# Electronic Supplementary Material (ESI) for CrystEngComm # 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_1Cd _database_code_depnum_ccdc_archive 'CCDC 916199' #======================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H8 Cd4 Cl N32 O4' _chemical_formula_sum 'C1.50 H0.50 Cd0.25 Cl0.06 N2 O0.25' _chemical_formula_weight 80.85 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 19.3620(3) _cell_length_b 19.3620(3) _cell_length_c 19.3620(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7258.56(19) _cell_formula_units_Z 48 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 912 _cell_measurement_theta_min -23.529 _cell_measurement_theta_max 23.529 _exptl_crystal_description chunky _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1851 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8811 _exptl_absorpt_correction_T_max 0.9639 _exptl_absorpt_process_details SADABS _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 'Bruker Smart Apex' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 46761 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1842 _reflns_number_gt 1737 _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 Ortep-3 _computing_publication_material 'wingx publication routines (Farrugia, 1999)' _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^)+(0.0462P)^2^+1.6492P] 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 1838 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 Cd1 Cd 0.355425(11) 0.5000 0.0000 0.02117(9) Uani 1 4 d S . . Cl1 Cl 0.5000 0.5000 0.0000 0.0262(3) Uani 1 16 d S . . N1 N 0.36585(7) 0.41388(7) 0.08266(7) 0.0310(3) Uani 1 1 d . . . N2 N 0.32375(8) 0.40471(8) 0.13615(7) 0.0371(4) Uani 1 1 d . . . O1 O 0.23894(17) 0.5000 0.0000 0.0976(15) Uani 1 4 d S . . C1 C 0.34895(9) 0.34895(9) 0.16773(13) 0.0326(5) Uani 1 2 d S . . C2 C 0.31849(10) 0.31849(10) 0.23034(12) 0.0367(6) Uani 1 2 d S . . C3 C 0.25984(10) 0.34782(12) 0.25984(10) 0.0389(6) Uani 1 2 d S . . H3 H 0.2403 0.3871 0.2403 0.047 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 Cd1 0.02889(13) 0.01770(12) 0.01692(12) 0.000 0.000 0.000 Cl1 0.0214(4) 0.0214(4) 0.0359(7) 0.000 0.000 0.000 N1 0.0350(7) 0.0320(7) 0.0262(6) 0.0101(6) 0.0105(5) 0.0068(6) N2 0.0421(8) 0.0363(8) 0.0329(7) 0.0174(6) 0.0182(6) 0.0134(7) O1 0.0334(17) 0.102(3) 0.157(5) 0.000 0.000 0.000 C1 0.0334(7) 0.0334(7) 0.0310(11) 0.0146(7) 0.0146(7) 0.0115(9) C2 0.0379(8) 0.0379(8) 0.0343(12) 0.0197(8) 0.0197(8) 0.0181(10) C3 0.0391(8) 0.0383(13) 0.0391(8) 0.0229(8) 0.0191(11) 0.0229(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 Cd1 O1 2.255(3) . ? Cd1 N1 2.3200(14) 26 ? Cd1 N1 2.3200(14) . ? Cd1 N1 2.3200(14) 27_565 ? Cd1 N1 2.3200(14) 4_565 ? Cd1 Cl1 2.7993(2) . ? Cl1 Cd1 2.7993(2) 13 ? Cl1 Cd1 2.7993(2) 37_665 ? Cl1 Cd1 2.7993(2) 25_665 ? N1 N1 1.315(3) 38 ? N1 N2 1.3298(17) . ? N2 C1 1.3332(18) . ? C1 N2 1.3332(18) 38 ? C1 C2 1.471(3) . ? C2 C3 1.3923(14) 9 ? C2 C3 1.3923(14) . ? C3 C2 1.3923(14) 5 ? 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 Cd1 N1 94.99(3) . 26 ? O1 Cd1 N1 94.99(3) . . ? N1 Cd1 N1 87.24(7) 26 . ? O1 Cd1 N1 94.99(3) . 27_565 ? N1 Cd1 N1 170.02(7) 26 27_565 ? N1 Cd1 N1 91.89(7) . 27_565 ? O1 Cd1 N1 94.99(3) . 4_565 ? N1 Cd1 N1 91.89(7) 26 4_565 ? N1 Cd1 N1 170.02(7) . 4_565 ? N1 Cd1 N1 87.24(7) 27_565 4_565 ? O1 Cd1 Cl1 180.0 . . ? N1 Cd1 Cl1 85.01(3) 26 . ? N1 Cd1 Cl1 85.01(3) . . ? N1 Cd1 Cl1 85.01(3) 27_565 . ? N1 Cd1 Cl1 85.01(3) 4_565 . ? Cd1 Cl1 Cd1 90.0 13 . ? Cd1 Cl1 Cd1 180.0 13 37_665 ? Cd1 Cl1 Cd1 90.0 . 