Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global loop_ _publ_author_name 'Ingmar Persson' 'Dorota Bobicz' 'Olof Kristiansson' _publ_contact_author_name 'Prof Ingmar Persson' _publ_contact_author_address ; Department of Chemistry Swedish University of Agricultural Sciences P O Box 7015 Uppsala SE-750 07 SWEDEN ; _publ_contact_author_email INGMAR.PERSSON@KEMI.SLU.SE _database_code_CSD 184727 data_hexakis(dimethylsulfoxide)nickel(II)chloride _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(dimethylsulfoxide)nickel(II) chloride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Cl2 Ni O8 S8' _chemical_formula_weight 754.63 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'triclinic' _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9520(16) _cell_length_b 10.2209(16) _cell_length_c 11.0282(18) _cell_angle_alpha 64.208(4) _cell_angle_beta 66.751(3) _cell_angle_gamma 87.620(3) _cell_volume 916.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12015 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 1.367 _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 398 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6864 _exptl_absorpt_correction_T_max 0.8007 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 diffractometer with CCD area detector ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ; Neglible as determined from a repetition of the first 50 frames at the end of the experiment ; _diffrn_reflns_number 3807 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3140 _reflns_number_gt 1895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998b)' _computing_cell_refinement 'Bruker SMART and SAINT (1998b)' _computing_data_reduction 'Bruker SAINT (1998b)' _computing_structure_solution 'Bruker SHELXTL (1998a)' _computing_structure_refinement 'Bruker SHELXTL (1998a)' _computing_molecular_graphics 'Bruker SHELXTL (1998a)' _computing_publication_material 'Bruker SHELXTL (1998a)' _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^)+(0.0634P)^2^+0.0000P] 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 0.043(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3140 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _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 Ni1 Ni 0.5000 0.5000 0.0000 0.0357(3) Uani 1 2 d S . . Cl1 Cl 0.22194(16) 0.81565(15) 0.44955(16) 0.0755(4) Uani 1 1 d . . . S11 S 0.63769(13) 0.30313(12) 0.21153(14) 0.0469(3) Uani 1 1 d . . . S21 S 0.28133(12) 0.22404(11) 0.26328(13) 0.0469(3) Uani 1 1 d . . . S31 S 0.45591(12) 0.67539(12) 0.18127(14) 0.0471(3) Uani 1 1 d . . . S41 S -0.04123(18) 0.74770(17) 0.2065(2) 0.0851(5) Uani 1 1 d . . . O11 O 0.6278(3) 0.3404(3) 0.0671(3) 0.0448(8) Uani 1 1 d . . . O21 O 0.3159(3) 0.3898(3) 0.1986(3) 0.0460(8) Uani 1 1 d . . . O31 O 0.5662(3) 0.6154(3) 0.0837(3) 0.0453(8) Uani 1 1 d . . . O41 O -0.0695(6) 0.7495(5) 0.0894(6) 0.1220(17) Uani 1 1 d . . . C11 C 0.6738(8) 0.1207(5) 0.2764(7) 0.089(2) Uani 1 1 d . . . H11A H 0.5882 0.0552 0.3058 0.134 Uiso 1 1 calc R . . H11B H 0.6967 0.0958 0.3600 0.134 Uiso 1 1 calc R . . H11C H 0.7564 0.1119 0.1988 0.134 Uiso 1 1 calc R . . C12 C 0.8127(5) 0.3918(6) 0.1632(6) 0.0700(15) Uani 1 1 d . . . H12A H 0.8129 0.4961 0.1243 0.105 Uiso 1 1 calc R . . H12B H 0.8876 0.3711 0.0894 0.105 Uiso 1 1 calc R . . H12C H 0.8326 0.3566 0.2496 0.105 Uiso 1 1 calc R . . C21 C 0.1850(6) 0.1664(5) 0.4561(5) 0.0676(15) Uani 1 1 d . . . H21A H 0.2527 0.1789 0.4941 0.101 Uiso 1 1 calc R . . H21B H 0.1422 0.0646 0.5056 0.101 Uiso 1 1 calc R . . H21C H 0.1080 0.2245 0.4732 0.101 Uiso 1 1 calc R . . C22 C 0.1301(5) 0.1875(5) 0.2315(6) 0.0662(15) Uani 1 1 d . . . H22A H 0.1627 0.2136 0.1285 0.099 Uiso 1 1 calc R . . H22B H 0.0552 0.2445 0.2586 0.099 Uiso 1 1 calc R . . H22C H 0.0899 0.0848 0.2903 0.099 Uiso 1 1 calc R . . C31 C 0.5583(6) 0.8343(6) 0.1416(9) 0.121(3) Uani 1 1 d . . . H31A H 0.5733 0.9096 0.0449 0.181 Uiso 1 1 calc R . . H31B H 0.6525 0.8134 0.1438 0.181 Uiso 1 1 calc R . . H31C H 0.5055 0.8674 0.2142 0.181 Uiso 1 1 calc R . . C32 C 0.4444(9) 0.5665(7) 0.3585(7) 0.128(3) Uani 1 1 d . . . H32A H 0.3918 0.4703 0.3974 0.192 Uiso 1 1 calc R . . H32B H 0.3926 0.6105 0.4215 0.192 Uiso 1 1 calc R . . H32C H 0.5423 0.5583 0.3545 0.192 Uiso 1 1 calc R . . C41 C 0.1201(7) 0.8725(6) 0.1291(7) 0.0875(19) Uani 1 1 d . . . H41A H 0.1034 0.9705 0.0773 0.131 Uiso 1 1 calc R . . H41B H 0.1997 0.8488 0.0611 0.131 Uiso 1 1 calc R . . H41C H 0.1456 0.8664 0.2066 0.131 Uiso 1 1 calc R . . C42 C 0.0290(7) 0.5859(5) 0.2886(7) 0.0829(18) Uani 1 1 d . . . H42A H -0.0471 0.5021 0.3398 0.124 Uiso 1 1 calc R . . H42B H 0.0605 0.5933 0.3575 0.124 Uiso 1 1 calc R . . H42C H 0.1117 0.5748 0.2127 0.124 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 Ni1 0.0336(4) 0.0363(4) 0.0372(5) -0.0125(4) -0.0195(4) 0.0035(3) Cl1 0.0808(9) 0.0798(9) 0.0681(10) -0.0381(9) -0.0300(8) 0.0305(7) S11 0.0494(7) 0.0497(7) 0.0456(8) -0.0178(6) -0.0288(6) 0.0142(5) S21 0.0393(6) 0.0393(6) 0.0491(8) -0.0126(6) -0.0144(5) 0.0032(5) S31 0.0419(6) 0.0511(7) 0.0548(9) -0.0259(7) -0.0247(6) 0.0092(5) S41 0.0746(10) 0.0918(12) 0.1046(15) -0.0433(11) -0.0542(10) 0.0172(8) O11 0.0478(17) 0.0498(17) 0.045(2) -0.0200(16) -0.0304(15) 0.0185(14) O21 0.0438(16) 0.0379(16) 0.043(2) -0.0119(15) -0.0118(14) -0.0014(12) O31 0.0394(15) 0.0512(17) 0.058(2) -0.0275(17) -0.0288(15) 0.0085(13) O41 0.144(4) 0.103(3) 0.161(5) -0.063(4) -0.101(4) 0.023(3) C11 0.139(6) 0.053(3) 0.090(5) -0.020(3) -0.078(4) 0.035(3) C12 0.060(3) 0.081(4) 0.086(5) -0.037(4) -0.047(3) 0.012(3) C21 0.072(3) 0.064(3) 0.046(4) -0.009(3) -0.022(3) 0.002(3) C22 0.059(3) 0.068(3) 0.065(4) -0.023(3) -0.026(3) -0.009(2) C31 0.078(4) 0.097(4) 0.178(8) -0.102(5) 0.002(5) -0.014(3) C32 0.226(9) 0.107(5) 0.056(5) -0.043(4) -0.065(5) 0.095(6) C41 0.108(5) 0.064(3) 0.103(5) -0.024(4) -0.071(4) 0.004(3) C42 0.093(4) 0.065(3) 0.084(5) -0.015(4) -0.049(4) -0.002(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 Ni1 O31 2.041(3) . ? Ni1 O21 2.069(3) . ? Ni1 O11 2.085(3) . ? S11 O11 1.511(3) . ? S11 C11 1.762(5) . ? S11 C12 1.765(5) . ? S21 O21 1.517(3) . ? S21 C22 1.762(5) . ? S21 C21 1.771(5) . ? S31 O31 1.525(3) . ? S31 C32 1.735(6) . ? S31 C31 1.742(5) . ? S41 O41 1.418(5) . ? S41 C41 1.753(6) . ? S41 C42 1.773(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 O31 Ni1 O31 180.00(11) 2_665 . ? O31 Ni1 O21 89.19(11) 2_665 . ? O31 Ni1 O21 90.81(11) . . ? O31 Ni1 O11 90.06(11) 2_665 2_665 ? O31 Ni1 O11 89.94(11) . 