# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 896261' #TrackingRef 'zhang.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Co3 N10 O10 S' _chemical_formula_weight 671.21 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.8097(11) _cell_length_b 20.6672(17) _cell_length_c 7.3626(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2101.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4945 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 28.01 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4478 _exptl_absorpt_correction_T_max 0.8844 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14747 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.47 _reflns_number_total 2588 _reflns_number_gt 2252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SAINT (Bruker, 2001)' _computing_publication_material 'SHELXL-97 (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^)+(0.0516P)^2^+3.4543P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2588 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.89887(3) 0.7500 -0.00978(6) 0.01329(13) Uani 1 2 d S . . Co2 Co 0.67212(2) 0.672519(17) 0.00374(4) 0.01492(12) Uani 1 1 d . . . S1 S 0.76310(6) 0.7500 0.33579(11) 0.0167(2) Uani 1 2 d S . . N1 N 0.92501(15) 0.39676(11) -0.3955(3) 0.0189(4) Uani 1 1 d . . . N2 N 0.95308(15) 0.60842(11) -0.1117(3) 0.0191(4) Uani 1 1 d . . . N3 N 0.88604(15) 0.64732(11) -0.0420(3) 0.0172(4) Uani 1 1 d . . . N4 N 0.80113(16) 0.61765(11) -0.0427(3) 0.0192(5) Uani 1 1 d . . . N5 N 0.81113(16) 0.55826(11) -0.1125(3) 0.0218(5) Uani 1 1 d . . . O1 O 0.7619(2) 0.7500 0.5352(4) 0.0269(6) Uani 1 2 d S . . O2 O 0.71224(14) 0.69139(9) 0.2717(3) 0.0228(4) Uani 1 1 d . . . O3 O 0.86356(19) 0.7500 0.2683(4) 0.0234(6) Uani 1 2 d S . . O4 O 0.75621(14) 0.7500 -0.0773(3) 0.0036(4) Uani 1 2 d S . . O5 O 0.57495(15) 0.7500 0.0298(3) 0.0083(4) Uani 1 2 d S . . C1 C 1.02178(19) 0.39022(13) -0.4093(4) 0.0212(5) Uani 1 1 d . . . H1A H 1.0466 0.3534 -0.4653 0.025 Uiso 1 1 calc R . . C2 C 1.08541(19) 0.43582(14) -0.3439(4) 0.0227(6) Uani 1 1 d . . . H2A H 1.1518 0.4299 -0.3563 0.027 Uiso 1 1 calc R . . C3 C 1.04961(19) 0.49042(13) -0.2594(4) 0.0202(5) Uani 1 1 d . . . H3A H 1.0914 0.5222 -0.2160 0.024 Uiso 1 1 calc R . . C4 C 0.94948(19) 0.49712(12) -0.2404(3) 0.0178(5) Uani 1 1 d . . . C5 C 0.89083(19) 0.44916(13) -0.3109(4) 0.0205(5) Uani 1 1 d . . . H5A H 0.8241 0.4536 -0.2989 0.025 Uiso 1 1 calc R . . C6 C 0.90504(18) 0.55426(12) -0.1538(3) 0.0176(5) Uani 1 1 d . . . O1W O 0.63507(18) 0.66015(12) -0.2672(3) 0.0292(5) Uani 1 1 d . . . O2W O 0.9338(2) 0.7500 -0.2855(4) 0.0278(7) Uani 1 2 d S . . O3W O 1.03657(19) 0.7500 0.0909(4) 0.0326(7) Uani 1 2 d S . . H1WA H 0.584(3) 0.648(2) -0.312(6) 0.046(11) Uiso 1 1 d . . . H1WB H 0.662(3) 0.680(2) -0.329(7) 