37_665 ? Cd1 Cl1 Cd1 90.0 13 25_665 ? Cd1 Cl1 Cd1 180.0 . 25_665 ? Cd1 Cl1 Cd1 90.0 37_665 25_665 ? N1 N1 N2 109.81(9) 38 . ? N1 N1 Cd1 124.73(3) 38 . ? N2 N1 Cd1 125.45(10) . . ? N1 N2 C1 103.94(14) . . ? N2 C1 N2 112.5(2) . 38 ? N2 C1 C2 123.76(10) . . ? N2 C1 C2 123.76(10) 38 . ? C3 C2 C3 119.8(2) 9 . ? C3 C2 C1 120.10(11) 9 . ? C3 C2 C1 120.10(11) . . ? C2 C3 C2 120.2(2) 5 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.903 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.074 data_1CdHT _database_code_depnum_ccdc_archive 'CCDC 916200' #======================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.50 H0.50 Cd0.29 Cl0.13 N2' _chemical_formula_weight 83.76 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' Cd Cd -0.8075 1.2024 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -y, -z' 'y, x, -z' '-x, y, -z' '-y, -x, -z' 'z, x, y' '-x, z, y' '-z, -x, y' 'x, -z, y' 'z, -x, -y' 'x, z, -y' '-z, x, -y' '-x, -z, -y' 'y, z, x' '-z, -y, -x' '-z, y, x' 'z, y, -x' 'z, -y, x' 'y, -z, -x' '-y, -z, x' '-y, z, -x' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, y, z' '-y, -x, z' 'x, -y, z' 'y, x, z' '-z, -x, -y' 'x, -z, -y' 'z, x, -y' '-x, z, -y' '-z, x, y' '-x, -z, y' 'z, -x, y' 'x, z, y' '-y, -z, -x' 'z, y, x' 'z, -y, -x' '-z, -y, x' '-z, y, -x' '-y, z, x' 'y, z, -x' 'y, -z, x' _cell_length_a 19.2945(2) _cell_length_b 19.2945(2) _cell_length_c 19.2945(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7182.91(13) _cell_formula_units_Z 48 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used 916 _cell_measurement_theta_min -23.529 _cell_measurement_theta_max 23.529 _exptl_crystal_description chunky _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1901 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8995 _exptl_absorpt_correction_T_max 0.9387 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 69272 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1319 _reflns_number_gt 1251 _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 Ortep-3 _computing_publication_material 'wingx publication routines (Farrugia, 1999)' _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^)+(0.1093P)^2^+2.7393P] 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 1319 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.257 _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 Cd1 Cd 0.35474(3) 0.5000 0.0000 0.0483(3) Uani 1 4 d S . . Cd2 Cd 0.2443(5) 0.5000 0.1460(6) 0.105(3) Uani 0.08 2 d SP . . Cl1 Cl 0.5000 0.5000 0.0000 0.0522(10) Uani 1 16 d S . . Cl2 Cl 0.2293(7) 0.5000 0.0000 0.116(5) Uani 0.25 4 d SP . . N1 N 0.3662(2) 0.4135(2) 0.0820(2) 0.0625(11) Uani 1 1 d . . . N2 N 0.3232(2) 0.4040(2) 0.1353(2) 0.0752(14) Uani 1 1 d . . . C1 C 0.3475(3) 0.3475(3) 0.1678(4) 0.069(2) Uani 1 2 d S . . C2 C 0.3157(3) 0.3157(3) 0.2280(4) 0.073(2) Uani 1 2 d S . . C3 C 0.2576(3) 0.3459(4) 0.2576(3) 0.077(2) Uani 1 2 d S . . H3 H 0.2387 0.3859 0.2387 0.092 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 Cd1 0.0693(5) 0.0369(4) 0.0387(4) 0.000 0.000 0.000 Cd2 0.097(6) 0.050(4) 0.166(9) 0.000 0.055(6) 0.000 Cl1 0.0437(12) 0.0437(12) 0.069(3) 0.000 0.000 0.000 Cl2 0.063(7) 0.104(10) 0.180(16) 0.000 0.000 0.000 N1 0.077(3) 0.061(2) 0.050(2) 0.0196(19) 0.0245(18) 0.0122(18) N2 0.088(3) 0.072(3) 0.066(3) 0.036(2) 0.041(2) 0.029(2) C1 0.075(3) 0.075(3) 0.057(4) 0.031(3) 0.031(3) 0.026(4) C2 0.076(3) 0.076(3) 0.068(4) 0.039(3) 0.039(3) 0.037(4) C3 0.076(3) 0.078(5) 0.076(3) 0.042(3) 0.026(4) 