Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'G. Leigh' 'Darren A. Handley' 'Peter B. Hitchcock' 'Ting Huei Lee' _publ_contact_author_name 'Prof G Leigh' _publ_contact_author_address ; Physics and Environmental Science University of Sussex School of Chemistry Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'G.J.LEIGH@SUSSEX.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Anomalous Reactions of the Diamine Me2NCH2NMe2 with Nickel(II) and Cobalt(II) ; data_feb999 _database_code_CSD 191669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[CoCl2(Me2NCH2NMeCH2NMe2)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H19 Cl2 Co N3' _chemical_formula_weight 275.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 12.079(3) _cell_length_b 10.960(3) _cell_length_c 9.231(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1222.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 1.806 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5563 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.97 _reflns_number_total 1547 _reflns_number_gt 1161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _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^)+(0.0187P)^2^+0.1466P] 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 ' refined ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1547 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Co Co 0.65471(4) 0.7500 0.12291(5) 0.01845(12) Uani 1 2 d S . . Cl1 Cl 0.80988(7) 0.7500 -0.01053(9) 0.0285(2) Uani 1 2 d S . . Cl2 Cl 0.49538(7) 0.7500 0.00052(9) 0.0282(2) Uani 1 2 d S . . N1 N 0.65285(16) 0.60356(16) 0.2646(2) 0.0199(4) Uani 1 1 d . . . N2 N 0.6327(2) 0.7500 0.4596(3) 0.0226(6) Uani 1 2 d S . . C1 C 0.6363(4) 0.7500 0.6174(4) 0.0417(10) Uani 1 2 d S . . H1A H 0.564(4) 0.7500 0.668(5) 0.062(15) Uiso 1 2 d S . . H1B H 0.678(2) 0.680(3) 0.650(3) 0.056(10) Uiso 1 1 d . . . C2 C 0.5895(2) 0.6393(2) 0.3961(3) 0.0244(5) Uani 1 1 d . . . H2B H 0.594(2) 0.575(3) 0.472(3) 0.034(7) Uiso 1 1 d . . . H2A H 0.515(2) 0.646(2) 0.369(3) 0.033(7) Uiso 1 1 d . . . C3 C 0.7672(2) 0.5682(2) 0.3056(3) 0.0258(5) Uani 1 1 d . . . H3A H 0.768(2) 0.497(2) 0.364(3) 0.030(7) Uiso 1 1 d . . . H3B H 0.808(2) 0.548(2) 0.218(3) 0.027(7) Uiso 1 1 d . . . H3C H 0.798(2) 0.631(2) 0.358(3) 0.028(7) Uiso 1 1 d . . . C4 C 0.5971(2) 0.4970(2) 0.1975(3) 0.0266(5) Uani 1 1 d . . . H4C H 0.520(2) 0.515(2) 0.170(3) 0.037(8) Uiso 1 1 d . . . H4A H 0.594(2) 0.429(2) 0.265(3) 0.029(7) Uiso 1 1 d . . . H4B H 0.635(2) 0.475(2) 0.111(3) 0.029(7) Uiso 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 Co 0.0184(2) 0.0184(2) 0.0186(2) 0.000 -0.00028(18) 0.000 Cl1 0.0253(4) 0.0311(5) 0.0292(5) 0.000 0.0073(3) 0.000 Cl2 0.0248(4) 0.0298(5) 0.0300(5) 0.000 -0.0095(3) 0.000 N1 0.0183(9) 0.0186(9) 0.0228(9) 0.0002(8) -0.0004(8) -0.0002(8) N2 0.0279(16) 0.0208(14) 0.0190(14) 0.000 0.0010(11) 0.000 C1 0.069(3) 0.033(2) 0.0237(19) 0.000 -0.003(2) 0.000 C2 0.0254(13) 0.0250(12) 0.0227(12) -0.0011(10) 0.0025(10) -0.0036(10) C3 0.0239(12) 0.0228(13) 0.0306(14) 0.0021(11) -0.0050(11) 0.0029(10) C4 0.0313(14) 0.0200(12) 0.0284(12) -0.0027(10) -0.0007(12) -0.0050(10) _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 Co N1 2.0706(18) 7_575 ? Co N1 2.0706(18) . ? Co Cl2 2.2317(10) . ? Co Cl1 2.2429(11) . ? N1 C4 1.484(3) . ? N1 C3 1.484(3) . ? N1 C2 1.488(3) . ? N2 C2 1.445(3) . ? N2 C2 1.445(3) 7_575 ? N2 C1 1.457(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 Co N1 101.64(10) 7_575 . ? N1 Co Cl2 108.09(6) 7_575 . ? N1 Co Cl2 108.09(6) . . ? N1 Co Cl1 110.85(6) 7_575 . ? N1 Co Cl1 110.85(6) . . ? Cl2 Co Cl1 116.27(4) . . ? C4 N1 C3 108.84(19) . . ? C4 N1 C2 108.35(18) . . ? C3 N1 C2 109.82(19) . . ? C4 N1 Co 110.56(15) . . ? C3 N1 Co 110.73(15) . . ? C2 N1 Co 108.50(14) . . ? C2 N2 C2 114.2(3) . 7_575 ? C2 N2 C1 114.58(17) . . ? C2 N2 C1 114.58(17) 7_575 . ? N2 C2 N1 111.5(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.406 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.069 #===END data_jan1099 _database_code_CSD 191670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Me2NCHNMe2][NiCl3(Me2NCH2NMe2)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H27 Cl3 N4 Ni' _chemical_formula_weight 368.42 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' '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 15.257(3) _cell_length_b 7.922(2) _cell_length_c 15.488(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.10(2) _cell_angle_gamma 90.00 _cell_volume 1695.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.608 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4216 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.98 _reflns_number_total 4077 _reflns_number_gt 3441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; The H atom on C8 was located on a difference map and freely refined. Other H atoms were in riding mode. 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^)+(0.0546P)^2^+0.1237P] 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 0.0028(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4077 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.763705(19) 0.15643(3) 0.072089(19) 0.01529(10) Uani 1 1 d . . . Cl1 Cl 0.91495(4) 0.07664(9) 0.18243(5) 0.03372(17) Uani 1 1 d . . . Cl2 Cl 0.69066(4) -0.10450(7) 0.05015(4) 0.02560(14) Uani 1 1 d . . . Cl3 Cl 0.79094(4) 0.20525(8) -0.06326(4) 0.02632(15) Uani 1 1 d . . . N1 N 0.62772(13) 0.2867(2) 0.02218(14) 0.0183(4) Uani 1 1 d . . . N2 N 0.77782(14) 0.4110(2) 0.11891(14) 0.0205(4) Uani 1 1 d . . . N3 N 0.67885(14) -0.3001(2) -0.18375(14) 0.0214(4) Uani 1 1 d . . . N4 N 0.84962(14) -0.2723(2) -0.10767(15) 0.0220(4) Uani 1 1 d . . . C1 C 0.56376(18) 0.2758(3) -0.08052(18) 0.0294(5) Uani 1 1 d . . . H1C H 0.5367 0.1617 -0.0958 0.044 Uiso 1 1 calc R . . H1B H 0.6010 0.3008 -0.1173 0.044 Uiso 1 1 calc R . . H1A H 0.5110 0.3578 -0.0967 0.044 Uiso 1 1 calc R . . C2 C 0.57009(17) 0.2494(3) 0.07578(19) 0.0270(5) Uani 1 1 d . . . H2C H 0.6106 0.2631 0.1442 0.040 