8_456 3_465 ? O1 Co1 O1 97.6(2) 2_675 3_465 ? O1 Co1 O1 97.6(2) . 3_465 ? O1 Co1 O1 82.4(2) 7_576 3_465 ? O1 Co1 O1 180.000(1) 9_666 3_465 ? O3 Co2 O1 112.9(2) . . ? O3 Co2 O3 162.92(13) . 8_456 ? O1 Co2 O3 79.5(2) . 8_456 ? O3 Co2 N1 87.3(3) . . ? O1 Co2 N1 103.1(3) . . ? O3 Co2 N1 101.6(3) 8_456 . ? O3 Co2 O1 77.9(2) . 9_666 ? O1 Co2 O1 82.8(3) . 9_666 ? O3 Co2 O1 92.8(2) 8_456 9_666 ? N1 Co2 O1 165.2(3) . 9_666 ? O3 Co2 O2 94.8(2) . 8_456 ? O1 Co2 O2 151.3(2) . 8_456 ? O3 Co2 O2 71.8(2) 8_456 8_456 ? N1 Co2 O2 85.0(3) . 8_456 ? O1 Co2 O2 96.4(2) 9_666 8_456 ? C2 N1 C1 115.5(8) . . ? C2 N1 Co2 128.5(6) . . ? C1 N1 Co2 116.0(6) . . ? O4 N2 O4 119.5(2) . 2_775 ? O4 N2 O4 119.5(2) . 3_575 ? O4 N2 O4 119.5(2) 2_775 3_575 ? Co2 O1 Co1 98.8(2) . . ? Co2 O1 Co2 98.6(2) . 8_456 ? Co1 O1 Co2 94.8(2) . 8_456 ? Co2 O1 H1 119.8 . . ? Co1 O1 H1 119.8 . . ? Co2 O1 H1 119.8 8_456 . ? C7 O2 C9 118.3(7) . . ? C7 O2 Co2 112.5(5) . 9_666 ? C9 O2 Co2 125.2(6) . 9_666 ? C8 O3 Co2 130.7(5) . . ? C8 O3 Co2 122.9(5) . 9_666 ? Co2 O3 Co2 103.2(2) . 9_666 ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 124.4(8) . . ? N1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? C4 C3 C8 120.1(8) . . ? C4 C3 C2 116.2(8) . . ? C8 C3 C2 123.6(8) . . ? C5 C4 C3 120.9(9) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.1(9) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C7 C6 C5 120.2(8) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 O2 124.3(8) . . ? C6 C7 C8 122.1(8) . . ? O2 C7 C8 113.6(7) . . ? O3 C8 C7 118.3(7) . . ? O3 C8 C3 124.1(7) . . ? C7 C8 C3 117.6(8) . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.000 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.182 # Attachment '- (2).cif' data_cmd16a-1 _database_code_depnum_ccdc_archive 'CCDC 843604' #TrackingRef '- (2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co7(OH)6(immp)6)(NO3)2.2MeOH _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H66 Co7 N8 O26' _chemical_formula_weight 1679.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 14.041(2) _cell_length_b 14.041(2) _cell_length_c 23.036(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3933.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1710 _exptl_absorpt_coefficient_mu 1.513 _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _exptl_absorpt_correction_T_min 0.83791 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) 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 9408 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.0312 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0095301862 _diffrn_orient_matrix_UB_12 0.0047780313 _diffrn_orient_matrix_UB_13 -0.0298618478 _diffrn_orient_matrix_UB_21 -0.0526693321 _diffrn_orient_matrix_UB_22 -0.0076332840 _diffrn_orient_matrix_UB_23 0.0069115542 _diffrn_orient_matrix_UB_31 0.0233686354 _diffrn_orient_matrix_UB_32 0.0577261323 _diffrn_orient_matrix_UB_33 0.0033892523 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 4.00 49.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - -17.3903 77.0000 0.0000 45 #__ type_ start__ end____ width___ exp.time_ 2 omega 5.00 82.00 1.0000 120.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 77.0000 -120.0000 77 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2362 _reflns_number_gt 2188 _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^)+(0.1283P)^2^+19.4239P] 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 2362 _refine_ls_number_parameters 153 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2221 _refine_ls_wR_factor_gt 0.2179 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _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 0.0000 0.0000 0.5000 0.0171(4) Uani 1 6 d S . . Co2 Co 0.10763(6) -0.14748(6) 0.48820(3) 0.0209(3) Uani 1 1 d . . . O1 O -0.0056(3) -0.1330(3) 0.54599(16) 0.0208(8) Uani 1 1 d . . . H1 H 0.0068 -0.1281 0.5889 0.025 Uiso 1 1 calc R . . O2 O -0.2443(3) -0.4006(3) 0.4467(2) 0.0293(10) Uani 1 1 d . . . O3 O -0.0354(3) -0.2780(3) 0.46572(17) 0.0229(8) Uani 1 1 d . . . O4 O -0.2358(5) -0.6473(5) 0.2056(3) 0.0587(16) Uani 1 1 d . . . O5 O 0.097(2) 0.0000 0.7500 0.068(7) Uiso 0.33 2 d SPD . . O6 O 0.3496(17) 0.3496(17) 0.7500 0.047(5) Uiso 0.33 2 d SPD . . N2 N -0.3333 -0.6667 0.2049(4) 0.039(2) Uani 1 3 d S . . N7 N 0.1820(4) -0.1956(4) 0.4248(2) 0.0289(11) Uani 1 1 d . . . C1 C 0.3025(6) -0.1319(7) 0.4216(4) 0.048(2) Uani 1 1 d . . . H1A H 0.3281 -0.1616 0.3906 0.072 Uiso 1 1 calc R . . H1B H 0.3337 -0.1369 0.4588 0.072 Uiso 1 1 calc R . . H1C H 0.3262 -0.0548 0.4133 0.072 Uiso 1 1 calc R . . C2 C 0.1333(5) -0.2731(5) 0.3877(3) 0.0293(13) Uani 1 1 d . . . H2 H 0.1786 -0.2853 0.3616 0.035 Uiso 1 1 calc R . . C3 C 0.0143(5) -0.3446(5) 0.3816(2) 0.0240(12) Uani 1 1 d . . . C4 C -0.0617(5) -0.3422(4) 0.4196(2) 0.0211(11) Uani 1 1 d . . . C5 C -0.1750(5) -0.4119(5) 0.4075(3) 0.0247(12) Uani 1 1 d . . . C6 C -0.2104(5) -0.4801(5) 0.3600(3) 0.0301(13) Uani 1 1 d . . . H6 H -0.2868 -0.5252 0.3525 0.036 Uiso 1 1 calc R . . C7 C -0.1336(6) -0.4827(5) 0.3230(3) 0.0340(14) Uani 1 1 d . . . H7 H -0.1577 -0.5302 0.2903 0.041 Uiso 1 1 calc R . . C8 C -0.0237(5) -0.4175(5) 0.3335(3) 0.0311(14) Uani 1 1 d . . . H8 H 0.0280 -0.4209 0.3082 0.037 Uiso 1 1 calc R . . C9 C -0.3506(5) -0.4938(5) 0.4564(3) 0.0381(16) Uani 1 1 d . . . H9A H -0.3968 -0.5064 0.4221 0.057 Uiso 1 1 calc R . . H9B H -0.3845 -0.4803 0.4902 0.057 Uiso 1 1 calc R . . H9C H -0.3434 -0.5588 0.4635 0.057 Uiso 1 1 calc R . . C10 C 0.192(2) 0.0000 0.7500 0.043(7) Uiso 0.33 2 d SPD . . C11 C 0.358(3) 0.266(3) 0.7295(15) 0.028(7) Uiso 0.17 1 d PD . . 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 0.0154(6) 0.0154(6) 0.0205(9) 0.000 0.000 0.0077(3) Co2 0.0172(5) 0.0191(5) 0.0275(5) -0.0058(3) -0.0035(3) 0.0098(4) O1 0.023(2) 0.0190(19) 0.0219(17) -0.0022(14) -0.0006(15) 0.0117(16) O2 0.017(2) 0.019(2) 0.044(2) -0.0073(17) 0.0038(18) 0.0034(17) O3 0.0189(19) 0.0190(19) 0.0283(19) -0.0064(16) 0.0018(15) 0.0076(16) O4 0.047(3) 0.068(4) 0.064(3) -0.023(3) -0.003(3) 0.030(3) N2 0.047(4) 0.047(4) 0.022(5) 0.000 0.000 0.0237(19) N7 0.020(3) 0.028(3) 0.039(3) -0.011(2) 0.002(2) 0.012(2) C1 0.021(3) 0.055(5) 0.066(5) -0.025(4) 0.000(3) 0.017(3) C2 0.029(3) 0.032(3) 0.030(3) -0.005(2) 0.003(2) 0.018(3) C3 0.028(3) 0.021(3) 0.024(3) 0.000(2) 0.001(2) 0.012(2) C4 0.020(3) 0.013(2) 0.027(3) 0.000(2) 0.000(2) 0.006(2) C5 0.022(3) 0.017(3) 0.035(3) 0.002(2) -0.002(2) 0.010(2) C6 0.025(3) 0.022(3) 0.034(3) -0.004(2) -0.006(2) 0.006(2) C7 0.040(4) 0.028(3) 0.028(3) -0.006(2) -0.002(3) 0.012(3) C8 0.036(3) 0.027(3) 0.024(3) -0.003(2) 0.006(2) 0.011(3) C9 0.024(3) 0.022(3) 0.063(4) 0.001(3) 0.006(3) 0.007(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 2.114(4) 8_556 ? Co1 O1 2.114(4) 9_556 ? Co1 O1 2.114(4) . ? Co1 O1 2.114(4) 7_556 ? Co1 O1 2.114(4) 2 ? Co1 O1 2.114(4) 3 ? Co2 O3 1.995(4) . ? Co2 O1 2.028(4) 9_556 ? Co2 O3 2.053(4) 9_556 ? Co2 N7 2.094(5) . ? Co2 O1 2.159(4) . ? Co2 O2 2.344(4) 9_556 ? O1 Co2 2.028(4) 8_556 ? O1 H1 1.0000 . ? O2 C5 1.393(7) . ? O2 C9 1.428(7) . ? O2 Co2 2.344(4) 8_556 ? O3 C4 1.321(7) . ? O3 Co2 2.053(4) 8_556 ? O4 N2 1.257(6) . ? O5 C10 1.34(4) . ? O6 C11 1.33(4) . ? O6 C11 1.33(4) 6_556 ? N2 O4 1.257(6) 3_545 ? N2 O4 1.257(6) 2_445 ? N7 C2 1.280(8) . ? N7 C1 1.468(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.463(8) . ? C2 H2 0.9500 . ? C3 C4 1.393(8) . ? C3 C8 1.419(8) . ? C4 C5 1.417(8) . ? C5 C6 1.374(9) . ? C6 C7 1.388(9) . ? C6 H6 0.9500 . ? C7 C8 1.366(9) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 O1 97.09(13) 8_556 9_556 ? O1 Co1 O1 82.91(13) 8_556 . ? O1 Co1 O1 82.91(13) 9_556 . ? O1 Co1 O1 97.09(13) 8_556 7_556 ? O1 Co1 O1 97.09(13) 9_556 7_556 ? O1 Co1 O1 180.00(17) . 7_556 ? O1 Co1 O1 180.0 8_556 2 ? O1 Co1 O1 82.91(13) 9_556 2 ? O1 Co1 O1 97.09(13) . 2 ? O1 Co1 O1 82.91(13) 7_556 2 ? O1 Co1 O1 82.91(13) 8_556 3 ? O1 Co1 O1 180.000(1) 9_556 3 ? O1 Co1 O1 97.09(13) . 3 ? O1 Co1 O1 82.91(13) 7_556 3 ? O1 Co1 O1 97.09(13) 2 3 ? O3 Co2 O1 112.49(16) . 