0.042(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 Cd1 N1 2.310(4) 31_565 ? Cd1 N1 2.310(4) 27 ? Cd1 N1 2.310(4) 5_565 ? Cd1 N1 2.310(4) . ? Cd1 Cl2 2.419(13) . ? Cd1 Cl1 2.8027(6) . ? Cd1 Cd2 3.532(8) 27 ? Cd2 N2 2.406(7) 31_565 ? Cd2 N2 2.406(7) . ? Cd2 Cd2 2.683(16) 42 ? Cd2 Cl2 2.832(11) . ? Cl1 Cd1 2.8027(6) 2_655 ? Cl1 Cd1 2.8027(6) 26_565 ? Cl1 Cd1 2.8027(6) 25_665 ? Cl2 Cd2 2.832(11) 27 ? N1 N1 1.291(8) 32 ? N1 N2 1.334(5) . ? N2 C1 1.343(5) . ? C1 N2 1.343(5) 32 ? C1 C2 1.449(8) . ? C2 C3 1.386(4) . ? C2 C3 1.386(4) 32 ? C3 C2 1.386(4) 9 ? C3 H3 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 N1 Cd1 N1 169.0(2) 31_565 27 ? N1 Cd1 N1 86.5(2) 31_565 5_565 ? N1 Cd1 N1 92.5(2) 27 5_565 ? N1 Cd1 N1 92.5(2) 31_565 . ? N1 Cd1 N1 86.5(2) 27 . ? N1 Cd1 N1 169.0(2) 5_565 . ? N1 Cd1 Cl2 95.51(10) 31_565 . ? N1 Cd1 Cl2 95.51(10) 27 . ? N1 Cd1 Cl2 95.51(10) 5_565 . ? N1 Cd1 Cl2 95.51(10) . . ? N1 Cd1 Cl1 84.49(10) 31_565 . ? N1 Cd1 Cl1 84.49(10) 27 . ? N1 Cd1 Cl1 84.49(10) 5_565 . ? N1 Cd1 Cl1 84.49(10) . . ? Cl2 Cd1 Cl1 180.0 . . ? N1 Cd1 Cd2 127.17(14) 31_565 27 ? N1 Cd1 Cd2 60.77(14) 27 27 ? N1 Cd1 Cd2 60.77(14) 5_565 27 ? N1 Cd1 Cd2 127.17(14) . 27 ? Cl2 Cd1 Cd2 52.91(19) . 27 ? Cl1 Cd1 Cd2 127.09(19) . 27 ? N2 Cd2 N2 100.6(4) 31_565 . ? N2 Cd2 Cd2 120.5(2) 31_565 42 ? N2 Cd2 Cd2 120.5(2) . 42 ? N2 Cd2 Cl2 88.8(3) 31_565 . ? N2 Cd2 Cl2 88.8(3) . . ? Cd2 Cd2 Cl2 129.1(3) 42 . ? Cd1 Cl1 Cd1 90.0 2_655 . ? Cd1 Cl1 Cd1 180.0 2_655 26_565 ? Cd1 Cl1 Cd1 90.0 . 26_565 ? Cd1 Cl1 Cd1 90.0 2_655 25_665 ? Cd1 Cl1 Cd1 180.0 . 25_665 ? Cd1 Cl1 Cd1 90.0 26_565 25_665 ? Cd1 Cl2 Cd2 84.1(3) . . ? Cd1 Cl2 Cd2 84.1(3) . 27 ? Cd2 Cl2 Cd2 168.3(7) . 27 ? N1 N1 N2 110.0(2) 32 . ? N1 N1 Cd1 125.36(9) 32 . ? N2 N1 Cd1 124.6(3) . . ? N1 N2 C1 104.8(4) . . ? N1 N2 Cd2 110.7(3) . . ? C1 N2 Cd2 143.7(4) . . ? N2 C1 N2 110.3(6) 32 . ? N2 C1 C2 124.8(3) 32 . ? N2 C1 C2 124.8(3) . . ? C3 C2 C3 120.6(6) . 32 ? C3 C2 C1 119.7(3) . . ? C3 C2 C1 119.7(3) 32 . ? C2 C3 C2 119.4(6) . 9 ? C2 C3 H3 120.3 . . ? C2 C3 H3 120.3 9 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.011 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.133 data_2Co _database_code_depnum_ccdc_archive 'CCDC 916201' #======================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.50 H0.50 Cl0.06 Co0.29 N2 O0.25' _chemical_formula_weight 69.94 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' 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 cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 18.7976(3) _cell_length_b 18.7976(3) _cell_length_c 18.7976(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6642.13(18) _cell_formula_units_Z 48 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 916 _cell_measurement_theta_min -23.529 _cell_measurement_theta_max 23.529 _exptl_crystal_description chunky _exptl_crystal_colour pink _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1653 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9257 _exptl_absorpt_correction_T_max 0.9450 _exptl_absorpt_process_details SADABS _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 'Bruker Smart Apex' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42725 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1692 _reflns_number_gt 1508 _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 Ortep-3 _computing_publication_material 'wingx publication routines (Farrugia, 1999)' _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^)+(0.1287P)^2^+6.2192P] 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 