Uiso 1 1 calc R . . H2B H 0.5462 0.1331 0.0629 0.040 Uiso 1 1 calc R . . H2A H 0.5151 0.3273 0.0559 0.040 Uiso 1 1 calc R . . C3 C 0.67820(16) 0.4504(3) 0.04876(17) 0.0208(4) Uani 1 1 d . . . H3B H 0.6457 0.5254 0.0773 0.025 Uiso 1 1 calc R . . H3A H 0.6790 0.5070 -0.0079 0.025 Uiso 1 1 calc R . . C4 C 0.85075(17) 0.5160(3) 0.1053(2) 0.0322(6) Uani 1 1 d . . . H4C H 0.8440 0.5028 0.0398 0.048 Uiso 1 1 calc R . . H4B H 0.9157 0.4804 0.1501 0.048 Uiso 1 1 calc R . . H4A H 0.8410 0.6347 0.1168 0.048 Uiso 1 1 calc R . . C5 C 0.7904(2) 0.4268(4) 0.21846(19) 0.0344(6) Uani 1 1 d . . . H5C H 0.8562 0.3924 0.2618 0.052 Uiso 1 1 calc R . . H5B H 0.7435 0.3542 0.2284 0.052 Uiso 1 1 calc R . . H5A H 0.7799 0.5444 0.2313 0.052 Uiso 1 1 calc R . . C6 C 0.58804(18) -0.2176(4) -0.1971(2) 0.0324(6) Uani 1 1 d . . . H6C H 0.6021 -0.1199 -0.1545 0.049 Uiso 1 1 calc R . . H6B H 0.5473 -0.2976 -0.1823 0.049 Uiso 1 1 calc R . . H6A H 0.5539 -0.1800 -0.2634 0.049 Uiso 1 1 calc R . . C7 C 0.66693(18) -0.4549(3) -0.23952(18) 0.0267(5) Uani 1 1 d . . . H7C H 0.6723 -0.4282 -0.2989 0.040 Uiso 1 1 calc R . . H7B H 0.6031 -0.5039 -0.2545 0.040 Uiso 1 1 calc R . . H7A H 0.7174 -0.5360 -0.2025 0.040 Uiso 1 1 calc R . . C8 C 0.76026(17) -0.2338(3) -0.12339(17) 0.0218(5) Uani 1 1 d . . . H8 H 0.7539(18) -0.153(3) -0.0861(18) 0.012(6) Uiso 1 1 d . . . C9 C 0.92945(19) -0.1965(4) -0.0255(2) 0.0335(6) Uani 1 1 d . . . H9C H 0.9034 -0.1158 0.0056 0.050 Uiso 1 1 calc R . . H9B H 0.9731 -0.1377 -0.0471 0.050 Uiso 1 1 calc R . . H9A H 0.9652 -0.2852 0.0199 0.050 Uiso 1 1 calc R . . C10 C 0.87913(19) -0.3833(4) -0.1662(2) 0.0325(6) Uani 1 1 d . . . H10C H 0.8884 -0.4982 -0.1404 0.049 Uiso 1 1 calc R . . H10B H 0.9399 -0.3422 -0.1657 0.049 Uiso 1 1 calc R . . H10A H 0.8288 -0.3839 -0.2318 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01484(15) 0.01202(15) 0.01810(16) 0.00004(10) 0.00610(11) 0.00227(10) Cl1 0.0209(3) 0.0357(3) 0.0326(3) 0.0001(3) -0.0003(2) 0.0118(2) Cl2 0.0310(3) 0.0127(3) 0.0353(3) -0.0015(2) 0.0162(3) -0.0021(2) Cl3 0.0317(3) 0.0265(3) 0.0263(3) 0.0027(2) 0.0177(3) 0.0046(2) N1 0.0160(9) 0.0143(8) 0.0242(9) 0.0004(7) 0.0083(8) 0.0006(7) N2 0.0192(9) 0.0140(9) 0.0263(10) -0.0034(7) 0.0077(8) -0.0005(7) N3 0.0201(9) 0.0202(9) 0.0259(10) -0.0004(8) 0.0116(8) -0.0002(8) N4 0.0182(9) 0.0189(9) 0.0291(10) -0.0005(8) 0.0102(8) -0.0003(8) C1 0.0231(12) 0.0294(13) 0.0281(13) -0.0012(10) 0.0036(10) 0.0029(10) C2 0.0200(11) 0.0247(12) 0.0398(14) 0.0041(11) 0.0161(11) 0.0020(9) C3 0.0191(10) 0.0117(10) 0.0302(12) 0.0014(8) 0.0093(9) 0.0028(8) C4 0.0208(11) 0.0191(11) 0.0561(17) -0.0047(11) 0.0156(12) -0.0059(9) C5 0.0360(14) 0.0350(14) 0.0278(13) -0.0117(11) 0.0094(11) 0.0015(12) C6 0.0208(12) 0.0374(14) 0.0395(15) -0.0005(12) 0.0134(11) 0.0043(11) C7 0.0281(12) 0.0236(12) 0.0289(12) -0.0047(10) 0.0125(10) -0.0073(10) C8 0.0231(11) 0.0183(11) 0.0256(12) -0.0022(9) 0.0118(10) 0.0001(9) C9 0.0233(12) 0.0329(14) 0.0391(15) -0.0051(12) 0.0083(11) -0.0071(11) C10 0.0248(12) 0.0326(14) 0.0441(16) -0.0060(12) 0.0185(12) 0.0037(11) _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 Ni N2 2.1229(19) . ? Ni N1 2.1465(19) . ? Ni Cl1 2.3020(9) . ? Ni Cl2 2.3041(8) . ? Ni Cl3 2.3357(9) . ? N1 C2 1.473(3) . ? N1 C1 1.474(3) . ? N1 C3 1.475(3) . ? N2 C4 1.475(3) . ? N2 C5 1.476(3) . ? N2 C3 1.479(3) . ? N3 C8 1.307(3) . ? N3 C6 1.465(3) . ? N3 C7 1.466(3) . ? N4 C8 1.315(3) . ? N4 C10 1.465(3) . ? N4 C9 1.466(3) . ? 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 Ni N1 66.96(7) . . ? N2 Ni Cl1 94.75(6) . . ? N1 Ni Cl1 155.62(6) . . ? N2 Ni Cl2 151.07(6) . . ? N1 Ni Cl2 92.59(6) . . ? Cl1 Ni Cl2 97.64(3) . . ? N2 Ni Cl3 96.80(6) . . ? N1 Ni Cl3 96.31(6) . . ? Cl1 Ni Cl3 101.99(3) . . ? Cl2 Ni Cl3 105.98(3) . . ? C2 N1 C1 108.44(19) . . ? C2 N1 C3 112.65(18) . . ? C1 N1 C3 112.40(19) . . ? C2 N1 Ni 114.68(14) . . ? C1 N1 Ni 117.17(15) . . ? C3 N1 Ni 90.67(12) . . ? C4 N2 C5 109.3(2) . . ? C4 N2 C3 112.24(19) . . ? C5 N2 C3 112.79(19) . . ? C4 N2 Ni 117.41(15) . . ? C5 N2 Ni 112.77(16) . . ? C3 N2 Ni 91.49(12) . . ? C8 N3 C6 118.5(2) . . ? C8 N3 C7 126.9(2) . . ? C6 N3 C7 114.6(2) . . ? C8 N4 C10 126.2(2) . . ? C8 N4 C9 118.7(2) . . ? C10 N4 C9 115.0(2) . . ? N1 C3 N2 105.77(17) . . ? N3 C8 N4 129.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.886 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.091 #===END data_nov399 _database_code_CSD 191671 _audit_creation_date 1999-11-02T11:30:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Me2NH2]2{CoCl4]' _chemical_formula_moiety '[C2 H8 N]2[Cl4 Co]' _chemical_formula_sum 'C4 H16 Cl4 Co N2' _chemical_formula_weight 292.92 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4399(6) _cell_length_b 11.3658(7) _cell_length_c 13.4408(11) _cell_angle_alpha 90 _cell_angle_beta 90.015(4) _cell_angle_gamma 90 _cell_volume 1289.32(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7695 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.783 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 7340 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.938 _diffrn_measured_fraction_theta_max 0.938 _reflns_number_total 2130 _reflns_number_gt 1926 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0547P)^2^+2.8794P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 2130 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.137 _refine_diff_density_min -0.68 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Co Co 0.17248(6) 0.20392(5) 0.07906(4) 0.0294(2) Uani 1 1 d . . . Cl1 Cl 0.19786(15) 0.26157(10) -0.08237(9) 0.0443(3) Uani 1 1 d . . . Cl2 Cl 0.18301(12) 0.00519(9) 0.09118(8) 0.0366(3) Uani 1 1 d . . . Cl3 Cl -0.07280(12) 0.26771(9) 0.12765(9) 0.0393(3) Uani 1 1 d . . . Cl4 Cl 0.36442(15) 0.28563(10) 0.17377(11) 0.0526(4) Uani 1 1 d . . . N1 N 0.2091(4) -0.0039(3) -0.1595(3) 0.0369(8) Uani 1 1 d . . . H1A H 0.1559 -0.0641 -0.1282 0.044 Uiso 1 1 calc R . . H1B H 0.1852 0.0649 -0.1267 0.044 Uiso 1 1 calc R . . N2 N 0.2966(5) 0.1923(4) 0.4005(3) 