Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gao, Song' 'Ma, Bao-Qing' 'Su, Gang' 'Sun, Hao-Ling' _publ_contact_author_name 'Prof Song Gao' _publ_contact_author_address ; College of Chemistry and Molecular Engineering Peking University College of Chemistry and Molecular Beijing 100871 CHINA ; _publ_contact_author_email 'GAOSONG@PKU.EDU.CN' _publ_section_title ; Pyrazine dioxide bridged two-dimensional antiferromagnets [M(NCS)2(pzdo)2] (M = Mn, Co; pzdo = pyrazine dioxide ; data_1-Mnpzdo _database_code_CSD 169675 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Mn N6 O4 S2' _chemical_formula_weight 395.28 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 6.9405(2) _cell_length_b 7.1938(3) _cell_length_c 8.2566(4) _cell_angle_alpha 82.237(3) _cell_angle_beta 66.892(3) _cell_angle_gamma 74.971(3) _cell_volume 365.94(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 199 _exptl_absorpt_coefficient_mu 1.216 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6971 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 27.51 _reflns_number_total 1662 _reflns_number_gt 1518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _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^)+(0.0000P)^2^+1.2221P] 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 SHELXL _refine_ls_extinction_coef 0.074(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1662 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _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 Mn1 Mn 0.0000 0.0000 0.0000 0.0265(3) Uani 1 2 d S . . S1 S 0.2857(2) 0.40697(19) -0.50764(17) 0.0536(4) Uani 1 1 d . . . O1 O 0.0284(5) 0.1745(4) 0.1866(3) 0.0333(6) Uani 1 1 d . . . O2 O 0.3499(5) -0.1318(4) -0.0781(4) 0.0409(7) Uani 1 1 d . . . N1 N 0.0137(5) 0.0911(4) 0.3421(4) 0.0261(6) Uani 1 1 d . . . N2 N 0.4218(5) -0.3124(5) -0.0395(4) 0.0296(7) Uani 1 1 d . . . N3 N 0.0799(7) 0.2219(5) -0.1927(5) 0.0418(9) Uani 1 1 d . . . C1 C -0.1802(6) 0.0927(6) 0.4704(5) 0.0309(8) Uani 1 1 d . . . H1 H -0.3047 0.1575 0.4516 0.037 Uiso 1 1 calc R . . C2 C 0.1937(6) 0.0017(6) 0.3710(5) 0.0308(8) Uani 1 1 d . . . H2 H 0.3276 0.0037 0.2832 0.037 Uiso 1 1 calc R . . C3 C 0.5735(6) -0.3586(6) 0.0328(5) 0.0322(8) Uani 1 1 d . . . H3 H 0.6255 -0.2619 0.0550 0.039 Uiso 1 1 calc R . . C4 C 0.3493(6) -0.4542(6) -0.0730(5) 0.0328(8) Uani 1 1 d . . . H4 H 0.2463 -0.4240 -0.1239 0.039 Uiso 1 1 calc R . . C5 C 0.1651(6) 0.3018(5) -0.3258(5) 0.0308(8) 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 Mn1 0.0303(5) 0.0279(4) 0.0227(4) 0.0020(3) -0.0138(3) -0.0042(3) S1 0.0485(7) 0.0492(7) 0.0501(7) 0.0111(5) -0.0040(6) -0.0190(6) O1 0.0485(17) 0.0333(14) 0.0231(13) 0.0038(11) -0.0190(12) -0.0110(12) O2 0.0324(15) 0.0281(14) 0.0596(19) 0.0064(13) -0.0194(14) -0.0030(12) N1 0.0344(17) 0.0254(15) 0.0231(14) -0.0003(11) -0.0155(13) -0.0072(12) N2 0.0233(15) 0.0275(15) 0.0342(17) 0.0001(13) -0.0101(13) -0.0012(12) N3 0.061(2) 0.0357(18) 0.0304(18) 0.0047(15) -0.0204(17) -0.0114(17) C1 0.0293(19) 0.0341(19) 0.0313(19) 0.0001(15) -0.0164(15) -0.0033(15) C2 0.0290(19) 