1692 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1939 _refine_ls_wR_factor_gt 0.1889 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 0.36196(3) 0.5000 0.0000 0.0159(3) Uani 1 4 d S . . Co2 Co 0.2441(3) 0.5000 0.1274(3) 0.0079(11) Uani 0.06 2 d SP . . Cl1 Cl 0.5000 0.5000 0.0000 0.0211(5) Uani 1 16 d S . . N1 N 0.36965(12) 0.41876(11) 0.07772(11) 0.0223(5) Uani 1 1 d . . . N2 N 0.32502(13) 0.40828(12) 0.13205(12) 0.0299(6) Uani 1 1 d . . . O1 O 0.2535(3) 0.5000 0.0000 0.0679(18) Uani 1 4 d S . . C1 C 0.35006(16) 0.35006(16) 0.1641(2) 0.0275(8) Uani 1 2 d S . . C2 C 0.31818(17) 0.31818(17) 0.2273(2) 0.0332(10) Uani 1 2 d S . . C3 C 0.25746(18) 0.3477(2) 0.25746(18) 0.0357(10) Uani 1 2 d S . . H3 H 0.2368 0.3877 0.2368 0.043 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 0.0220(4) 0.0139(4) 0.0118(3) 0.000 0.000 0.000 Co2 0.012(3) 0.004(2) 0.008(2) 0.000 0.004(2) 0.000 Cl1 0.0172(6) 0.0172(6) 0.0291(12) 0.000 0.000 0.000 N1 0.0248(11) 0.0226(10) 0.0195(10) 0.0049(8) 0.0071(8) 0.0027(8) N2 0.0342(12) 0.0287(12) 0.0268(11) 0.0132(9) 0.0144(9) 0.0124(10) O1 0.028(2) 0.063(3) 0.113(5) 0.000 0.000 0.000 C1 0.0290(12) 0.0290(12) 0.0245(17) 0.0137(11) 0.0137(11) 0.0114(15) C2 0.0343(13) 0.0343(13) 0.031(2) 0.0192(13) 0.0192(13) 0.0160(17) C3 0.0367(14) 0.034(2) 0.0367(14) 0.0220(14) 0.0188(18) 0.0220(14) _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 2.039(5) . ? Co1 N1 2.118(2) 27_565 ? Co1 N1 2.118(2) 4_565 ? Co1 N1 2.118(2) . ? Co1 N1 2.118(2) 26 ? Co1 Cl1 2.5948(7) . ? Co2 N2 2.301(5) 27_565 ? Co2 N2 2.301(5) . ? Co2 O1 2.402(6) . ? Cl1 Co1 2.5948(7) 37_665 ? Cl1 Co1 2.5948(7) 25_665 ? Cl1 Co1 2.5948(7) 13 ? N1 N1 1.306(4) 38 ? N1 N2 1.336(3) . ? N2 C1 1.335(3) . ? O1 Co2 2.402(6) 26 ? C1 N2 1.335(3) 38 ? C1 C2 1.460(5) . ? C2 C3 1.390(2) . ? C2 C3 1.390(2) 9 ? C3 C2 1.390(2) 5 ? 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 N1 93.91(6) . 27_565 ? O1 Co1 N1 93.91(6) . 4_565 ? N1 Co1 N1 87.21(11) 27_565 4_565 ? O1 Co1 N1 93.91(6) . . ? N1 Co1 N1 92.26(11) 27_565 . ? N1 Co1 N1 172.18(12) 4_565 . ? O1 Co1 N1 93.91(6) . 26 ? N1 Co1 N1 172.18(12) 27_565 26 ? N1 Co1 N1 92.26(11) 4_565 26 ? N1 Co1 N1 87.20(11) . 26 ? O1 Co1 Cl1 180.0 . . ? N1 Co1 Cl1 86.09(6) 27_565 . ? N1 Co1 Cl1 86.09(6) 4_565 . ? N1 Co1 Cl1 86.09(6) . . ? N1 Co1 Cl1 86.09(6) 26 . ? N2 Co2 N2 97.1(3) 27_565 . ? N2 Co2 O1 89.38(19) 27_565 . ? N2 Co2 O1 89.38(19) . . ? Co1 Cl1 Co1 90.0 37_665 25_665 ? Co1 Cl1 Co1 90.0 37_665 . ? Co1 Cl1 Co1 180.0 25_665 . ? Co1 Cl1 Co1 180.0 37_665 13 ? Co1 Cl1 Co1 90.0 25_665 13 ? Co1 Cl1 Co1 90.0 . 13 ? N1 N1 N2 109.86(13) 38 . ? N1 N1 Co1 123.92(6) 38 . ? N2 N1 Co1 126.20(16) . . ? C1 N2 N1 104.1(2) . . ? C1 N2 Co2 149.8(2) . . ? N1 N2 Co2 106.0(2) . . ? Co1 O1 Co2 94.19(19) . 26 ? Co1 O1 Co2 94.19(19) . . ? Co2 O1 Co2 171.6(4) 26 . ? N2 C1 N2 112.0(3) . 38 ? N2 C1 C2 123.98(15) . . ? N2 C1 C2 123.98(15) 38 . ? C3 C2 C3 119.3(4) . 9 ? C3 C2 C1 120.33(19) . . ? C3 C2 C1 120.33(19) 9 . ? C2 C3 C2 120.7(4) . 