# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rao, Chintamani Nagesa Ramachandra' _publ_contact_author_email cnrrao@jncasr.ac.in _publ_section_title ; Organically-Templated Kagom\~A Compounds Containing TwoTransition Metal Ions ; _publ_author_name C.N.R.Rao # Attachment '- Compound1.cif' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 768970' #TrackingRef '- Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H8 Co2 F6 N4 Ni O8 S2' _chemical_formula_sum 'C4 H8 Co2 F6 N4 Ni O8 S2' _chemical_formula_weight 594.83 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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 '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 Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.7299(12) _cell_length_b 7.3839(8) _cell_length_c 9.7260(16) _cell_angle_alpha 90.00 _cell_angle_beta 118.782(5) _cell_angle_gamma 90.00 _cell_volume 801.26(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.4 _exptl_crystal_description Rhambohedral _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 3.582 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.659027 _exptl_absorpt_correction_T_max 0.9623 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4459 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.44 _reflns_number_total 988 _reflns_number_gt 898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+5.0530P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 988 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.5000 0.0141(2) Uani 1 2 d S . . Ni1 Ni 0.0000 0.0000 0.5000 0.0112(2) Uani 1 4 d S . . S1 S 0.27482(10) 0.0000 0.78424(13) 0.0124(3) Uani 1 2 d S . . O3 O 0.3383(3) 0.0000 0.9563(4) 0.0170(7) Uani 1 2 d S . . O1 O 0.1447(3) 0.0000 0.7242(4) 0.0237(9) Uani 1 2 d S . . O2 O 0.3097(3) 0.1635(5) 0.7282(3) 0.0372(8) Uani 1 1 d . . . F1 F 0.07556(18) 0.1972(3) 0.4317(3) 0.0230(5) Uani 1 1 d . . . F2 F 0.2741(3) 0.0000 0.4306(3) 0.0209(7) Uani 1 2 d S . . N1 N 0.490(3) 0.3067(12) 0.989(4) 0.039(5) Uani 0.50 1 d P . . C1 C 0.4298 0.4015 1.0460 0.0486(15) Uani 1 1 d . . . N2 N -0.0654(4) 0.5000 0.3091(5) 0.0165(8) Uani 1 2 d S . . H4 H -0.0944 0.5000 0.2091 0.020 Uiso 1 2 d SR . . H1 H -0.0208 0.5909 0.3430 0.020 Uiso 0.50 1 d PR . . H2 H -0.0270 0.5000 0.4108 0.020 Uiso 1 2 d SR . . H3 H -0.1177 0.5636 0.3214 0.020 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 0.0122(3) 0.0127(4) 0.0193(3) 0.0052(2) 0.0090(3) -0.0008(2) Ni1 0.0112(4) 0.0056(4) 0.0178(4) 0.000 0.0077(3) 0.000 S1 0.0132(5) 0.0088(6) 0.0154(5) 0.000 0.0070(4) 0.000 O3 0.0226(18) 0.0136(18) 0.0173(16) 0.000 0.0117(14) 0.000 O1 0.0107(16) 0.043(3) 0.0159(16) 0.000 0.0050(13) 0.000 O2 0.0402(17) 0.035(2) 0.0215(13) 0.0075(12) 0.0034(12) -0.0276(15) F1 0.0143(9) 0.0161(11) 0.0363(12) 0.0112(10) 0.0104(9) -0.0025(9) F2 0.0223(15) 0.0220(17) 0.0251(15) 0.000 0.0168(13) 0.000 N1 0.030(10) 0.025(3) 0.062(9) 0.028(8) 0.022(8) 0.001(6) C1 0.066(3) 0.035(3) 0.081(4) -0.018(3) 0.064(3) -0.023(3) N2 0.019(2) 0.011(2) 0.022(2) 0.000 0.0116(17) 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 F1 2.026(2) 7_556 ? Co1 F1 2.026(2) . ? Co1 F2 2.0387(12) . ? Co1 F2 2.0387(12) 7_556 ? Co1 O2 2.070(3) 7_556 ? Co1 O2 2.070(3) . ? Ni1 F1 2.025(2) 6 ? Ni1 F1 2.025(2) . ? Ni1 F1 2.025(2) 5_556 ? Ni1 F1 2.025(2) 2_556 ? Ni1 O1 2.069(3) . ? Ni1 O1 2.069(3) 5_556 ? S1 O3 1.467(4) . ? S1 O1 1.468(4) . ? S1 O2 1.478(3) 6 ? S1 O2 1.478(3) . ? F2 Co1 2.0387(12) 4_546 ? N1 N1 0.25(7) 2_657 ? N1 C1 1.34(3) . ? N1 C1 1.41(3) 2_657 ? C1 N1 1.41(3) 2_657 ? C1 C1 1.45517(16) 6_565 ? 