0.055(15) Uiso 1 1 d . . . H2WA H 0.891(4) 0.7500 -0.330(7) 0.029(15) Uiso 1 2 d S . . H2WB H 0.996(4) 0.7500 -0.344(7) 0.09(2) Uiso 1 2 d S . . H3WA H 1.0820 0.7150 0.1204 0.104 Uiso 0.50 1 d PR . . H3WB H 0.9941 0.7450 0.1415 0.104 Uiso 0.50 1 d 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 0.0112(2) 0.0139(3) 0.0148(2) 0.000 0.00000(16) 0.000 Co2 0.0132(2) 0.0131(2) 0.0185(2) 0.00086(12) 0.00021(12) -0.00130(12) S1 0.0138(4) 0.0248(5) 0.0116(4) 0.000 -0.0002(3) 0.000 N1 0.0187(10) 0.0153(11) 0.0228(11) -0.0020(9) 0.0006(9) -0.0023(8) N2 0.0190(10) 0.0154(10) 0.0230(11) -0.0030(9) 0.0019(9) 0.0012(8) N3 0.0155(10) 0.0149(11) 0.0212(10) -0.0020(9) 0.0017(8) 0.0007(8) N4 0.0183(10) 0.0138(11) 0.0255(11) -0.0025(9) -0.0002(9) -0.0004(8) N5 0.0194(11) 0.0164(11) 0.0297(12) -0.0042(9) 0.0012(9) 0.0006(9) O1 0.0246(14) 0.0413(18) 0.0149(13) 0.000 -0.0005(11) 0.000 O2 0.0251(10) 0.0247(10) 0.0187(9) 0.0047(8) -0.0020(8) -0.0047(8) O3 0.0165(13) 0.0373(16) 0.0164(12) 0.000 0.0003(10) 0.000 O4 0.0018(9) 0.0022(9) 0.0069(10) 0.000 0.0001(7) 0.000 O5 0.0033(9) 0.0081(11) 0.0135(10) 0.000 -0.0010(8) 0.000 C1 0.0204(12) 0.0167(13) 0.0265(13) -0.0044(10) 0.0013(10) 0.0028(10) C2 0.0180(12) 0.0228(14) 0.0274(14) -0.0027(11) -0.0002(11) 0.0019(10) C3 0.0188(12) 0.0174(12) 0.0245(13) -0.0021(10) -0.0028(10) -0.0023(10) C4 0.0212(13) 0.0130(12) 0.0192(12) 0.0011(10) 0.0004(10) -0.0001(10) C5 0.0167(12) 0.0176(13) 0.0272(13) -0.0029(10) 0.0012(10) -0.0001(10) C6 0.0188(12) 0.0146(12) 0.0195(12) -0.0004(10) 0.0002(10) -0.0005(9) O1W 0.0278(12) 0.0383(13) 0.0214(10) 0.0031(10) -0.0039(9) -0.0107(10) O2W 0.0170(15) 0.049(2) 0.0178(14) 0.000 0.0003(12) 0.000 O3W 0.0130(13) 0.052(2) 0.0335(17) 0.000 -0.0042(12) 0.000 _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 2.032(2) . ? Co1 O3W 2.041(3) . ? Co1 O2W 2.087(3) . ? Co1 O3 2.104(3) . ? Co1 N3 2.143(2) . ? Co1 N3 2.143(2) 7_575 ? Co1 H3WB 1.7262 . ? Co2 O4 2.0661(13) . ? Co2 O1W 2.075(2) . ? Co2 O2 2.0856(19) . ? Co2 N1 2.097(2) 2_665 ? Co2 O5 2.0981(14) . ? Co2 N4 2.139(2) . ? S1 O1 1.468(3) . ? S1 O3 1.474(3) . ? S1 O2 1.478(2) . ? S1 O2 1.478(2) 7_575 ? N1 C5 1.335(3) . ? N1 C1 1.347(3) . ? N1 Co2 2.097(2) 2_664 ? N2 N3 1.329(3) . ? N2 C6 1.337(3) . ? N3 N4 1.323(3) . ? N4 N5 1.338(3) . ? N5 C6 1.335(3) . ? O4 Co2 2.0661(13) 7_575 ? O5 Co2 2.0981(14) 7_575 ? C1 C2 1.376(4) . ? C1 H1A 0.9300 . ? C2 C3 1.380(4) . ? C2 H2A 0.9300 . ? C3 C4 1.397(4) . ? C3 H3A 0.9300 . ? C4 C5 1.381(4) . ? C4 C6 1.476(3) . ? C5 H5A 0.9300 . ? O1W H1WA 0.82(4) . ? O1W H1WB 0.72(5) . ? O2W H2WA 0.67(5) . ? O2W H2WB 0.96(6) . ? O3W H3WA 0.9828 . ? O3W H3WB 0.7023 . ? 