5 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.425 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.157 data_2CoHT _database_code_depnum_ccdc_archive 'CCDC 916202' #======================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.50 H0.50 Cl0.19 Co0.31 N2' _chemical_formula_weight 71.60 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' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 18.5015(3) _cell_length_b 18.5015(3) _cell_length_c 18.5015(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6333.16(18) _cell_formula_units_Z 48 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used 903 _cell_measurement_theta_min -23.529 _cell_measurement_theta_max 23.529 _exptl_crystal_description chunky _exptl_crystal_colour pink _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1686 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9131 _exptl_absorpt_correction_T_max 0.9355 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 60559 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1171 _reflns_number_gt 1105 _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 Ortep-3 _computing_publication_material 'wingx publication routines (Farrugia, 1999)' _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^)+(0.1365P)^2^+15.1308P] 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 1171 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2583 _refine_ls_wR_factor_gt 0.2512 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.221 _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 0.36674(8) 0.5000 0.0000 0.0403(6) Uani 1 4 d S . . Co2 Co 0.2681(4) 0.5000 0.1484(5) 0.052(3) Uani 0.13 2 d SP . . Cl1 Cl 0.5000 0.5000 0.0000 0.0469(13) Uani 1 16 d S . . Cl2 Cl 0.2403(7) 0.5000 0.0000 0.070(4) Uani 0.25 4 d SP . . Cl3 Cl 0.2876(10) 0.5000 0.2876(10) 0.141(9) Uani 0.25 4 d SP . . N1 N 0.3713(2) 0.4215(2) 0.0750(2) 0.0469(11) Uani 1 1 d . . . N2 N 0.3258(3) 0.4103(2) 0.1292(2) 0.0525(13) Uani 1 1 d . . . C1 C 0.3507(3) 0.3507(3) 0.1618(4) 0.0491(19) Uani 1 2 d S . . C2 C 0.3169(3) 0.3169(3) 0.2257(4) 0.056(2) Uani 1 2 d S . . C3 C 0.2575(3) 0.3477(5) 0.2575(3) 0.059(2) Uani 1 2 d S . . H3 H 0.2384 0.3901 0.2384 0.071 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 0.0567(10) 0.0375(8) 0.0266(8) 0.000 0.000 0.000 Co2 0.050(5) 0.008(3) 0.098(7) 0.000 0.057(5) 0.000 Cl1 0.0465(18) 0.0465(18) 0.048(3) 0.000 0.000 0.000 Cl2 0.058(7) 0.055(7) 0.096(10) 0.000 0.000 0.000 Cl3 0.156(14) 0.109(16) 0.156(14) 0.000 -0.039(18) 0.000 N1 0.057(3) 0.049(2) 0.035(2) 0.0000(19) 0.000(2) 0.0058(19) N2 0.064(3) 0.051(3) 0.042(3) 0.009(2) 0.018(2) 0.012(2) C1 0.053(3) 0.053(3) 0.040(4) 0.007(3) 0.007(3) 0.014(4) C2 0.059(3) 0.059(3) 0.048(5) 0.018(3) 0.018(3) 0.017(4) C3 0.056(3) 0.064(5) 0.056(3) 0.020(3) 0.012(4) 0.020(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 N1 2.011(4) 27_565 ? Co1 N1 2.011(4) 26 ? Co1 N1 2.011(4) . ? Co1 N1 2.011(4) 4_565 ? Co1 Cl2 2.339(14) . ? Co1 Cl1 2.4655(15) . ? Co2 N2 2.005(6) . ? Co2 N2 2.005(6) 27_565 ? Co2 Cl3 2.60(2) . ? Co2 Cl2 2.793(11) . ? Cl1 Co1 2.4655(15) 37_665 ? Cl1 Co1 2.4655(15) 13 ? Cl1 Co1 2.4655(15) 25_665 ? Cl3 Co2 2.60(2) 22_565 ? N1 N1 1.313(8) 38 ? N1 N2 1.325(6) . ? N2 C1 1.339(6) . ? C1 N2 1.339(6) 38 ? C1 C2 1.476(11) . ? C2 C3 1.371(5) . ? C2 C3 1.371(5) 9 ? C3 C2 1.371(5) 5 ? 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 N1 Co1 N1 175.2(3) 27_565 26 ? N1 Co1 N1 92.6(2) 27_565 . ? N1 Co1 N1 87.2(2) 26 . ? N1 Co1 N1 87.2(2) 27_565 4_565 ? N1 Co1 N1 92.6(2) 26 4_565 ? N1 Co1 N1 175.2(3) . 4_565 ? N1 Co1 Cl2 92.38(14) 27_565 . ? N1 Co1 Cl2 92.38(14) 26 . ? N1 Co1 Cl2 92.38(14) . . ? N1 Co1 Cl2 92.38(14) 4_565 . ? N1 Co1 Cl1 87.62(14) 27_565 . ? N1 Co1 Cl1 87.62(14) 26 . ? N1 Co1 Cl1 87.62(14) . . ? N1 Co1 Cl1 87.62(14) 4_565 . ? Cl2 Co1 Cl1 180.0 . . ? N2 Co2 N2 111.8(4) . 27_565 ? N2 Co2 Cl3 95.8(4) . . ? N2 Co2 Cl3 95.8(4) 27_565 . ? N2 Co2 Cl2 85.6(3) . . ? N2 Co2 Cl2 85.6(3) 27_565 . ? Cl3 Co2 Cl2 177.4(5) . . ? Co1 Cl1 Co1 90.0 37_665 . ? Co1 Cl1 Co1 180.0 37_665 13 ? Co1 Cl1 Co1 90.0 . 