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 F1 Co1 F1 180.0 7_556 . ? F1 Co1 F2 88.12(11) 7_556 . ? F1 Co1 F2 91.88(11) . . ? F1 Co1 F2 91.88(11) 7_556 7_556 ? F1 Co1 F2 88.12(11) . 7_556 ? F2 Co1 F2 180.00(17) . 7_556 ? F1 Co1 O2 94.06(11) 7_556 7_556 ? F1 Co1 O2 85.94(11) . 7_556 ? F2 Co1 O2 87.74(13) . 7_556 ? F2 Co1 O2 92.26(13) 7_556 7_556 ? F1 Co1 O2 85.94(11) 7_556 . ? F1 Co1 O2 94.06(11) . . ? F2 Co1 O2 92.26(13) . . ? F2 Co1 O2 87.74(13) 7_556 . ? O2 Co1 O2 180.00(8) 7_556 . ? F1 Ni1 F1 91.93(14) 6 . ? F1 Ni1 F1 88.07(14) 6 5_556 ? F1 Ni1 F1 180.00(10) . 5_556 ? F1 Ni1 F1 180.00(12) 6 2_556 ? F1 Ni1 F1 88.07(14) . 2_556 ? F1 Ni1 F1 91.93(14) 5_556 2_556 ? F1 Ni1 O1 91.34(9) 6 . ? F1 Ni1 O1 91.34(9) . . ? F1 Ni1 O1 88.66(9) 5_556 . ? F1 Ni1 O1 88.66(9) 2_556 . ? F1 Ni1 O1 88.66(9) 6 5_556 ? F1 Ni1 O1 88.66(9) . 5_556 ? F1 Ni1 O1 91.34(9) 5_556 5_556 ? F1 Ni1 O1 91.34(9) 2_556 5_556 ? O1 Ni1 O1 180.0 . 5_556 ? O3 S1 O1 110.5(2) . . ? O3 S1 O2 108.82(14) . 6 ? O1 S1 O2 109.59(16) . 6 ? O3 S1 O2 108.82(14) . . ? O1 S1 O2 109.59(16) . . ? O2 S1 O2 109.5(3) 6 . ? S1 O1 Ni1 132.9(2) . . ? S1 O2 Co1 128.84(18) . . ? Ni1 F1 Co1 130.51(11) . . ? Co1 F2 Co1 129.77(14) . 4_546 ? N1 N1 C1 101(10) 2_657 . ? N1 N1 C1 69(10) 2_657 2_657 ? C1 N1 C1 117.8(8) . 2_657 ? N1 C1 N1 10(3) . 2_657 ? N1 C1 C1 121.5(6) . 6_565 ? N1 C1 C1 119.8(8) 2_657 6_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.266 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.148 # Attachment '- Compound2.cif' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 768971' #TrackingRef '- Compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H8 Co F6 N4 Ni2 O8 S2' _chemical_formula_sum 'C4 H8 Co F6 N4 Ni2 O8 S2' _chemical_formula_weight 594.61 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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 '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 Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.7062(13) _cell_length_b 7.3347(7) _cell_length_c 9.5851(10) _cell_angle_alpha 90.00 _cell_angle_beta 116.427(7) _cell_angle_gamma 90.00 _cell_volume 799.95(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.9 _exptl_crystal_description Rhambohedral _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 3.728 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.42599 _exptl_absorpt_correction_T_max 0.9248 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4205 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.92 _reflns_number_total 831 _reflns_number_gt 778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+12.0035P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 831 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.2500 0.2500 0.5000 0.0206(3) Uani 1 2 d S . . Co1 Co 0.5000 0.5000 0.5000 0.0173(4) Uani 1 4 d S . . S1 S 0.23874(18) 0.5000 0.2183(2) 0.0231(5) Uani 1 2 d S . . F1 F 0.4216(3) 0.3028(4) 0.5684(4) 0.0250(7) Uani 1 1 d . . . F2 F 0.2752(4) 0.0000 0.4308(5) 0.0238(10) Uani 1 2 d S . . O1 O 0.3667(5) 0.5000 