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 O3W 172.86(11) . . ? O4 Co1 O2W 89.19(11) . . ? O3W Co1 O2W 97.95(13) . . ? O4 Co1 O3 90.77(9) . . ? O3W Co1 O3 82.10(12) . . ? O2W Co1 O3 179.96(11) . . ? O4 Co1 N3 83.84(6) . . ? O3W Co1 N3 96.73(6) . . ? O2W Co1 N3 84.91(6) . . ? O3 Co1 N3 95.08(6) . . ? O4 Co1 N3 83.84(6) . 7_575 ? O3W Co1 N3 96.73(6) . 7_575 ? O2W Co1 N3 84.91(6) . 7_575 ? O3 Co1 N3 95.08(6) . 7_575 ? N3 Co1 N3 164.11(12) . 7_575 ? O4 Co1 H3WB 153.7 . . ? O3W Co1 H3WB 19.3 . . ? O2W Co1 H3WB 116.9 . . ? O3 Co1 H3WB 63.2 . . ? N3 Co1 H3WB 94.3 . . ? N3 Co1 H3WB 101.2 7_575 . ? O4 Co2 O1W 87.51(9) . . ? O4 Co2 O2 88.79(8) . . ? O1W Co2 O2 176.08(9) . . ? O4 Co2 N1 172.15(8) . 2_665 ? O1W Co2 N1 95.63(9) . 2_665 ? O2 Co2 N1 87.88(8) . 2_665 ? O4 Co2 O5 78.14(6) . . ? O1W Co2 O5 91.39(9) . . ? O2 Co2 O5 86.59(8) . . ? N1 Co2 O5 94.56(8) 2_665 . ? O4 Co2 N4 84.06(8) . . ? O1W Co2 N4 89.22(9) . . ? O2 Co2 N4 91.66(8) . . ? N1 Co2 N4 103.14(9) 2_665 . ? O5 Co2 N4 162.14(8) . . ? O1 S1 O3 110.33(16) . . ? O1 S1 O2 108.32(10) . . ? O3 S1 O2 109.86(10) . . ? O1 S1 O2 108.32(10) . 7_575 ? O3 S1 O2 109.86(10) . 7_575 ? O2 S1 O2 110.12(16) . 7_575 ? C5 N1 C1 117.9(2) . . ? C5 N1 Co2 119.50(17) . 2_664 ? C1 N1 Co2 122.63(18) . 2_664 ? N3 N2 C6 104.5(2) . . ? N4 N3 N2 109.6(2) . . ? N4 N3 Co1 122.18(16) . . ? N2 N3 Co1 125.76(17) . . ? N3 N4 N5 109.6(2) . . ? N3 N4 Co2 119.46(17) . . ? N5 N4 Co2 129.32(17) . . ? C6 N5 N4 104.2(2) . . ? S1 O2 Co2 125.57(11) . . ? S1 O3 Co1 123.11(16) . . ? Co1 O4 Co2 118.31(6) . . ? Co1 O4 Co2 118.31(6) . 7_575 ? Co2 O4 Co2 101.62(9) . 7_575 ? Co2 O5 Co2 99.50(9) 7_575 . ? N1 C1 C2 122.6(2) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 118.1(2) . . ? C5 C4 C6 119.5(2) . . ? C3 C4 C6 122.3(2) . . ? N1 C5 C4 123.4(2) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? N5 C6 N2 112.2(2) . . ? N5 C6 C4 123.5(2) . . ? N2 C6 C4 124.3(2) . . ? Co2 O1W H1WA 130(3) . . ? Co2 O1W H1WB 114(4) . . ? H1WA O1W H1WB 112(5) . . ? Co1 O2W H2WA 106(5) . . ? Co1 O2W H2WB 130(3) . . ? H2WA O2W H2WB 124(6) . . ? Co1 O3W H3WA 132.5 . . ? Co1 O3W H3WB 54.1 . . ? H3WA O3W H3WB 107.9 . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.929 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.115 data_2 _database_code_depnum_ccdc_archive 'CCDC 896262' #TrackingRef 'zhang.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Co2 N4 O7' _chemical_formula_weight 394.08 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 6.4307(13) _cell_length_b 6.8381(14) _cell_length_c 15.023(3) _cell_angle_alpha 81.520(3) _cell_angle_beta 82.013(4) _cell_angle_gamma 62.680(3) _cell_volume 578.