0.0541(11) Uani 1 1 d . . . H2A H 0.3474 0.2179 0.4571 0.065 Uiso 1 1 calc R . . H2B H 0.3376 0.234 0.3477 0.065 Uiso 1 1 calc R . . C1 C 0.1534(6) 0.0048(4) -0.2620(4) 0.0430(11) Uani 1 1 d . . . H1C H 0.2022 0.0732 -0.294 0.065 Uiso 1 1 calc R . . H1D H 0.0379 0.0137 -0.2624 0.065 Uiso 1 1 calc R . . H1E H 0.1826 -0.0667 -0.2983 0.065 Uiso 1 1 calc R . . C2 C 0.3815(6) -0.0256(5) -0.1519(5) 0.0578(14) Uani 1 1 d . . . H2C H 0.4067 -0.1018 -0.182 0.087 Uiso 1 1 calc R . . H2D H 0.4129 -0.0261 -0.0817 0.087 Uiso 1 1 calc R . . H2E H 0.4389 0.0368 -0.187 0.087 Uiso 1 1 calc R . . C3 C 0.1286(7) 0.2211(5) 0.4094(6) 0.0728(19) Uani 1 1 d . . . H3A H 0.0794 0.2197 0.3434 0.109 Uiso 1 1 calc R . . H3B H 0.1171 0.2997 0.4385 0.109 Uiso 1 1 calc R . . H3C H 0.0766 0.1632 0.4524 0.109 Uiso 1 1 calc R . . C4 C 0.3344(7) 0.0669(5) 0.3860(5) 0.0644(15) Uani 1 1 d . . . H4A H 0.2897 0.0209 0.4409 0.097 Uiso 1 1 calc R . . H4B H 0.4497 0.0566 0.3845 0.097 Uiso 1 1 calc R . . H4C H 0.289 0.0399 0.3229 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0244(3) 0.0242(3) 0.0396(4) -0.0026(2) 0.0000(2) 0.0008(2) Cl1 0.0516(7) 0.0346(6) 0.0466(6) 0.0074(5) 0.0126(5) -0.0015(5) Cl2 0.0356(5) 0.0253(5) 0.0488(6) 0.0037(4) 0.0030(5) 0.0029(4) Cl3 0.0325(5) 0.0352(6) 0.0501(6) -0.0009(4) 0.0092(5) 0.0094(4) Cl4 0.0430(6) 0.0396(6) 0.0753(9) -0.0125(6) -0.0197(6) -0.0027(5) N1 0.0267(17) 0.038(2) 0.046(2) -0.0053(16) 0.0038(16) 0.0002(15) N2 0.054(3) 0.054(3) 0.054(3) -0.004(2) -0.008(2) -0.005(2) C1 0.040(2) 0.042(3) 0.048(3) 0.005(2) 0.002(2) -0.003(2) C2 0.029(2) 0.077(4) 0.067(3) -0.003(3) 0.000(2) 0.010(2) C3 0.042(3) 0.058(4) 0.119(6) -0.020(4) -0.009(3) -0.002(3) C4 0.058(3) 0.045(3) 0.090(4) -0.014(3) -0.005(3) 0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Co Cl4 2.2597(13) . ? Co Cl2 2.2664(11) . ? Co Cl1 2.2766(13) . ? Co Cl3 2.2888(11) . ? N1 C1 1.459(6) . ? N1 C2 1.479(6) . ? N2 C3 1.460(7) . ? N2 C4 1.474(7) . ? 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 Cl4 Co Cl2 109.94(5) . . ? Cl4 Co Cl1 110.55(5) . . ? Cl2 Co Cl1 110.59(4) . . ? Cl4 Co Cl3 110.94(5) . . ? Cl2 Co Cl3 109.31(4) . . ? Cl1 Co Cl3 105.44(5) . . ? C1 N1 C2 113.2(4) . . ? C3 N2 C4 116.0(4) . . ? #===END data_sep1699 _database_code_CSD 191672 _audit_creation_date 1999-09-18T12:32:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Me2NH2][Me2N=CH2][CoCl4]' _chemical_formula_moiety 'C5 H16 Cl4 Co N2' _chemical_formula_structural 'C5 H16 Cl4 Co N2' _chemical_formula_sum 'C5 H16 Cl4 Co N2' _chemical_formula_weight 304.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8749(4) _cell_length_b 10.0074(6) _cell_length_c 15.0839(6) _cell_angle_alpha 90 _cell_angle_beta 95.553(3) _cell_angle_gamma 90 _cell_volume 1333.38(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5077 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.779 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 9316 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 3869 _reflns_number_gt 3098 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXs-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Hydrogen atoms were freely refined , except for the methyl groups of the [Me2N=CH2] cation which were disordered and included in riding mode (AFIX 123). 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^)+(0.0252P)^2^+0.9207P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0057(12) _refine_ls_number_reflns 3869 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.083 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.841 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Co Co 0.30406(3) 0.72858(3) 0.066462(19) 0.03109(11) Uani 1 1 d . . . Cl1 Cl 0.09828(7) 0.82534(7) 0.11711(4) 0.04800(18) Uani 1 1 d . . . Cl2 Cl 0.31234(7) 0.79090(6) -0.07859(4) 0.03929(15) Uani 1 1 d . . . Cl3 Cl 0.30435(8) 0.50233(6) 0.07460(4) 0.04742(17) Uani 1 1 d . . . Cl4 Cl 0.51814(7) 0.79918(6) 0.14960(4) 0.04584(17) Uani 1 1 d . . . N1 N 0.6831(2) 0.5113(2) 0.15073(13) 0.0358(4) Uani 1 1 d . . . H1B H 0.667(3) 0.448(3) 0.114(2) 0.048(8) Uiso 1 1 d . . . H1A H 0.628(4) 0.578(4) 0.133(2) 0.055(9) Uiso 1 1 d . . . N2 N 0.2330(3) 1.1475(2) 0.10506(15) 0.0478(5) Uani 1 1 d . . . C1 C 0.6366(4) 0.4672(3) 0.23760(18) 0.0480(6) Uani 1 1 d . . . H1C H 0.696(4) 0.391(4) 0.258(2) 0.071(11) Uiso 1 1 d . . . H1B' H 0.661(4) 0.534(3) 0.277(2) 0.060(9) Uiso 1 1 d . . . H1A' H 0.529(4) 0.446(3) 0.228(2) 0.063(9) Uiso 1 1 d . . . C2 C 0.8433(3) 0.5507(4) 0.1546(3) 0.0536(7) Uani 1 1 d . . . H2C H 0.907(4) 0.482(4) 0.179(2) 0.070(10) Uiso 1 1 d . . . H2B H 0.858(4) 0.620(4) 0.192(2) 0.072(11) Uiso 1 1 d . . . H2A H 0.869(4) 0.572(4) 0.099(3) 0.070(11) Uiso 1 1 d . . . C3 C 0.0920(4) 1.2085(4) 0.1152(3) 0.0693(9) Uani 1 1 d . . . H3A H 0.0811 1.2211 0.1787 0.104 Uiso 0.5 1 calc PR . . H3B H 0.01 1.1511 0.0888 0.104 Uiso 0.5 1 calc PR . . H3C H 0.087 1.2954 0.0851 0.104 Uiso 0.5 1 calc PR . . H3D H 0.0376 1.224 0.0564 0.104 Uiso 0.5 1 calc PR . . H3E H 0.1087 1.294 0.1463 0.104 Uiso 0.5 1 calc PR . . H3F H 0.0317 1.1497 0.15 0.104 Uiso 0.5 1 calc PR . . C4 C 0.3310(4) 1.1279(4) 0.1830(2) 0.0721(10) Uani 1 1 d . . . H4A H 0.2796 1.154 0.235 0.108 Uiso 0.5 1 calc PR . . H4B H 0.422 1.1826 0.1804 0.108 Uiso 0.5 1 calc PR . . H4C H 0.3597 1.0334 0.188 0.108 Uiso 0.5 1 calc PR . . H4D H 0.428 1.0927 0.1673 0.108 Uiso 0.5 1 calc PR . . H4E H 0.2855 1.0641 0.2219 0.108 Uiso 0.5 1 calc PR . . H4F H 0.3478 1.2133 0.2142 0.108 Uiso 0.5 1 calc PR . . C5 C 0.2769(4) 1.1188(4) 0.0259(2) 0.0589(8) Uani 1 1 d . . . H5B H 0.367(5) 1.077(5) 0.036(3) 0.097(14) Uiso 1 1 d . . . H5A H 0.195(5) 1.121(4) -0.020(3) 0.102(14) Uiso 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 Co 0.03251(17) 0.03099(18) 0.02931(16) 0.00106(12) 0.00075(11) -0.00137(12) Cl1 0.0434(3) 0.0490(4) 0.0544(4) -0.0018(3) 0.0189(3) -0.0008(3) Cl2 0.0478(3) 0.0388(3) 0.0311(3) 0.0045(2) 0.0032(2) 0.0013(2) Cl3 0.0606(4) 0.0310(3) 0.0487(3) 0.0044(3) -0.0049(3) -0.0059(3) Cl4 0.0460(3) 0.0384(3) 0.0492(3) -0.0057(3) -0.0153(3) -0.0011(3) N1 0.0360(10) 0.0357(11) 0.0340(10) -0.0011(9) -0.0053(8) -0.0020(9) N2 0.0477(12) 0.0441(13) 0.0511(12) 0.0021(10) 0.0020(10) -0.0053(10) C1 0.0572(17) 0.0533(18) 0.0333(12) 0.0045(12) 0.0030(12) 0.0076(15) C2 0.0387(13) 0.059(2) 0.0613(19) 0.0007(17) -0.0056(13) -0.0109(14) C3 0.0460(16) 0.075(2) 0.090(2) 0.0094(19) 0.0211(16) 0.0078(16) C4 0.072(2) 0.094(3) 0.0475(16) -0.0061(17) -0.0082(15) 0.0040(19) C5 0.0568(18) 0.073(2) 0.0490(16) -0.0042(15) 0.0147(15) -0.0027(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Co Cl1 2.2643(7) . ? Co Cl3 2.2675(7) . ? Co Cl2 2.2830(6) . ? Co Cl4 2.2849(6) . ? N1 C2 1.471(3) . ? N1 C1 1.479(3) . ? N2 C5 1.323(4) . ? N2 C4 1.407(4) . ? N2 C3 1.415(4) . ? 