9_556 ? O3 Co2 O3 163.37(9) . 9_556 ? O1 Co2 O3 80.03(15) 9_556 9_556 ? O3 Co2 N7 87.56(18) . . ? O1 Co2 N7 101.57(19) 9_556 . ? O3 Co2 N7 100.95(18) 9_556 . ? O3 Co2 O1 78.26(15) . . ? O1 Co2 O1 83.8(2) 9_556 . ? O3 Co2 O1 92.87(15) 9_556 . ? N7 Co2 O1 165.81(18) . . ? O3 Co2 O2 94.86(16) . 9_556 ? O1 Co2 O2 151.85(15) 9_556 9_556 ? O3 Co2 O2 71.85(15) 9_556 9_556 ? N7 Co2 O2 85.55(19) . 9_556 ? O1 Co2 O2 95.84(15) . 9_556 ? Co2 O1 Co1 97.98(15) 8_556 . ? Co2 O1 Co2 98.01(14) 8_556 . ? Co1 O1 Co2 94.04(15) . . ? Co2 O1 H1 120.4 8_556 . ? Co1 O1 H1 120.4 . . ? Co2 O1 H1 120.4 . . ? C5 O2 C9 117.8(5) . . ? C5 O2 Co2 112.3(3) . 8_556 ? C9 O2 Co2 125.7(4) . 8_556 ? C4 O3 Co2 130.2(4) . . ? C4 O3 Co2 123.2(4) . 8_556 ? Co2 O3 Co2 102.72(17) . 8_556 ? C11 O6 C11 133(4) . 6_556 ? O4 N2 O4 119.98(3) . 3_545 ? O4 N2 O4 119.98(3) . 2_445 ? O4 N2 O4 119.98(3) 3_545 2_445 ? C2 N7 C1 116.6(5) . . ? C2 N7 Co2 126.8(4) . . ? C1 N7 Co2 116.6(4) . . ? N7 C1 H1A 109.5 . . ? N7 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N7 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N7 C2 C3 126.0(5) . . ? N7 C2 H2 117.0 . . ? C3 C2 H2 117.0 . . ? C4 C3 C8 119.4(6) . . ? C4 C3 C2 123.3(5) . . ? C8 C3 C2 117.3(5) . . ? O3 C4 C3 124.4(5) . . ? O3 C4 C5 117.6(5) . . ? C3 C4 C5 118.0(5) . . ? C6 C5 O2 124.5(5) . . ? C6 C5 C4 121.8(6) . . ? O2 C5 C4 113.7(5) . . ? C5 C6 C7 119.5(6) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 120.3(6) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C3 120.9(6) . . ? C7 C8 H8 119.5 . . ? C3 C8 H8 119.5 . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 4.265 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.184 # Attachment '- (3).cif' data_sm673 _database_code_depnum_ccdc_archive 'CCDC 843605' #TrackingRef '- (3).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2-ImPh-6-MePhenol _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 N O2' _chemical_formula_weight 227.25 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.0471(6) _cell_length_b 9.0763(12) _cell_length_c 20.933(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1148.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.088 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9134 _cell_measurement_reflns_used 941 _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 0.58764 _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 3612 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.9134 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0157109000 _diffrn_orient_matrix_UB_12 0.0731850000 _diffrn_orient_matrix_UB_13 -0.0110137000 _diffrn_orient_matrix_UB_21 0.0244704000 _diffrn_orient_matrix_UB_22 -0.0230634000 _diffrn_orient_matrix_UB_23 -0.0315976000 _diffrn_orient_matrix_UB_31 -0.1135816000 _diffrn_orient_matrix_UB_32 -0.0150518000 _diffrn_orient_matrix_UB_33 -0.0052969000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -63.00 -30.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -18.4841 112.0000 -115.0000 33 #__ type_ start__ end____ width___ exp.time_ 2 omega -64.00 -31.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -18.4841 -37.0000 -60.0000 33 #__ type_ start__ end____ width___ exp.time_ 3 omega -6.00 84.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 18.7966 37.0000 -90.0000 90 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 2000 _reflns_number_gt 1347 _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^)+(0.0806P)^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 5(3) _refine_ls_number_reflns 2000 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 N1 N 0.1487(6) -0.1178(4) 0.19262(18) 0.0274(10) Uani 1 1 d . . . O1A O -0.0074(5) 0.0323(4) 0.09578(15) 0.0293(9) Uani 1 1 d . . . H1A H 0.0673 0.0194 0.1291 0.035 Uiso 1 1 calc R . . O2A O -0.3302(5) 0.0702(4) 0.01321(15) 0.0285(8) Uani 1 1 d . . . C1 C -0.5257(4) 0.1093(4) -0.0226(2) 0.0368(13) Uani 1 1 d . . . H1B H -0.5408 0.0432 -0.0594 0.055 Uiso 1 1 calc R . . H1C H -0.5128 0.2112 -0.0376 0.055 Uiso 1 1 calc R . . H1D H -0.6562 0.1000 0.0049 0.055 Uiso 1 1 calc R . . C2 C -0.1624(4) -0.0761(3) 0.09073(12) 0.0237(11) Uani 1 1 d R . . C3 C -0.3333(4) -0.0577(3) 0.04608(12) 0.0227(10) Uani 1 1 d R . . C4 C -0.4910(4) -0.1670(3) 0.03933(12) 0.0258(11) Uani 1 1 d R . . H4 H -0.6070 -0.1551 0.0092 0.031 Uiso 1 1 calc R . . C5 C -0.4811(7) -0.2938(6) 0.0762(2) 0.0299(12) Uani 1 1 d . . . H5 H -0.5888 -0.3688 0.0703 0.036 Uiso 1 1 calc R . . C6 C -0.3182(7) -0.3126(5) 0.1209(2) 0.0264(11) Uani 1 1 d . . . H6 H -0.3151 -0.3990 0.1465 0.032 Uiso 1 1 calc R . . C7 C -0.1537(7) -0.2018(5) 0.1289(2) 0.0236(11) Uani 1 1 d . . . C8 C 0.0052(7) -0.2195(5) 0.1799(2) 0.0268(11) Uani 1 1 d . . . H8 H 0.0042 -0.3073 0.2046 0.032 Uiso 1 1 calc R . . C9 C 0.2913(6) -0.1343(5) 0.2459(2) 0.0241(11) Uani 1 1 d . . . C10 C 0.2355(7) -0.2106(5) 0.3008(2) 0.0265(11) Uani 1 1 d . . . H10 H 0.0941 -0.2555 0.3042 0.032 Uiso 1 1 calc R . . C11 C 0.3845(7) -0.2221(6) 0.3512(2) 0.0294(12) Uani 1 1 d . . . H11 H 0.3433 -0.2723 0.3892 0.035 Uiso 1 1 calc R . . C12 C 0.5929(7) -0.1603(6) 0.3459(3) 0.0352(14) Uani 1 1 d . . . H12 H 0.6985 -0.1722 0.3791 0.042 Uiso 1 1 calc R . . C13 C 0.6452(7) -0.0808(6) 0.2914(2) 0.0329(13) Uani 1 1 d . . . H13 H 0.7862 -0.0351 0.2886 0.039 Uiso 1 1 calc R . . C14 C 0.5009(7) -0.0658(5) 0.2416(2) 0.0292(11) Uani 1 1 d . . . H14 H 0.5405 -0.0104 0.2048 0.035 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 N1 0.0190(18) 0.034(2) 0.030(2) 0.001(2) 0.0007(19) 0.0025(19) O1A 0.0189(15) 0.034(2) 0.035(2) 0.0048(17) -0.0082(17) -0.0065(15) O2A 0.0181(15) 0.0286(19) 0.039(2) 0.0052(17) -0.0044(15) -0.0007(15) C1 0.023(2) 0.040(3) 0.047(3) 0.010(3) -0.012(3) 0.001(2) C2 0.018(2) 0.023(3) 0.030(3) -0.007(2) 0.003(2) -0.004(2) C3 0.020(2) 0.020(3) 0.028(3) -0.002(2) 0.003(2) 0.003(2) C4 0.017(2) 0.028(3) 0.033(3) -0.001(2) 0.000(2) 0.000(2) C5 0.022(2) 0.026(3) 0.043(3) -0.002(2) -0.003(2) -0.006(2) C6 0.025(2) 0.025(3) 0.029(3) 0.000(2) 0.003(2) 0.000(2) C7 0.017(2) 0.023(3) 0.031(3) 0.001(2) -0.001(2) 0.002(2) C8 0.023(2) 0.026(3) 0.032(3) 0.003(2) -0.001(2) 0.001(2) C9 0.015(2) 0.029(3) 0.029(3) 0.000(2) 0.000(2) 0.004(2) C10 0.016(2) 0.024(3) 0.040(3) 0.002(3) -0.002(2) -0.001(2) C11 0.030(2) 0.030(3) 0.027(3) 0.003(2) 0.001(2) 0.002(2) C12 0.022(2) 0.042(3) 0.042(3) -0.008(3) -0.010(2) 0.003(2) C13 0.017(2) 0.039(3) 0.042(3) -0.004(3) -0.002(3) -0.004(2) C14 0.0195(19) 0.030(3) 0.038(3) 0.000(2) 0.007(3) -0.004(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 N1 C8 1.295(5) . ? N1 C9 1.418(6) . ? O1A C2 1.363(4) . ? O1A H1A 0.8400 . ? O2A C3 1.349(4) . ? O2A C1 1.444(4) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 C7 1.393(5) . ? C2 C3 1.4034 . ? C3 C4 1.3833 . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.370(6) . ? C5 H5 0.9500 . ? C6 C7 1.425(6) . ? C6 H6 0.9500 . ? C7 C8 1.446(6) . ? C8 H8 0.9500 . ? C9 C10 1.384(6) . ? C9 C14 1.415(6) . ? C10 C11 1.392(6) . ? C10 H10 0.9500 . ? C11 C12 1.383(6) . ? C11 H11 0.9500 . ? C12 C13 1.387(7) . ? C12 H12 0.9500 . ? C13 C14 1.367(6) . ? C13 H13 0.9500 . ? C14 H14 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 C8 N1 C9 119.6(4) . . ? C2 O1A H1A 109.5 . . ? C3 O2A C1 117.7(3) . . ? O2A C1 H1B 109.5 . . ? O2A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2A C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1A C2 C7 121.3(3) . . ? O1A C2 C3 118.16(18) . . ? C7 C2 C3 120.5(2) . . ? O2A C3 C4 125.07(16) . . ? O2A C3 C2 115.59(17) . . ? C4 C3 C2 119.3 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 121.0(4) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 119.0(4) . . ? C2 C7 C8 122.7(4) . . ? C6 C7 C8 118.2(4) . . ? N1 C8 C7 121.2(4) . . ? N1 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C14 119.4(4) . . ? C10 C9 N1 124.0(4) . . ? C14 C9 N1 116.6(4) . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 119.0(5) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 122.3(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C9 118.7(4) . . ? C13 C14 H14 120.7 . . ? C9 C14 H14 120.