Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Blake, A,' 'Brett, Matthew T.' 'Champness, Neil' 'Khlobystov, Andrei N.' 'Long, De-Liang' 'Schroder, Martin' 'Wilson, Claire' _publ_contact_author_name 'Dr Neil Champness' _publ_contact_author_address ; Dr Neil Champness Department of Chemistry The University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'NEIL.CHAMPNESS@NOTTINGHAM.AC.UK' _publ_section_title ; Inorganic-Organic Interpenetrating Frameworks: 4,4'-bipyridine-dioxide as a Bridging Hydrogen-Bond Acceptor ; data_cobpdo _database_code_CSD 169145 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co(II) 2(NO3) 4(H2O)] [bipydiox]' _chemical_melting_point unknown _chemical_formula_moiety '[Co(II) 2(NO3) 4(H2O)] [bipydiox]' _chemical_formula_sum 'C20 H24 Co N6 O14' _chemical_formula_weight 631.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.3309(10) _cell_length_b 19.3309(10) _cell_length_c 13.4691(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5033.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6167 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.5 _exptl_crystal_description 'irregular block' _exptl_crystal_colour pink _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 5 _diffrn_standards_decay_% none _diffrn_reflns_number 3004 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3004 _reflns_number_gt 2374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SAINT _computing_data_reduction 'SAINT version 6.02a (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0604P)^2^+0.2436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ; Hydrogens of H2O molecules located from difmap, others geometrically placed ; _refine_ls_hydrogen_treatment ; Hydrogens of H2O molecules refined with restraints, others with riding model ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3004 _refine_ls_number_parameters 199 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.013 _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 Co Co 0.0000 0.7500 0.127119(16) 0.01426(10) Uani 1 2 d S . . O1W O 0.04224(5) 0.68694(5) 0.02113(7) 0.0187(2) Uani 1 1 d D . . H1W1 H 0.0147(7) 0.6632(7) -0.0120(10) 0.028 Uiso 1 1 d D . . H1W2 H 0.0682(7) 0.7064(7) -0.0206(10) 0.028 Uiso 1 1 d D . . O2W O 0.04791(5) 0.69245(5) 0.23604(6) 0.0183(2) Uani 1 1 d D . . H2W1 H 0.0261(7) 0.6708(7) 0.2788(9) 0.027 Uiso 1 1 d D . . H2W2 H 0.0765(7) 0.7164(7) 0.2675(10) 0.027 Uiso 1 1 d D . . N1A N 0.11766(6) 0.86075(6) 0.11450(8) 0.0199(3) Uani 1 1 d . . . O2A O 0.18019(6) 0.87511(6) 0.10680(8) 0.0332(3) Uani 1 1 d . . . O1A O 0.10088(5) 0.79777(5) 0.12780(7) 0.0246(3) Uani 1 1 d . . . O3A O 0.07274(7) 0.90576(6) 0.10915(9) 0.0426(3) Uani 1 1 d . . . O1 O 0.02380(6) 0.37762(5) 0.12608(6) 0.0224(2) Uani 1 1 d . . . N1 N 0.07188(6) 0.42708(6) 0.12596(7) 0.0178(3) Uani 1 1 d . . . C2 C 0.05125(8) 0.49374(7) 0.12959(9) 0.0217(3) Uani 1 1 d . . . H2 H 0.0033 0.5044 0.1295 0.026 Uiso 1 1 calc R . . C3 C 0.09914(8) 0.54641(8) 0.13343(10) 0.0209(3) Uani 1 1 d . . . H3 H 0.0839 0.5931 0.1358 0.025 Uiso 1 1 calc R . . C4 C 0.17000(7) 0.53183(7) 0.13384(9) 0.0170(3) Uani 1 1 d . . . C5 C 0.18924(8) 0.46206(8) 0.12795(9) 0.0194(3) Uani 1 1 d . . . H5 H 0.2369 0.4500 0.1268 0.023 Uiso 1 1 calc R . . C6 C 0.13975(8) 0.41069(8) 0.12374(9) 0.0204(3) Uani 1 1 d . . . H6 H 0.1535 0.3636 0.1193 0.024 Uiso 1 1 calc R . . C7 C 0.22133(7) 0.58869(7) 0.13914(9) 0.0164(3) Uani 1 1 d . . . C8 C 0.20069(7) 0.65813(7) 0.13084(9) 0.0194(3) Uani 1 1 d . . . H8 H 