Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Raj Sharma' _publ_contact_author_address ; Department of Chemsitry Panjab University Chandigarh 160014 INDIA ; _publ_contact_author_phone '091 172 2534433' _publ_contact_author_fax '091 172 2545074' _publ_contact_author_email rpsharma@pu.ac.in _publ_requested_coeditor_name ? _publ_contact_letter ; Please send back the ccdc code by mail ; loop_ _publ_author_name _publ_author_address 'Raj Pal Sharma' ; Department of Chemistry Panjab University Chandigarh, 160014 India ; 'Ritu Bala' ; Department of Chemistry Panjab University Chandigarh, 160014 India ; 'Rajni Sharma' ; Department of Chemistry Panjab University Chandigarh, 160014 India ; 'Paloth Venugopalan' ; Department of Chemistry Panjab University Chandigarh, 160014 India ; _publ_section_title ; 'Rings and rectangles' mediated through weak interactions in ionic solids: Synthesis and packing analysis of [Co(NH3)6]Cl2SeCN and [Co(NH3)6]3Cl4(N3)5 in the crystalline state ; # Attachment 'seleno.cif' #========================================================================= data_absrp6 _database_code_depnum_ccdc_archive 'CCDC 268674' _audit_creation_method 'Manual edit of SHELXL-97 cif' _chemical_name_systematic ; hexaamminecobalt(III) dichloride selenocaynide ; _chemical_melting_point 458 _chemical_formula_sum 'C H18 Cl2 Co N7 Se' _chemical_formula_weight 337.01 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' Cl Cl 0.1484 0.1585 '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' Se Se -0.0929 2.2259 '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 12.9480(10) _cell_length_b 7.3340(10) _cell_length_c 13.8490(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.350(10) _cell_angle_gamma 90.00 _cell_volume 1188.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10.479 _cell_measurement_theta_max 32.017 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 4.926 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.754 _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 'siemens P4' _diffrn_measurement_method '2/q/\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 1184 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1128 _reflns_number_gt 1059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens)' _computing_cell_refinement 'XSCANS (Siemens)' _computing_data_reduction 'XSCANS (Siemens)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _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^)+(0.0152P)^2^+9.4033P] 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 0.0061(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1128 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.002 _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 Se1 Se 0.63265(6) 0.0000 0.19456(5) 0.0385(2) Uani 1 2 d S . . Co1 Co 0.0000 0.0000 0.0000 0.0200(3) Uani 1 4 d S . . Co2 Co 0.5000 0.0000 0.5000 0.0206(3) Uani 1 4 d S . . Cl1 