2_665 ? O21 Ni1 O11 87.87(11) . 2_665 ? O21 Ni1 O11 92.13(11) 2_665 2_665 ? O31 Ni1 O11 89.94(11) 2_665 . ? O31 Ni1 O11 90.06(11) . . ? O21 Ni1 O11 92.13(11) . . ? O11 S11 C11 105.6(2) . . ? O11 S11 C12 106.2(2) . . ? C11 S11 C12 98.0(3) . . ? O21 S21 C22 106.9(2) . . ? O21 S21 C21 103.1(2) . . ? C22 S21 C21 97.7(2) . . ? O31 S31 C32 105.3(2) . . ? O31 S31 C31 103.6(2) . . ? C32 S31 C31 98.3(4) . . ? O41 S41 C41 108.4(3) . . ? O41 S41 C42 110.9(3) . . ? C41 S41 C42 97.0(3) . . ? S11 O11 Ni1 117.89(15) . . ? S21 O21 Ni1 117.90(16) . . ? S31 O31 Ni1 121.69(15) . . ? _diffrn_measured_fraction_theta_max 0.786 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.786 _refine_diff_density_max 0.655 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.074 #===END data_hexakis(dimethylsulfoxide)nickel(II)bromide _database_code_CSD 184728 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(dimethylsulfoxide)nickel(II) bromide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H48 Br2 Ni O8 S8' _chemical_formula_weight 843.55 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.900(5) _cell_length_b 10.380(6) _cell_length_c 11.295(6) _cell_angle_alpha 63.608(12) _cell_angle_beta 67.713(8) _cell_angle_gamma 87.889(9) _cell_volume 949.8(9) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12015 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 434 _exptl_absorpt_coefficient_mu 3.085 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3870 _exptl_absorpt_correction_T_max 0.5248 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 diffractometer with CCD area detector ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ; Approximately 20 % as determined from a repetition of the first 50 frames at the end of the experiment ; _diffrn_reflns_number 3516 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.1482 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3076 _reflns_number_gt 1346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998b)' _computing_cell_refinement 'Bruker SMART and SAINT (1998b)' _computing_data_reduction 'Bruker SAINT (1998b)' _computing_structure_solution 'Bruker SHELXTL (1998a)' _computing_structure_refinement 'Bruker SHELXTL (1998a)' _computing_molecular_graphics 'Bruker SHELXTL (1998a)' _computing_publication_material 'Bruker SHELXTL (1998a)' _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^)+(0.0600P)^2^+0.0000P] 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 0.048(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3076 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1676 _refine_ls_R_factor_gt 0.1100 _refine_ls_wR_factor_ref 0.2433 _refine_ls_wR_factor_gt 0.2355 _refine_ls_goodness_of_fit_ref 1.440 _refine_ls_restrained_S_all 1.440 _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 0.5000 0.5000 0.5000 0.0500(9) Uani 1 2 d S . . Br1 Br 0.23981(19) 0.8140(2) -0.0522(2) 0.0895(9) Uani 1 1 d . . . S11 S 0.5296(4) 0.3307(4) 0.3247(4) 0.0613(12) Uani 1 1 d . . . S21 S 0.7172(4) 0.7729(4) 0.2343(4) 0.0601(12) Uani 1 1 d . . . S31 S 0.3580(4) 0.6994(4) 0.2971(4) 0.0570(12) Uani 1 1 d . . . S41 S 0.0416(5) 