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.255 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.071 # Attachment '- (4).cif' data_sm74a-5 _database_code_depnum_ccdc_archive 'CCDC 843606' #TrackingRef '- (4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co7(OH)6(immp-Ph)6)(NO3)2.3MeCN _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H87 Co7 N12 O27' _chemical_formula_weight 2181.23 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.2767(15) _cell_length_b 12.9879(5) _cell_length_c 24.4043(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.797(5) _cell_angle_gamma 90.00 _cell_volume 9268.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 1.306 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.7684 _cell_measurement_reflns_used 5670 _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 0.86435 _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 20749 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.7684 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0227771000 _diffrn_orient_matrix_UB_12 -0.0182805000 _diffrn_orient_matrix_UB_13 -0.0035997000 _diffrn_orient_matrix_UB_21 -0.0047011000 _diffrn_orient_matrix_UB_22 0.0179670000 _diffrn_orient_matrix_UB_23 0.0265877000 _diffrn_orient_matrix_UB_31 -0.0068856000 _diffrn_orient_matrix_UB_32 0.0482125000 _diffrn_orient_matrix_UB_33 -0.0112849000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 63.00 95.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.6403 179.0000 -120.0000 32 #__ type_ start__ end____ width___ exp.time_ 2 omega -50.00 75.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.6403 0.0000 -120.0000 125 #__ type_ start__ end____ width___ exp.time_ 3 omega 28.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.6403 77.0000 -150.0000 61 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 8489 _reflns_number_gt 5388 _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^)+(0.0486P)^2^+24.4175P] 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 8489 _refine_ls_number_parameters 617 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.053 _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 0.2500 0.2500 0.0000 0.0159(3) Uani 1 2 d S . . Co2 Co 0.23950(3) 0.14004(6) 0.11039(3) 0.0184(2) Uani 1 1 d . . . Co3 Co 0.15227(3) 0.19304(6) 0.02978(3) 0.0195(2) Uani 1 1 d . . . Co4 Co 0.17000(3) 0.39204(6) -0.04356(3) 0.0190(2) Uani 1 1 d . . . O1 O 0.21500(14) 0.1335(3) 0.01855(16) 0.0199(10) Uani 1 1 d . . . H1 H 0.2179 0.0680 -0.0025 0.024 Uiso 1 1 calc R . . O2 O 0.28085(13) 0.2335(3) 0.06999(16) 0.0162(9) Uani 1 1 d . . . H2 H 0.2937 0.2959 0.0892 0.019 Uiso 1 1 calc R . . O3 O 0.20036(14) 0.3306(3) 0.02532(16) 0.0189(10) Uani 1 1 d . . . H3H H 0.2056 0.3752 0.0584 0.023 Uiso 1 1 calc R . . O4 O 0.17518(14) 0.1856(3) 0.10930(16) 0.0205(10) Uani 1 1 d . . . O5 O 0.09139(15) 0.2324(3) 0.08507(17) 0.0282(11) Uani 1 1 d . . . O6 O 0.28717(14) 0.0349(3) 0.09041(16) 0.0193(10) Uani 1 1 d . . . O7 O 0.21902(15) -0.0131(3) 0.14808(17) 0.0239(11) Uani 1 1 d . . . O8 O 0.12549(14) 0.2735(3) -0.03348(17) 0.0227(10) Uani 1 1 d . . . O9 O 0.11192(15) 0.4031(3) -0.11138(17) 0.0264(11) Uani 1 1 d . . . O10 O 0.22285(19) 0.4415(4) 0.1209(2) 0.0477(15) Uani 1 1 d . . . O11 O 0.29278(18) 0.4429(3) 0.0955(2) 0.0396(13) Uani 1 1 d . . . O12 O 0.27811(18) 0.4772(4) 0.17919(19) 0.0392(14) Uani 1 1 d . . . O13 O 0.0000 0.5595(8) 0.2500 0.176(8) Uani 1 2 d S . . O14 O 0.0080(2) 0.4229(5) 0.2933(2) 0.0615(18) Uani 1 1 d . . . N1 N 0.35730(19) -0.0345(4) 0.0223(2) 0.0225(13) Uani 1 1 d . . . N2 N 0.25065(18) 0.1911(4) 0.1896(2) 0.0215(12) Uani 1 1 d . . . N3 N 0.11211(19) 0.0689(4) 0.0045(2) 0.0241(13) Uani 1 1 d . . . N4 N 0.2644(2) 0.4546(4) 0.1324(2) 0.0314(15) Uani 1 1 d . . . N5 N 0.0000 0.4702(8) 0.2500 0.046(3) Uani 1 2 d S . . N6 N 0.0673(3) -0.1750(9) -0.1145(5) 0.106(4) Uani 1 1 d . . . C1 C 0.0442(2) 0.2445(6) 0.0704(3) 0.040(2) Uani 1 1 d . . . H1A H 0.0262 0.1991 0.0932 0.060 Uiso 1 1 calc R . . H1B H 0.0385 0.2265 0.0317 0.060 Uiso 1 1 calc R . . H1C H 0.0352 0.3162 0.0763 0.060 Uiso 1 1 calc R . . C2 C 0.1051(2) 0.2502(5) 0.1386(3) 0.0244(15) Uani 1 1 d . . . C3 C 0.0780(3) 0.2880(5) 0.1779(3) 0.0314(17) Uani 1 1 d . . . H3 H 0.0465 0.3014 0.1696 0.038 Uiso 1 1 calc R . . C4 C 0.0975(3) 0.3066(5) 0.2308(3) 0.0367(19) Uani 1 1 d . . . H4 H 0.0789 0.3326 0.2586 0.044 Uiso 1 1 calc R . . C5 C 0.1430(3) 0.2876(5) 0.2428(3) 0.0343(18) Uani 1 1 d . . . H5 H 0.1557 0.3024 0.2785 0.041 Uiso 1 1 calc R . . C6 C 0.1710(2) 0.2463(5) 0.2028(3) 0.0244(16) Uani 1 1 d . . . C7 C 0.1513(2) 0.2260(5) 0.1493(2) 0.0237(16) Uani 1 1 d . . . C8 C 0.2190(2) 0.2285(5) 0.2187(3) 0.0267(16) Uani 1 1 d . . . H8 H 0.2281 0.2468 0.2553 0.032 Uiso 1 1 calc R . . C9 C 0.2943(2) 0.1804(5) 0.2192(2) 0.0225(15) Uani 1 1 d . . . C10 C 0.3009(2) 0.1000(5) 0.2564(3) 0.0294(17) Uani 1 1 d . . . H10 H 0.2775 0.0501 0.2605 0.035 Uiso 1 1 calc R . . C11 C 0.3410(3) 0.0933(6) 0.2869(3) 0.0356(19) Uani 1 1 d . . . H11 H 0.3452 0.0393 0.3129 0.043 Uiso 1 1 calc R . . C12 C 0.3761(2) 0.1641(6) 0.2806(3) 0.0329(18) Uani 1 1 d . . . H12 H 0.4040 0.1590 0.3018 0.039 Uiso 1 1 calc R . . C13 C 0.3689(2) 0.2429(5) 0.2423(3) 0.0316(17) Uani 1 1 d . . . H13 H 0.3923 0.2923 0.2376 0.038 Uiso 1 1 calc R . . C14 C 0.3287(2) 0.2505(5) 0.2114(3) 0.0274(16) Uani 1 1 d . . . H14 H 0.3246 0.3036 0.1848 0.033 Uiso 1 1 calc R . . C15 C 0.1046(3) 0.4808(5) -0.1536(3) 0.0309(18) Uani 1 1 d . . . H15A H 0.1069 0.4491 -0.1898 0.046 Uiso 1 1 calc R . . H15B H 0.1279 0.5348 -0.1487 0.046 Uiso 1 1 calc R . . H15C H 0.0742 0.5112 -0.1508 0.046 Uiso 1 1 calc R . . C16 C 0.0839(2) 0.3186(5) -0.1141(3) 0.0226(15) Uani 1 1 d . . . C17 C 0.0936(2) 0.2486(5) -0.0715(2) 0.0205(15) Uani 1 1 d . . . C18 C 0.0694(2) 0.1546(5) -0.0716(3) 0.0254(16) Uani 1 1 d . . . C19 C 0.0354(3) 0.1356(6) -0.1130(3) 0.0362(19) Uani 1 1 d . . . H19 H 0.0190 0.0725 -0.1134 0.043 Uiso 1 1 calc R . . C20 C 0.0259(2) 0.2076(6) -0.1527(3) 0.0340(18) Uani 1 1 d . . . H20 H 0.0025 0.1943 -0.1802 0.041 Uiso 1 1 calc R . . C21 C 0.0501(2) 0.3008(5) -0.1537(3) 0.0262(16) Uani 1 1 d . . . H21 H 0.0431 0.3507 -0.1813 0.031 Uiso 1 1 calc R . . C22 C 0.0805(2) 0.0713(5) -0.0345(3) 0.0292(17) Uani 1 1 d . . . H22 H 0.0624 0.0108 -0.0392 0.035 Uiso 1 1 calc R . . C23 C 0.1177(3) -0.0299(5) 0.0321(3) 0.0268(17) Uani 1 1 d . . . C24 C 0.0845(3) -0.0654(6) 0.0647(3) 0.043(2) Uani 1 1 d . . . H24 H 0.0581 -0.0253 0.0708 0.052 Uiso 1 1 calc R . . C25 C 0.0906(3) -0.1639(6) 0.0892(4) 0.058(3) Uani 1 1 d . . . H25 H 0.0679 -0.1903 0.1119 0.070 Uiso 1 1 calc R . . C26 C 0.1283(3) -0.2207(5) 0.0805(3) 0.041(2) Uani 1 1 d . . . H26 H 0.1317 -0.2870 0.0966 0.049 Uiso 1 1 calc R . . C27 C 0.1615(3) -0.1833(5) 0.0486(3) 0.0315(18) Uani 1 1 d . . . H27 H 0.1881 -0.2232 0.0431 0.038 Uiso 1 1 calc R . . C28 C 0.1566(3) -0.0864(5) 0.0241(3) 0.0306(18) Uani 1 1 d . . . H28 H 0.1798 -0.0599 0.0021 0.037 Uiso 1 1 calc R . . C29 C 0.1818(2) -0.0342(5) 0.1835(3) 0.0316(17) Uani 1 1 d . . . H29A H 0.1613 -0.0855 0.1661 0.047 Uiso 1 1 calc R . . H29B H 0.1648 0.0295 0.1895 0.047 Uiso 1 1 calc R . . H29C H 0.1942 -0.0607 0.2188 0.047 Uiso 1 1 calc R . . C30 C 0.2458(2) -0.0945(5) 0.1336(3) 0.0221(15) Uani 1 1 d . . . C31 C 0.2816(2) -0.0648(4) 0.1012(2) 0.0209(16) Uani 1 1 d . . . C32 C 0.3105(2) -0.1410(5) 0.0806(3) 0.0248(16) Uani 1 1 d . . . C33 C 0.3021(3) -0.2450(5) 0.0960(3) 0.0307(18) Uani 1 1 d . . . H33 H 0.3217 -0.2977 0.0837 0.037 Uiso 1 1 calc R . . C34 C 0.2670(3) -0.2713(5) 0.1276(3) 0.0323(18) Uani 1 1 d . . . H34 H 0.2620 -0.3415 0.1365 0.039 Uiso 1 1 calc R . . C35 C 0.2382(2) -0.1959(4) 0.1472(3) 0.0247(16) Uani 1 1 d . . . H35 H 0.2138 -0.2140 0.1695 0.030 Uiso 1 1 calc R . . C36 C 0.3469(2) -0.1204(5) 0.0444(3) 0.0268(16) Uani 1 1 d . . . H36 H 0.3656 -0.1776 0.0359 0.032 Uiso 1 1 calc R . . C37 C 0.3946(2) -0.0376(4) -0.0138(3) 0.0205(15) Uani 1 1 d . . . C38 C 0.3888(2) 