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 Cl1 Co Cl3 113.92(3) . . ? Cl1 Co Cl2 107.96(3) . . ? Cl3 Co Cl2 108.95(3) . . ? Cl1 Co Cl4 109.73(3) . . ? Cl3 Co Cl4 106.41(3) . . ? Cl2 Co Cl4 109.84(3) . . ? C2 N1 C1 113.3(2) . . ? C5 N2 C4 120.8(3) . . ? C5 N2 C3 122.2(3) . . ? C4 N2 C3 116.8(3) . . ? #===END data_mar1999 _database_code_CSD 194217 _audit_creation_date 2000-05-02T13:23:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; [Ni3Cl4(OH)9tmeda)3][Ni3Cl4(OMe)(tmeda)3][NiCl3(tmeda)}2 ; _chemical_formula_sum 'C41 H116 Cl14 N16 Ni8 O2' _chemical_formula_weight 1831.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 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' _cell_length_a 28.975(5) _cell_length_b 10.987(2) _cell_length_c 25.727(4) _cell_angle_alpha 90 _cell_angle_beta 102.266(14) _cell_angle_gamma 90 _cell_volume 8003(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.60 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3808 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.35 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 7566 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7430 _reflns_number_gt 6013 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The [Ni3Cl4(OH)(tmeda)3] cation shows disorder between the apical bridging positions; Cl:OH 0.62:0.38 suggesting that it is mainly as stated but with some [Ni3Cl5(tmeda)3] also present. The formula is given for the idealised product Cl:OH 0.5:0.5 . H atoms for the OH groups were omitted. 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^)+(0.0485P)^2^+35.2428P] 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 'riding; or omitted (for OH)' _refine_ls_extinction_method none _refine_ls_number_reflns 7430 _refine_ls_number_parameters 749 _refine_ls_number_restraints 410 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(4) _refine_diff_density_max 1.215 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.02429(6) 0.32339(18) 0.34487(7) 0.0287(5) Uani 1 1 d U A 1 Ni2 Ni -0.10747(6) 0.26184(17) 0.25770(7) 0.0254(4) Uani 1 1 d U A 1 Ni3 Ni -0.09292(7) 0.1350(2) 0.36367(7) 0.0344(5) Uani 1 1 d U A 1 Cl1 Cl -0.04453(11) 0.4067(4) 0.25589(13) 0.0279(8) Uani 1 1 d U A 1 Cl2 Cl -0.15718(12) 0.1080(4) 0.28605(14) 0.0340(9) Uani 1 1 d U A 1 Cl3 Cl -0.02296(13) 0.2061(4) 0.42335(14) 0.0383(9) Uani 1 1 d U A 1 Cl4 Cl -0.1134(2) 0.3658(5) 0.3453(2) 0.0346(12) Uani 0.617(7) 1 d PU A 1 Cl5 Cl -0.03843(18) 0.1132(6) 0.2953(2) 0.0268(12) Uani 0.617(7) 1 d PU A 1 N1 N 0.0507(4) 0.3335(11) 0.3527(5) 0.028(2) Uani 1 1 d U A 1 N2 N 0.0025(4) 0.4886(11) 0.3811(5) 0.027(2) Uani 1 1 d U A 1 N3 N -0.1163(3) 0.2061(10) 0.1772(4) 0.0201(19) Uani 1 1 d U A 1 N4 N -0.1589(4) 0.3693(12) 0.2092(5) 0.026(2) Uani 1 1 d U A 1 N5 N -0.0867(4) -0.0501(12) 0.3885(5) 0.032(2) Uani 1 1 d U A 1 N6 N -0.1323(4) 0.1054(11) 0.4209(5) 0.030(2) Uani 1 1 d U A 1 C1 C 0.0478(5) 0.4653(15) 0.3624(6) 0.034(3) Uani 1 1 d U A 1 H1A H 0.0477 0.5112 0.3293 0.04 Uiso 1 1 calc R A 1 H1B H 0.0753 0.492 0.3898 0.04 Uiso 1 1 calc R A 1 C2 C 0.0676(5) 0.3189(16) 0.3025(6) 0.047(4) Uani 1 1 d U A 1 H2A H 0.0459 0.3606 0.2736 0.07 Uiso 1 1 calc R A 1 H2B H 0.0688 0.2321 0.2941 0.07 Uiso 1 1 calc R A 1 H2C H 0.0992 0.3542 0.3068 0.07 Uiso 1 1 calc R A 1 C3 C 0.0805(5) 0.2746(16) 0.3921(6) 0.040(3) Uani 1 1 d U A 1 H3A H 0.0687 0.28 0.425 0.06 Uiso 1 1 calc R A 1 H3B H 0.1119 0.312 0.3976 0.06 Uiso 1 1 calc R A 1 H3C H 0.0826 0.1889 0.3823 0.06 Uiso 1 1 calc R A 1 C4 C -0.0201(6) 0.6025(15) 0.3568(7) 0.045(4) Uani 1 1 d U A 1 H4A H -0.024 0.5983 0.318 0.067 Uiso 1 1 calc R A 1 H4B H -0.0001 0.6723 0.3704 0.067 Uiso 1 1 calc R A 1 H4C H -0.0511 0.6119 0.3659 0.067 Uiso 1 1 calc R A 1 C5 C 0.0094(5) 0.4904(14) 0.4381(5) 0.037(3) Uani 1 1 d U A 1 H5A H -0.0209 0.5053 0.4481 0.056 Uiso 1 1 calc R A 1 H5B H 0.0317 0.5554 0.4525 0.056 Uiso 1 1 calc R A 1 H5C H 0.0222 0.4119 0.4525 0.056 Uiso 1 1 calc R A 1 C6 C -0.1441(5) 0.3274(13) 0.1604(5) 0.025(3) Uani 1 1 d U A 1 H6A H -0.1236 0.3886 0.1484 0.03 Uiso 1 1 calc R A 1 H6B H -0.1719 0.3125 0.1314 0.03 Uiso 1 1 calc R A 1 C7 C -0.1429(5) 0.1008(13) 0.1613(6) 0.031(3) Uani 1 1 d U A 1 H7A H -0.1705 0.0998 0.1777 0.047 Uiso 1 1 calc R A 1 H7B H -0.1235 0.0287 0.1727 0.047 Uiso 1 1 calc R A 1 H7C H -0.1534 0.1002 0.1225 0.047 Uiso 1 1 calc R A 1 C8 C -0.0737(5) 0.2047(15) 0.1522(6) 0.032(3) Uani 1 1 d U A 1 H8A H -0.0552 0.279 0.162 0.048 Uiso 1 1 calc R A 1 H8B H -0.0841 0.2006 0.1134 0.048 Uiso 1 1 calc R A 1 H8C H -0.0541 0.1335 0.1649 0.048 Uiso 1 1 calc R A 1 C9 C -0.2104(4) 0.331(2) 0.2084(7) 0.052(5) Uani 1 1 d U A 1 H9A H -0.2191 0.3577 0.2414 0.078 Uiso 1 1 calc R A 1 H9B H -0.2133 0.2427 0.2052 0.078 Uiso 1 1 calc R A 1 H9C H -0.2315 0.3697 0.178 0.078 Uiso 1 1 calc R A 1 C10 C -0.1559(6) 0.5034(14) 0.2143(7) 0.040(4) Uani 1 1 d U A 1 H10A H -0.1648 0.5282 0.2475 0.06 Uiso 1 1 calc R A 1 H10B H -0.1775 0.541 0.1841 0.06 Uiso 1 1 calc R A 1 H10C H -0.1235 0.5298 0.2149 0.06 Uiso 1 1 calc R A 1 C11 C -0.1150(9) -0.0197(19) 0.4269(9) 0.113(8) Uani 1 1 d U A 1 H11A H -0.0957 -0.031 0.4632 0.135 Uiso 1 1 calc R A 1 H11B H -0.1422 -0.076 0.4224 0.135 Uiso 1 1 calc R A 1 C12 C -0.0408(6) -0.0913(19) 0.4148(9) 0.076(6) Uani 1 1 d U