0.2758(6) 0.0348(15) Uani 1 2 d S . . O2 O 0.2038(4) 0.3375(6) 0.2750(4) 0.0368(11) Uani 1 1 d . . . O3 O 0.1817(5) 0.5000 0.0468(6) 0.0323(14) Uani 1 2 d S . . C1 C -0.0978(11) 0.0952(18) -0.0064(17) 0.106(5) Uani 1 1 d . . . N1 N 0.000(4) 0.182(3) 0.035(5) 0.123(16) Uani 0.50 1 d P . . N2 N 0.5625(5) 0.0000 0.6910(7) 0.0231(15) Uani 1 2 d S . . H2 H 0.6062 0.0000 0.6689 0.028 Uiso 1 2 d SR . . H3 H 0.5943 0.0000 0.7841 0.028 Uiso 1 2 d SR . . H1 H 0.5248 -0.1077 0.6666 0.028 Uiso 1 1 d 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 0.0226(5) 0.0202(5) 0.0211(5) 0.0029(4) 0.0117(4) 0.0016(4) Co1 0.0163(7) 0.0183(7) 0.0151(7) 0.000 0.0048(6) 0.000 S1 0.0254(10) 0.0282(11) 0.0121(9) 0.000 0.0051(8) 0.000 F1 0.0225(16) 0.0251(17) 0.0272(16) 0.0063(14) 0.0108(13) 0.0026(13) F2 0.026(2) 0.024(2) 0.027(2) 0.000 0.016(2) 0.000 O1 0.022(3) 0.066(4) 0.017(3) 0.000 0.008(2) 0.000 O2 0.048(3) 0.036(3) 0.020(2) 0.0037(19) 0.0091(19) -0.013(2) O3 0.034(3) 0.047(4) 0.010(3) 0.000 0.005(2) 0.000 C1 0.077(8) 0.109(11) 0.137(11) 0.042(8) 0.051(8) 0.031(7) N1 0.116(15) 0.071(11) 0.14(4) -0.035(16) 0.02(2) 0.061(16) N2 0.020(3) 0.026(4) 0.022(3) 0.000 0.008(3) 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 Ni1 F1 2.016(3) 7_556 ? Ni1 F1 2.016(3) . ? Ni1 F2 2.0233(18) 7_556 ? Ni1 F2 2.0233(18) . ? Ni1 O2 2.069(4) . ? Ni1 O2 2.069(4) 7_556 ? Co1 F1 2.023(3) 6_565 ? Co1 F1 2.023(3) . ? Co1 F1 2.023(3) 5_666 ? Co1 F1 2.023(3) 2_656 ? Co1 O1 2.061(5) . ? Co1 O1 2.061(5) 5_666 ? S1 O2 1.459(4) 6_565 ? S1 O2 1.459(4) . ? S1 O1 1.466(6) . ? S1 O3 1.472(5) . ? F2 Ni1 2.0233(18) 4_546 ? C1 N1 1.29(4) . ? C1 C1 1.40(3) 6 ? C1 N1 1.53(4) 2 ? N1 N1 0.68(8) 2 ? N1 C1 1.53(4) 2 ? N2 H2 0.6768 . ? N2 H3 0.7985 . ? N2 H1 0.8993 . ? 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 F1 Ni1 F1 180.00(7) 7_556 . ? F1 Ni1 F2 88.57(15) 7_556 7_556 ? F1 Ni1 F2 91.43(15) . 7_556 ? F1 Ni1 F2 91.43(15) 7_556 . ? F1 Ni1 F2 88.57(15) . . ? F2 Ni1 F2 180.0 7_556 . ? F1 Ni1 O2 87.51(15) 7_556 . ? F1 Ni1 O2 92.49(15) . . ? F2 Ni1 O2 92.74(17) 7_556 . ? F2 Ni1 O2 87.26(17) . . ? F1 Ni1 O2 92.49(15) 7_556 7_556 ? F1 Ni1 O2 87.51(15) . 7_556 ? F2 Ni1 O2 87.26(17) 7_556 7_556 ? F2 Ni1 O2 92.74(17) . 7_556 ? O2 Ni1 O2 180.000(1) . 7_556 ? F1 Co1 F1 91.23(18) 6_565 . ? F1 Co1 F1 88.77(18) 6_565 5_666 ? F1 Co1 F1 180.00(12) . 5_666 ? F1 Co1 F1 180.000(1) 6_565 2_656 ? F1 Co1 F1 88.77(18) . 2_656 ? F1 Co1 F1 91.23(18) 5_666 2_656 ? F1 Co1 O1 92.49(14) 6_565 . ? F1 Co1 O1 92.49(14) . . ? F1 Co1 O1 87.51(14) 5_666 . ? F1 Co1 O1 87.51(14) 2_656 . ? F1 Co1 O1 87.51(14) 6_565 5_666 ? F1 Co1 O1 87.51(14) . 5_666 ? F1 Co1 O1 92.49(14) 5_666 5_666 ? F1 Co1 O1 92.49(14) 2_656 5_666 ? O1 Co1 O1 180.000(1) . 5_666 ? O2 S1 O2 109.6(4) 6_565 . ? O2 S1 O1 109.3(2) 6_565 . ? O2 S1 O1 109.3(2) . . ? O2 S1 O3 109.6(2) 6_565 . ? O2 S1 O3 109.6(2) . . ? O1 S1 O3 109.4(4) . . ? Ni1 F1 Co1 130.48(15) . . ? Ni1 F2 Ni1 130.0(2) 4_546 . ? S1 O1 Co1 130.6(4) . . ? S1 O2 Ni1 130.5(3) . . ? N1 C1 C1 119.5(10) . 6 ? N1 C1 N1 26(3) . 2 ? C1 C1 N1 114.5(13) 6 2 ? N1 N1 C1 97(7) 2 . ? N1 N1 C1 57(6) 2 2 ? C1 N1 C1 119(2) . 2 ? H2 N2 H3 105.8 . . ? H2 N2 H1 109.5 . . ? H3 N2 H1 103.7 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.530 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.135