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1215 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 27.44 _exptl_crystal_description sheet _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 2.912 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6692 _exptl_absorpt_correction_T_max 0.8924 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3127 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2402 _reflns_number_gt 1947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (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^)+(0.1598P)^2^+3.7179P] 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 2402 _refine_ls_number_parameters 193 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.2485 _refine_ls_wR_factor_gt 0.1964 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.059 _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 0.21854(19) 0.71741(18) 0.29409(7) 0.0164(4) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.5000 0.0120(4) Uani 1 2 d S . . Co3 Co 0.0000 1.0000 0.5000 0.0124(4) Uani 1 2 d S . . O1 O 0.1124(8) 0.7243(8) 0.4321(3) 0.0044(9) Uani 1 1 d U . . O2 O 0.3353(12) 0.7193(12) 0.1630(4) 0.0268(14) Uani 1 1 d . . . O3 O 0.7016(11) 0.6610(12) 0.1797(4) 0.0279(15) Uani 1 1 d . . . O1W O -0.3075(9) 0.6893(9) 0.4466(4) 0.0122(11) Uani 1 1 d . . . H1WA H -0.2822 0.7596 0.3982 0.015 Uiso 1 1 d R . . H1WB H -0.3589 0.6047 0.4322 0.015 Uiso 1 1 d R . . O2W O 0.5565(11) 0.5356(10) 0.3369(4) 0.0215(13) Uani 1 1 d . . . H2WA H 0.5748 0.4119 0.3648 0.026 Uiso 1 1 d R . . H2WB H 0.6566 0.5188 0.2917 0.026 Uiso 1 1 d R . . O3W O -0.1376(10) 0.8751(10) 0.2786(4) 0.0228(13) Uani 1 1 d . . . H3WA H -0.2000 0.9129 0.2286 0.027 Uiso 1 1 d R . . H3WB H -0.2067 0.9791 0.3128 0.027 Uiso 1 1 d R . . O4W O -0.3184(10) 1.1359(9) 0.4418(4) 0.0202(13) Uani 1 1 d . . . H4WA H -0.3538 1.0323 0.4377 0.024 Uiso 1 1 d R . . H4WB H -0.4236 1.2231 0.4774 0.024 Uiso 1 1 d R . . N1 N 0.7945(12) 0.6169(11) -0.3011(4) 0.0153(14) Uani 1 1 d . . . N2 N 0.8663(12) 0.6772(11) -0.3842(4) 0.0165(14) Uani 1 1 d . . . N3 N 0.8660(12) 0.8692(11) -0.3849(4) 0.0134(13) Uani 1 1 d U . . N4 N 0.7912(12) 0.9433(11) -0.3025(4) 0.0158(14) Uani 1 1 d . . . C1 C 0.5366(16) 0.7040(14) 0.1321(6) 0.0207(17) Uani 1 1 d . . . C2 C 0.5882(15) 0.7339(13) 0.0324(5) 0.0151(16) Uani 1 1 d . . . C3 C 0.4280(16) 0.7513(13) -0.0273(6) 0.0201(18) Uani 1 1 d . . . H3 H 0.2869 0.7496 -0.0043 0.024 Uiso 1 1 calc R . . C4 C 0.4785(15) 0.7708(14) -0.1193(6) 0.0187(17) Uani 1 1 d . . . H4 H 0.3731 0.7798 -0.1581 0.022 Uiso 1 1 calc R . . C5 C 0.6871(15) 0.7771(14) -0.1539(5) 0.0171(16) Uani 1 1 d . . . C6 C 0.8400(16) 0.7666(16) -0.0954(6) 0.0249(19) Uani 1 1 d . . . H6 H 0.9774 0.7755 -0.1189 0.030 Uiso 1 1 calc R . . C7 C 0.7940(13) 0.7429(15) -0.0019(6) 0.0186(17) Uani 1 1 d . . . H7 H 0.9004 0.7334 0.0366 0.022 Uiso 1 1 calc R . . C8 C 0.7563(13) 0.7813(14) -0.2525(5) 0.0143(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0194(6) 0.0183(6) 0.0118(6) -0.0019(4) 0.0010(4) -0.0092(5) Co2 0.0157(8) 0.0121(7) 