0.0036(5) -0.0663(3) 0.0255(16) Uani 1 1 d . . . H38 H 0.3613 0.0386 -0.0768 0.031 Uiso 1 1 calc R . . C39 C 0.4226(2) -0.0057(5) -0.1030(3) 0.0250(16) Uani 1 1 d . . . H39 H 0.4178 0.0208 -0.1391 0.030 Uiso 1 1 calc R . . C40 C 0.4635(3) -0.0533(5) -0.0880(3) 0.0376(19) Uani 1 1 d . . . H40 H 0.4870 -0.0589 -0.1134 0.045 Uiso 1 1 calc R . . C41 C 0.4701(3) -0.0929(6) -0.0353(3) 0.045(2) Uani 1 1 d . . . H41 H 0.4981 -0.1256 -0.0247 0.054 Uiso 1 1 calc R . . C42 C 0.4359(3) -0.0850(5) 0.0018(3) 0.0363(19) Uani 1 1 d . . . H42 H 0.4407 -0.1118 0.0379 0.044 Uiso 1 1 calc R . . C43 C 0.1169(3) -0.0525(7) -0.1712(4) 0.074(3) Uani 1 1 d . . . H43A H 0.1274 -0.0905 -0.2030 0.111 Uiso 1 1 calc R . . H43B H 0.1434 -0.0278 -0.1489 0.111 Uiso 1 1 calc R . . H43C H 0.0983 0.0063 -0.1839 0.111 Uiso 1 1 calc R . . C44 C 0.0895(4) -0.1207(9) -0.1382(5) 0.072(3) Uani 1 1 d . . . N7 N 0.0000 0.1509(12) 0.2500 0.117(5) Uiso 1 2 d SD . . C51 C 0.0175(7) 0.0842(13) 0.2285(9) 0.093(8) Uiso 0.50 1 d PD . . C52 C 0.0420(6) 0.0007(12) 0.2076(7) 0.067(6) Uiso 0.50 1 d PD . . H52A H 0.0738 0.0036 0.2221 0.100 Uiso 0.50 1 calc PR . . H52B H 0.0412 0.0046 0.1675 0.100 Uiso 0.50 1 calc PR . . H52C H 0.0281 -0.0641 0.2188 0.100 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0230(7) 0.0080(6) 0.0167(6) 0.0004(5) 0.0004(5) 0.0007(5) Co2 0.0252(5) 0.0124(4) 0.0180(4) 0.0015(3) 0.0044(4) 0.0027(4) Co3 0.0235(5) 0.0146(4) 0.0206(5) 0.0021(4) 0.0019(4) 0.0014(4) Co4 0.0263(5) 0.0112(4) 0.0194(5) 0.0010(3) 0.0020(4) 0.0025(4) O1 0.033(3) 0.0072(19) 0.020(2) 0.0003(17) 0.003(2) -0.007(2) O2 0.017(2) 0.011(2) 0.020(2) 0.0001(17) 0.0004(19) 0.0036(19) O3 0.023(3) 0.012(2) 0.023(2) -0.0009(18) 0.005(2) 0.0010(19) O4 0.026(3) 0.021(2) 0.014(2) 0.0008(18) 0.0032(19) 0.002(2) O5 0.025(3) 0.036(3) 0.023(3) 0.002(2) 0.000(2) 0.010(2) O6 0.024(3) 0.011(2) 0.024(2) 0.0031(18) 0.008(2) 0.009(2) O7 0.032(3) 0.012(2) 0.029(3) 0.0035(19) 0.010(2) 0.000(2) O8 0.024(3) 0.021(2) 0.023(2) 0.0007(19) -0.003(2) -0.001(2) O9 0.034(3) 0.022(2) 0.023(2) 0.008(2) -0.002(2) 0.004(2) O10 0.040(4) 0.051(3) 0.052(4) -0.026(3) -0.003(3) 0.005(3) O11 0.054(4) 0.028(3) 0.038(3) -0.013(2) 0.014(3) -0.013(3) O12 0.058(4) 0.034(3) 0.025(3) -0.006(2) -0.008(3) 0.007(3) O13 0.302(19) 0.035(6) 0.171(13) 0.000 -0.180(14) 0.000 O14 0.054(4) 0.079(4) 0.052(4) 0.018(3) 0.001(3) -0.024(4) N1 0.032(4) 0.014(3) 0.021(3) -0.001(2) 0.001(3) 0.005(3) N2 0.029(3) 0.016(3) 0.020(3) 0.002(2) 0.007(3) 0.001(3) N3 0.031(4) 0.021(3) 0.020(3) 0.001(2) 0.004(3) -0.003(3) N4 0.043(4) 0.015(3) 0.036(4) -0.007(3) 0.004(3) 0.009(3) N5 0.041(6) 0.036(6) 0.060(7) 0.000 -0.019(5) 0.000 N6 0.072(8) 0.124(10) 0.124(10) -0.017(8) 0.011(7) -0.019(7) C1 0.037(5) 0.041(5) 0.041(5) -0.010(4) -0.008(4) 0.006(4) C2 0.026(4) 0.017(3) 0.031(4) 0.004(3) 0.007(3) 0.004(3) C3 0.035(5) 0.027(4) 0.033(4) 0.009(3) 0.007(3) 0.009(4) C4 0.041(5) 0.039(4) 0.031(4) -0.003(3) 0.015(4) 0.010(4) C5 0.044(5) 0.032(4) 0.026(4) -0.002(3) 0.002(4) 0.005(4) C6 0.029(4) 0.021(3) 0.023(4) -0.001(3) 0.000(3) 0.002(3) C7 0.041(4) 0.015(3) 0.017(3) 0.003(3) 0.012(3) 0.000(3) C8 0.035(4) 0.025(4) 0.020(4) 0.000(3) 0.000(3) 0.004(3) C9 0.028(4) 0.023(3) 0.017(3) -0.007(3) 0.000(3) 0.003(3) C10 0.031(4) 0.028(4) 0.029(4) 0.004(3) 0.001(3) -0.001(3) C11 0.043(5) 0.034(4) 0.029(4) 0.009(3) -0.004(4) 0.003(4) C12 0.029(4) 0.045(5) 0.024(4) -0.007(3) 0.000(3) 0.006(4) C13 0.024(4) 0.027(4) 0.044(5) -0.009(3) 0.005(4) -0.006(3) C14 0.034(4) 0.022(4) 0.026(4) -0.001(3) 0.003(3) 0.004(3) C15 0.045(5) 0.026(4) 0.022(4) 0.007(3) 0.003(3) -0.001(4) C16 0.017(4) 0.025(4) 0.025(4) -0.001(3) 0.000(3) 0.003(3) C17 0.024(4) 0.022(3) 0.016(3) -0.001(3) 0.005(3) 0.005(3) C18 0.023(4) 0.025(4) 0.028(4) -0.001(3) -0.002(3) -0.004(3) C19 0.038(5) 0.030(4) 0.040(4) -0.004(4) -0.003(4) -0.009(4) C20 0.024(4) 0.044(5) 0.033(4) -0.002(4) -0.005(3) -0.001(4) C21 0.023(4) 0.031(4) 0.025(4) 0.003(3) 0.006(3) 0.005(3) C22 0.037(5) 0.017(3) 0.034(4) -0.005(3) 0.006(4) -0.005(3) C23 0.039(5) 0.012(3) 0.029(4) 0.002(3) -0.008(3) -0.004(3) C24 0.051(6) 0.031(4) 0.049(5) 0.008(4) 0.017(4) -0.001(4) C25 0.080(7) 0.034(5) 0.063(6) 0.020(4) 0.019(5) -0.011(5) C26 0.072(6) 0.014(4) 0.036(4) 0.004(3) -0.005(4) -0.004(4) C27 0.043(5) 0.017(3) 0.034(4) -0.005(3) 0.001(4) -0.003(4) C28 0.039(5) 0.020(4) 0.031(4) 0.003(3) -0.007(4) -0.006(4) C29 0.036(5) 0.027(4) 0.033(4) 0.003(3) 0.016(4) 0.003(4) C30 0.033(4) 0.014(3) 0.019(3) 0.000(3) 0.005(3) 0.005(3) C31 0.042(5) 0.013(3) 0.008(3) 0.005(2) -0.004(3) -0.002(3) C32 0.043(5) 0.012(3) 0.020(3) -0.001(3) 0.000(3) 0.007(3) C33 0.042(5) 0.014(3) 0.037(4) -0.002(3) 0.001(4) 0.006(3) C34 0.053(5) 0.009(3) 0.035(4) 0.005(3) -0.001(4) 0.000(3) C35 0.036(4) 0.015(3) 0.023(4) 0.004(3) 0.004(3) -0.001(3) C36 0.034(4) 0.019(3) 0.028(4) -0.006(3) -0.001(3) 0.012(3) C37 0.021(4) 0.008(3) 0.032(4) -0.001(3) -0.001(3) 0.001(3) C38 0.029(4) 0.015(3) 0.032(4) -0.001(3) 0.002(3) 0.000(3) C39 0.035(4) 0.018(3) 0.022(4) -0.002(3) 0.006(3) 0.003(3) C40 0.037(5) 0.028(4) 0.050(5) -0.010(4) 0.020(4) 0.000(4) C41 0.033(5) 0.047(5) 0.055(5) 0.002(4) 0.012(4) 0.016(4) C42 0.039(5) 0.034(4) 0.036(4) 0.006(3) 0.000(4) 0.015(4) C43 0.066(7) 0.062(6) 0.094(8) -0.023(6) 0.000(6) -0.011(6) C44 0.049(7) 0.072(8) 0.094(9) -0.038(7) -0.004(6) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.895(4) 7 ? Co1 O1 1.895(4) . ? Co1 O2 1.905(4) . ? Co1 O2 1.905(4) 7 ? Co1 O3 1.917(4) 7 ? Co1 O3 1.917(4) . ? Co2 O4 1.973(4) . ? Co2 O2 2.007(4) . ? Co2 O6 2.029(4) . ? Co2 N2 2.055(5) . ? Co2 O7 2.284(4) . ? Co2 O1 2.321(4) . ? Co3 O8 1.993(4) . ? Co3 O1 2.023(4) . ? Co3 O4 2.024(4) . ? Co3 N3 2.072(5) . ? Co3 O3 2.280(4) . ? Co3 O5 2.344(5) . ? Co4 O6 1.980(4) 7 ? Co4 O3 2.027(4) . ? Co4 O8 2.040(4) . ? Co4 N1 2.090(5) 7 ? Co4 O2 2.289(4) 7 ? Co4 O9 2.319(4) . ? O1 H1 1.0000 . ? O2 Co4 2.289(4) 7 ? O2 H2 1.0000 . ? O3 H3H 1.0000 . ? O4 C7 1.337(7) . ? O5 C2 1.369(7) . ? O5 C1 1.419(7) . ? O6 C31 1.333(7) . ? O6 Co4 1.980(4) 7 ? O7 C30 1.372(7) . ? O7 C29 1.448(8) . ? O8 C17 1.324(7) . ? O9 C16 1.369(7) . ? O9 C15 1.452(7) . ? O10 N4 1.245(7) . ? O11 N4 1.264(7) . ? O12 N4 1.228(7) . ? O13 N5 1.160(12) . ? O14 N5 1.234(7) . ? N1 C36 1.283(8) . ? N1 C37 1.437(8) . ? N1 Co4 2.090(5) 7 ? N2 C8 1.290(8) . ? N2 C9 1.445(8) . ? N3 C22 1.296(8) . ? N3 C23 1.454(8) . ? N5 O14 1.234(7) 2 ? N6 C44 1.135(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.365(9) . ? C2 C7 1.399(9) . ? C3 C4 1.408(9) . ? C3 H3 0.9500 . ? C4 C5 1.372(10) . ? C4 H4 0.9500 . ? C5 C6 1.413(9) . ? C5 H5 0.9500 . ? C6 C7 1.425(8) . ? C6 C8 1.458(9) . ? C8 H8 0.9500 . ? C9 C14 1.377(9) . ? C9 C10 1.391(9) . ? C10 C11 1.363(9) . ? C10 H10 0.9500 . ? C11 C12 1.391(9) . ? C11 H11 0.9500 . ? C12 C13 1.395(9) . ? C12 H12 0.9500 . ? C13 C14 1.369(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.368(8) . ? C16 C17 1.401(8) . ? C17 C18 1.410(8) . ? C18 C19 1.407(9) . ? C18 C22 1.437(9) . ? C19 C20 1.365(9) . ? C19 H19 0.9500 . ? C20 C21 1.404(9) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.364(10) . ? C23 C28 1.378(9) . ? C24 C25 1.420(10) . ? C24 H24 0.9500 . ? C25 C26 1.355(11) . ? C25 H25 0.9500 . ? C26 C27 1.364(10) . ? C26 H26 0.9500 . ? C27 C28 1.398(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C35 1.378(8) . ? C30 C31 1.400(9) . ? C31 C32 1.410(9) . ? C32 C33 1.427(8) . ? C32 C36 1.442(9) . ? C33 C34 1.359(10) . ? C33 H33 0.9500 . ? C34 C35 1.390(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.390(9) . ? C37 C42 1.395(9) . ? C38 C39 1.372(9) . ? C38 H38 0.9500 . ? C39 C40 1.381(9) . ? C39 H39 0.9500 . ? C40 C41 1.388(10) . ? C40 H40 0.9500 . ? C41 C42 1.386(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.464(14) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N7 C51 1.147(9) . ? N7 C51 1.147(9) 2 ? C51 C52 1.410(9) . ? C51 C51 1.50(4) 2 ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 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 O1 180.0(3) 7 . ? O1 Co1 O2 93.76(16) 7 . ? O1 Co1 O2 86.24(16) . . ? O1 Co1 O2 86.24(16) 7 7 ? O1 Co1 O2 93.76(16) . 