0.1530 0.6690 0.1243 0.023 Uiso 1 1 calc R . . C9 C 0.24887(7) 0.71073(7) 0.13206(9) 0.0189(3) Uani 1 1 d . . . H9 H 0.2341 0.7575 0.1265 0.023 Uiso 1 1 calc R . . N10 N 0.31700(6) 0.69613(6) 0.14111(8) 0.0167(2) Uani 1 1 d . . . O10 O 0.36282(5) 0.74765(5) 0.13553(6) 0.0198(2) Uani 1 1 d . . . C11 C 0.33876(7) 0.63009(7) 0.15228(10) 0.0197(3) Uani 1 1 d . . . H11 H 0.3866 0.6208 0.1608 0.024 Uiso 1 1 calc R . . C12 C 0.29227(7) 0.57634(7) 0.15148(10) 0.0195(3) Uani 1 1 d . . . H12 H 0.3084 0.5302 0.1594 0.023 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 Co 0.01274(15) 0.01349(15) 0.01655(16) 0.000 0.000 0.00026(9) O1W 0.0161(5) 0.0192(5) 0.0209(5) -0.0032(4) 0.0015(4) -0.0024(4) O2W 0.0172(5) 0.0173(5) 0.0203(5) 0.0027(4) -0.0024(4) -0.0027(4) N1A 0.0203(6) 0.0175(6) 0.0219(6) 0.0009(4) -0.0018(4) -0.0024(5) O2A 0.0196(6) 0.0318(7) 0.0482(7) 0.0062(5) -0.0007(5) -0.0111(5) O1A 0.0173(5) 0.0175(5) 0.0392(6) 0.0045(4) -0.0012(4) -0.0039(4) O3A 0.0301(7) 0.0206(6) 0.0772(9) 0.0005(6) -0.0034(6) 0.0062(5) O1 0.0241(6) 0.0173(5) 0.0256(5) 0.0019(4) -0.0042(4) -0.0091(4) N1 0.0194(6) 0.0151(6) 0.0190(6) 0.0008(4) -0.0025(4) -0.0042(4) C2 0.0179(7) 0.0179(7) 0.0294(7) 0.0020(5) -0.0023(5) 0.0003(5) C3 0.0185(7) 0.0146(7) 0.0297(7) 0.0007(5) -0.0010(5) 0.0000(5) C4 0.0190(7) 0.0145(7) 0.0175(6) 0.0007(5) 0.0006(5) -0.0006(5) C5 0.0171(7) 0.0175(7) 0.0236(7) -0.0002(5) 0.0017(5) 0.0014(5) C6 0.0233(8) 0.0142(7) 0.0236(7) -0.0004(5) 0.0011(5) 0.0010(5) C7 0.0158(7) 0.0162(7) 0.0172(6) -0.0002(5) 0.0011(5) -0.0005(5) C8 0.0150(7) 0.0185(7) 0.0246(7) -0.0002(5) 0.0008(5) 0.0000(5) C9 0.0180(7) 0.0147(7) 0.0240(7) -0.0010(5) 0.0001(5) 0.0016(5) N10 0.0157(6) 0.0160(6) 0.0184(5) -0.0008(4) 0.0009(4) -0.0033(4) O10 0.0167(5) 0.0182(5) 0.0243(5) -0.0015(4) 0.0005(4) -0.0058(4) C11 0.0148(7) 0.0199(7) 0.0242(6) 0.0017(5) -0.0003(5) 0.0023(5) C12 0.0175(7) 0.0163(7) 0.0249(6) 0.0017(5) 0.0000(5) 0.0011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O1W 2.0471(9) 6_464 ? Co O1W 2.0471(9) . ? Co O2W 2.0609(9) . ? Co O2W 2.0609(9) 6_464 ? Co O1A 2.1578(10) 6_464 ? Co O1A 2.1578(10) . ? N1A O3A 1.2313(17) . ? N1A O2A 1.2445(16) . ? N1A O1A 1.2725(15) . ? O1 N1 1.3333(15) . ? N1 C2 1.3498(18) . ? N1 C6 1.3500(19) . ? C2 C3 1.377(2) . ? C3 C4 1.398(2) . ? C4 C5 1.401(2) . ? C4 C7 1.4825(19) . ? C5 C6 1.380(2) . ? C7 C12 1.4019(19) . ? C7 C8 1.4049(19) . ? C8 C9 1.379(2) . ? C9 N10 1.3525(18) . ? N10 O10 1.3351(14) . ? N10 C11 1.3525(17) . ? C11 C12 1.3737(19) . ? 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 O1W Co O1W 91.57(5) 6_464 . ? O1W Co O2W 175.61(4) 6_464 . ? O1W Co O2W 89.75(4) . . ? O1W Co O2W 89.75(4) 6_464 6_464 ? O1W Co O2W 175.61(4) . 6_464 ? O2W Co O2W 89.23(5) . 6_464 ? O1W Co O1A 84.10(4) 6_464 6_464 ? O1W Co O1A 96.24(4) . 6_464 ? O2W Co O1A 99.91(4) . 6_464 ? O2W Co O1A 79.74(4) 6_464 6_464 ? O1W Co O1A 96.24(4) 6_464 . ? O1W Co O1A 84.10(4) . . ? O2W Co O1A 79.74(4) . . ? O2W Co O1A 99.91(4) 6_464 . ? O1A Co O1A 179.51(5) 6_464 . ? O3A N1A O2A 121.49(12) . . ? O3A N1A O1A 120.30(12) . . ? O2A N1A O1A 118.21(12) . . ? N1A O1A Co 129.73(9) . . ? O1 N1 C2 118.60(12) . . ? O1 N1 C6 120.60(12) . . ? C2 N1 C6 120.79(12) . . ? N1 C2 C3 120.57(14) . . ? C2 C3 C4 120.65(14) . . ? C3 C4 C5 116.99(13) . . ? C3 C4 C7 120.42(12) . . ? C5 C4 C7 122.59(13) . . ? C6 C5 C4 120.71(13) . . ? N1 C6 C5 120.26(13) . . ? C12 C7 C8 116.75(12) . . ? C12 C7 C4 122.29(12) . . ? C8 C7 C4 120.96(12) . . ? C9 C8 C7 120.78(13) . . ? N10 C9 C8 