0.0096(7) -0.0027(5) 0.0013(5) -0.0077(6) Co3 0.0175(8) 0.0107(7) 0.0101(7) -0.0020(5) 0.0017(5) -0.0078(6) O1 0.0083(16) 0.0032(16) 0.0035(16) -0.0010(13) 0.0020(13) -0.0045(13) O2 0.032(4) 0.037(4) 0.018(3) -0.004(3) 0.006(3) -0.022(3) O3 0.029(3) 0.040(4) 0.015(3) -0.004(3) -0.001(3) -0.016(3) O1W 0.012(2) 0.017(3) 0.010(3) -0.003(2) -0.0053(19) -0.007(2) O2W 0.029(3) 0.024(3) 0.014(3) 0.002(2) -0.001(2) -0.014(3) O3W 0.020(3) 0.025(3) 0.021(3) -0.006(3) -0.001(2) -0.008(3) O4W 0.022(3) 0.011(3) 0.024(3) 0.000(2) -0.004(2) -0.004(2) N1 0.020(3) 0.017(3) 0.007(3) 0.001(3) 0.000(2) -0.008(3) N2 0.025(4) 0.012(3) 0.012(3) -0.001(2) 0.001(3) -0.008(3) N3 0.023(3) 0.013(3) 0.003(3) 0.002(2) 0.001(2) -0.009(3) N4 0.020(3) 0.018(3) 0.008(3) -0.005(3) 0.001(3) -0.007(3) C1 0.025(4) 0.016(4) 0.024(5) -0.002(3) -0.003(3) -0.011(3) C2 0.026(4) 0.009(3) 0.008(4) 0.001(3) -0.002(3) -0.007(3) C3 0.029(4) 0.007(4) 0.024(4) 0.004(3) 0.001(4) -0.010(3) C4 0.024(4) 0.023(4) 0.017(4) -0.002(3) -0.004(3) -0.016(4) C5 0.028(4) 0.022(4) 0.008(4) 0.001(3) -0.003(3) -0.016(4) C6 0.025(4) 0.032(5) 0.020(4) -0.004(4) 0.000(3) -0.015(4) C7 0.005(3) 0.031(5) 0.020(4) -0.006(3) -0.001(3) -0.007(3) C8 0.011(3) 0.026(4) 0.007(3) -0.006(3) 0.003(3) -0.009(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 O2 2.009(6) . ? Co1 O3W 2.067(6) . ? Co1 O2W 2.087(6) . ? Co1 O1 2.091(5) . ? Co1 N1 2.312(7) 2_665 ? Co1 N4 2.314(7) 2_675 ? Co2 O1W 2.004(5) . ? Co2 O1W 2.004(5) 2_566 ? Co2 O1 2.066(5) . ? Co2 O1 2.066(5) 2_566 ? Co2 N2 2.118(7) 2_665 ? Co2 N2 2.118(7) 1_456 ? Co3 O1 2.057(5) . ? Co3 O1 2.057(5) 2_576 ? Co3 O4W 2.082(6) 2_576 ? Co3 O4W 2.082(6) . ? Co3 N3 2.091(6) 1_456 ? Co3 N3 2.091(6) 2_675 ? O2 C1 1.275(11) . ? O3 C1 1.259(11) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8501 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8501 . ? N1 C8 1.340(11) . ? N1 N2 1.343(9) . ? N1 Co1 2.312(7) 2_665 ? N2 N3 1.311(10) . ? N2 Co2 2.118(7) 1_654 ? N3 N4 1.348(9) . ? N3 Co3 2.091(6) 1_654 ? N4 C8 1.333(11) . ? N4 Co1 2.314(7) 2_675 ? C1 C2 1.493(12) . ? C2 C7 1.377(11) . ? C2 C3 1.412(13) . ? C3 C4 1.376(12) . ? C3 H3 0.9300 . ? C4 C5 1.387(11) . ? C4 H4 0.9300 . ? C5 C6 1.378(12) . ? C5 C8 1.486(11) . ? C6 C7 1.397(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O3W 98.3(3) . . ? O2 Co1 O2W 93.2(3) . . ? O3W Co1 O2W 167.8(2) . . ? O2 Co1 O1 176.1(2) . . ? O3W Co1 O1 84.2(2) . . ? O2W Co1 O1 84.5(2) . . ? O2 Co1 N1 94.8(3) . 2_665 ? O3W Co1 N1 88.5(2) . 2_665 ? O2W Co1 N1 86.6(2) . 2_665 ? O1 Co1 N1 88.2(2) . 2_665 ? O2 Co1 N4 91.3(3) . 2_675 ? O3W Co1 N4 89.4(2) . 2_675 ? O2W Co1 N4 94.3(2) . 2_675 ? O1 Co1 N4 85.7(2) . 2_675 ? N1 Co1 N4 173.7(2) 2_665 2_675 ? O1W Co2 O1W 179.999(1) . 2_566 ? O1W Co2 O1 86.7(2) . . ? O1W Co2 O1 93.3(2) 2_566 . ? O1W Co2 O1 93.3(2) . 