7 ? O2 Co1 O2 180.0(3) . 7 ? O1 Co1 O3 86.08(17) 7 7 ? O1 Co1 O3 93.92(17) . 7 ? O2 Co1 O3 83.92(16) . 7 ? O2 Co1 O3 96.08(16) 7 7 ? O1 Co1 O3 93.92(17) 7 . ? O1 Co1 O3 86.08(17) . . ? O2 Co1 O3 96.08(16) . . ? O2 Co1 O3 83.92(16) 7 . ? O3 Co1 O3 180.0(3) 7 . ? O4 Co2 O2 114.20(16) . . ? O4 Co2 O6 150.01(17) . . ? O2 Co2 O6 81.41(16) . . ? O4 Co2 N2 91.35(19) . . ? O2 Co2 N2 101.26(18) . . ? O6 Co2 N2 111.32(19) . . ? O4 Co2 O7 89.86(16) . . ? O2 Co2 O7 154.33(16) . . ? O6 Co2 O7 73.02(16) . . ? N2 Co2 O7 86.25(18) . . ? O4 Co2 O1 75.41(16) . . ? O2 Co2 O1 73.33(14) . . ? O6 Co2 O1 85.83(15) . . ? N2 Co2 O1 161.39(17) . . ? O7 Co2 O1 106.39(14) . . ? O8 Co3 O1 114.89(17) . . ? O8 Co3 O4 150.09(17) . . ? O1 Co3 O4 81.45(16) . . ? O8 Co3 N3 88.94(18) . . ? O1 Co3 N3 99.66(19) . . ? O4 Co3 N3 113.90(19) . . ? O8 Co3 O3 76.86(15) . . ? O1 Co3 O3 74.12(15) . . ? O4 Co3 O3 84.64(16) . . ? N3 Co3 O3 159.75(18) . . ? O8 Co3 O5 92.86(17) . . ? O1 Co3 O5 151.89(15) . . ? O4 Co3 O5 71.59(16) . . ? N3 Co3 O5 84.54(19) . . ? O3 Co3 O5 110.19(15) . . ? O6 Co4 O3 113.79(17) 7 . ? O6 Co4 O8 149.07(17) 7 . ? O3 Co4 O8 81.93(16) . . ? O6 Co4 N1 88.85(19) 7 7 ? O3 Co4 N1 107.48(18) . 7 ? O8 Co4 N1 112.5(2) . 7 ? O6 Co4 O2 75.77(15) 7 7 ? O3 Co4 O2 72.34(15) . 7 ? O8 Co4 O2 84.86(16) . 7 ? N1 Co4 O2 162.53(19) 7 7 ? O6 Co4 O9 91.22(16) 7 . ? O3 Co4 O9 153.25(16) . . ? O8 Co4 O9 71.46(15) . . ? N1 Co4 O9 81.17(18) 7 . ? O2 Co4 O9 106.98(15) 7 . ? Co1 O1 Co3 103.43(17) . . ? Co1 O1 Co2 93.22(15) . . ? Co3 O1 Co2 95.45(17) . . ? Co1 O1 H1 119.8 . . ? Co3 O1 H1 119.8 . . ? Co2 O1 H1 119.8 . . ? Co1 O2 Co2 103.74(18) . . ? Co1 O2 Co4 95.99(16) . 7 ? Co2 O2 Co4 96.30(15) . 7 ? Co1 O2 H2 118.8 . . ? Co2 O2 H2 118.8 . . ? Co4 O2 H2 118.8 7 . ? Co1 O3 Co4 104.85(19) . . ? Co1 O3 Co3 93.86(15) . . ? Co4 O3 Co3 95.82(16) . . ? Co1 O3 H3H 119.1 . . ? Co4 O3 H3H 119.1 . . ? Co3 O3 H3H 119.1 . . ? C7 O4 Co2 129.9(4) . . ? C7 O4 Co3 121.4(4) . . ? Co2 O4 Co3 107.37(19) . . ? C2 O5 C1 117.3(5) . . ? C2 O5 Co3 113.0(4) . . ? C1 O5 Co3 129.6(4) . . ? C31 O6 Co4 131.7(4) . 7 ? C31 O6 Co2 121.0(4) . . ? Co4 O6 Co2 106.19(17) 7 . ? C30 O7 C29 117.6(5) . . ? C30 O7 Co2 113.8(4) . . ? C29 O7 Co2 128.6(4) . . ? C17 O8 Co3 130.7(4) . . ? C17 O8 Co4 122.2(4) . . ? Co3 O8 Co4 105.05(18) . . ? C16 O9 C15 117.1(5) . . ? C16 O9 Co4 113.7(3) . . ? C15 O9 Co4 128.8(4) . . ? C36 N1 C37 115.8(5) . . ? C36 N1 Co4 124.4(5) . 7 ? C37 N1 Co4 119.3(4) . 7 ? C8 N2 C9 113.7(5) . . ? C8 N2 Co2 123.7(5) . . ? C9 N2 Co2 122.4(4) . . ? C22 N3 C23 114.9(6) . . ? C22 N3 Co3 125.1(5) . . ? C23 N3 Co3 120.0(4) . . ? O12 N4 O10 120.9(7) . . ? O12 N4 O11 119.6(6) . . ? O10 N4 O11 119.5(6) . . ? O13 N5 O14 119.9(5) . . ? O13 N5 O14 119.9(5) . 2 ? O14 N5 O14 120.3(10) . 2 ? O5 C1 H1A 109.5 . . ? O5 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O5 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O5 125.2(6) . . ? C3 C2 C7 122.7(6) . . ? O5 C2 C7 112.1(6) . . ? C2 C3 C4 118.8(7) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.7(7) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.8(6) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C7 118.6(6) . . ? C5 C6 C8 117.4(6) . . ? C7 C6 C8 123.9(6) . . ? O4 C7 C2 119.2(6) . . ? O4 C7 C6 122.5(6) . . ? C2 C7 C6 118.3(6) . . ? N2 C8 C6 128.4(6) . . ? N2 C8 H8 115.8 . . ? C6 C8 H8 115.8 . . ? C14 C9 C10 120.6(6) . . ? C14 C9 N2 120.2(6) . . ? C10 C9 N2 119.2(6) . . ? C11 C10 C9 119.4(7) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 121.3(7) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C13 118.1(7) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C14 C13 C12 121.2(7) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C9 119.3(7) . . ? C13 C14 H14 120.3 . . ? C9 C14 H14 120.3 . . ? O9 C15 H15A 109.5 . . ? O9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 O9 125.5(6) . . ? C21 C16 C17 121.8(6) . . ? O9 C16 C17 112.6(5) . . ? O8 C17 C16 118.1(6) . . ? O8 C17 C18 123.3(6) . . ? C16 C17 C18 118.6(6) . . ? C19 C18 C17 119.3(6) . . ? C19 C18 C22 116.7(6) . . ? C17 C18 C22 123.6(6) . . ? C20 C19 C18 120.2(7) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 118.9(6) . . ? C16 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? N3 C22 C18 127.7(6) . . ? N3 C22 H22 116.2 . . ? C18 C22 H22 116.2 . . ? C24 C23 C28 121.2(6) . . ? C24 C23 N3 120.1(7) . . ? C28 C23 N3 118.6(7) . . ? C23 C24 C25 118.3(8) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C26 C25 C24 120.7(8) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.4(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 120.2(7) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 119.2(7) . . ? C23 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? O7 C29 H29A 109.5 . . ? O7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 C30 C35 125.1(6) . . ? O7 C30 C31 112.7(5) . . ? C35 C30 C31 122.2(6) . . ? O6 C31 C30 118.7(6) . . ? O6 C31 C32 122.1(6) . . ? C30 C31 C32 119.2(6) . . ? C31 C32 C33 117.2(6) . . ? C31 C32 C36 124.2(6) . . ? C33 C32 C36 118.7(6) . . ? C34 C33 C32 122.2(6) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C33 C34 C35 120.4(6) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C30 C35 C34 118.9(7) . . ? C30 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? N1 C36 C32 128.0(6) . . ? N1 C36 H36 116.0 . . ? C32 C36 H36 116.0 . . ? C38 C37 C42 119.1(7) . . ? C38 C37 N1 119.5(6) . . ? C42 C37 N1 121.3(6) . . ? C39 C38 C37 120.6(6) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 120.6(6) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 119.3(7) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C42 C41 C40 120.5(7) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C37 119.8(7) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C44 C43 177.2(13) . . ? C51 N7 C51 82(3) . 2 ? N7 C51 C52 173(2) . . ? N7 C51 C51 49.1(13) . 2 ? C52 C51 C51 129.0(13) . 2 ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 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 1.090 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.122 # Attachment '- (5).cif' data_sm259d-8 _database_code_depnum_ccdc_archive 'CCDC 854829' #TrackingRef '- (5).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co(L)2) _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' 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 11.6622(8) _cell_length_b 23.9507(13) _cell_length_c 9.2521(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.596(7) _cell_angle_gamma 90.00 _cell_volume 2434.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.9 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.742 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9750 _cell_measurement_reflns_used 3975 _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 0.74030 _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 11316 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.9750 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 0.0182323000 _diffrn_orient_matrix_UB_12 -0.0251364000 _diffrn_orient_matrix_UB_13 -0.0265469000 _diffrn_orient_matrix_UB_21 0.0618730000 _diffrn_orient_matrix_UB_22 0.0068350000 _diffrn_orient_matrix_UB_23 0.0390778000 _diffrn_orient_matrix_UB_31 -0.0025561000 _diffrn_orient_matrix_UB_32 -0.0140990000 _diffrn_orient_matrix_UB_33 0.0662677000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -3.00 67.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 18.7966 37.0000 -60.0000 70 #__ type_ start__ end____ width___ exp.time_ 2 omega -43.00 81.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 18.7966 0.0000 -120.0000 124 #__ type_ start__ end____ width___ exp.time_ 3 omega 64.00 94.