120.32(13) . . ? O10 N10 C9 119.03(11) . . ? O10 N10 C11 120.27(11) . . ? C9 N10 C11 120.66(12) . . ? N10 C11 C12 120.64(12) . . ? C11 C12 C7 120.80(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 O1 0.832(9) 1.882(11) 2.6682(13) 157.3(15) 9_565 O1W H1W2 O1 0.842(9) 1.845(10) 2.6678(13) 165.2(15) 4_454 O2W H2W1 O10 0.827(9) 1.880(10) 2.6832(13) 163.4(16) 3 O2W H2W2 O10 0.836(9) 1.888(10) 2.7038(13) 164.8(15) 13_565 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.321 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.052 #===END data_nibyno _database_code_CSD 169146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4,4'-Bipyridyl-(N,N')-dioxide Nickel(II) bisnitrate tetrahydrate complex ; _chemical_name_common 4,4 _chemical_melting_point unknown _chemical_formula_moiety 'C10 H12 N3 Ni0.50 O7' _chemical_formula_sum 'C10 H12 N3 Ni0.50 O7' _chemical_formula_weight 315.58 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)cd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' 'x, -y, z+1/2' '-x+1/2, y+1/2, z' '-y, -x+1/2, z+3/4' 'y+1/2, x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' 'x+1/2, -y+1/2, z+1' '-x+1, y+1, z+1/2' '-y+1/2, -x+1, z+5/4' 'y+1, x+1/2, z+3/4' _cell_length_a 19.3091(11) _cell_length_b 19.3091(11) _cell_length_c 13.4271(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5006.2(5) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5087 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.5 _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.682 _exptl_absorpt_correction_T_max 0.751 _exptl_absorpt_process_details ? _exptl_special_details ; 4,4'-Bipyridyl-(N,N')-dioxide Nickel(II) bisnitrate tetrahydrate complex ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 5 _diffrn_standards_decay_% none _diffrn_reflns_number 2454 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.83 _reflns_number_total 2454 _reflns_number_gt 2259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)' _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^)+(0.0395P)^2^+1.2373P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'H2O from difference electron map, others placed geometrically' _refine_ls_hydrogen_treatment 'H2O refined freely, riding model for others' _refine_ls_extinction_method none _refine_ls_extinction_coef 'refined to zero' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 2454 _refine_ls_number_parameters 203 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Ni1 Ni 0.5000 0.5000 0.76160(12) 0.01333(9) Uani 1 2 d S . . O1A O 0.59848(6) 0.45604(6) 0.76175(14) 0.0226(3) Uani 1 1 d . . . O1W O 0.45974(8) 0.43730(7) 0.65506(12) 0.0176(3) Uani 1 1 d D . . H1WB H 0.4859(11) 0.4102(11) 0.6255(16) 0.030(7) Uiso 1 1 d D . . H1WA H 0.4387(13) 0.4611(12) 0.6128(15) 0.041(9) Uiso 1 1 d D . . O1 O 0.88132(5) 0.01207(6) 0.50650(16) 0.0206(3) Uani 1 1 d . . . O10 O 0.51354(6) 0.35345(6) 0.51759(14) 0.0192(3) Uani 1 1 d . . . O2W O 0.45336(8) 0.44064(7) 0.86838(13) 0.0176(3) Uani 1 1 d D . . H2WB H 0.4711(14) 0.4127(12) 0.9073(17) 0.059(10) Uiso 1 1 d D . . H2WA H 0.4285(11) 0.4676(11) 0.9021(16) 0.036(8) Uiso 1 1 d D . . O2A O 0.57053(7) 0.34736(7) 0.75283(19) 0.0421(4) Uani 1 1 d . . . O3A O 0.67798(7) 0.37806(7) 0.74877(17) 0.0337(4) Uani 1 1 d . . . N1A N 0.61531(7) 0.39216(7) 0.75425(19) 0.0199(3) Uani 1 1 d . . . N1 N 0.83202(7) 0.05994(7) 0.50059(14) 0.0170(3) Uani 1 1 d . . . N10 N 0.56496(7) 0.30782(7) 0.51643(15) 0.0169(3) Uani 1 1 d . . . C2 C 0.76487(8) 0.03991(8) 0.50622(18) 0.0203(4) Uani 