Cl 0.34919(12) 0.0000 0.16807(11) 0.0331(4) Uani 1 2 d S . . Cl2 Cl 0.35899(14) 0.5000 0.56629(14) 0.0424(4) Uani 1 2 d S . . N1 N 0.8612(5) 0.0000 0.1937(5) 0.0525(16) Uani 1 2 d S . . N2 N 0.1052(3) 0.1865(5) -0.0069(3) 0.0298(8) Uani 1 1 d . . . H2A H 0.1763 0.1587 0.0390 0.045 Uiso 1 1 calc R . . H2B H 0.0863 0.2946 0.0100 0.045 Uiso 1 1 calc R . . H2C H 0.1008 0.1908 -0.0728 0.045 Uiso 1 1 calc R . . N3 N -0.0804(4) 0.0000 -0.1573(4) 0.0313(11) Uani 1 2 d S . . H3A H -0.0295 0.0000 -0.1847 0.047 Uiso 1 2 d SR . . H3B H -0.1240 0.0991 -0.1791 0.047 Uiso 1 1 d R . . N4 N 0.3997(6) 0.1853(8) 0.4071(3) 0.105(3) Uani 1 1 d . . . H4A H 0.3874 0.1627 0.3399 0.158 Uiso 1 1 calc R . . H4B H 0.4322 0.2943 0.4266 0.158 Uiso 1 1 calc R . . H4C H 0.3335 0.1838 0.4123 0.158 Uiso 1 1 calc R . . N5 N 0.5804(5) 0.0000 0.4113(5) 0.116(5) Uani 1 2 d S . . H5A H 0.6553 0.0000 0.4524 0.175 Uiso 1 2 d SR . . H5B H 0.5615 -0.0991 0.3703 0.175 Uiso 1 1 d R . . C1 C 0.7736(6) 0.0000 0.1956(5) 0.0360(14) Uani 1 2 d S . . 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 Se1 0.0468(4) 0.0386(4) 0.0410(4) 0.000 0.0292(3) 0.000 Co1 0.0182(5) 0.0226(5) 0.0205(5) 0.000 0.0095(4) 0.000 Co2 0.0208(5) 0.0233(5) 0.0187(5) 0.000 0.0095(4) 0.000 Cl1 0.0277(7) 0.0410(8) 0.0280(7) 0.000 0.0094(6) 0.000 Cl2 0.0378(9) 0.0425(9) 0.0488(9) 0.000 0.0204(7) 0.000 N1 0.049(4) 0.062(4) 0.058(4) 0.000 0.034(3) 0.000 N2 0.0267(16) 0.0303(19) 0.0348(17) 0.0011(15) 0.0153(14) -0.0019(15) N3 0.029(3) 0.038(3) 0.026(2) 0.000 0.011(2) 0.000 N4 0.167(6) 0.079(4) 0.028(2) -0.001(2) 0.002(3) 0.087(4) N5 0.031(3) 0.298(15) 0.027(3) 0.000 0.019(3) 0.000 C1 0.049(4) 0.034(3) 0.029(3) 0.000 0.020(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 Se1 C1 1.819(7) . ? Co1 N2 1.961(3) . ? Co1 N2 1.961(3) 6 ? Co1 N2 1.961(3) 5 ? Co1 N2 1.961(3) 2 ? Co1 N3 1.972(5) . ? Co1 N3 1.972(5) 5 ? Co2 N5 1.920(6) . ? Co2 N5 1.920(6) 5_656 ? Co2 N4 1.938(4) 2_656 ? Co2 N4 1.938(4) 6 ? Co2 N4 1.938(4) 5_656 ? Co2 N4 1.938(4) . ? N1 C1 1.146(9) . ? 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 N2 Co1 N2 88.4(2) . 6 ? N2 Co1 N2 180.0(2) . 5 ? N2 Co1 N2 91.6(2) 6 5 ? N2 Co1 N2 91.6(2) . 2 ? N2 Co1 N2 180.00(18) 6 2 ? N2 Co1 N2 88.4(2) 5 2 ? N2 Co1 N3 89.73(14) . . ? N2 Co1 N3 89.73(14) 6 . ? N2 Co1 N3 90.27(14) 5 . ? N2 Co1 N3 90.27(14) 2 . ? N2 Co1 N3 90.27(14) . 5 ? N2 Co1 N3 90.28(14) 6 5 ? N2 Co1 N3 89.73(14) 5 5 ? N2 Co1 N3 89.72(14) 2 5 ? N3 Co1 N3 180.00(14) . 5 ? N5 Co2 N5 180.000(1) . 5_656 ? N5 Co2 N4 91.8(2) . 2_656 ? N5 Co2 N4 88.2(2) 5_656 2_656 ? N5 Co2 N4 88.2(2) . 6 ? N5 Co2 N4 91.8(2) 5_656 6 ? N4 Co2 N4 180.0(2) 2_656 6 ? N5 Co2 N4 91.8(2) . 