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 18.7966 179.0000 -120.0000 30 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 296.9 _reflns_number_total 4448 _reflns_number_gt 3291 _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^)+(0.0414P)^2^+1.1298P] 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 4448 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.26893(4) 0.05619(2) 0.46896(5) 0.03976(17) Uani 1 1 d . . . O1 O 0.3651(3) 0.18768(11) 0.8310(3) 0.0630(8) Uani 1 1 d . . . O2 O 0.3215(2) 0.11660(10) 0.6091(3) 0.0465(6) Uani 1 1 d . . . O3 O 0.2598(3) -0.11122(11) 0.6781(3) 0.0578(7) Uani 1 1 d . . . O4 O 0.2520(2) -0.01722(10) 0.5365(3) 0.0436(6) Uani 1 1 d . . . N1 N 0.3977(3) 0.06718(11) 0.3766(3) 0.0381(7) Uani 1 1 d . . . N2 N 0.1073(3) 0.05934(12) 0.3025(3) 0.0389(7) Uani 1 1 d . . . C1 C 0.3826(5) 0.2280(2) 0.9484(5) 0.0842(16) Uani 1 1 d . . . H1A H 0.4544 0.2181 1.0360 0.126 Uiso 1 1 calc R . . H1B H 0.3108 0.2289 0.9809 0.126 Uiso 1 1 calc R . . H1C H 0.3946 0.2648 0.9095 0.126 Uiso 1 1 calc R . . C2 C 0.4573(4) 0.17996(15) 0.7724(4) 0.0447(9) Uani 1 1 d . . . C3 C 0.5684(4) 0.20555(15) 0.8223(4) 0.0556(11) Uani 1 1 d . . . H3 H 0.5868 0.2311 0.9054 0.067 Uiso 1 1 calc R . . C4 C 0.6550(4) 0.19461(17) 0.7528(5) 0.0594(11) Uani 1 1 d . . . H4 H 0.7331 0.2114 0.7916 0.071 Uiso 1 1 calc R . . C5 C 0.6280(3) 0.15988(16) 0.6295(5) 0.0519(10) Uani 1 1 d . . . H5 H 0.6864 0.1539 0.5801 0.062 Uiso 1 1 calc R . . C6 C 0.5138(3) 0.13246(14) 0.5738(4) 0.0401(8) Uani 1 1 d . . . C7 C 0.4271(3) 0.14071(14) 0.6476(4) 0.0366(8) Uani 1 1 d . . . C8 C 0.4919(3) 0.09882(14) 0.4379(4) 0.0402(8) Uani 1 1 d . . . H8 H 0.5517 0.0999 0.3890 0.048 Uiso 1 1 calc R . . C9 C 0.3814(3) 0.04220(14) 0.2305(4) 0.0385(8) Uani 1 1 d . . . C10 C 0.3902(3) 0.07303(17) 0.1097(4) 0.0516(10) Uani 1 1 d . . . H10 H 0.4124 0.1113 0.1234 0.062 Uiso 1 1 calc R . . C11 C 0.3666(4) 0.0480(2) -0.0324(4) 0.0626(12) Uani 1 1 d . . . H11 H 0.3721 0.0693 -0.1164 0.075 Uiso 1 1 calc R . . C12 C 0.3353(4) -0.0074(2) -0.0523(4) 0.0617(12) Uani 1 1 d . . . H12 H 0.3207 -0.0246 -0.1494 0.074 Uiso 1 1 calc R . . C13 C 0.3252(4) -0.03791(18) 0.0684(5) 0.0612(11) Uani 1 1 d . . . H13 H 0.3033 -0.0762 0.0548 0.073 Uiso 1 1 calc R . . C14 C 0.3468(3) -0.01310(15) 0.2092(4) 0.0478(9) Uani 1 1 d . . . H14 H 0.3379 -0.0341 0.2919 0.057 Uiso 1 1 calc R . . C15 C 0.2613(5) -0.15783(19) 0.7718(6) 0.0886(16) Uani 1 1 d . . . H15A H 0.1916 -0.1558 0.8083 0.133 Uiso 1 1 calc R . . H15B H 0.3369 -0.1579 0.8599 0.133 Uiso 1 1 calc R . . H15C H 0.2563 -0.1922 0.7124 0.133 Uiso 1 1 calc R . . C16 C 0.1534(3) -0.10024(15) 0.5587(4) 0.0432(9) Uani 1 1 d . . . C17 C 0.0556(4) -0.13538(16) 0.5102(5) 0.0562(11) Uani 1 1 d . . . H17 H 0.0596 -0.1708 0.5578 0.067 Uiso 1 1 calc R . . C18 C -0.0501(4) -0.12005(18) 0.3918(5) 0.0590(11) Uani 1 1 d . . . H18 H -0.1182 -0.1445 0.3597 0.071 Uiso 1 1 calc R . . C19 C -0.0538(3) -0.06986(16) 0.3237(4) 0.0519(10) Uani 1 1 d . . . H19 H -0.1260 -0.0593 0.2438 0.062 Uiso 1 1 calc R . . C20 C 0.0459(3) -0.03238(14) 0.3669(4) 0.0378(8) Uani 1 1 d . . . C21 C 0.1537(3) -0.04757(14) 0.4871(4) 0.0361(8) Uani 1 1 d . . . C22 C 0.0304(3) 0.01887(15) 0.2845(4) 0.0419(9) Uani 1 1 d . . . H22 H -0.0462 0.0240 0.2064 0.050 Uiso 1 1 calc R . . C23 C 0.0762(3) 0.10550(15) 0.1999(4) 0.0447(9) Uani 1 1 d . . . C24 C 0.0050(4) 0.09991(19) 0.0452(4) 0.0605(12) Uani 1 1 d . . . H24 H -0.0259 0.0643 0.0056 0.073 Uiso 1 1 calc R . . C25 C -0.0205(5) 0.1459(2) -0.0495(5) 0.0761(15) Uani 1 1 d . . . H25 H -0.0691 0.1418 -0.1543 0.091 Uiso 1 1 calc R . . C26 C 0.0235(5) 0.1975(2) 0.0057(6) 0.0821(16) Uani 1 1 d . . . H26 H 0.0043 0.2291 -0.0602 0.099 Uiso 1 1 calc R . . C27 C 0.0959(5) 0.20356(19) 0.1573(6) 0.0776(14) Uani 1 1 d . . . H27 H 0.1277 0.2392 0.1954 0.093 Uiso 1 1 calc R . . C28 C 0.1220(4) 0.15765(17) 0.2534(5) 0.0582(11) Uani 1 1 d . . . H28 H 0.1720 0.1620 0.3576 0.070 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 0.0428(3) 0.0402(3) 0.0337(3) -0.0027(2) 0.0094(2) -0.0101(2) O1 0.074(2) 0.0593(18) 0.0567(17) -0.0267(15) 0.0232(15) -0.0148(15) O2 0.0387(15) 0.0561(16) 0.0447(14) -0.0153(12) 0.0138(12) -0.0159(12) O3 0.0596(18) 0.0509(17) 0.0641(18) 0.0167(14) 0.0222(15) 0.0016(13) O4 0.0365(14) 0.0428(14) 0.0446(14) 0.0000(12) 0.0044(11) -0.0100(11) N1 0.0415(17) 0.0369(17) 0.0334(15) 0.0024(13) 0.0091(13) -0.0011(13) N2 0.0439(17) 0.0383(17) 0.0333(15) -0.0044(14) 0.0115(13) -0.0002(14) C1 0.093(4) 0.079(3) 0.074(3) -0.039(3) 0.020(3) -0.002(3) C2 0.052(2) 0.037(2) 0.038(2) -0.0005(17) 0.0063(17) -0.0013(17) C3 0.061(3) 0.038(2) 0.051(2) -0.0047(19) -0.005(2) -0.007(2) C4 0.040(2) 0.050(3) 0.075(3) -0.004(2) 0.002(2) -0.0107(19) C5 0.041(2) 0.046(2) 0.064(3) 0.001(2) 0.0106(19) -0.0059(18) C6 0.041(2) 0.0325(19) 0.0394(19) 0.0069(16) 0.0039(16) -0.0026(16) C7 0.039(2) 0.035(2) 0.0302(17) 0.0037(16) 0.0035(15) -0.0036(15) C8 0.037(2) 0.042(2) 0.041(2) 0.0086(17) 0.0121(16) 0.0029(16) C9 0.0369(19) 0.044(2) 0.0324(18) 0.0020(17) 0.0085(15) 0.0026(16) C10 0.055(2) 0.056(3) 0.043(2) 0.0081(19) 0.0146(18) -0.0052(19) C11 0.062(3) 0.088(4) 0.036(2) 0.008(2) 0.0146(19) -0.001(2) C12 0.050(3) 0.090(4) 0.038(2) -0.013(2) 0.0065(19) 0.008(2) C13 0.069(3) 0.055(3) 0.054(3) -0.009(2) 0.014(2) 0.003(2) C14 0.059(3) 0.044(2) 0.041(2) 0.0006(18) 0.0170(18) 0.0009(19) C15 0.102(4) 0.059(3) 0.106(4) 0.037(3) 0.036(3) 0.010(3) C16 0.049(2) 0.038(2) 0.050(2) -0.0041(18) 0.0250(19) 0.0002(17) C17 0.069(3) 0.041(2) 0.073(3) -0.008(2) 0.043(3) -0.014(2) C18 0.053(3) 0.054(3) 0.077(3) -0.022(2) 0.031(2) -0.022(2) C19 0.039(2) 0.060(3) 0.057(2) -0.021(2) 0.0165(19) -0.0127(19) C20 0.036(2) 0.041(2) 0.0377(19) -0.0118(17) 0.0142(16) -0.0053(16) C21 0.037(2) 0.038(2) 0.0378(18) -0.0085(16) 0.0184(15) -0.0037(16) C22 0.035(2) 0.053(2) 0.0338(19) -0.0111(18) 0.0063(15) 0.0029(17) C23 0.048(2) 0.047(2) 0.041(2) 0.0008(19) 0.0166(17) 0.0080(18) C24 0.076(3) 0.061(3) 0.039(2) 0.000(2) 0.013(2) 0.019(2) C25 0.098(4) 0.086(4) 0.042(2) 0.013(3) 0.021(2) 0.036(3) C26 0.110(5) 0.073(4) 0.069(3) 0.030(3) 0.037(3) 0.033(3) C27 0.098(4) 0.054(3) 0.082(3) 0.016(3) 0.033(3) 0.006(3) C28 0.068(3) 0.052(3) 0.051(2) 0.007(2) 0.016(2) 0.001(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 O4 1.898(2) . ? Co1 O2 1.902(2) . ? Co1 N1 1.978(3) . ? Co1 N2 1.996(3) . ? O1 C2 1.370(4) . ? O1 C1 1.416(4) . ? O2 C7 1.297(4) . ? O3 C16 1.382(4) . ? O3 C15 1.410(5) . ? O4 C21 1.303(4) . ? N1 C8 1.299(4) . ? N1 C9 1.432(4) . ? N2 C22 1.293(4) . ? N2 C23 1.423(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.366(5) . ? C2 C7 1.438(5) . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C5 1.361(5) . ? C4 H4 0.9500 . ? C5 C6 1.417(5) . ? C5 H5 0.9500 . ? C6 C7 1.412(5) . ? C6 C8 1.442(5) . ? C8 H8 0.9500 . ? C9 C10 1.372(5) . ? C9 C14 1.379(5) . ? C10 C11 1.386(5) . ? C10 H10 0.9500 . ? C11 C12 1.373(6) . ? C11 H11 0.9500 . ? C12 C13 1.372(6) . ? C12 H12 0.9500 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.367(5) . ? C16 C21 1.425(5) . ? C17 C18 1.396(6) . ? C17 H17 0.9500 . ? C18 C19 1.351(5) . ? C18 H18 0.9500 . ? C19 C20 1.416(5) . ? C19 H19 0.9500 . ? C20 C21 1.419(5) . ? C20 C22 1.424(5) . ? C22 H22 0.9500 . ? C23 C28 1.383(5) . ? C23 C24 1.399(5) . ? C24 C25 1.377(6) . ? C24 H24 0.9500 . ? C25 C26 1.370(7) . ? C25 H25 0.9500 . ? C26 C27 1.380(6) . ? C26 H26 0.9500 . ? C27 C28 1.383(5) . ? C27 H27 0.9500 . ? C28 H28 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 O4 Co1 O2 121.71(10) . . ? O4 Co1 N1 116.31(11) . . ? O2 Co1 N1 94.33(11) . . ? O4 Co1 N2 96.50(11) . . ? O2 Co1 N2 120.16(11) . . ? N1 Co1 N2 108.60(11) . . ? C2 O1 C1 117.7(3) . . ? C7 O2 Co1 125.8(2) . . ? C16 O3 C15 117.7(3) . . ? C21 O4 Co1 125.3(2) . . ? C8 N1 C9 118.7(3) . . ? C8 N1 Co1 122.9(2) . . ? C9 N1 Co1 118.2(2) . . ? C22 N2 C23 119.1(3) . . ? C22 N2 Co1 120.4(2) . . ? C23 N2 Co1 120.5(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 126.0(3) . . ? C3 C2 C7 120.9(4) . . ? O1 C2 C7 113.1(3) . . ? C2 C3 C4 120.8(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 C8 123.6(3) . . ? C5 C6 C8 116.5(3) . . ? O2 C7 C6 125.0(3) . . ? O2 C7 C2 117.8(3) . . ? C6 C7 C2 117.2(3) . . ? N1 C8 C6 125.7(3) . . ? N1 C8 H8 117.2 . . ? C6 C8 H8 117.2 . . ? C10 C9 C14 119.9(3) . . ? C10 C9 N1 121.5(3) . . ? C14 C9 N1 118.4(3) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.3(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 120.1(4) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 O3 124.9(4) . . ? C17 C16 C21 121.6(4) . . ? O3 C16 C21 113.5(3) . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 118.8(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 122.6(4) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C21 119.1(3) . . ? C19 C20 C22 116.8(3) . . ? C21 C20 C22 124.1(3) . . ? O4 C21 C20 125.2(3) . . ? O4 C21 C16 118.0(3) . . ? C20 C21 C16 116.9(3) . . ? N2 C22 C20 128.3(3) . . ? N2 C22 H22 115.9 . . ? C20 C22 H22 115.9 . . ? C28 C23 C24 118.6(4) . . ? C28 C23 N2 118.8(3) . . ? C24 C23 N2 122.6(3) . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 120.7(4) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.0(4) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 119.8(5) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 120.8(4) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.320 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.057 # Attachment '- Co2Na1(6).cif' data_sm127b-1 _database_code_depnum_ccdc_archive 'CCDC 854830' #TrackingRef '- Co2Na1(6).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co2Na1(immp-Br)6)(BF4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H54 B Br6 Co2 F4 N6 Na O12' _chemical_formula_weight 1686.15 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.774(5) _cell_length_b 15.542(3) _cell_length_c 15.416(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.61(3) _cell_angle_gamma 90.00 _cell_volume 5924(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 4.693 _cell_measurement_theta_max 25.35 _cell_measurement_theta_min 2.9307 _cell_measurement_reflns_used 7911 _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 0.43441 _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 14165 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.9307 _diffrn_reflns_theta_max 25.35 _diffrn_orient_matrix_UB_11 -0.0215959000 _diffrn_orient_matrix_UB_12 -0.0213929000 _diffrn_orient_matrix_UB_13 -0.0234051000 _diffrn_orient_matrix_UB_21 -0.0034037000 _diffrn_orient_matrix_UB_22 -0.0270543000 _diffrn_orient_matrix_UB_23 0.0363499000 _diffrn_orient_matrix_UB_31 -0.0185500000 _diffrn_orient_matrix_UB_32 0.0298506000 _diffrn_orient_matrix_UB_33 0.0161392000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 37.00 63.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 179.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega 41.00 84.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 179.0000 0.0000 43 #__ type_ start__ end____ width___ exp.time_ 3 omega -52.00 45.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 -37.0000 0.0000 97 #__ type_ start__ end____ width___ exp.time_ 4 omega -29.00 33.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 19.7341 -37.0000 90.0000 62 ; _diffrn_measurement_method '\w scans' _diffrn_ambient_temperature 150(2) _reflns_number_total 5423 _reflns_number_gt 4199 _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^)+(0.0345P)^2^+0.5809P] 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 5423 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.459067(16) 0.21196(3) 0.93876(3) 0.01353(11) Uani 1 1 d . . . Na1 Na 0.5000 0.29908(12) 0.7500 0.0206(4) Uani 1 2 d S . . Br1 Br 0.699450(13) 0.46503(2) 1.08799(2) 0.02483(10) Uani 1 1 d . . . Br2 Br 0.173740(13) 0.15845(2) 0.83812(3) 0.02607(10) Uani 1 1 d . . . Br3 Br 0.321410(15) -0.09845(2) 0.67015(3) 0.03224(11) Uani 1 1 d . . . B1 B 0.5000 0.5910(4) 0.7500 0.0301(15) Uani 1 2 d S . . N1 N 0.48794(10) 0.21811(16) 1.05808(18) 0.0161(6) Uani 1 1 d . . . N2 N 0.41192(10) 0.30768(16) 0.95952(18) 0.0163(6) Uani 1 1 d . . . N3 N 0.50015(10) 0.10981(17) 0.91125(18) 0.0159(6) Uani 1 1 d . . . O1 O 0.57481(8) 0.38163(14) 0.81064(15) 0.0192(5) Uani 1 1 d . . . O2 O 0.51406(8) 0.28334(13) 0.89795(14) 0.0168(5) Uani 1 1 d . . . O3 O 0.34839(8) -0.00891(14) 0.95208(16) 0.0219(6) Uani 1 1 d . . . O4 O 0.40621(8) 0.13260(13) 0.97050(14) 0.0150(5) Uani 1 1 d . . . O5 O 0.34444(9) 0.23500(14) 0.71235(16) 0.0242(6) Uani 1 1 d . . . O6 O 0.43129(8) 0.21621(13) 0.82050(14) 0.0161(5) Uani 1 1 d . . . F1 F 0.49121(9) 0.54115(15) 0.82157(15) 0.0452(6) Uani 1 1 d . . . F2 F 0.54483(8) 0.64342(14) 0.76931(15) 0.0398(6) Uani 1 1 d . . . C1 C 0.60883(14) 0.4333(2) 0.7593(2) 0.0260(8) Uani 1 1 d . . . H1A H 0.6099 0.4923 0.7816 0.039 Uiso 1 1 calc R . . H1B H 0.5943 0.4334 0.6987 0.039 Uiso 1 1 calc R . . H1C H 0.6455 0.4093 0.7625 0.039 Uiso 1 1 calc R . . C2 C 0.58947(12) 0.3740(2) 0.8968(2) 0.0153(7) Uani 1 1 d . . . C3 C 0.63242(12) 0.4144(2) 0.9400(2) 0.0168(7) Uani 1 1 d . . . H3 H 0.6556 0.4506 0.9093 0.020 Uiso 1 1 calc R . . C4 C 0.64200(12) 0.4021(2) 1.0297(2) 0.0183(8) Uani 1 1 d . . . C5 C 0.60996(12) 0.3517(2) 1.0761(2) 0.0202(8) Uani 1 1 d . . . H5 H 0.6169 0.3450 1.1370 0.024 Uiso 1 1 calc R . . C6 C 0.56591(12) 0.3090(2) 1.0320(2) 0.0181(8) Uani 1 1 d . . . C7 C 0.55444(12) 0.3189(2) 0.9426(2) 0.0156(7) Uani 1 1 d . . . C8 C 0.53039(13) 0.2598(2) 1.0846(2) 0.0180(7) Uani 1 1 d . . . H8 H 0.5396 0.2585 1.1453 0.022 Uiso 1 1 calc R . . C9 C 0.45593(13) 0.1793(2) 1.1250(2) 0.0224(8) Uani 1 1 d . . . H9A H 0.4765 0.1817 1.1814 0.034 Uiso 1 1 calc R . . H9B H 0.4479 0.1192 1.1099 0.034 Uiso 1 1 calc R . . H9C H 0.4220 0.2112 1.1285 0.034 Uiso 1 1 calc R . . C10 C 0.31946(14) -0.0861(2) 0.9309(3) 0.0280(9) Uani 1 1 d . . . H10A H 0.2883 -0.0906 0.9668 0.042 Uiso 1 1 calc R . . H10B H 0.3433 -0.1357 0.9420 0.042 Uiso 1 1 calc R . . H10C H 0.3069 -0.0851 0.8694 0.042 Uiso 1 1 calc R . . C11 C 0.32263(12) 0.0673(2) 0.9320(2) 0.0160(7) Uani 1 1 d . . . C12 C 0.26960(12) 0.0731(2) 0.8998(2) 0.0196(8) Uani 1 1 d . . . H12 H 0.2487 0.0226 0.8887 0.024 Uiso 1 1 calc R . . C13 C 0.24703(12) 0.1546(2) 0.8838(2) 0.0196(8) Uani 1 1 d . . . C14 C 0.27577(13) 0.2273(2) 0.8989(2) 0.0215(8) Uani 1 1 d . . . H14 H 0.2591 0.2818 0.8891 0.026 Uiso 1 1 calc R . . C15 C 0.33084(12) 0.2223(2) 0.9294(2) 0.0163(7) Uani 1 1 d . . . C16 C 0.35527(12) 0.1421(2) 0.9447(2) 0.0163(7) Uani 1 1 d . . . C17 C 0.36036(13) 0.3005(2) 0.9472(2) 0.0193(8) Uani 1 1 d . . . H17 H 0.3398 0.3518 0.9502 0.023 Uiso 1 1 calc R . . C18 C 0.43431(13) 0.3918(2) 0.9855(2) 0.0231(8) Uani 1 1 d . . . H18A H 0.4050 0.4342 0.9857 0.035 Uiso 1 1 calc R . . H18B H 0.4607 0.4098 0.9443 0.035 Uiso 1 1 calc R . . H18C H 0.4522 0.3877 1.0439 0.035 Uiso 1 1 calc R . . C19 C 0.29354(15) 0.2437(2) 0.6634(3) 0.0344(10) Uani 1 1 d . . . H19A H 0.2972 0.2238 0.6038 0.052 Uiso 1 1 calc R . . H19B H 0.2825 0.3043 0.6625 0.052 Uiso 1 1 calc R . . H19C H 0.2662 0.2091 0.6905 0.052 Uiso 1 1 calc R . . C20 C 0.36227(13) 0.1533(2) 0.7270(2) 0.0180(8) Uani 1 1 d . . . C21 C 0.40957(12) 0.1470(2) 0.7849(2) 0.0161(7) Uani 1 1 d . . . C22 C 0.43091(12) 0.0643(2) 0.8019(2) 0.0173(7) Uani 1 1 d . . . C23 C 0.40549(13) -0.0098(2) 0.7658(2) 0.0207(8) Uani 1 1 d . . . H23 H 0.4203 -0.0654 0.7771 0.025 Uiso 1 1 calc R . . C24 C 0.35896(13) 0.0003(2) 0.7142(2) 0.0208(8) Uani 1 1 d . . . C25 C 0.33774(13) 0.0807(2) 0.6935(2) 0.0211(8) Uani 1 1 d . . . H25 H 0.3060 0.0854 0.6559 0.025 Uiso 1 1 calc R . . C26 C 0.48035(13) 0.0552(2) 0.8564(2) 0.0181(8) Uani 1 1 d . . . H26 H 0.5000 0.0032 0.8507 0.022 Uiso 1 1 calc R . . C27 C 0.55293(12) 0.0912(2) 0.9550(2) 0.0224(8) Uani 1 1 d . . . H27A H 0.5669 0.0371 0.9326 0.034 Uiso 1 1 calc R . . H27B H 0.5492 0.0859 1.0177 0.034 Uiso 1 1 calc R . . H27C H 0.5781 0.1380 0.9440 0.034 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 0.0130(2) 0.0166(2) 0.0108(2) -0.0003(2) -0.00094(17) -0.00155(18) Na1 0.0204(10) 0.0278(11) 0.0131(10) 0.000 -0.0025(8) 0.000 Br1 0.01790(18) 0.0290(2) 0.0266(2) -0.00322(17) -0.00593(14) -0.00560(15) Br2 0.01447(18) 0.0303(2) 0.0326(2) -0.00020(18) -0.00471(14) 0.00134(15) Br3 0.0299(2) 0.0277(2) 0.0386(3) -0.01442(19) -0.00200(17) -0.00777(17) B1 