13 ? Co1 Cl1 Co1 90.0 37_665 25_665 ? Co1 Cl1 Co1 180.0 . 25_665 ? Co1 Cl1 Co1 90.0 13 25_665 ? Co1 Cl2 Co2 79.4(3) . . ? Co2 Cl3 Co2 74.1(7) 22_565 . ? N1 N1 N2 109.8(3) 38 . ? N1 N1 Co1 122.72(12) 38 . ? N2 N1 Co1 127.5(3) . . ? N1 N2 C1 104.6(4) . . ? N1 N2 Co2 110.0(4) . . ? C1 N2 Co2 141.8(5) . . ? N2 C1 N2 111.3(7) . 38 ? N2 C1 C2 124.3(3) . . ? N2 C1 C2 124.3(3) 38 . ? C3 C2 C3 118.9(8) . 9 ? C3 C2 C1 120.5(4) . . ? C3 C2 C1 120.5(4) 9 . ? C2 C3 C2 121.0(8) 5 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.375 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.129 data_3Ni _database_code_depnum_ccdc_archive 'CCDC 916203' #======================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.50 H0.50 Cl0.13 N2 Ni0.31 O0.25' _chemical_formula_weight 73.32 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' Cl Cl 0.1484 0.1585 '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 cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 18.6483(3) _cell_length_b 18.6483(3) _cell_length_c 18.6483(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6485.12(18) _cell_formula_units_Z 48 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 924 _cell_measurement_theta_min -23.529 _cell_measurement_theta_max 23.529 _exptl_crystal_description chunky _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1746 _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8745 _exptl_absorpt_correction_T_max 0.8941 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40409 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1653 _reflns_number_gt 1440 _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 Ortep-3 _computing_publication_material 'wingx publication routines (Farrugia, 1999)' _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^)+(0.1464P)^2^+5.3616P] 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 0.0008(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1653 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2056 _refine_ls_wR_factor_gt 0.2012 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.36564(3) 0.5000 0.0000 0.0180(3) Uani 1 4 d S . . Ni2 Ni 0.2486(2) 0.5000 0.13427(19) 0.0205(7) Uani 0.13 2 d SP . . Cl1 Cl 0.5000 0.5000 0.0000 0.0231(5) Uani 1 16 d S . . Cl2 Cl 0.1426(8) 0.4240(11) 0.1426(8) 0.142(12) Uani 0.13 2 d SP . . O1 O 0.2487(2) 0.5000 0.0000 0.0412(11) Uani 1 4 d S . . N1 N 0.37103(12) 0.42035(12) 0.07702(12) 0.0240(5) Uani 1 1 d . . . N2 N 0.32613(13) 0.41040(13) 0.13175(12) 0.0312(6) Uani 1 1 d . . . C1 C 0.35186(17) 0.35186(17) 0.1643(2) 0.0310(9) Uani 1 2 d S . . C2 C 0.31895(17) 0.31895(17) 0.2275(2) 0.0364(10) Uani 1 2 d S . . C3 C 0.25879(18) 0.3497(2) 0.25879(18) 0.0384(11) Uani 1 2 d S . . H1 H 0.2393 0.3913 0.2393 0.016(10) 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 Ni1 0.0228(4) 0.0166(4) 0.0146(4) 0.000 0.000 0.000 Ni2 0.0227(17) 0.0162(15) 0.0226(16) 0.000 0.0071(13) 0.000 Cl1 0.0202(7) 0.0202(7) 0.0288(12) 0.000 0.000 0.000 Cl2 0.177(18) 0.074(11) 0.177(18) -0.001(7) -0.10(2) -0.001(7) O1 0.025(2) 0.030(2) 0.068(3) 0.000 0.000 0.000 N1 0.0288(11) 0.0253(11) 0.0178(10) 0.0045(9) 0.0079(8) 0.0008(8) N2 0.0328(12) 0.0332(12) 0.0276(12) 0.0114(9) 0.0127(9) 0.0079(10) C1 0.0326(12) 0.0326(12) 0.0279(19) 0.0119(12) 0.0119(12) 0.0069(16) C2 0.0369(14) 0.0369(14) 0.035(2) 0.0158(13) 0.0158(13) 0.0120(18) C3 0.0393(15) 0.037(2) 0.0393(15) 0.0203(15) 0.0202(19) 0.0203(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 Ni1 N1 2.069(2) 27_565 ? Ni1 N1 2.069(2) 4_565 ? Ni1 N1 2.069(2) 26 ? Ni1 N1 2.069(2) . ? Ni1 O1 2.180(4) . ? Ni1 Cl1 2.5056(6) . ? Ni2 N2 2.210(3) 27_565 ? Ni2 N2 2.210(3) . ? Ni2 Cl2 2.438(17) . ? Ni2 Cl2 2.438(17) 27_565 ? Ni2 O1 2.504(4) . ? Cl1 Ni1 2.5056(6) 37_665 ? Cl1 Ni1 2.5056(6) 13 ? Cl1 Ni1 2.5056(6) 25_665 ? Cl2 Ni2 2.438(17) 22_565 ? N1 N1 1.301(4) 38 ? N1 N2 1.333(3) . ? N2 C1 1.338(3) . ? C1 N2 1.338(3) 38 ? C1 C2 1.464(5) . ? C2 C3 1.388(3) . ? C2 C3 1.388(3) 9 ? C3 C2 1.388(3) 5 ? 