0.036(2) 0.0258(18) -0.0017(15) -0.0096(15) -0.0050(15) C3 0.0262(18) 0.034(2) 0.038(2) -0.0042(16) -0.0132(16) -0.0053(15) C4 0.0282(19) 0.035(2) 0.038(2) -0.0010(16) -0.0169(16) -0.0047(16) C5 0.0317(19) 0.0283(18) 0.038(2) -0.0030(16) -0.0185(16) -0.0060(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N3 2.114(4) . ? Mn1 N3 2.114(4) 2 ? Mn1 O1 2.208(3) 2 ? Mn1 O1 2.208(3) . ? Mn1 O2 2.226(3) . ? Mn1 O2 2.226(3) 2 ? S1 C5 1.600(4) . ? O1 N1 1.319(4) . ? O2 N2 1.309(4) . ? N1 C2 1.344(5) . ? N1 C1 1.345(5) . ? N2 C4 1.350(5) . ? N2 C3 1.354(5) . ? N3 C5 1.176(5) . ? C1 C2 1.372(5) 2_556 ? C2 C1 1.372(5) 2_556 ? C3 C4 1.362(5) 2_645 ? C3 C4 9.997(6) 2_556 ? C4 C3 1.362(5) 2_645 ? C4 C3 9.997(6) 2_556 ? 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 N3 Mn1 N3 180.0(2) . 2 ? N3 Mn1 O1 92.44(12) . 2 ? N3 Mn1 O1 87.56(12) 2 2 ? N3 Mn1 O1 87.56(12) . . ? N3 Mn1 O1 92.44(12) 2 . ? O1 Mn1 O1 180.00(14) 2 . ? N3 Mn1 O2 88.34(13) . . ? N3 Mn1 O2 91.66(13) 2 . ? O1 Mn1 O2 91.74(11) 2 . ? O1 Mn1 O2 88.26(11) . . ? N3 Mn1 O2 91.66(13) . 2 ? N3 Mn1 O2 88.34(13) 2 2 ? O1 Mn1 O2 88.26(11) 2 2 ? O1 Mn1 O2 91.74(11) . 2 ? O2 Mn1 O2 180.0 . 2 ? N1 O1 Mn1 115.9(2) . . ? N2 O2 Mn1 122.0(2) . . ? O1 N1 C2 119.6(3) . . ? O1 N1 C1 120.3(3) . . ? C2 N1 C1 120.1(3) . . ? O2 N2 C4 121.1(3) . . ? O2 N2 C3 119.7(3) . . ? C4 N2 C3 119.2(3) . . ? C5 N3 Mn1 161.1(3) . . ? N1 C1 C2 119.8(3) . 2_556 ? N1 C2 C1 120.1(4) . 2_556 ? N2 C3 C4 120.5(4) . 2_645 ? N2 C3 C4 93.0(2) . 2_556 ? C4 C3 C4 114.9(3) 2_645 2_556 ? N2 C4 C3 120.3(4) . 2_645 ? N2 C4 C3 60.8(2) . 2_556 ? C3 C4 C3 114.9(3) 2_645 2_556 ? N3 C5 S1 178.8(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.707 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.091 data_2-Copzdo _database_code_CSD 169676 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 Co N6 O4 S2' _chemical_formula_weight 399.27 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' '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' _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 6.8922(14) _cell_length_b 7.1528(14) _cell_length_c 8.1074(16) _cell_angle_alpha 82.49(3) _cell_angle_beta 67.26(3) _cell_angle_gamma 74.06(3) _cell_volume 354.31(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 201 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7110 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.81 _reflns_number_total 1664 _reflns_number_gt 1406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _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^)+(0.0370P)^2^+0.1374P] 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 SHELXL _refine_ls_extinction_coef 0.049(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1664 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Co1 Co 0.0000 0.0000 0.0000 0.02286(15) Uani 1 2 d S . . S1 S 0.28415(10) 0.40832(10) -0.50028(9) 0.0466(2) Uani 1 1 d . . . O1 O 0.0294(2) 0.1693(2) 0.17979(17) 0.0289(3) Uani 1 1 d . . . O2 O 0.3394(2) -0.1276(2) -0.0775(2) 0.0342(4) Uani 1 1 d . . . N1 N 0.0149(3) 0.0877(2) 0.3384(2) 0.0229(4) Uani 1 1 d . . . N2 N 0.4163(3) -0.3116(2) -0.0390(2) 0.0251(4) Uani 1 1 d . . . N3 N 0.0770(3) 0.2155(3) -0.1876(2) 0.0325(4) Uani 1 1 d . . . C1 C -0.1811(3) 0.0900(3) 0.4657(3) 0.0274(4) Uani 1 1 d . . . H1 H -0.3063 0.1523 0.4434 0.033 Uiso 1 1 calc R . . C2 C 0.1960(3) -0.0001(3) 0.3713(3) 0.0263(4) Uani 1 1 d . . . H2 H 0.3314 0.0001 0.2834 0.032 Uiso 1 1 calc R . . C3 C 0.5743(3) -0.3561(3) 0.0292(3) 0.0277(4) Uani 1 1 d . . . H3 H 0.6263 -0.2576 0.0495 0.033 Uiso 1 1 calc R . . C4 C 0.3419(3) -0.4547(3) -0.0685(3) 0.0289(5) Uani 1 1 d . . . H4 H 0.2333 -0.4247 -0.1158 0.035 Uiso 1 1 calc R . . C5 C 0.1616(3) 0.2970(3) -0.3183(3) 0.0266(4) 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 0.0275(2) 0.0229(2) 0.0193(2) 0.00252(14) -0.01207(16) -0.00442(15) S1 0.0420(4) 0.0419(4) 0.0446(4) 0.0110(3) -0.0034(3) -0.0167(3) O1 0.0415(9) 0.0301(8) 0.0201(7) 0.0051(6) -0.0168(6) -0.0110(7) O2 0.0283(8) 0.0215(8) 0.0503(9) 0.0054(7) -0.0168(7) -0.0017(6) N1 0.0313(9) 0.0210(8) 0.0197(8) -0.0001(6) -0.0132(7) -0.0060(7) N2 0.0222(8) 0.0213(9) 0.0277(9) 0.0007(7) -0.0081(7) -0.0015(7) N3 0.0442(11) 0.0282(10) 0.0268(9) 0.0034(7) -0.0165(8) -0.0083(8) C1 0.0262(10) 0.0306(11) 0.0275(10) 0.0006(8) -0.0145(9) -0.0041(8) C2 0.0260(10) 0.0282(11) 0.0232(10) -0.0006(8) -0.0090(8) -0.0044(8) C3 0.0244(10) 0.0265(11) 0.0333(11) -0.0034(8) -0.0114(9) -0.0057(8) C4 0.0268(10) 0.0292(11) 0.0336(11) -0.0010(9) -0.0159(9) -0.0042(9) C5 0.0271(10) 0.0240(10) 0.0321(11) -0.0023(8) -0.0154(9) -0.0042(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.0450(19) 2 ? Co1 N3 2.0450(19) . ? Co1 O1 2.1114(15) 2 ? Co1 O1 2.1114(15) . ? Co1 O2 2.1309(16) 2 ? Co1 O2 2.1309(16) . ? S1 C5 1.619(2) . ? O1 N1 1.319(2) . ? O2 N2 1.322(2) . ? N1 C2 1.344(3) . ? N1 C1 1.344(3) . ? N2 C4 1.348(3) . ? N2 C3 1.350(3) . ? N3 C5 1.163(3) . ? C1 C2 1.371(3) 2_556 ? C2 C1 1.371(3) 2_556 ? C3 C4 1.367(3) 2_645 ? C3 C4 9.800(5) 2_556 ? C4 C3 1.367(3) 2_645 ? C4 C3 9.800(5) 2_556 ? 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 N3 Co1 N3 180.00(9) 2 . ? N3 Co1 O1 86.64(6) 2 2 ? N3 Co1 O1 93.36(6) . 2 ? N3 Co1 O1 93.36(6) 2 . ? N3 Co1 O1 86.64(6) . . ? O1 Co1 O1 180.00(7) 2 . ? N3 Co1 O2 87.40(8) 2 2 ? N3 Co1 O2 92.60(8) . 2 ? O1 Co1 O2 87.76(7) 2 2 ? O1 Co1 O2 92.24(7) . 2 ? N3 Co1 O2 92.60(8) 2 . ? N3 Co1 O2 87.40(8) . . ? O1 Co1 O2 92.24(7) 2 . ? O1 Co1 O2 87.76(7) . . ? O2 Co1 O2 180.00(4) 2 . ? N1 O1 Co1 115.92(11) . . ? N2 O2 Co1 121.98(12) . . ? O1 N1 C2 119.96(17) . . ? O1 N1 C1 119.84(16) . . ? C2 N1 C1 120.18(17) . . ? O2 N2 C4 121.30(17) . . ? O2 N2 C3 119.01(17) . . ? C4 N2 C3 119.69(17) . . ? C5 N3 Co1 162.14(17) . . ? N1 C1 C2 119.79(19) . 2_556 ? N1 C2 C1 120.02(19) . 2_556 ? N2 C3 C4 120.19(19) . 2_645 ? N2 C3 C4 92.13(11) . 2_556 ? C4 C3 C4 115.12(13) 2_645 2_556 ? N2 C4 C3 120.12(19) . 2_645 ? N2 C4 C3 62.24(11) . 2_556 ? C3 C4 C3 115.12(13) 2_645 2_556 ? N3 C5 S1 178.9(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.81 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.304 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.067