0.031(4) 0.035(4) 0.025(4) 0.000 0.000(3) 0.000 N1 0.0166(14) 0.0186(15) 0.0128(15) 0.0010(13) -0.0004(11) 0.0009(12) N2 0.0210(15) 0.0140(14) 0.0138(16) -0.0016(12) -0.0004(12) -0.0011(12) N3 0.0134(14) 0.0196(15) 0.0147(16) 0.0034(13) -0.0004(11) -0.0005(12) O1 0.0238(13) 0.0206(13) 0.0133(13) 0.0017(10) 0.0015(10) -0.0064(10) O2 0.0158(11) 0.0215(12) 0.0124(13) 0.0018(11) -0.0035(9) -0.0068(10) O3 0.0164(12) 0.0163(12) 0.0323(16) 0.0050(11) -0.0034(10) -0.0021(10) O4 0.0109(11) 0.0188(12) 0.0151(13) 0.0035(10) -0.0011(9) -0.0010(9) O5 0.0238(13) 0.0217(13) 0.0255(16) 0.0032(11) -0.0106(11) -0.0020(10) O6 0.0180(12) 0.0180(12) 0.0118(13) 0.0004(10) -0.0027(9) -0.0053(10) F1 0.0487(15) 0.0523(15) 0.0339(15) 0.0157(13) -0.0023(11) -0.0048(12) F2 0.0374(13) 0.0455(14) 0.0356(15) 0.0018(12) -0.0060(10) -0.0078(11) C1 0.030(2) 0.030(2) 0.018(2) 0.0047(17) 0.0032(15) -0.0108(17) C2 0.0158(17) 0.0162(17) 0.0138(19) -0.0024(15) -0.0003(13) 0.0033(14) C3 0.0159(17) 0.0145(17) 0.020(2) -0.0017(15) 0.0021(14) -0.0014(13) C4 0.0141(17) 0.0193(18) 0.021(2) -0.0074(16) -0.0044(14) -0.0032(14) C5 0.0174(18) 0.028(2) 0.0146(19) -0.0034(16) -0.0040(14) 0.0001(15) C6 0.0165(17) 0.0205(18) 0.017(2) -0.0013(16) -0.0018(14) -0.0007(14) C7 0.0162(17) 0.0161(17) 0.0143(19) -0.0007(15) -0.0007(13) 0.0022(14) C8 0.0212(18) 0.0227(19) 0.0096(18) -0.0006(15) -0.0038(13) -0.0001(15) C9 0.0257(19) 0.0277(19) 0.013(2) 0.0046(16) -0.0008(14) -0.0074(16) C10 0.025(2) 0.0189(19) 0.039(3) 0.0049(18) -0.0024(16) -0.0031(16) C11 0.0163(17) 0.0188(17) 0.0130(19) 0.0011(15) 0.0021(13) 0.0009(14) C12 0.0154(18) 0.0259(19) 0.018(2) 0.0006(16) 0.0020(14) -0.0042(15) C13 0.0120(17) 0.026(2) 0.020(2) 0.0007(16) -0.0023(13) 0.0014(15) C14 0.0178(18) 0.0214(19) 0.025(2) 0.0031(17) 0.0015(15) 0.0104(15) C15 0.0149(17) 0.0185(18) 0.0156(19) -0.0008(15) 0.0028(13) 0.0021(14) C16 0.0147(17) 0.0249(19) 0.0094(18) 0.0001(15) 0.0025(13) 0.0009(15) C17 0.0191(18) 0.0191(19) 0.019(2) -0.0001(15) -0.0003(14) 0.0035(14) C18 0.0222(19) 0.0180(18) 0.028(2) -0.0059(17) -0.0042(15) -0.0016(15) C19 0.033(2) 0.028(2) 0.040(3) 0.006(2) -0.0142(19) 0.0021(18) C20 0.0178(17) 0.0211(19) 0.0151(19) 0.0007(15) 0.0015(14) -0.0026(15) C21 0.0136(17) 0.0222(19) 0.0127(19) -0.0028(15) 0.0022(13) -0.0048(14) C22 0.0166(17) 0.0204(18) 0.0152(19) -0.0029(15) 0.0030(13) -0.0027(14) C23 0.0231(19) 0.0184(18) 0.021(2) -0.0044(16) 0.0055(15) 0.0015(15) C24 0.0226(19) 0.0235(19) 0.016(2) -0.0090(16) 0.0021(14) -0.0080(15) C25 0.0175(18) 0.032(2) 0.0138(19) -0.0019(17) 0.0002(14) -0.0042(16) C26 0.0158(17) 0.0196(18) 0.019(2) 0.0002(16) 0.0052(14) 0.0034(15) C27 0.0144(17) 0.030(2) 0.023(2) -0.0032(17) -0.0022(14) 0.0034(15) _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 O4 1.886(2) . ? Co1 O2 1.895(2) . ? Co1 O6 1.909(2) . ? Co1 N2 1.930(3) . ? Co1 N1 1.934(3) . ? Co1 N3 1.947(3) . ? Co1 Na1 3.4207(11) . ? Na1 O2 2.299(2) 2_656 ? Na1 O2 2.299(2) . ? Na1 O1 2.395(2) . ? Na1 O1 2.395(2) 2_656 ? Na1 O6 2.443(2) 2_656 ? Na1 O6 2.443(2) . ? Na1 Co1 3.4207(11) 2_656 ? Br1 C4 1.905(3) . ? Br2 C13 1.906(3) . ? Br3 C24 1.898(3) . ? B1 F1 1.376(4) 2_656 ? B1 F1 1.376(4) . ? B1 F2 1.395(4) . ? B1 F2 1.395(4) 2_656 ? N1 C8 1.281(4) . ? N1 C9 1.470(4) . ? N2 C17 1.285(4) . ? N2 C18 1.467(4) . ? N3 C26 1.275(4) . ? N3 C27 1.462(4) . ? O1 C2 1.359(4) . ? O1 C1 1.437(4) . ? O2 C7 1.301(4) . ? O3 C11 1.371(4) . ? O3 C10 1.425(4) . ? O4 C16 1.307(4) . ? O5 C20 1.358(4) . ? O5 C19 1.434(4) . ? O6 C21 1.308(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.372(4) . ? C2 C7 1.436(4) . ? C3 C4 1.402(5) . ? C3 H3 0.9500 . ? C4 C5 1.352(5) . ? C5 C6 1.413(4) . ? C5 H5 0.9500 . ? C6 C7 1.398(5) . ? C6 C8 1.452(5) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.378(4) . ? C11 C16 1.423(4) . ? C12 C13 1.401(4) . ? C12 H12 0.9500 . ? C13 C14 1.348(5) . ? C14 C15 1.417(4) . ? C14 H14 0.9500 . ? C15 C16 1.399(4) . ? C15 C17 1.436(4) . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.368(5) . ? C20 C21 1.432(5) . ? C21 C22 1.407(5) . ? C22 C23 1.411(5) . ? C22 C26 1.448(5) . ? C23 C24 1.368(5) . ? C23 H23 0.9500 . ? C24 C25 1.384(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 O4 Co1 O2 174.04(10) . . ? O4 Co1 O6 93.20(9) . . ? O2 Co1 O6 83.46(9) . . ? O4 Co1 N2 91.36(10) . . ? O2 Co1 N2 93.38(10) . . ? O6 Co1 N2 86.91(11) . . ? O4 Co1 N1 90.39(10) . . ? O2 Co1 N1 93.23(10) . . ? O6 Co1 N1 175.15(10) . . ? N2 Co1 N1 89.75(11) . . ? O4 Co1 N3 84.50(10) . . ? O2 Co1 N3 90.49(10) . . ? O6 Co1 N3 88.98(10) . . ? N2 Co1 N3 174.00(11) . . ? N1 Co1 N3 94.61(11) . . ? O4 Co1 Na1 136.67(7) . . ? O2 Co1 Na1 39.46(7) . . ? O6 Co1 Na1 44.12(6) . . ? N2 Co1 Na1 92.91(9) . . ? N1 Co1 Na1 132.69(8) . . ? N3 Co1 Na1 87.16(8) . . ? O2 Na1 O2 167.78(13) 2_656 . ? O2 Na1 O1 120.63(8) 2_656 . ? O2 Na1 O1 66.70(8) . . ? O2 Na1 O1 66.70(8) 2_656 2_656 ? O2 Na1 O1 120.63(8) . 2_656 ? O1 Na1 O1 115.23(13) . 2_656 ? O2 Na1 O6 64.46(8) 2_656 2_656 ? O2 Na1 O6 108.60(8) . 2_656 ? O1 Na1 O6 84.97(7) . 2_656 ? O1 Na1 O6 130.72(7) 2_656 2_656 ? O2 Na1 O6 108.60(8) 2_656 . ? O2 Na1 O6 64.46(8) . . ? O1 Na1 O6 130.72(7) . . ? O1 Na1 O6 84.97(7) 2_656 . ? O6 Na1 O6 116.38(12) 2_656 . ? O2 Na1 Co1 31.60(5) 2_656 2_656 ? O2 Na1 Co1 140.13(7) . 2_656 ? O1 Na1 Co1 106.29(6) . 2_656 ? O1 Na1 Co1 98.25(6) 2_656 2_656 ? O6 Na1 Co1 32.95(5) 2_656 2_656 ? O6 Na1 Co1 114.95(7) . 2_656 ? O2 Na1 Co1 140.13(7) 2_656 . ? O2 Na1 Co1 31.60(5) . . ? O1 Na1 Co1 98.25(6) . . ? O1 Na1 Co1 106.29(6) 2_656 . ? O6 Na1 Co1 114.95(7) 2_656 . ? O6 Na1 Co1 32.95(5) . . ? Co1 Na1 Co1 133.37(6) 2_656 . ? F1 B1 F1 111.5(5) 2_656 . ? F1 B1 F2 109.63(14) 2_656 . ? F1 B1 F2 108.77(14) . . ? F1 B1 F2 108.77(14) 2_656 2_656 ? F1 B1 F2 109.63(14) . 2_656 ? F2 B1 F2 108.4(5) . 2_656 ? C8 N1 C9 116.9(3) . . ? C8 N1 Co1 125.2(2) . . ? C9 N1 Co1 117.7(2) . . ? C17 N2 C18 118.3(3) . . ? C17 N2 Co1 121.0(2) . . ? C18 N2 Co1 120.7(2) . . ? C26 N3 C27 118.0(3) . . ? C26 N3 Co1 120.2(2) . . ? C27 N3 Co1 121.7(2) . . ? C2 O1 C1 117.2(3) . . ? C2 O1 Na1 119.15(18) . . ? C1 O1 Na1 123.4(2) . . ? C7 O2 Co1 128.2(2) . . ? C7 O2 Na1 122.9(2) . . ? Co1 O2 Na1 108.94(10) . . ? C11 O3 C10 117.0(2) . . ? C16 O4 Co1 121.3(2) . . ? C20 O5 C19 116.2(3) . . ? C21 O6 Co1 119.1(2) . . ? C21 O6 Na1 121.79(19) . . ? Co1 O6 Na1 102.93(9) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.9(3) . . ? O1 C2 C7 113.6(3) . . ? C3 C2 C7 120.5(3) . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 122.1(3) . . ? C5 C4 Br1 119.7(3) . . ? C3 C4 Br1 118.1(2) . . ? C4 C5 C6 118.6(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C7 C6 C5 121.7(3) . . ? C7 C6 C8 121.1(3) . . ? C5 C6 C8 117.1(3) . . ? O2 C7 C6 125.2(3) . . ? O2 C7 C2 117.5(3) . . ? C6 C7 C2 117.3(3) . . ? N1 C8 C6 127.1(3) . . ? N1 C8 H8 116.5 . . ? C6 C8 H8 116.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C11 C12 123.9(3) . . ? O3 C11 C16 115.0(3) . . ? C12 C11 C16 121.1(3) . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 121.8(3) . . ? C14 C13 Br2 121.2(2) . . ? C12 C13 Br2 117.0(2) . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 C17 120.8(3) . . ? C14 C15 C17 119.0(3) . . ? O4 C16 C15 123.4(3) . . ? O4 C16 C11 118.6(3) . . ? C15 C16 C11 117.9(3) . . ? N2 C17 C15 126.3(3) . . ? N2 C17 H17 116.8 . . ? C15 C17 H17 116.8 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 C25 125.2(3) . . ? O5 C20 C21 114.4(3) . . ? C25 C20 C21 120.4(3) . . ? O6 C21 C22 122.2(3) . . ? O6 C21 C20 120.3(3) . . ? C22 C21 C20 117.5(3) . . ? C21 C22 C23 121.3(3) . . ? C21 C22 C26 119.5(3) . . ? C23 C22 C26 119.2(3) . . ? C24 C23 C22 118.3(3) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C23 C24 C25 122.1(3) . . ? C23 C24 Br3 119.4(3) . . ? C25 C24 Br3 118.5(3) . . ? C20 C25 C24 120.3(3) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? N3 C26 C22 126.5(3) . . ? N3 C26 H26 116.7 . . ? C22 C26 H26 116.7 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 0.564 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.091