1 1 d . . . H2A H 0.7538 -0.0080 0.5096 0.024 Uiso 1 1 calc R . . C3 C 0.71257(8) 0.08815(8) 0.5071(2) 0.0205(4) Uani 1 1 d . . . H3A H 0.6658 0.0733 0.5113 0.025 Uiso 1 1 calc R . . C4 C 0.72760(8) 0.15894(8) 0.50190(17) 0.0160(4) Uani 1 1 d . . . C5 C 0.79733(9) 0.17751(10) 0.49298(17) 0.0202(4) Uani 1 1 d . . . H5A H 0.8096 0.2250 0.4874 0.024 Uiso 1 1 calc R . . C6 C 0.84843(10) 0.12766(10) 0.49223(17) 0.0206(4) Uani 1 1 d . . . H6A H 0.8956 0.1411 0.4858 0.025 Uiso 1 1 calc R . . C7 C 0.67170(8) 0.21170(8) 0.50759(19) 0.0163(3) Uani 1 1 d . . . C8 C 0.60195(8) 0.19149(8) 0.50511(19) 0.0191(4) Uani 1 1 d . . . H8A H 0.5907 0.1437 0.5001 0.023 Uiso 1 1 calc R . . C9 C 0.54961(8) 0.23968(8) 0.50984(19) 0.0190(4) Uani 1 1 d . . . H9A H 0.5026 0.2251 0.5085 0.023 Uiso 1 1 calc R . . C11 C 0.63145(9) 0.32949(9) 0.52053(17) 0.0193(4) Uani 1 1 d . . . H11A H 0.6413 0.3775 0.5265 0.023 Uiso 1 1 calc R . . C12 C 0.68505(9) 0.28250(9) 0.51620(18) 0.0190(4) Uani 1 1 d . . . H12A H 0.7316 0.2984 0.5191 0.023 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 Ni1 0.01168(13) 0.01231(13) 0.01601(17) 0.000 0.000 -0.00010(12) O1A 0.0160(6) 0.0151(5) 0.0368(8) -0.0024(7) -0.0006(7) 0.0021(4) O1W 0.0166(7) 0.0172(7) 0.0191(9) -0.0027(6) -0.0023(6) 0.0028(6) O1 0.0161(5) 0.0210(6) 0.0249(8) -0.0027(9) 0.0002(8) 0.0078(4) O10 0.0178(6) 0.0154(5) 0.0243(8) 0.0019(7) 0.0023(8) 0.0061(4) O2W 0.0171(7) 0.0148(6) 0.0208(9) 0.0017(6) 0.0026(6) 0.0020(6) O2A 0.0275(7) 0.0191(6) 0.0797(14) 0.0001(10) -0.0053(10) -0.0036(5) O3A 0.0194(7) 0.0312(7) 0.0504(11) -0.0057(9) -0.0016(8) 0.0098(5) N1A 0.0183(7) 0.0179(7) 0.0235(9) -0.0017(8) -0.0033(8) 0.0036(6) N1 0.0147(6) 0.0191(7) 0.0171(9) -0.0019(7) -0.0010(7) 0.0033(5) N10 0.0171(6) 0.0155(6) 0.0180(8) -0.0007(8) 0.0013(7) 0.0028(5) C2 0.0170(8) 0.0149(7) 0.0290(12) -0.0024(10) -0.0020(11) -0.0022(6) C3 0.0149(7) 0.0190(8) 0.0275(11) -0.0013(10) -0.0003(10) -0.0022(6) C4 0.0144(7) 0.0164(8) 0.0171(10) 0.0004(8) -0.0005(8) 0.0001(6) C5 0.0175(8) 0.0182(8) 0.0249(13) 0.0026(8) -0.0006(8) -0.0026(7) C6 0.0150(8) 0.0219(9) 0.0250(13) 0.0019(8) 0.0008(8) -0.0012(7) C7 0.0163(7) 0.0146(7) 0.0182(9) 0.0007(9) -0.0002(9) 0.0012(6) C8 0.0178(8) 0.0135(7) 0.0259(11) 0.0008(9) -0.0003(10) -0.0003(6) C9 0.0154(7) 0.0173(8) 0.0243(10) 0.0002(9) 0.0012(10) -0.0016(6) C11 0.0197(8) 0.0145(7) 0.0237(12) -0.0005(8) -0.0002(9) -0.0012(6) C12 0.0150(7) 0.0179(8) 0.0241(11) 0.0003(10) -0.0025(9) -0.0031(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 Ni1 O1W 2.0289(19) . ? Ni1 O1W 2.0289(19) 10_554 ? Ni1 O2W 2.0446(19) 10_554 ? Ni1 O2W 2.0446(19) . ? Ni1 O1A 2.0824(11) 10_554 ? Ni1 O1A 2.0824(11) . ? O1A N1A 1.2796(18) . ? O1 N1 1.3293(16) . ? O10 N10 1.3275(17) . ? O2A N1A 1.2232(18) . ? O3A N1A 1.2425(19) . ? N1 C6 1.350(2) . ? N1 C2 1.355(2) . ? N10 C11 1.351(2) . ? N10 C9 1.352(2) . ? C2 C3 1.374(2) . ? C3 C4 1.399(2) . ? C4 C5 1.398(2) . ? C4 C7 1.486(2) . ? C5 C6 1.378(3) . ? C7 C12 1.396(2) . ? C7 C8 1.403(2) . ? C8 C9 1.375(2) . ? C11 C12 1.378(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Ni1 O1W 90.33(11) . 10_554 ? O1W Ni1 O2W 176.11(6) . 10_554 ? O1W Ni1 O2W 89.49(5) 10_554 10_554 ? O1W Ni1 O2W 89.49(5) . . ? O1W Ni1 O2W 176.11(6) 10_554 . ? O2W Ni1 O2W 90.95(12) 10_554 . ? O1W Ni1 O1A 83.92(7) . 10_554 ? O1W Ni1 O1A 96.16(7) 10_554 10_554 ? O2W Ni1 O1A 99.97(7) 10_554 10_554 ? O2W Ni1 O1A 79.96(6) . 