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 N1 Ni1 N1 87.95(12) 27_565 4_565 ? N1 Ni1 N1 174.43(13) 27_565 26 ? N1 Ni1 N1 91.78(12) 4_565 26 ? N1 Ni1 N1 91.78(12) 27_565 . ? N1 Ni1 N1 174.43(13) 4_565 . ? N1 Ni1 N1 87.95(12) 26 . ? N1 Ni1 O1 92.79(6) 27_565 . ? N1 Ni1 O1 92.79(6) 4_565 . ? N1 Ni1 O1 92.79(6) 26 . ? N1 Ni1 O1 92.79(6) . . ? N1 Ni1 Cl1 87.21(6) 27_565 . ? N1 Ni1 Cl1 87.21(6) 4_565 . ? N1 Ni1 Cl1 87.21(6) 26 . ? N1 Ni1 Cl1 87.21(6) . . ? O1 Ni1 Cl1 180.0 . . ? N2 Ni2 N2 98.3(2) 27_565 . ? N2 Ni2 Cl2 166.3(4) 27_565 . ? N2 Ni2 Cl2 95.3(4) . . ? N2 Ni2 Cl2 95.3(4) 27_565 27_565 ? N2 Ni2 Cl2 166.3(4) . 27_565 ? Cl2 Ni2 Cl2 71.1(9) . 27_565 ? N2 Ni2 O1 88.75(13) 27_565 . ? N2 Ni2 O1 88.75(13) . . ? Cl2 Ni2 O1 93.7(4) . . ? Cl2 Ni2 O1 93.7(4) 27_565 . ? Ni1 Cl1 Ni1 90.0 37_665 . ? Ni1 Cl1 Ni1 180.0 37_665 13 ? Ni1 Cl1 Ni1 90.0 . 13 ? Ni1 Cl1 Ni1 90.0 37_665 25_665 ? Ni1 Cl1 Ni1 180.0 . 25_665 ? Ni1 Cl1 Ni1 90.0 13 25_665 ? Ni2 Cl2 Ni2 76.4(6) 22_565 . ? Ni1 O1 Ni2 90.04(13) . . ? N1 N1 N2 110.23(14) 38 . ? N1 N1 Ni1 122.83(6) 38 . ? N2 N1 Ni1 126.94(17) . . ? N1 N2 C1 103.6(2) . . ? N1 N2 Ni2 108.78(18) . . ? C1 N2 Ni2 147.3(2) . . ? N2 C1 N2 112.3(3) . 38 ? N2 C1 C2 123.84(16) . . ? N2 C1 C2 123.84(16) 38 . ? C3 C2 C3 119.4(4) . 9 ? C3 C2 C1 120.2(2) . . ? C3 C2 C1 120.2(2) 9 . ? C2 C3 C2 120.5(4) . 5 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.749 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.177 data_3NiHT _database_code_depnum_ccdc_archive 'CCDC 916204' #=======================================================================ta_cwt04ch _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.50 H0.50 Cl0.10 N2 Ni0.42 O0.38' _chemical_formula_weight 80.69 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' Cl Cl 0.1484 0.1585 '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 cubic _symmetry_space_group_name_H-M 'P m -3 m' _symmetry_space_group_name_Hall '-P 4 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 18.5564(3) _cell_length_b 18.5564(3) _cell_length_c 18.5564(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6389.71(18) _cell_formula_units_Z 48 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used 903 _cell_measurement_theta_min -23.529 _cell_measurement_theta_max 23.529 _exptl_crystal_description chunky _exptl_crystal_colour blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1917 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6820 _exptl_absorpt_correction_T_max 0.8348 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'phi-omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39832 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1624 _reflns_number_gt 1225 _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 Ortep-3 _computing_publication_material 'wingx publication routines (Farrugia, 1999)' _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^)+(0.0794P)^2^+12.2123P] 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 1624 