A 1 H12A H -0.0276 -0.0352 0.4438 0.114 Uiso 1 1 calc R A 1 H12B H -0.02 -0.094 0.3892 0.114 Uiso 1 1 calc R A 1 H12C H -0.0432 -0.1729 0.4293 0.114 Uiso 1 1 calc R A 1 C13 C -0.1049(9) -0.140(2) 0.3480(9) 0.102(8) Uani 1 1 d U A 1 H13A H -0.1363 -0.1156 0.3285 0.153 Uiso 1 1 calc R A 1 H13B H -0.1072 -0.2194 0.365 0.153 Uiso 1 1 calc R A 1 H13C H -0.0836 -0.1472 0.3233 0.153 Uiso 1 1 calc R A 1 C14 C -0.1193(7) 0.154(3) 0.4719(7) 0.079(7) Uani 1 1 d U A 1 H14A H -0.0851 0.1466 0.4847 0.118 Uiso 1 1 calc R A 1 H14B H -0.1356 0.1101 0.4959 0.118 Uiso 1 1 calc R A 1 H14C H -0.1283 0.2404 0.4711 0.118 Uiso 1 1 calc R A 1 C15 C -0.1838(6) 0.121(3) 0.4049(7) 0.070(6) Uani 1 1 d U A 1 H15A H -0.1951 0.0875 0.3693 0.105 Uiso 1 1 calc R A 1 H15B H -0.1915 0.2081 0.4048 0.105 Uiso 1 1 calc R A 1 H15C H -0.199 0.0787 0.4302 0.105 Uiso 1 1 calc R A 1 O4A O -0.0582(6) 0.1841(16) 0.3089(6) 0.0227(18) Uani 0.383(7) 1 d PU A 1 O5A O -0.0904(8) 0.305(3) 0.3383(9) 0.0243(19) Uani 0.383(7) 1 d PU A 1 Ni4 Ni 0.16680(6) 0.65491(18) 0.49412(7) 0.0280(4) Uani 1 1 d U B 2 Cl6 Cl 0.17515(14) 0.8527(4) 0.47599(14) 0.0381(9) Uani 1 1 d U B 2 Cl7 Cl 0.17905(16) 0.5230(4) 0.43164(16) 0.0471(11) Uani 1 1 d U B 2 Cl8 Cl 0.10428(15) 0.6390(6) 0.5315(2) 0.0649(15) Uani 1 1 d U B 2 N7 N 0.2209(4) 0.6237(11) 0.5569(4) 0.022(2) Uani 1 1 d U B 2 N8 N 0.2521(4) 0.6854(13) 0.6484(4) 0.031(3) Uani 1 1 d U B 2 C16 C 0.2174(5) 0.7033(15) 0.6005(5) 0.031(3) Uani 1 1 d U B 2 H16A H 0.2196 0.7885 0.5887 0.037 Uiso 1 1 calc R B 2 H16B H 0.1858 0.6926 0.6087 0.037 Uiso 1 1 calc R B 2 C17 C 0.2206(6) 0.4928(14) 0.5714(6) 0.042(4) Uani 1 1 d U B 2 H17A H 0.2235 0.4429 0.5407 0.062 Uiso 1 1 calc R B 2 H17B H 0.1909 0.4734 0.582 0.062 Uiso 1 1 calc R B 2 H17C H 0.2472 0.476 0.601 0.062 Uiso 1 1 calc R B 2 C18 C 0.2669(4) 0.6495(16) 0.5388(5) 0.033(3) Uani 1 1 d U B 2 H18A H 0.2695 0.5946 0.5096 0.05 Uiso 1 1 calc R B 2 H18B H 0.2938 0.6365 0.5686 0.05 Uiso 1 1 calc R B 2 H18C H 0.267 0.734 0.5267 0.05 Uiso 1 1 calc R B 2 C19 C 0.2798(6) 0.792(2) 0.6665(7) 0.063(6) Uani 1 1 d U B 2 H19A H 0.3029 0.7728 0.6992 0.094 Uiso 1 1 calc R B 2 H19B H 0.2589 0.8574 0.6737 0.094 Uiso 1 1 calc R B 2 H19C H 0.2964 0.8187 0.639 0.094 Uiso 1 1 calc R B 2 C20 C 0.2329(5) 0.6288(17) 0.6932(6) 0.045(4) Uani 1 1 d U B 2 H20A H 0.2586 0.6193 0.7246 0.067 Uiso 1 1 calc R B 2 H20B H 0.2194 0.5488 0.682 0.067 Uiso 1 1 calc R B 2 H20C H 0.2084 0.6816 0.7019 0.067 Uiso 1 1 calc R B 2 Ni5 Ni 0.08992(6) 0.96503(17) 0.13765(7) 0.0225(4) Uani 1 1 d U C 3 Ni6 Ni 0.02156(6) 0.77394(17) 0.15600(7) 0.0222(4) Uani 1 1 d U C 3 Ni7 Ni 0.10567(5) 0.83442(16) 0.24251(7) 0.0210(4) Uani 1 1 d U C 3 Cl9 Cl 0.15523(11) 0.9871(4) 0.21376(13) 0.0283(8) Uani 1 1 d U C 3 Cl10 Cl 0.02068(13) 0.8930(4) 0.07811(15) 0.0356(9) Uani 1 1 d U C 3 Cl11 Cl 0.04393(11) 0.6854(3) 0.24479(13) 0.0262(7) Uani 1 1 d U C 3 Cl12 Cl 0.03912(12) 0.9738(4) 0.20467(14) 0.0313(7) Uani 1 1 d U C 3 O1 O 0.0940(3) 0.7921(8) 0.1650(3) 0.0208(13) Uani 1 1 d U C 3 N9 N 0.1160(4) 0.8731(10) 0.3227(4) 0.023(2) Uani 1 1 d U C 3 N10 N 0.1604(4) 0.7267(12) 0.2909(5) 0.028(2) Uani 1 1 d U C 3 N11 N 0.0857(4) 1.1442(13) 0.1130(5) 0.035(2) Uani 1 1 d U C 3 N12 N 0.1324(4) 1.0019(12) 0.0786(5) 0.032(2) Uani 1 1 d U C 3 N13 N -0.0507(4) 0.7514(12) 0.1508(4) 0.028(2) Uani 1 1 d U C 3 N14 N -0.0037(4) 0.6095(12) 0.1203(5) 0.029(2) Uani 1 1 d U C 3 C21 C 0.1440(6) 0.7739(16) 0.3378(6) 0.036(3) Uani 1 1 d U C 3 H21A H 0.1259 0.7102 0.352 0.043 Uiso 1 1 calc R C 3 H21B H 0.1714 0.7969 0.3661 0.043 Uiso 1 1 calc R C 3 C22 C 0.0741(5) 0.8797(18) 0.3452(6) 0.042(4) Uani 1 1 d U C 3 H22A H 0.0566 0.9543 0.3329 0.063 Uiso 1 1 calc R C 3 H22B H 0.0834 0.8804 0.3841 0.063 Uiso 1 1 calc R C 3 H22C H 0.054 0.8089 0.3336 0.063 Uiso 1 1 calc R C 3 C23 C 0.1444(6) 0.9918(15) 0.3386(5) 0.038(4) Uani 1 1 d U C 3 H23A H 0.1239 1.0622 0.3274 0.056 Uiso 1 1 calc R C 3 H23B H 0.1713 0.9945 0.3213 0.056 Uiso 1 1 calc R C 3 H23C H 0.1557 0.9939 0.3773 0.056 Uiso 1 1 calc R C 3 C24 C 0.1564(6) 0.5928(15) 0.2866(6) 0.037(3) Uani 1 1 d U C 3 H24A H 0.1236 0.5686 0.2853 0.056 Uiso 1 1 calc R C 3 H24B H 0.177 0.5554 0.3176 0.056 Uiso 1 1 calc R C 3 H24C H 0.166 0.5657 0.2542 0.056 Uiso 1 1 calc R C 3 C25 C 0.2070(4) 0.7576(16) 0.2912(6) 0.040(3) Uani 1 1 d U C 3 H25A H 0.2104 0.8464 0.2926 0.06 Uiso 1 1 calc R C 3 H25B H 0.2156 0.7269 0.2588 0.06 Uiso 1 1 calc R C 3 H25C H 0.2278 0.7215 0.3224 0.06 Uiso 1 1 calc R C 3 C26 C 0.1239(7) 1.1306(16) 0.0837(8) 0.072(5) Uani 1 1 d U C 3 H26A H 0.1145 1.1684 0.0481 0.086 Uiso 1 1 calc R C 3 H26B H 0.1529 1.1713 0.1032 0.086 Uiso 1 1 calc R C 3 C27 C 0.0403(6) 1.1861(18) 0.0781(8) 0.070(5) Uani 1 1 d U C 3 H27A H 0.0159 1.1921 0.0992 0.106 Uiso 1 1 calc R C 3 H27B H 0.0303 1.1275 0.0492 0.106 Uiso 1 1 calc R C 3 H27C H 0.045 1.266 0.0631 0.106 Uiso 1 1 calc R C 3 C28 C 0.1026(6) 1.2367(14) 0.1527(6) 0.051(4) Uani 1 1 d U C 3 H28A H 0.0788 1.2514 0.1739 0.076 Uiso 1 1 calc R C 3 H28B H 0.1085 1.3123 0.1349 0.076 Uiso 1 1 calc R C 3 H28C H 0.132 1.2091 0.176 0.076 Uiso 1 1 calc R C 3 C29 C 0.1129(7) 0.940(2) 0.0248(6) 0.071(6) Uani 1 1 d U C 3 H29A H 0.1219 0.8544 0.0268 0.106 Uiso 1 1 calc R C 3 H29B H 0.1259 0.9806 -0.003 0.106 Uiso 1 1 calc R C 3 H29C H 0.0784 0.9473 0.0162 0.106 Uiso 1 1 calc R C 3 C30 C 0.1822(5) 0.987(2) 0.0930(6) 0.062(6) Uani 1 1 d U C 3 H30A H 0.1902 0.9013 0.0894 0.093 Uiso 1 1 calc R C 3 H30B H 0.1935 1.0128 0.13 0.093 Uiso 1 1 calc R C 3 H30C H 0.1972 1.0368 0.0697 0.093 Uiso 1 1 calc R C 3 C31 C -0.0483(5) 0.6213(16) 0.1365(6) 0.035(3) Uani 1 1 d U C 3 H31A H -0.0491 0.5684 0.1674 0.042 Uiso 1 1 calc R C 3 H31B H -0.0749 0.5993 0.107 0.042 Uiso 1 1 calc R C 3 C32 C -0.0814(4) 0.8316(18) 0.1048(6) 0.043(4) Uani 1 1 d U C 3 H32A H -0.0809 0.9167 0.1163 0.064 Uiso 1 1 calc R C 3 H32B H -0.1141 0.802 0.0969 0.064 Uiso 1 1 calc R C 3 H32C H -0.0683 0.8255 0.0727 0.064 Uiso 1 1 calc R C 3 C33 C -0.0691(4) 0.7774(16) 0.2000(5) 0.037(4) Uani 1 1 d U C 3 H33A H -0.0694 