10_554 ? O1W Ni1 O1A 96.16(7) . . ? O1W Ni1 O1A 83.92(7) 10_554 . ? O2W Ni1 O1A 79.96(6) 10_554 . ? O2W Ni1 O1A 99.97(7) . . ? O1A Ni1 O1A 179.89(14) 10_554 . ? N1A O1A Ni1 128.67(10) . . ? O2A N1A O3A 122.19(15) . . ? O2A N1A O1A 120.22(14) . . ? O3A N1A O1A 117.59(13) . . ? O1 N1 C6 120.69(14) . . ? O1 N1 C2 118.91(13) . . ? C6 N1 C2 120.37(14) . . ? O10 N10 C11 120.30(13) . . ? O10 N10 C9 118.88(13) . . ? C11 N10 C9 120.82(14) . . ? N1 C2 C3 120.68(15) . . ? C2 C3 C4 120.63(15) . . ? C5 C4 C3 117.03(15) . . ? C5 C4 C7 121.87(14) . . ? C3 C4 C7 121.10(14) . . ? C6 C5 C4 120.72(17) . . ? N1 C6 C5 120.51(17) . . ? C12 C7 C8 116.85(15) . . ? C12 C7 C4 122.79(14) . . ? C8 C7 C4 120.36(14) . . ? C9 C8 C7 121.09(16) . . ? N10 C9 C8 120.04(15) . . ? N10 C11 C12 120.53(16) . . ? C11 C12 C7 120.65(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O1 0.836(10) 1.879(13) 2.688(2) 162(3) 13_454 O1W H1WB O10 0.829(10) 1.893(14) 2.666(2) 155(2) . O2W H2WA O1 0.841(10) 1.879(13) 2.697(2) 164(2) 9_455 O2W H2WB O10 0.825(10) 1.895(14) 2.694(2) 163(3) 14_545 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.240 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.069 #===END data_COPYNO _database_code_CSD 169147 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H48 Co N14 O18' _chemical_formula_weight 1312.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9447(8) _cell_length_b 11.7160(11) _cell_length_c 14.0734(13) _cell_angle_alpha 104.712(3) _cell_angle_beta 96.797(2) _cell_angle_gamma 98.233(2) _cell_volume 1393.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5439 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29 _exptl_crystal_description Tablet _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 677 _exptl_absorpt_coefficient_mu 0.401 _exptl_absorpt_correction_type 'multi-scans' _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8843 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.69 _reflns_number_total 6175 _reflns_number_gt 5351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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^)+(0.0767P)^2^+0.2857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'refined in riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 6175 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.123 _refine_ls_wR_factor_gt 0.118 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.0000 1.0000 0.5000 0.02772(11) Uani 1 2 d S . . O10 O -0.22974(14) 0.97992(11) 0.44300(10) 0.0393(3) Uani 1 1 d . . . O20 O -0.82196(18) 1.61376(13) 0.58172(13) 0.0546(4) Uani 1 1 d . . . O30 O -0.01636(16) 0.81496(10) 0.46381(9) 0.0372(3) Uani 1 1 d . . . O40 O -0.2004(2) 0.26354(14) -0.19437(10) 0.0561(4) Uani 1 1 d . . . O50 O -0.06670(15) 0.99300(12) 0.63672(9) 0.0397(3) Uani 1 1 d . . . O60 O 0.56343(19) 0.84417(17) 1.18568(12) 0.0617(4) Uani 1 1 d . . . N10 N -0.31765(16) 1.06235(13) 0.46683(11) 0.0325(3) Uani 1 1 d . . . N20 N -0.74522(18) 1.52571(14) 0.56492(13) 0.0388(3) Uani 1 1 d . . . N30 N -0.05826(17) 0.73543(12) 0.37538(10) 0.0314(3) Uani 1 1 d . . . N40 N -0.1907(2) 0.33108(14) -0.10427(12) 0.0420(4) Uani 1 1 d . . . N50 N 0.01767(17) 0.96764(13) 0.71038(10) 0.0325(3) Uani 1 1 d . . . N60 N 0.47730(19) 0.86239(16) 1.11156(13) 0.0437(4) Uani 1 1 d . . . C11 C -0.3119(2) 1.12541(16) 0.56192(14) 0.0369(4) Uani 1 1 d . . . H11A H -0.2480 1.1102 0.6126 0.044 Uiso 1 1 calc R . . C12 C -0.4006(2) 1.21266(17) 0.58422(13) 0.0364(4) Uani 1 1 d . . . H12A H -0.3965 1.2558 0.6501 0.044 Uiso 1 1 calc R . . C13 C -0.49672(19) 1.23701(15) 0.50898(13) 0.0328(4) Uani 1 1 d . . . C14 C -0.5037(2) 1.16549(17) 0.41188(14) 0.0383(4) Uani 1 1 d . . . H14A H -0.5696 1.1766 0.3601 0.046 Uiso 1 1 calc R . . C15 C -0.4144(2) 1.07913(17) 0.39218(14) 0.0372(4) Uani 1 1 d . . . H15A H -0.4203 1.0320 0.3273 0.045 Uiso 1 1 calc R . . C21 C -0.7987(2) 1.42729(17) 0.48693(15) 0.0392(4) Uani 1 1 d . . . H21A H -0.8896 1.4232 0.4456 0.047 Uiso 1 1 calc R . . C22 C -0.7199(2) 1.33325(17) 0.46826(14) 0.0368(4) Uani 1 1 d . . . H22A H -0.7578 1.2670 0.4139 0.044 Uiso 1 1 calc R . . C23 C -0.5845(2) 1.33579(15) 0.52954(13) 0.0326(4) Uani 1 1 d . . . C24 C -0.5329(2) 1.43848(17) 0.60915(14) 0.0394(4) Uani 1 1 d . . . H24A H -0.4428 1.4441 0.6519 0.047 Uiso 1 1 calc R . . C25 C -0.6130(2) 1.53122(17) 0.62534(15) 0.0423(4) Uani 1 1 d . . . H25A H -0.5761 1.5989 0.6786 0.051 Uiso 1 1 calc R . . C31 C 0.0080(2) 0.63679(15) 0.35772(14) 0.0367(4) Uani 1 1 d . . . H31A H 0.0791 0.6266 0.4073 0.044 Uiso 1 1 calc R . . C32 C -0.0290(2) 0.55191(16) 0.26745(14) 0.0377(4) Uani 1 1 d . . . H32A H 0.0172 0.4845 0.2567 0.045 Uiso 1 1 calc R . . C33 C -0.1348(2) 0.56484(15) 0.19116(13) 0.0332(4) Uani 1 1 d . . . C34 C -0.2048(2) 0.66516(16) 0.21390(14) 0.0377(4) Uani 1 1 d . . . H34A H -0.2789 0.6758 0.1662 0.045 Uiso 1 1 calc R . . C35 C -0.1666(2) 0.74907(16) 0.30575(14) 0.0366(4) Uani 1 1 d . . . H35A H -0.2155 0.8149 0.3196 0.044 Uiso 1 1 calc R . . C41 C -0.2816(3) 0.41483(19) -0.08274(16) 0.0497(5) Uani 1 1 d . . . H41A H -0.3537 0.4223 -0.1331 0.060 Uiso 1 1 calc R . . C42 C -0.2687(2) 0.48857(18) 0.01191(15) 0.0463(5) Uani 1 1 d . . . H42A H -0.3318 0.5454 0.0242 0.056 Uiso 1 1 calc R . . C43 C -0.1630(2) 0.48018(15) 0.09019(13) 0.0345(4) Uani 1 1 d . . . C44 C -0.0741(2) 0.39167(16) 0.06570(14) 0.0394(4) Uani 1 1 d . . . H44A H -0.0033 0.3808 0.1151 0.047 Uiso 1 1 calc R . . C45 C -0.0891(2) 0.32054(18) -0.02979(15) 0.0437(4) Uani 1 1 d . . . H45A H -0.0272 0.2630 -0.0436 0.052 Uiso 1 1 calc R . . C51 C 0.0847(2) 0.86986(16) 0.69389(13) 0.0375(4) Uani 1 1 d . . . H51A H 0.0722 0.8185 0.6300 0.045 Uiso 1 1 calc R . . C52 C 0.1720(2) 0.84599(16) 0.77191(14) 0.0374(4) Uani 1 1 d . . . H52A H 0.2171 0.7780 0.7600 0.045 Uiso 1 1 calc R . . C53 C 0.1935(2) 0.92228(15) 0.86822(13) 0.0331(4) Uani 1 1 d . . . C54 C 0.1195(2) 1.02092(16) 0.88201(13) 0.0375(4) Uani 1 1 d . . . H54A H 0.1294 1.0732 0.9453 0.045 Uiso 1 1 calc R . . C55 C 0.0321(2) 1.04161(16) 0.80303(13) 0.0369(4) Uani 1 1 d . . . H55A H -0.0175 1.1072 0.8135 0.044 Uiso 1 1 calc R . . C61 C 0.3717(2) 0.93406(18) 1.12864(15) 0.0427(4) Uani 1 1 d . . . H61A H 0.3603 0.9696 1.1938 0.051 Uiso 1 1 calc R . . C62 C 0.2810(2) 0.95508(17) 1.05113(14) 0.0390(4) Uani 1 1 d . . . H62A H 0.2110 1.0062 1.0649 0.047 Uiso 1 1 calc R . . C63 C 0.2918(2) 0.90122(15) 0.95227(13) 0.0340(4) Uani 1 1 d . . . C64 C 0.4020(2) 0.82843(18) 0.93736(15) 0.0418(4) Uani 1 1 d . . . H64A H 0.4144 0.7910 0.8728 0.050 Uiso 1 1 calc R . . C65 C 0.4925(2) 0.81121(19) 1.01647(16) 0.0463(5) Uani 1 1 d . . . H65A H 0.5661 0.7631 1.0044 0.056 Uiso 1 1 calc R . . N1 N -0.7443(3) 1.2783(2) 0.17413(16) 0.0651(6) Uani 1 1 d . . . O1 O -0.8130(3) 1.2381(2) 0.08911(17) 0.1104(10) Uani 1 1 d . A . O2 O -0.6562(5) 1.2277(4) 0.2155(2) 0.0987(13) Uani 0.70 1 d P A 1 O3 O -0.7697(5) 1.3736(3) 0.2274(3) 0.1155(15) Uani 0.70 1 d P A 1 O2' O -0.7458(11) 1.1949(9) 0.2199(8) 0.094(3) Uiso 0.30 1 d P A 2 O3' O -0.6306(11) 1.3611(9) 0.1706(7) 0.112(3) Uiso 0.30 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.03220(18) 0.02690(17) 0.02291(17) 