2_566 ? O1W Co2 O1 86.7(2) 2_566 2_566 ? O1 Co2 O1 180.0 . 2_566 ? O1W Co2 N2 90.9(2) . 2_665 ? O1W Co2 N2 89.1(2) 2_566 2_665 ? O1 Co2 N2 86.9(2) . 2_665 ? O1 Co2 N2 93.1(2) 2_566 2_665 ? O1W Co2 N2 89.1(2) . 1_456 ? O1W Co2 N2 90.9(2) 2_566 1_456 ? O1 Co2 N2 93.1(2) . 1_456 ? O1 Co2 N2 86.9(2) 2_566 1_456 ? N2 Co2 N2 179.999(1) 2_665 1_456 ? O1 Co3 O1 180.000(2) . 2_576 ? O1 Co3 O4W 90.6(2) . 2_576 ? O1 Co3 O4W 89.4(2) 2_576 2_576 ? O1 Co3 O4W 89.4(2) . . ? O1 Co3 O4W 90.6(2) 2_576 . ? O4W Co3 O4W 179.999(1) 2_576 . ? O1 Co3 N3 94.0(2) . 1_456 ? O1 Co3 N3 86.0(2) 2_576 1_456 ? O4W Co3 N3 88.1(2) 2_576 1_456 ? O4W Co3 N3 91.9(2) . 1_456 ? O1 Co3 N3 86.0(2) . 2_675 ? O1 Co3 N3 94.0(2) 2_576 2_675 ? O4W Co3 N3 91.9(2) 2_576 2_675 ? O4W Co3 N3 88.1(2) . 2_675 ? N3 Co3 N3 180.0(4) 1_456 2_675 ? Co3 O1 Co2 112.1(2) . . ? Co3 O1 Co1 123.5(2) . . ? Co2 O1 Co1 121.2(2) . . ? C1 O2 Co1 125.4(6) . . ? Co2 O1W H1WA 108.1 . . ? Co2 O1W H1WB 108.1 . . ? H1WA O1W H1WB 107.4 . . ? Co1 O2W H2WA 111.4 . . ? Co1 O2W H2WB 109.4 . . ? H2WA O2W H2WB 111.4 . . ? Co1 O3W H3WA 125.7 . . ? Co1 O3W H3WB 110.1 . . ? H3WA O3W H3WB 110.2 . . ? Co3 O4W H4WA 108.4 . . ? Co3 O4W H4WB 108.0 . . ? H4WA O4W H4WB 107.4 . . ? C8 N1 N2 104.2(6) . . ? C8 N1 Co1 143.7(5) . 2_665 ? N2 N1 Co1 112.0(5) . 2_665 ? N3 N2 N1 109.5(6) . . ? N3 N2 Co2 120.1(5) . 1_654 ? N1 N2 Co2 130.1(5) . 1_654 ? N2 N3 N4 109.9(6) . . ? N2 N3 Co3 120.1(5) . 1_654 ? N4 N3 Co3 129.7(5) . 1_654 ? C8 N4 N3 103.9(6) . . ? C8 N4 Co1 142.4(5) . 2_675 ? N3 N4 Co1 113.6(5) . 2_675 ? O3 C1 O2 124.8(8) . . ? O3 C1 C2 116.0(8) . . ? O2 C1 C2 119.1(8) . . ? C7 C2 C3 119.6(8) . . ? C7 C2 C1 120.0(7) . . ? C3 C2 C1 120.4(8) . . ? C4 C3 C2 120.7(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.8(8) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 119.3(8) . . ? C6 C5 C8 119.1(8) . . ? C4 C5 C8 121.4(7) . . ? C5 C6 C7 121.8(8) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C2 C7 C6 118.8(7) . . ? C2 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? N4 C8 N1 112.3(7) . . ? N4 C8 C5 124.9(7) . . ? N1 C8 C5 122.8(7) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.434 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.301 data_3 _database_code_depnum_ccdc_archive 'CCDC 896263' #TrackingRef 'zhang.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H2 Co N4 O' _chemical_formula_weight 144.99 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 P4(2)/nmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 9.6822(3) _cell_length_b 9.6822(3) _cell_length_c 7.4882(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 701.98(6) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1251 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.93 _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 