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.36647(5) 0.5000 0.0000 0.0352(3) Uani 1 4 d S . . Ni2 Ni 0.26048(11) 0.5000 0.14052(11) 0.0484(5) Uani 0.33 2 d SP . . Cl1 Cl 0.5000 0.5000 0.0000 0.0504(8) Uani 1 16 d S . . Cl2 Cl 0.2712(4) 0.5000 0.2712(4) 0.060(2) Uani 0.20 4 d SP . . O1 O 0.2450(2) 0.5000 0.0000 0.0468(12) Uani 1 4 d S . . O2 O 0.1539(13) 0.5000 0.1539(13) 0.32(3) Uani 0.50 4 d SP . . N1 N 0.37153(14) 0.42154(14) 0.07629(13) 0.0400(6) Uani 1 1 d . . . N2 N 0.32637(17) 0.41064(16) 0.13058(15) 0.0487(8) Uani 1 1 d . . . C1 C 0.3511(2) 0.3511(2) 0.1626(3) 0.0472(12) Uani 1 2 d S . . C2 C 0.3170(2) 0.3170(2) 0.2255(3) 0.0558(14) Uani 1 2 d S . . C3 C 0.2558(2) 0.3481(3) 0.2558(2) 0.0606(16) Uani 1 2 d S . . H3 H 0.2355 0.3891 0.2355 0.073 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 Ni1 0.0505(5) 0.0324(4) 0.0227(4) 0.000 0.000 0.000 Ni2 0.0505(11) 0.0376(10) 0.0571(12) 0.000 0.0174(9) 0.000 Cl1 0.0509(12) 0.0509(12) 0.0493(19) 0.000 0.000 0.000 Cl2 0.058(4) 0.063(6) 0.058(4) 0.000 0.024(5) 0.000 O1 0.0193(19) 0.034(2) 0.087(4) 0.000 0.000 0.000 O2 0.124(14) 0.72(9) 0.124(14) 0.000 0.083(17) 0.000 N1 0.0515(16) 0.0389(14) 0.0294(12) 0.0025(11) 0.0072(11) 0.0036(11) N2 0.0554(18) 0.0508(16) 0.0400(15) 0.0115(12) 0.0155(13) 0.0145(14) C1 0.0500(17) 0.0500(17) 0.042(2) 0.0129(16) 0.0129(16) 0.010(2) C2 0.058(2) 0.058(2) 0.052(3) 0.0215(19) 0.0215(19) 0.019(3) C3 0.057(2) 0.067(3) 0.057(2) 0.024(2) 0.022(3) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.033(3) 26 ? Ni1 N1 2.033(3) 27_565 ? Ni1 N1 2.033(3) . ? Ni1 N1 2.033(3) 4_565 ? Ni1 O1 2.254(4) . ? Ni1 Cl1 2.4779(9) . ? Ni2 O2 1.99(2) . ? Ni2 N2 2.069(3) 27_565 ? Ni2 N2 2.069(3) . ? Ni2 Cl2 2.433(9) . ? Ni2 O1 2.623(2) . ? Cl1 Ni1 2.4779(9) 25_665 ? Cl1 Ni1 2.4779(9) 13 ? Cl1 Ni1 2.4779(9) 37_665 ? Cl2 Ni2 2.433(9) 22_565 ? O2 Ni2 1.99(2) 22_565 ? N1 N1 1.312(5) 38 ? N1 N2 1.326(4) . ? N2 C1 1.336(4) . ? C1 N2 1.336(4) 38 ? C1 C2 1.470(7) . ? C2 C3 1.393(4) 9 ? C2 C3 1.393(4) . ? C3 C2 1.393(4) 5 ? C3 H3 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 N1 Ni1 N1 174.71(16) 26 27_565 ? N1 Ni1 N1 88.27(14) 26 . ? N1 Ni1 N1 91.48(14) 27_565 . ? N1 Ni1 N1 91.48(14) 26 4_565 ? N1 Ni1 N1 88.27(14) 27_565 4_565 ? N1 Ni1 N1 174.71(16) . 4_565 ? N1 Ni1 O1 92.65(8) 26 . ? N1 Ni1 O1 92.65(8) 27_565 . ? N1 Ni1 O1 92.65(8) . . ? N1 Ni1 O1 92.65(8) 4_565 . ? N1 Ni1 Cl1 87.35(8) 26 . ? N1 Ni1 Cl1 87.35(8) 27_565 . ? N1 Ni1 Cl1 87.35(8) . . ? N1 Ni1 Cl1 87.35(8) 4_565 . ? O1 Ni1 Cl1 180.0 . . ? O2 Ni2 N2 126.70(10) . 27_565 ? O2 Ni2 N2 126.70(10) . . ? N2 Ni2 N2 106.6(2) 27_565 . ? O2 Ni2 Cl2 87.5(8) . . ? N2 Ni2 Cl2 92.33(15) 27_565 . ? N2 Ni2 Cl2 92.33(15) . . ? O2 Ni2 O1 90.9(8) . . ? N2 Ni2 O1 88.63(11) 27_565 . ? N2 Ni2 O1 88.63(11) . . ? Cl2 Ni2 O1 178.4(2) . . ? Ni1 Cl1 Ni1 90.0 25_665 13 ? Ni1 Cl1 Ni1 180.0 25_665 . ? Ni1 Cl1 Ni1 90.0 13 . ? Ni1 Cl1 Ni1 90.0 25_665 37_665 ? Ni1 Cl1 Ni1 180.0 13 37_665 ? Ni1 Cl1 Ni1 90.0 . 37_665 ? Ni2 Cl2 Ni2 80.6(4) . 22_565 ? Ni1 O1 Ni2 83.71(10) . . ? Ni2 O2 Ni2 104.4(15) . 22_565 ? N1 N1 N2 109.81(17) 38 . ? N1 N1 Ni1 122.62(7) 38 . ? N2 N1 Ni1 127.5(2) . . ? N1 N2 C1 104.3(3) . . ? N1 N2 Ni2 108.6(2) . . ? C1 N2 Ni2 145.7(2) . . ? N2 C1 N2 111.7(4) 38 . ? N2 C1 C2 124.1(2) 38 . ? N2 C1 C2 124.1(2) . . ? C3 C2 C3 120.8(5) 9 . ? C3 C2 C1 119.6(3) 9 . ? C3 C2 C1 119.6(3) . . ? C2 C3 C2 119.2(5) . 5 ? C2 C3 H3 120.4 . . ? C2 C3 H3 120.4 5 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.009 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.097