0.00276(12) -0.00021(12) 0.01285(12) O10 0.0357(6) 0.0355(6) 0.0406(7) -0.0030(5) -0.0035(5) 0.0193(5) O20 0.0558(9) 0.0409(8) 0.0689(10) 0.0083(7) 0.0080(8) 0.0291(7) O30 0.0548(8) 0.0280(6) 0.0250(6) 0.0008(5) -0.0004(5) 0.0125(5) O40 0.0698(10) 0.0585(9) 0.0282(7) -0.0030(6) 0.0086(7) 0.0002(8) O50 0.0441(7) 0.0540(8) 0.0257(6) 0.0115(5) 0.0021(5) 0.0257(6) O60 0.0566(9) 0.0805(11) 0.0529(10) 0.0303(9) -0.0111(7) 0.0226(8) N10 0.0298(7) 0.0328(7) 0.0327(7) 0.0031(6) 0.0003(6) 0.0127(6) N20 0.0393(8) 0.0335(8) 0.0475(9) 0.0118(7) 0.0105(7) 0.0155(6) N30 0.0409(8) 0.0257(7) 0.0262(7) 0.0034(5) 0.0043(6) 0.0092(6) N40 0.0513(9) 0.0376(8) 0.0292(8) 0.0010(6) 0.0066(7) -0.0030(7) N50 0.0364(7) 0.0375(7) 0.0256(7) 0.0090(6) 0.0030(6) 0.0140(6) N60 0.0400(9) 0.0493(9) 0.0431(9) 0.0210(8) -0.0053(7) 0.0071(7) C11 0.0382(9) 0.0410(9) 0.0314(9) 0.0074(7) -0.0001(7) 0.0164(7) C12 0.0381(9) 0.0423(9) 0.0281(8) 0.0047(7) 0.0026(7) 0.0170(7) C13 0.0298(8) 0.0351(8) 0.0344(9) 0.0082(7) 0.0047(7) 0.0119(6) C14 0.0367(9) 0.0444(10) 0.0329(9) 0.0076(8) -0.0024(7) 0.0165(8) C15 0.0354(9) 0.0420(9) 0.0297(9) 0.0003(7) -0.0017(7) 0.0154(7) C21 0.0320(9) 0.0423(10) 0.0433(10) 0.0099(8) 0.0019(7) 0.0135(7) C22 0.0333(9) 0.0384(9) 0.0383(10) 0.0067(7) 0.0045(7) 0.0127(7) C23 0.0320(8) 0.0355(9) 0.0331(9) 0.0104(7) 0.0061(7) 0.0126(7) C24 0.0375(9) 0.0421(10) 0.0376(10) 0.0079(8) 0.0010(8) 0.0137(7) C25 0.0458(10) 0.0362(9) 0.0412(10) 0.0030(8) 0.0033(8) 0.0125(8) C31 0.0477(10) 0.0309(8) 0.0323(9) 0.0081(7) 0.0013(8) 0.0148(7) C32 0.0496(10) 0.0296(8) 0.0346(9) 0.0054(7) 0.0046(8) 0.0170(7) C33 0.0385(9) 0.0283(8) 0.0303(9) 0.0041(6) 0.0042(7) 0.0059(6) C34 0.0397(9) 0.0352(9) 0.0348(9) 0.0046(7) -0.0024(7) 0.0121(7) C35 0.0410(9) 0.0317(8) 0.0360(9) 0.0050(7) 0.0019(7) 0.0144(7) C41 0.0567(12) 0.0480(11) 0.0371(11) 0.0066(9) -0.0063(9) 0.0060(9) C42 0.0510(11) 0.0423(10) 0.0398(11) 0.0027(8) -0.0036(9) 0.0138(9) C43 0.0396(9) 0.0289(8) 0.0312(9) 0.0034(7) 0.0040(7) 0.0047(7) C44 0.0479(10) 0.0360(9) 0.0313(9) 0.0037(7) 0.0034(8) 0.0101(8) C45 0.0521(11) 0.0384(10) 0.0369(10) 0.0017(8) 0.0089(9) 0.0103(8) C51 0.0474(10) 0.0363(9) 0.0280(8) 0.0039(7) 0.0028(7) 0.0166(8) C52 0.0465(10) 0.0332(9) 0.0334(9) 0.0075(7) 0.0032(8) 0.0157(7) C53 0.0364(9) 0.0342(8) 0.0302(9) 0.0116(7) 0.0025(7) 0.0082(7) C54 0.0493(10) 0.0372(9) 0.0248(8) 0.0041(7) 0.0019(7) 0.0151(8) C55 0.0471(10) 0.0369(9) 0.0293(9) 0.0073(7) 0.0064(7) 0.0190(8) C61 0.0482(11) 0.0443(10) 0.0340(10) 0.0119(8) -0.0028(8) 0.0085(8) C62 0.0446(10) 0.0379(9) 0.0342(9) 0.0111(7) -0.0013(8) 0.0108(7) C63 0.0370(9) 0.0325(8) 0.0329(9) 0.0118(7) 0.0007(7) 0.0063(7) C64 0.0445(10) 0.0461(10) 0.0387(10) 0.0140(8) 0.0071(8) 0.0157(8) C65 0.0408(10) 0.0515(11) 0.0531(12) 0.0211(10) 0.0057(9) 0.0183(9) N1 0.0689(13) 0.0697(14) 0.0521(12) 0.0079(10) -0.0062(10) 0.0268(11) O1 0.129(2) 0.1122(18) 0.0673(13) -0.0210(12) -0.0350(13) 0.0738(16) O2 0.120(3) 0.117(3) 0.065(2) 0.0163(19) -0.009(2) 0.074(3) O3 0.155(3) 0.090(2) 0.075(2) -0.0235(18) -0.036(2) 0.067(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 Co O10 2.0730(12) . yes Co O10 2.0730(12) 2_576 ? Co O30 2.0763(12) . yes Co O30 2.0763(12) 2_576 ? Co O50 2.0983(13) . yes Co O50 2.0983(13) 2_576 ? O10 N10 1.3337(17) . yes O20 N20 1.3072(19) . yes O30 N30 1.3259(17) . yes O40 N40 1.299(2) . yes O50 N50 1.3297(18) . yes O60 N60 1.303(2) . yes N10 C11 1.345(2) . ? N10 C15 1.353(2) . ? N20 C25 1.356(3) . ? N20 C21 1.356(3) . ? N30 C35 1.351(2) . ? N30 