0.8656 0.2058 0.056 Uiso 1 1 calc R C 3 H33B H -0.0487 0.7384 0.2307 0.056 Uiso 1 1 calc R C 3 H33C H -0.1013 0.7454 0.1956 0.056 Uiso 1 1 calc R C 3 C34 C -0.0096(6) 0.604(2) 0.0596(6) 0.055(5) Uani 1 1 d U C 3 H34A H -0.025 0.6792 0.0438 0.083 Uiso 1 1 calc R C 3 H34B H -0.0291 0.5341 0.0456 0.083 Uiso 1 1 calc R C 3 H34C H 0.0215 0.5968 0.0506 0.083 Uiso 1 1 calc R C 3 C35 C 0.0192(5) 0.4941(13) 0.1385(6) 0.032(3) Uani 1 1 d U C 3 H35A H 0.0491 0.4878 0.1267 0.047 Uiso 1 1 calc R C 3 H35B H -0.0015 0.4265 0.1236 0.047 Uiso 1 1 calc R C 3 H35C H 0.0253 0.4905 0.1774 0.047 Uiso 1 1 calc R C 3 C36 C 0.1181(4) 0.7056(11) 0.1450(4) 0.021(2) Uani 1 1 d U C 3 H36A H 0.1067 0.701 0.1064 0.031 Uiso 1 1 calc R C 3 H36B H 0.1134 0.6269 0.161 0.031 Uiso 1 1 calc R C 3 H36C H 0.1518 0.7259 0.153 0.031 Uiso 1 1 calc R C 3 Ni8 Ni 0.33277(6) 0.93433(17) 0.00529(7) 0.0274(4) Uani 1 1 d U D 4 Cl13 Cl 0.32570(14) 0.7364(4) 0.02343(15) 0.0348(9) Uani 1 1 d U D 4 Cl14 Cl 0.39432(13) 0.9601(4) -0.03482(16) 0.0407(9) Uani 1 1 d U D 4 Cl15 Cl 0.32100(14) 1.0677(4) 0.06722(16) 0.0441(10) Uani 1 1 d U D 4 N15 N 0.2764(4) 0.9633(12) -0.0561(4) 0.025(2) Uani 1 1 d U D 4 N16 N 0.2456(4) 0.9078(13) -0.1509(5) 0.033(3) Uani 1 1 d U D 4 C37 C 0.2831(5) 0.8854(14) -0.1026(5) 0.028(3) Uani 1 1 d U D 4 H37A H 0.3143 0.9034 -0.1108 0.034 Uiso 1 1 calc R D 4 H37B H 0.2828 0.7984 -0.0927 0.034 Uiso 1 1 calc R D 4 C38 C 0.2328(4) 0.9374(17) -0.0417(6) 0.039(4) Uani 1 1 d U D 4 H38A H 0.2324 0.8521 -0.0307 0.058 Uiso 1 1 calc R D 4 H38B H 0.2068 0.952 -0.0723 0.058 Uiso 1 1 calc R D 4 H38C H 0.2291 0.9903 -0.0121 0.058 Uiso 1 1 calc R D 4 C39 C 0.2774(5) 1.0936(14) -0.0719(6) 0.034(3) Uani 1 1 d U D 4 H39A H 0.3077 1.1117 -0.0815 0.051 Uiso 1 1 calc R D 4 H39B H 0.2737 1.1455 -0.0421 0.051 Uiso 1 1 calc R D 4 H39C H 0.2516 1.1094 -0.1025 0.051 Uiso 1 1 calc R D 4 C40 C 0.2163(5) 0.8001(16) -0.1675(7) 0.049(5) Uani 1 1 d U D 4 H40A H 0.2024 0.7722 -0.1381 0.074 Uiso 1 1 calc R D 4 H40B H 0.2359 0.7352 -0.1776 0.074 Uiso 1 1 calc R D 4 H40C H 0.1911 0.8208 -0.1981 0.074 Uiso 1 1 calc R D 4 C41 C 0.2656(5) 0.9495(14) -0.1924(5) 0.034(3) Uani 1 1 d U D 4 H41A H 0.2856 1.0204 -0.1804 0.052 Uiso 1 1 calc R D 4 H41B H 0.2405 0.9726 -0.2227 0.052 Uiso 1 1 calc R D 4 H41C H 0.2849 0.8848 -0.2032 0.052 Uiso 1 1 calc R D 4 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 0.0332(9) 0.0324(11) 0.0185(10) 0.0055(8) 0.0010(8) -0.0164(9) Ni2 0.0301(9) 0.0311(11) 0.0148(9) 0.0021(8) 0.0040(7) -0.0081(9) Ni3 0.0427(11) 0.0405(11) 0.0187(10) 0.0063(9) 0.0037(8) -0.0172(10) Cl1 0.0322(17) 0.0317(19) 0.0187(17) 0.0059(15) 0.0027(14) -0.0118(16) Cl2 0.0372(17) 0.042(2) 0.0208(18) 0.0040(17) 0.0028(14) -0.0147(17) Cl3 0.048(2) 0.044(2) 0.0186(17) 0.0140(16) -0.0027(15) -0.0195(19) Cl4 0.046(3) 0.033(3) 0.024(2) -0.0008(19) 0.0059(19) -0.004(2) Cl5 0.027(2) 0.034(3) 0.017(2) 0.004(2) -0.0003(19) -0.014(2) N1 0.035(4) 0.018(5) 0.029(6) 0.000(4) 0.000(4) -0.013(4) N2 0.035(5) 0.023(4) 0.023(5) 0.004(4) 0.004(4) -0.006(4) N3 0.026(5) 0.017(5) 0.017(4) 0.001(3) 0.004(3) 0.002(3) N4 0.030(4) 0.031(5) 0.019(5) -0.002(4) 0.009(4) 0.002(4) N5 0.043(6) 0.025(4) 0.034(6) 0.005(4) 0.018(4) -0.002(4) N6 0.043(5) 0.023(5) 0.027(5) -0.003(4) 0.013(4) -0.007(4) C1 0.032(6) 0.026(6) 0.042(8) 0.012(6) 0.006(6) -0.013(4) C2 0.043(8) 0.051(10) 0.052(8) 0.025(7) 0.020(7) 0.033(8) C3 0.042(6) 0.034(7) 0.038(7) 0.003(7) -0.005(6) 0.001(7) C4 0.050(9) 0.031(6) 0.043(8) 0.004(6) -0.013(7) 0.010(7) C5 0.059(9) 0.023(8) 0.028(6) 0.002(5) 0.006(6) -0.018(7) C6 0.045(7) 0.015(5) 0.017(5) 0.002(5) 0.013(5) -0.004(5) C7 0.043(8) 0.015(6) 0.038(8) -0.007(6) 0.015(7) -0.004(6) C8 0.035(6) 0.030(7) 0.033(7) -0.008(6) 0.016(6) -0.006(5) C9 0.029(5) 0.076(12) 0.056(11) 0.014(10) 0.021(6) -0.003(7) C10 0.049(9) 0.022(6) 0.050(11) -0.009(6) 0.015(8) 0.011(6) C11 0.193(19) 0.055(9) 0.137(16) 0.059(9) 0.143(16) 0.057(12) C12 0.060(9) 0.036(10) 0.117(17) 0.006(10) -0.013(8) 0.002(8) C13 0.16(2) 0.043(9) 0.079(15) -0.011(10) -0.027(12) -0.034(14) C14 0.078(11) 0.132(17) 0.034(8) -0.028(11) 0.031(7) -0.050(14) C15 0.051(7) 0.111(17) 0.053(11) -0.006(12) 0.023(6) -0.010(9) O4A 0.029(5) 0.021(5) 0.015(5) 0.007(4) -0.002(3) -0.009(3) O5A 0.024(4) 0.036(5) 0.013(5) 0.008(4) 0.004(4) -0.008(4) Ni4 0.0350(10) 0.0280(10) 0.0198(10) -0.0030(9) 0.0031(8) -0.0007(9) Cl6 0.063(2) 0.030(2) 0.0210(18) 0.0031(17) 0.0087(17) 0.002(2) Cl7 0.074(3) 0.039(2) 0.027(2) -0.0080(19) 0.008(2) 0.008(2) Cl8 0.036(2) 0.101(4) 0.061(3) -0.029(3) 0.017(2) -0.023(3) N7 0.029(4) 0.017(5) 0.020(4) 0.004(4) 0.005(4) 0.006(4) N8 0.033(6) 0.046(8) 0.015(5) 0.004(5) 0.007(4) 0.000(6) C16 0.028(7) 0.033(7) 0.029(5) 0.005(5) 0.002(4) 0.009(6) C17 0.077(11) 0.022(6) 0.029(8) 0.011(5) 0.018(7) -0.002(7) C18 0.045(6) 0.048(9) 0.007(5) 0.012(6) 0.006(4) -0.001(7) C19 0.054(9) 0.093(14) 0.033(9) 0.004(9) -0.007(7) -0.027(10) C20 0.066(9) 0.053(10) 0.022(7) 0.008(7) 0.026(7) 0.007(8) Ni5 0.0307(9) 0.0217(8) 0.0166(9) 0.0030(7) 0.0083(7) -0.0054(8) Ni6 0.0272(8) 0.0261(10) 0.0136(9) 0.0013(8) 0.0051(7) -0.0029(8) Ni7 0.0259(8) 0.0232(9) 0.0143(8) 0.0009(8) 0.0048(7) -0.0034(8) Cl9 0.0330(16) 0.029(2) 0.0228(17) 0.0013(15) 0.0063(14) -0.0097(15) Cl10 0.0390(18) 0.046(2) 0.0197(17) 0.0067(16) 0.0018(14) -0.0128(18) Cl11 0.0354(17) 0.0272(18) 0.0171(16) 0.0026(14) 0.0084(14) -0.0035(15) Cl12 0.0426(18) 0.0256(16) 0.0285(18) 0.0010(15) 0.0139(15) 0.0054(15) O1 0.032(3) 0.013(3) 0.016(3) -0.001(2) 0.002(3) -0.011(3) N9 0.033(5) 0.020(5) 0.016(4) -0.003(4) 0.007(4) -0.004(4) N10 0.032(5) 0.027(5) 0.025(5) 0.003(4) 0.004(4) 0.005(4) N11 0.044(6) 0.035(5) 0.026(6) 0.010(4) 0.011(4) -0.004(4) N12 0.042(5) 0.035(6) 0.018(5) 0.004(4) 0.007(4) -0.009(5) N13 0.028(4) 0.037(6) 0.020(5) 0.015(4) 0.009(4) 0.006(4) N14 0.037(5) 0.031(5) 0.018(5) -0.008(4) 0.005(5) -0.006(4) C21 0.046(8) 0.040(7) 0.021(5) 0.008(6) 0.002(6) 0.013(7) C22 0.048(7) 0.066(11) 0.017(6) -0.012(7) 0.016(6) 0.006(7) C23 0.054(9) 0.041(7) 