4.710 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3977 _exptl_absorpt_correction_T_max 0.7044 _exptl_absorpt_process_details 'SADBAS, Sheldrick 1997' _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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3893 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.97 _reflns_number_total 435 _reflns_number_gt 363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SAINT (Bruker, 2001)' _computing_publication_material 'SHELXL-97 (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^)+(0.0662P)^2^+1.2072P] 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 435 _refine_ls_number_parameters 36 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 0.43223(5) 0.56777(5) 0.2500 0.0152(3) Uani 1 2 d S . . O1 O 0.2500 0.5760(3) 0.1298(4) 0.0136(7) Uani 1 2 d S . . N1 N 0.4859(3) 0.3178(3) -0.0228(4) 0.0183(6) Uani 1 1 d . . . N2 N 0.4617(3) 0.3631(3) 0.1432(4) 0.0215(7) Uani 1 1 d . . . C1 C 0.4484(6) 0.2500 0.2416(7) 0.0231(12) Uani 1 2 d S . . H1A H 0.4318 0.2500 0.3640 0.028 Uiso 1 2 calc SR . . 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 0.0138(4) 0.0138(4) 0.0180(5) 0.00021(16) 0.00021(16) 0.0003(2) O1 0.0051(14) 0.0246(17) 0.0112(14) 0.0016(12) 0.000 0.000 N1 0.0196(14) 0.0156(14) 0.0196(15) -0.0015(11) -0.0003(12) -0.0001(11) N2 0.0250(15) 0.0175(14) 0.0219(15) -0.0013(12) 0.0017(13) 0.0003(12) C1 0.035(3) 0.022(3) 0.013(2) 0.000 0.0033(19) 0.000 _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 1.9825(14) 12_666 ? Co1 O1 1.9825(15) . ? Co1 N2 2.156(3) 8_665 ? Co1 N2 2.156(3) . ? Co1 N1 2.180(3) 9_665 ? Co1 N1 2.180(3) 16_556 ? O1 Co1 1.9825(14) 11_566 ? N1 N1 1.312(5) 13_565 ? N1 N2 1.339(4) . ? N1 Co1 2.180(3) 9_665 ? N2 C1 1.326(4) . ? C1 N2 1.326(4) 13_565 ? C1 H1A 0.9300 . ? 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 97.73(17) 12_666 . ? O1 Co1 N2 89.21(12) 12_666 8_665 ? O1 Co1 N2 172.70(11) . 8_665 ? O1 Co1 N2 172.70(11) 12_666 . ? O1 Co1 N2 89.21(12) . . ? N2 Co1 N2 83.95(16) 8_665 . ? O1 Co1 N1 85.22(10) 12_666 9_665 ? O1 Co1 N1 87.05(11) . 9_665 ? N2 Co1 N1 91.29(11) 8_665 9_665 ? N2 Co1 N1 97.46(11) . 9_665 ? O1 Co1 N1 87.05(11) 12_666 16_556 ? O1 Co1 N1 85.22(10) . 16_556 ? N2 Co1 N1 97.46(11) 8_665 16_556 ? N2 Co1 N1 91.29(11) . 16_556 ? N1 Co1 N1 168.24(14) 9_665 16_556 ? Co1 O1 Co1 125.75(16) . 11_566 ? N1 N1 N2 109.14(17) 13_565 . ? N1 N1 Co1 120.56(7) 13_565 9_665 ? N2 N1 Co1 128.4(2) . 9_665 ? C1 N2 N1 105.2(3) . . ? C1 N2 Co1 122.7(3) . . ? N1 N2 Co1 132.0(2) . . ? N2 C1 N2 111.3(4) 13_565 . ? N2 C1 H1A 124.3 13_565 . ? N2 C1 H1A 124.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.957 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.140 #============================================================