5_656 ? N5 Co2 N4 88.2(2) 5_656 5_656 ? N4 Co2 N4 89.0(4) 2_656 5_656 ? N4 Co2 N4 91.0(4) 6 5_656 ? N5 Co2 N4 88.2(2) . . ? N5 Co2 N4 91.8(2) 5_656 . ? N4 Co2 N4 91.0(4) 2_656 . ? N4 Co2 N4 89.0(4) 6 . ? N4 Co2 N4 180.0(2) 5_656 . ? N1 C1 Se1 178.4(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.717 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.094 _chemical_name_common 'hexaamminecobalt(iii) dichloride selenocaynide' #========================================================================= data_abrit28 _database_code_depnum_ccdc_archive 'CCDC 290464' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaamminecobalt(III) chloride diazide ; _chemical_melting_point 472 _chemical_formula_sum 'H54 Cl4 Co3 N33' _chemical_formula_weight 835.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M I222 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' _cell_length_a 7.1150(10) _cell_length_b 10.121(2) _cell_length_c 23.154(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1667.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 9.939 _cell_measurement_theta_max 34.871 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.850 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.861 _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 'siemens P4' _diffrn_measurement_method '2/q/\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 877 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.01 _reflns_number_total 872 _reflns_number_gt 782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens)' _computing_cell_refinement 'XSCANS (Siemens)' _computing_data_reduction 'XSCANS (Siemens)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _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^)+(0.0283P)^2^+2.3063P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(7) _refine_ls_number_reflns 872 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.808 _refine_ls_shift/su_mean 0.059 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 1.0000 0.32197(3) 0.0276(2) Uani 1 2 d S . . Co2 Co 0.0000 1.0000 0.0000 0.0257(2) Uani 1 4 d S . . Cl1 Cl -0.0005(9) 1.28222(10) 0.18675(4) 0.0423(3) Uani 1 1 d . . . N1 N 0.1944(5) 1.0053(16) 0.38195(15) 0.0448(10) Uani 1 1 d . . . H1A H 0.2984 1.0416 0.3676 0.067 Uiso 1 1 calc R . . H1B H 0.2194 0.9235 0.3938 0.067 Uiso 1 1 calc R . . H1C H 0.1538 1.0531 0.4117 0.067 Uiso 1 1 calc R . . N2 N 0.1915(5) 0.9942(15) 0.26146(15) 0.0430(10) Uani 1 1 d . . . H2A H 0.1439 0.9561 0.2301 0.064 Uiso 1 1 calc R . . H2B H 0.2898 0.9478 0.2738 0.064 Uiso 1 1 calc R . . H2C H 0.2279 1.0760 0.2530 0.064 Uiso 1 1 calc R . . N3 N -0.003(2) 1.1937(3) 0.32240(14) 0.0435(8) Uani 1 1 d . . . H3A H 0.0475 1.2238 0.2897 0.065 Uiso 1 1 calc R . . H3B H 0.0641 1.2231 0.3523 0.065 Uiso 1 1 calc R . . H3C H -0.1205 1.2222 0.3254 0.065 Uiso 1 1 calc R . . N4 N 0.003(2) 0.8670(3) 0.06090(16) 0.0532(11) Uani 1 1 d . . . H4A H -0.0236 0.7883 0.0459 0.080 Uiso 1 1 calc R . . H4B H -0.0825 0.8874 0.0875 0.080 Uiso 1 1 calc R . . H4C H 0.1163 0.8647 0.0771 0.080 Uiso 1 1 calc R . . N5 N -0.2727(6) 1.0000 0.0000 0.0576(17) Uani 1 2 d S . . H5A H -0.3144 0.9495 -0.0287 