0.011(6) -0.007(6) -0.008(6) -0.006(7) C24 0.061(10) 0.031(6) 0.023(8) 0.007(6) 0.016(8) 0.010(6) C25 0.035(5) 0.043(9) 0.039(9) -0.002(7) -0.002(5) 0.010(6) C26 0.110(10) 0.028(6) 0.104(13) 0.013(6) 0.080(10) -0.015(7) C27 0.071(9) 0.045(10) 0.076(12) 0.035(9) -0.027(8) -0.010(8) C28 0.086(12) 0.019(6) 0.042(8) 0.014(6) 0.003(7) -0.012(8) C29 0.093(11) 0.110(15) 0.015(6) -0.010(8) 0.022(6) -0.049(13) C30 0.041(6) 0.128(17) 0.020(7) 0.024(10) 0.015(5) -0.004(9) C31 0.031(6) 0.036(6) 0.036(8) -0.003(6) 0.006(6) -0.008(5) C32 0.029(6) 0.060(10) 0.037(7) 0.027(8) 0.004(6) 0.010(7) C33 0.037(7) 0.051(9) 0.028(6) -0.008(6) 0.017(6) -0.016(7) C34 0.068(11) 0.076(13) 0.021(6) -0.017(6) 0.006(7) -0.014(11) C35 0.043(7) 0.026(6) 0.035(7) -0.013(5) 0.029(6) -0.010(5) C36 0.017(4) 0.028(5) 0.016(5) 0.010(4) -0.001(4) -0.006(4) Ni8 0.0326(10) 0.0273(11) 0.0211(10) 0.0001(8) 0.0031(8) 0.0011(9) Cl13 0.052(2) 0.0292(19) 0.026(2) 0.0015(17) 0.0140(17) 0.0037(18) Cl14 0.0344(18) 0.044(2) 0.044(2) 0.0009(19) 0.0101(16) -0.0083(19) Cl15 0.060(2) 0.041(2) 0.028(2) -0.0131(19) 0.0005(18) 0.010(2) N15 0.036(5) 0.020(5) 0.020(4) -0.005(4) 0.009(4) -0.004(5) N16 0.038(6) 0.032(7) 0.027(5) -0.006(5) 0.002(4) -0.007(6) C37 0.040(7) 0.028(7) 0.018(5) -0.007(5) 0.012(4) 0.004(6) C38 0.021(5) 0.054(10) 0.046(9) -0.015(8) 0.021(5) 0.006(6) C39 0.038(7) 0.027(6) 0.033(8) -0.006(5) -0.002(6) 0.004(6) C40 0.052(9) 0.044(10) 0.053(10) -0.023(8) 0.014(7) -0.022(7) C41 0.049(8) 0.027(7) 0.023(6) 0.003(5) 0.000(5) -0.002(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O5A 1.90(2) . ? Ni1 O4A 1.944(16) . ? Ni1 N2 2.112(13) . ? Ni1 N1 2.141(11) . ? Ni1 Cl3 2.388(4) . ? Ni1 Cl1 2.419(4) . ? Ni1 Cl4 2.624(6) . ? Ni1 Cl5 2.628(6) . ? Ni1 Ni3 2.980(3) . ? Ni2 O4A 1.925(16) . ? Ni2 O5A 2.08(2) . ? Ni2 N4 2.093(12) . ? Ni2 N3 2.123(11) . ? Ni2 Cl1 2.429(4) . ? Ni2 Cl2 2.431(4) . ? Ni2 Cl4 2.564(6) . ? Ni2 Cl5 2.604(6) . ? Ni3 O4A 1.972(16) . ? Ni3 O5A 1.99(3) . ? Ni3 N6 2.069(11) . ? Ni3 N5 2.127(13) . ? Ni3 Cl3 2.399(4) . ? Ni3 Cl2 2.442(4) . ? Ni3 Cl5 2.613(6) . ? Ni3 Cl4 2.624(6) . ? Cl4 O5A 0.98(3) . ? Cl5 O4A 1.069(18) . ? N1 C3 1.350(18) . ? N1 C1 1.47(2) . ? N1 C2 1.484(18) . ? N2 C5 1.438(17) . ? N2 C4 1.487(19) . ? N2 C1 1.511(17) . ? N3 C7 1.403(18) . ? N3 C8 1.508(15) . ? N3 C6 1.570(17) . ? N4 C10 1.48(2) . ? N4 C6 1.482(16) . ? N4 C9 1.546(16) . ? N5 C12 1.43(2) . ? N5 C13 1.45(2) . ? N5 C11 1.448(19) . ? N6 C14 1.40(2) . ? N6 C11 1.46(2) . ? N6 C15 1.47(2) . ? Ni4 N7 2.025(11) . ? Ni4 Cl8 2.231(4) . ? Ni4 Cl6 2.247(5) . ? Ni4 Cl7 2.248(4) . ? N7 C16 1.443(18) . ? N7 C17 1.486(18) . ? N7 C18 1.530(15) . ? N8 C19 1.44(2) . ? N8 C16 1.430(17) . ? N8 C20 1.516(16) . ? Ni5 O1 2.021(9) . ? Ni5 N11 2.064(14) . ? Ni5 N12 2.188(11) . ? Ni5 Cl10 2.386(4) . ? Ni5 Cl9 2.429(4) . ? Ni5 Cl12 2.496(4) . ? Ni5 Ni6 2.992(3) . ? Ni6 O1 2.073(8) . ? Ni6 N13 2.085(11) . ? Ni6 N14 2.088(12) . ? Ni6 Cl10 2.389(4) . ? Ni6 Cl11 2.441(4) . ? Ni6 Cl12 2.526(4) . ? Ni7 O1 2.005(8) . ? Ni7 N9 2.065(11) . ? Ni7 N10 2.151(12) . ? Ni7 Cl9 2.424(4) . ? Ni7 Cl11 2.435(4) . ? Ni7 Cl12 2.493(4) . ? O1 C36 1.344(14) . ? N9 C21 1.363(19) . ? N9 C22 1.454(15) . ? N9 C23 1.550(19) . ? N10 C25 1.389(17) . ? N10 C24 1.48(2) . ? N10 C21 1.483(18) . ? N11 C28 1.45(2) . ? N11 C26 1.473(18) . ? N11 C27 1.50(2) . ? N12 C30 1.420(18) . ? N12 C26 1.45(2) . ? N12 C29 1.54(2) . ? N13 C31 1.48(2) . ? N13 C33 1.502(15) . ? N13 C32 1.589(18) . ? N14 C31 1.446(17) . ? N14 C35 1.46(2) . ? N14 C34 1.535(17) . ? Ni8 N15 2.040(11) . ? Ni8 Cl13 2.243(5) . ? Ni8 Cl15 2.244(4) . ? Ni8 Cl14 2.260(4) . ? N15 C38 1.420(15) . ? N15 C39 1.49(2) . ? N15 C37 1.517(16) . ? N16 C41 1.397(17) . ? N16 C40 1.466(19) . ? N16 C37 1.487(18) . ? 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 O5A Ni1 O4A 58.4(10) . . ? O5A Ni1 N2 113.5(9) . . ? O4A Ni1 N2 171.2(6) . . ? O5A Ni1 N1 177.0(9) . . ? O4A Ni1 N1 119.1(6) . . ? N2 Ni1 N1 69.1(4) . . ? O5A Ni1 Cl3 81.6(7) . . ? O4A Ni1 Cl3 83.9(4) . . ? N2 Ni1 Cl3 98.8(3) . . ? N1 Ni1 Cl3 96.6(3) . . ? O5A Ni1 Cl1 85.3(7) . . ? O4A Ni1 Cl1 81.5(4) . . ? N2 Ni1 Cl1 94.8(3) . . ? N1 Ni1 Cl1 96.1(3) . . ? Cl3 Ni1 Cl1 163.99(15) . . ? O5A Ni1 Cl4 17.0(9) . . ? O4A Ni1 Cl4 75.1(6) . . ? N2 Ni1 Cl4 96.6(3) . . ? N1 Ni1 Cl4 165.7(4) . . ? Cl3 Ni1 Cl4 86.08(17) . . ? Cl1 Ni1 Cl4 84.02(16) . . ? O5A Ni1 Cl5 79.3(9) . . ? O4A Ni1 Cl5 21.0(5) . . ? N2 Ni1 Cl5 167.0(3) . . ? N1 Ni1 Cl5 98.2(3) . . ? Cl3 Ni1 Cl5 84.80(17) . . ? Cl1 Ni1 Cl5 83.78(16) . . ? Cl4 Ni1 Cl5 96.09(18) . . ? O5A Ni1 Ni3 41.1(8) . . ? O4A Ni1 Ni3 40.8(5) . . ? N2 Ni1 Ni3 136.2(3) . . ? N1 Ni1 Ni3 136.0(3) . . ? Cl3 Ni1 Ni3 51.66(11) . . ? Cl1 Ni1 Ni3 112.37(11) . . ? Cl4 Ni1 Ni3 55.40(14) . . ? Cl5 Ni1 Ni3 55.11(12) . . ? O4A Ni2 O5A 55.7(9) . . ? O4A Ni2 N4 171.5(6) . . ? O5A Ni2 N4 116.9(8) . . ? O4A Ni2 N3 117.2(6) . . ? O5A Ni2 N3 172.6(8) . . ? N4 Ni2 N3 70.0(4) . . ? O4A Ni2 Cl1 81.6(5) . . ? O5A Ni2 Cl1 81.3(6) . . ? N4 Ni2 Cl1 93.5(3) . . ? N3 Ni2 Cl1 96.0(3) . . ? O4A Ni2 Cl2 83.5(5) . . ? O5A Ni2 Cl2 83.8(6) . . ? N4 Ni2 Cl2 100.3(3) . . ? N3 Ni2 Cl2 97.8(3) . . ? Cl1 Ni2 Cl2 163.07(14) . . ? O4A Ni2 Cl4 77.0(6) . . ? O5A Ni2 Cl4 21.4(7) . . ? N4 Ni2 Cl4 95.8(3) . . ? N3 Ni2 Cl4 165.8(3) . . ? Cl1 Ni2 Cl4 85.14(16) . . ? Cl2 Ni2 Cl4 83.78(16) . . ? O4A Ni2 Cl5 21.3(5) . . ? O5A Ni2 Cl5 76.9(8) . . ? N4 Ni2 Cl5 165.6(3) . . ? N3 Ni2 Cl5 96.0(3) . . ? Cl1 Ni2 Cl5 84.11(15) . . ? Cl2 Ni2 Cl5 84.84(16) . . ? Cl4 Ni2 Cl5 98.19(19) . . ? O4A Ni3 O5A 56.5(9) . . ? O4A Ni3 N6 173.0(7) . . ? O5A Ni3 N6 116.5(8) . . ? O4A Ni3 N5 116.9(6) . . ? O5A Ni3 N5 172.5(7) . . ? N6 Ni3 N5 70.1(5) . . ? O4A Ni3 Cl3 83.0(4) . . ? O5A Ni3 Cl3 79.6(7) . . ? N6 Ni3 Cl3 96.6(4) . . ? N5 Ni3 Cl3 96.5(4) . . ? O4A Ni3 Cl2 82.2(4) . . ? O5A Ni3 Cl2 85.4(7) . . ? N6 Ni3 Cl2 97.1(4) . . ? N5 Ni3 Cl2 97.5(4) . . ? Cl3 Ni3 Cl2 163.08(15) . . ? O4A Ni3 Cl5 21.7(5) . . ? O5A Ni3 Cl5 78.2(7) . . ? N6 Ni3 Cl5 165.3(4) . . ? N5 Ni3 Cl5 95.2(3) . . ? Cl3 Ni3 Cl5 84.92(16) . . ? Cl2 Ni3 Cl5 