C31 1.354(2) . ? N40 C45 1.346(3) . ? N40 C41 1.360(3) . ? N50 C51 1.349(2) . ? N50 C55 1.350(2) . ? N60 C65 1.352(3) . ? N60 C61 1.354(3) . ? C11 C12 1.379(2) . ? C12 C13 1.396(2) . ? C13 C14 1.399(2) . ? C13 C23 1.477(2) . ? C14 C15 1.371(2) . ? C21 C22 1.378(2) . ? C22 C23 1.394(2) . ? C23 C24 1.396(3) . ? C24 C25 1.372(3) . ? C31 C32 1.370(2) . ? C32 C33 1.398(3) . ? C33 C34 1.394(2) . ? C33 C43 1.481(2) . ? C34 C35 1.381(2) . ? C41 C42 1.373(3) . ? C42 C43 1.397(3) . ? C43 C44 1.395(2) . ? C44 C45 1.369(3) . ? C51 C52 1.382(2) . ? C52 C53 1.395(2) . ? C53 C54 1.395(2) . ? C53 C63 1.482(2) . ? C54 C55 1.375(2) . ? C61 C62 1.376(3) . ? C62 C63 1.395(3) . ? C63 C64 1.394(3) . ? C64 C65 1.372(3) . ? N1 O1 1.220(3) . ? N1 O2 1.230(4) . ? N1 O3 1.245(4) . ? N1 O2' 1.299(11) . ? N1 O3' 1.316(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Co O10 180 2_576 . ? O10 Co O30 89.56(5) 2_576 . ? O10 Co O30 90.44(5) . . yes O10 Co O30 90.44(5) 2_576 2_576 ? O10 Co O30 89.56(5) . 2_576 yes O10 Co O50 92.20(5) . 2_576 yes O10 Co O50 87.80(5) 2_576 2_576 ? O10 Co O50 92.20(5) 2_576 . ? O10 Co O50 87.80(5) . . yes O30 Co O30 180 . 2_576 ? O30 Co O50 91.90(5) . 2_576 yes O30 Co O50 88.10(5) 2_576 2_576 ? O30 Co O50 88.10(5) . . yes O30 Co O50 91.90(5) 2_576 . ? O50 Co O50 180 2_576 . ? N10 O10 Co 125.38(10) . . yes N30 O30 Co 128.74(10) . . yes N50 O50 Co 125.50(10) . . yes O10 N10 C11 121.19(14) . . ? O10 N10 C15 117.65(14) . . ? C11 N10 C15 121.16(14) . . ? O20 N20 C25 120.63(16) . . ? O20 N20 C21 119.87(16) . . ? C25 N20 C21 119.50(15) . . ? O30 N30 C35 121.87(13) . . ? O30 N30 C31 117.66(14) . . ? C35 N30 C31 120.44(15) . . ? O40 N40 C45 120.64(17) . . ? O40 N40 C41 121.08(17) . . ? C45 N40 C41 118.27(16) . . ? O50 N50 C51 121.33(14) . . ? O50 N50 C55 117.95(14) . . ? C51 N50 C55 120.70(15) . . ? O60 N60 C65 120.79(17) . . ? O60 N60 C61 120.39(18) . . ? C65 N60 C61 118.82(16) . . ? N10 C11 C12 120.01(16) . . ? C11 C12 C13 120.75(16) . . ? C12 C13 C14 117.03(15) . . ? C12 C13 C23 122.03(16) . . ? C14 C13 C23 120.91(15) . . ? C15 C14 C13 120.76(16) . . ? N10 C15 C14 120.16(16) . . ? N20 C21 C22 120.76(17) . . ? C21 C22 C23 121.09(17) . . ? C22 C23 C24 116.57(15) . . ? C22 C23 C13 121.69(16) . . ? C24 C23 C13 121.69(16) . . ? C25 C24 C23 121.02(17) . . ? N20 C25 C24 121.04(17) . . ? N30 C31 C32 120.54(16) . . ? C31 C32 C33 121.19(16) . . ? C34 C33 C32 116.34(15) . . ? C34 C33 C43 122.18(16) . . ? C32 C33 C43 121.37(15) . . ? C35 C34 C33 121.37(17) . . ? N30 C35 C34 119.99(15) . . ? N40 C41 C42 121.20(19) . . ? C41 C42 C43 121.55(19) . . ? C44 C43 C42 115.60(17) . . ? C44 C43 C33 120.72(16) . . ? C42 C43 C33 123.48(16) . . ? C45 C44 C43 121.18(18) . . ? N40 C45 C44 122.17(18) . . ? N50 C51 C52 120.01(16) . . ? C51 C52 C53 121.00(16) . . ? C54 C53 C52 116.93(15) . . ? C54 C53 C63 121.11(16) . . ? C52 C53 C63 121.96(15) . . ? C55 C54 C53 120.69(16) . . ? N50 C55 C54 120.62(15) . . ? N60 C61 C62 121.03(19) . . ? C61 C62 C63 121.34(18) . . ? C64 C63 C62 116.12(16) . . ? C64 C63 C53 122.10(17) . . ? C62 C63 C53 121.77(16) . . ? C65 C64 C63 120.97(19) . . ? N60 C65 C64 121.69(18) . . ? O1 N1 O2 124.9(3) . . ? O1 N1 O3 119.6(3) . . ? O2 N1 O3 115.4(3) . . ? O1 N1 O2' 110.9(5) . . ? O2 N1 O2' 39.4(4) . . ? O3 N1 O2' 112.3(5) . . ? O1 N1 O3' 105.9(5) . . ? O2 N1 O3' 91.4(5) . . ? O3 N1 O3' 75.1(5) . . ? O2' N1 O3' 129.9(6) . . ? _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.74 _refine_diff_density_min -0.39 _refine_diff_density_rms 0.09 #===END