0.086 Uiso 0.50 1 calc PR . . H5B H -0.3144 1.0822 -0.0048 0.086 Uiso 0.50 1 calc PR . . H5C H -0.3144 0.9683 0.0335 0.086 Uiso 0.50 1 calc PR . . N6 N 0.0000 0.3918(6) 0.0000 0.155(5) Uani 1 2 d S . . N7 N 0.0000 0.5000 0.0000 0.0554(19) Uani 1 4 d S . . N8 N -0.008(5) 0.2262(6) 0.4518(2) 0.117(3) Uani 1 1 d . . . N9 N 0.0000 0.2187(4) 0.5000 0.0472(12) Uani 1 2 d S . . N10 N 0.1634(6) 0.493(2) 0.36784(19) 0.0615(16) Uani 1 1 d . . . N11 N 0.0000 0.5000 0.36819(18) 0.0360(10) Uani 1 2 d S . . 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 0.0253(3) 0.0236(3) 0.0338(4) 0.000 0.000 0.0003(17) Co2 0.0240(4) 0.0212(4) 0.0318(5) 0.000 0.000 0.000 Cl1 0.0386(5) 0.0392(5) 0.0493(5) -0.0005(4) 0.005(3) 0.000(3) N1 0.0358(16) 0.050(3) 0.0484(17) 0.005(6) -0.0067(15) 0.008(6) N2 0.0447(18) 0.036(3) 0.0477(17) -0.002(5) 0.0069(15) 0.009(5) N3 0.059(2) 0.0290(16) 0.0430(16) -0.0024(13) -0.001(10) -0.005(8) N4 0.066(3) 0.0378(17) 0.056(2) 0.0125(17) -0.024(6) -0.009(7) N5 0.032(2) 0.086(4) 0.055(3) -0.022(11) 0.000 0.000 N6 0.304(15) 0.027(4) 0.136(7) 0.000 0.04(5) 0.000 N7 0.084(6) 0.040(5) 0.043(4) 0.000 0.000 0.000 N8 0.198(9) 0.081(3) 0.073(3) -0.011(3) 0.027(15) -0.003(17) N9 0.100(4) 0.033(2) 0.0085(19) 0.000 0.004(15) 0.000 N10 0.048(2) 0.071(5) 0.065(2) -0.010(8) -0.0069(19) 0.004(8) N11 0.044(3) 0.030(2) 0.033(2) 0.000 0.000 0.000(13) _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 N2 1.955(3) 2_575 ? Co1 N2 1.955(3) . ? Co1 N3 1.961(3) 2_575 ? Co1 N3 1.961(3) . ? Co1 N1 1.961(3) . ? Co1 N1 1.961(3) 2_575 ? Co2 N5 1.940(4) . ? Co2 N5 1.940(4) 2_575 ? Co2 N4 1.950(3) 3 ? Co2 N4 1.950(3) 2_575 ? Co2 N4 1.950(3) . ? Co2 N4 1.950(3) 4_575 ? N6 N7 1.095(7) . ? N7 N6 1.095(7) 2_565 ? N8 N9 1.120(6) . ? N9 N8 1.120(6) 3_556 ? N10 N11 1.165(5) . ? N11 N10 1.165(5) 2_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 N2 Co1 N2 88.5(2) 2_575 . ? N2 Co1 N3 92.3(5) 2_575 2_575 ? N2 Co1 N3 88.1(5) . 2_575 ? N2 Co1 N3 88.1(5) 2_575 . ? N2 Co1 N3 92.3(5) . . ? N3 Co1 N3 179.42(19) 2_575 . ? N2 Co1 N1 176.6(7) 2_575 . ? N2 Co1 N1 90.96(16) . . ? N3 Co1 N1 91.0(6) 2_575 . ? N3 Co1 N1 88.6(6) . . ? N2 Co1 N1 90.96(16) 2_575 2_575 ? N2 Co1 N1 176.6(7) . 2_575 ? N3 Co1 N1 88.6(6) 2_575 2_575 ? N3 Co1 N1 91.0(6) . 2_575 ? N1 Co1 N1 89.8(2) . 2_575 ? N5 Co2 N5 180.0 . 2_575 ? N5 Co2 N4 89.4(4) . 3 ? N5 Co2 N4 90.6(4) 2_575 3 ? N5 Co2 N4 89.4(4) . 2_575 ? N5 Co2 N4 90.6(4) 2_575 2_575 ? N4 Co2 N4 178.8(9) 3 2_575 ? N5 Co2 N4 90.6(4) . . ? N5 Co2 N4 89.4(4) 2_575 . ? N4 Co2 N4 92.7(2) 3 . ? N4 Co2 N4 87.3(2) 2_575 . ? N5 Co2 N4 90.6(4) . 4_575 ? N5 Co2 N4 89.4(4) 2_575 4_575 ? N4 Co2 N4 87.3(2) 3 4_575 ? N4 Co2 N4 92.7(2) 2_575 4_575 ? N4 Co2 N4 178.8(9) . 4_575 ? N6 N7 N6 180.0 2_565 . ? N8 N9 N8 172.2(8) 3_556 . ? N10 N11 N10 179.2(7) 2_565 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.600 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.061