84.44(15) . . ? O4A Ni3 Cl4 74.7(6) . . ? O5A Ni3 Cl4 18.9(7) . . ? N6 Ni3 Cl4 98.2(4) . . ? N5 Ni3 Cl4 168.3(3) . . ? Cl3 Ni3 Cl4 85.87(18) . . ? Cl2 Ni3 Cl4 82.30(17) . . ? Cl5 Ni3 Cl4 96.46(19) . . ? O4A Ni3 Ni1 40.1(5) . . ? O5A Ni3 Ni1 38.8(7) . . ? N6 Ni3 Ni1 135.4(4) . . ? N5 Ni3 Ni1 134.1(3) . . ? Cl3 Ni3 Ni1 51.34(10) . . ? Cl2 Ni3 Ni1 111.75(12) . . ? Cl5 Ni3 Ni1 55.58(14) . . ? Cl4 Ni3 Ni1 55.41(14) . . ? Ni1 Cl1 Ni2 76.46(12) . . ? Ni2 Cl2 Ni3 76.33(12) . . ? Ni1 Cl3 Ni3 77.00(13) . . ? O5A Cl4 Ni2 50.5(14) . . ? O5A Cl4 Ni3 41.0(14) . . ? Ni2 Cl4 Ni3 70.94(16) . . ? O5A Cl4 Ni1 34.5(14) . . ? Ni2 Cl4 Ni1 70.63(15) . . ? Ni3 Cl4 Ni1 69.20(16) . . ? O4A Cl5 Ni2 40.7(8) . . ? O4A Cl5 Ni3 43.1(8) . . ? Ni2 Cl5 Ni3 70.49(16) . . ? O4A Cl5 Ni1 40.5(9) . . ? Ni2 Cl5 Ni1 69.96(17) . . ? Ni3 Cl5 Ni1 69.31(16) . . ? C3 N1 C1 113.3(13) . . ? C3 N1 C2 108.9(12) . . ? C1 N1 C2 107.1(12) . . ? C3 N1 Ni1 121.4(10) . . ? C1 N1 Ni1 88.5(9) . . ? C2 N1 Ni1 115.3(9) . . ? C5 N2 C4 111.7(13) . . ? C5 N2 C1 112.6(11) . . ? C4 N2 C1 110.1(12) . . ? C5 N2 Ni1 114.8(9) . . ? C4 N2 Ni1 116.7(9) . . ? C1 N2 Ni1 88.7(8) . . ? C7 N3 C8 108.5(11) . . ? C7 N3 C6 113.7(9) . . ? C8 N3 C6 108.1(10) . . ? C7 N3 Ni2 117.8(9) . . ? C8 N3 Ni2 118.7(8) . . ? C6 N3 Ni2 88.3(7) . . ? C10 N4 C6 111.3(12) . . ? C10 N4 C9 107.9(13) . . ? C6 N4 C9 110.9(12) . . ? C10 N4 Ni2 119.2(11) . . ? C6 N4 Ni2 91.9(8) . . ? C9 N4 Ni2 114.8(10) . . ? C12 N5 C13 106.3(16) . . ? C12 N5 C11 110.8(17) . . ? C13 N5 C11 118.2(18) . . ? C12 N5 Ni3 117.1(11) . . ? C13 N5 Ni3 116.3(12) . . ? C11 N5 Ni3 87.7(10) . . ? C14 N6 C11 104.2(19) . . ? C14 N6 C15 105.6(14) . . ? C11 N6 C15 116.5(18) . . ? C14 N6 Ni3 122.1(10) . . ? C11 N6 Ni3 89.7(9) . . ? C15 N6 Ni3 117.6(10) . . ? N1 C1 N2 107.7(11) . . ? N4 C6 N3 104.8(10) . . ? N5 C11 N6 112.1(14) . . ? Cl5 O4A Ni2 118.0(12) . . ? Cl5 O4A Ni1 118.5(12) . . ? Ni2 O4A Ni1 101.7(8) . . ? Cl5 O4A Ni3 115.2(11) . . ? Ni2 O4A Ni3 101.2(8) . . ? Ni1 O4A Ni3 99.1(8) . . ? Cl4 O5A Ni1 128(2) . . ? Cl4 O5A Ni3 120.1(17) . . ? Ni1 O5A Ni3 100.1(12) . . ? Cl4 O5A Ni2 108.1(17) . . ? Ni1 O5A Ni2 97.7(10) . . ? Ni3 O5A Ni2 95.4(12) . . ? N7 Ni4 Cl8 101.8(3) . . ? N7 Ni4 Cl6 103.3(4) . . ? Cl8 Ni4 Cl6 107.4(2) . . ? N7 Ni4 Cl7 104.3(3) . . ? Cl8 Ni4 Cl7 121.6(2) . . ? Cl6 Ni4 Cl7 115.79(16) . . ? C16 N7 C17 112.7(11) . . ? C16 N7 C18 109.5(11) . . ? C17 N7 C18 107.9(12) . . ? C16 N7 Ni4 110.3(8) . . ? C17 N7 Ni4 108.6(10) . . ? C18 N7 Ni4 107.7(7) . . ? C19 N8 C16 114.1(13) . . ? C19 N8 C20 110.9(12) . . ? C16 N8 C20 114.0(11) . . ? N8 C16 N7 115.7(12) . . ? O1 Ni5 N11 177.5(4) . . ? O1 Ni5 N12 114.6(4) . . ? N11 Ni5 N12 67.4(5) . . ? O1 Ni5 Cl10 83.8(3) . . ? N11 Ni5 Cl10 97.6(4) . . ? N12 Ni5 Cl10 97.8(3) . . ? O1 Ni5 Cl9 80.5(3) . . ? N11 Ni5 Cl9 97.9(4) . . ? N12 Ni5 Cl9 94.9(3) . . ? Cl10 Ni5 Cl9 162.87(15) . . ? O1 Ni5 Cl12 78.2(3) . . ? N11 Ni5 Cl12 99.8(3) . . ? N12 Ni5 Cl12 167.1(4) . . ? Cl10 Ni5 Cl12 85.26(14) . . ? Cl9 Ni5 Cl12 84.95(13) . . ? O1 Ni5 Ni6 43.7(2) . . ? N11 Ni5 Ni6 136.0(3) . . ? N12 Ni5 Ni6 136.8(3) . . ? Cl10 Ni5 Ni6 51.24(10) . . ? Cl9 Ni5 Ni6 111.80(11) . . ? Cl12 Ni5 Ni6 53.89(10) . . ? O1 Ni6 N13 177.0(4) . . ? O1 Ni6 N14 112.6(4) . . ? N13 Ni6 N14 67.4(5) . . ? O1 Ni6 Cl10 82.6(3) . . ? N13 Ni6 Cl10 100.4(3) . . ? N14 Ni6 Cl10 99.5(3) . . ? O1 Ni6 Cl11 82.7(3) . . ? N13 Ni6 Cl11 94.3(3) . . ? N14 Ni6 Cl11 93.8(4) . . ? Cl10 Ni6 Cl11 163.13(15) . . ? O1 Ni6 Cl12 76.6(3) . . ? N13 Ni6 Cl12 103.2(4) . . ? N14 Ni6 Cl12 170.3(3) . . ? Cl10 Ni6 Cl12 84.54(15) . . ? Cl11 Ni6 Cl12 84.09(13) . . ? O1 Ni6 Ni5 42.4(3) . . ? N13 Ni6 Ni5 139.7(4) . . ? N14 Ni6 Ni5 136.0(3) . . ? Cl10 Ni6 Ni5 51.15(11) . . ? Cl11 Ni6 Ni5 111.99(11) . . ? Cl12 Ni6 Ni5 52.96(9) . . ? O1 Ni7 N9 178.0(4) . . ? O1 Ni7 N10 113.3(4) . . ? N9 Ni7 N10 66.6(5) . . ? O1 Ni7 Cl9 80.9(3) . . ? N9 Ni7 Cl9 101.1(3) . . ? N10 Ni7 Cl9 98.3(3) . . ? O1 Ni7 Cl11 84.2(3) . . ? N9 Ni7 Cl11 93.8(3) . . ? N10 Ni7 Cl11 94.1(4) . . ? Cl9 Ni7 Cl11 163.47(14) . . ? O1 Ni7 Cl12 78.5(3) . . ? N9 Ni7 Cl12 101.5(3) . . ? N10 Ni7 Cl12 168.0(3) . . ? Cl9 Ni7 Cl12 85.12(13) . . ? Cl11 Ni7 Cl12 84.90(13) . . ? Ni7 Cl9 Ni5 76.48(11) . . ? Ni5 Cl10 Ni6 77.61(13) . . ? Ni7 Cl11 Ni6 76.10(11) . . ? Ni7 Cl12 Ni5 74.05(11) . . ? Ni7 Cl12 Ni6 73.57(12) . . ? Ni5 Cl12 Ni6 73.15(11) . . ? C36 O1 Ni7 123.6(7) . . ? C36 O1 Ni5 121.9(7) . . ? Ni7 O1 Ni5 96.5(4) . . ? C36 O1 Ni6 119.0(7) . . ? Ni7 O1 Ni6 94.9(3) . . ? Ni5 O1 Ni6 93.9(4) . . ? C21 N9 C22 115.0(13) . . ? C21 N9 C23 110.4(11) . . ? C22 N9 C23 107.0(12) . . ? C21 N9 Ni7 94.1(9) . . ? C22 N9 Ni7 116.8(9) . . ? C23 N9 Ni7 113.2(8) . . ? C25 N10 C24 107.7(13) . . ? C25 N10 C21 112.9(13) . . ? C24 N10 C21 112.0(13) . . ? C25 N10 Ni7 117.7(10) . . ? C24 N10 Ni7 117.9(11) . . ? C21 N10 Ni7 87.3(8) . . ? C28 N11 C26 104.6(13) . . ? C28 N11 C27 109.2(15) . . ? C26 N11 C27 112.5(15) . . ? C28 N11 Ni5 117.7(9) . . ? C26 N11 Ni5 93.3(10) . . ? C27 N11 Ni5 117.6(10) . . ? C30 N12 C26 105.8(16) . . ? C30 N12 C29 110.2(14) . . ? C26 N12 C29 118.3(16) . . ? C30 N12 Ni5 119.1(9) . . ? C26 N12 Ni5 89.1(9) . . ? C29 N12 Ni5 113.0(9) . . ? C31 N13 C33 115.9(12) . . ? C31 N13 C32 113.4(13) . . ? C33 N13 C32 106.2(11) . . ? C31 N13 Ni6 91.8(8) . . ? C33 N13 Ni6 117.1(8) . . ? C32 N13 Ni6 112.2(8) . . ? C31 N14 C35 111.0(12) . . ? C31 N14 C34 112.6(12) . . ? C35 N14 C34 103.9(12) . . ? C31 N14 Ni6 92.7(9) . . ? C35 N14 Ni6 121.1(9) . . ? C34 N14 Ni6 115.6(10) . . ? N9 C21 N10 108.8(12) . . ? N12 C26 N11 107.9(13) . . ? N14 C31 N13 104.5(12) . . ? N15 Ni8 Cl13 102.6(4) . . ? N15 Ni8 Cl15 103.3(3) . . ? Cl13 Ni8 Cl15 116.82(17) . . ? N15 Ni8 Cl14 101.9(3) . . ? Cl13 Ni8 Cl14 109.41(17) . . ? Cl15 Ni8 Cl14 119.75(18) . . ? C38 N15 C39 109.5(13) . . ? C38 N15 C37 111.3(11) . . ? C39 N15 C37 108.3(11) . . ? C38 N15 Ni8 112.2(9) . . ? C39 N15 Ni8 107.6(9) . . ? C37 N15 Ni8 107.9(8) . . ? C41 N16 C40 110.5(12) . . ? C41 N16 C37 110.0(10) . . ? C40 N16 C37 112.7(13) . . ? N16 C37 N15 111.8(11) . . ? #===END