0.2527(6) 0.2908(6) 0.0933(16) Uani 1 1 d . . . O11 O 0.4224(8) 0.3870(9) 0.4226(10) 0.056(3) Uani 1 1 d . . . O21 O 0.6862(9) 0.6084(11) 0.3041(10) 0.071(3) Uani 1 1 d . . . O31 O 0.3745(9) 0.6598(9) 0.4345(10) 0.059(3) Uani 1 1 d . . . O41 O 0.0684(13) 0.2483(15) 0.4103(15) 0.118(4) Uani 1 1 d . . . C11 C 0.518(3) 0.428(2) 0.163(2) 0.136(8) Uani 1 1 d . . . H11A H 0.5666 0.5266 0.1187 0.204 Uiso 1 1 calc R . . H11B H 0.4155 0.4291 0.1782 0.204 Uiso 1 1 calc R . . H11C H 0.5640 0.3850 0.1016 0.204 Uiso 1 1 calc R . . C12 C 0.4304(19) 0.1599(18) 0.381(2) 0.108(7) Uani 1 1 d . . . H12A H 0.4275 0.0906 0.4732 0.162 Uiso 1 1 calc R . . H12B H 0.4789 0.1257 0.3111 0.162 Uiso 1 1 calc R . . H12C H 0.3314 0.1712 0.3877 0.162 Uiso 1 1 calc R . . C21 C 0.8056(17) 0.8286(19) 0.0490(16) 0.099(6) Uani 1 1 d . . . H21A H 0.7354 0.8137 0.0147 0.149 Uiso 1 1 calc R . . H21B H 0.8834 0.7727 0.0317 0.149 Uiso 1 1 calc R . . H21C H 0.8467 0.9301 -0.0012 0.149 Uiso 1 1 calc R . . C22 C 0.8702(16) 0.8127(17) 0.2648(18) 0.077(5) Uani 1 1 d . . . H22A H 0.8389 0.7868 0.3651 0.116 Uiso 1 1 calc R . . H22B H 0.9085 0.9149 0.2069 0.116 Uiso 1 1 calc R . . H22C H 0.9459 0.7579 0.2389 0.116 Uiso 1 1 calc R . . C31 C 0.1783(15) 0.6111(16) 0.3519(19) 0.085(5) Uani 1 1 d . . . H31A H 0.1780 0.5080 0.3889 0.127 Uiso 1 1 calc R . . H31B H 0.1521 0.6472 0.2705 0.127 Uiso 1 1 calc R . . H31C H 0.1080 0.6303 0.4260 0.127 Uiso 1 1 calc R . . C32 C 0.322(2) 0.8819(17) 0.2338(19) 0.095(6) Uani 1 1 d . . . H32A H 0.4106 0.9466 0.2001 0.142 Uiso 1 1 calc R . . H32B H 0.2451 0.8913 0.3111 0.142 Uiso 1 1 calc R . . H32C H 0.2923 0.9065 0.1558 0.142 Uiso 1 1 calc R . . C41 C -0.118(2) 0.129(2) 0.373(2) 0.140(9) Uani 1 1 d . . . H41A H -0.0991 0.0326 0.4224 0.211 Uiso 1 1 calc R . . H41B H -0.1497 0.1341 0.3003 0.211 Uiso 1 1 calc R . . H41C H -0.1942 0.1521 0.4403 0.211 Uiso 1 1 calc R . . C42 C -0.030(2) 0.414(2) 0.210(2) 0.137(9) Uani 1 1 d . . . H42A H 0.0474 0.4962 0.1567 0.205 Uiso 1 1 calc R . . H42B H -0.1092 0.4258 0.2835 0.205 Uiso 1 1 calc R . . H42C H -0.0655 0.4053 0.1449 0.205 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 Ni1 0.0247(13) 0.071(2) 0.0456(16) -0.0204(14) -0.0128(11) -0.0005(11) Br1 0.0643(12) 0.1164(17) 0.0852(15) -0.0564(13) -0.0170(9) 0.0215(10) S11 0.038(2) 0.084(3) 0.068(3) -0.040(2) -0.0213(18) 0.0084(18) S21 0.0311(19) 0.069(3) 0.063(3) -0.022(2) -0.0120(16) 0.0023(16) S31 0.041(2) 0.072(3) 0.049(2) -0.019(2) -0.0200(16) 0.0112(17) S41 0.058(3) 0.121(4) 0.113(4) -0.066(4) -0.033(3) 0.020(3) O11 0.026(5) 0.070(7) 0.073(7) -0.038(6) -0.016(4) 0.013(4) O21 0.025(5) 0.100(9) 0.068(7) -0.032(6) -0.006(4) 0.004(5) O31 0.038(5) 0.079(7) 0.064(7) -0.036(6) -0.022(5) 0.023(4) O41 0.076(9) 0.180(13) 0.133(11) -0.085(10) -0.064(8) 0.034(8) C11 0.20(3) 0.139(18) 0.086(16) -0.063(15) -0.070(17) 0.077(17) C12 0.080(13) 0.087(13) 0.163(19) -0.087(14) -0.020(12) 0.001(10) C21 0.069(12) 0.141(16) 0.058(11) -0.012(11) -0.034(9) -0.033(10) C22 0.055(10) 0.094(12) 0.095(13) -0.052(11) -0.031(9) 0.005(8) C31 0.040(9) 0.105(13) 0.109(14) -0.044(11) -0.039(9) 0.019(8) C32 0.113(16) 0.099(14) 0.078(13) -0.037(11) -0.050(12) 0.029(11) C41 0.15(2) 0.114(17) 0.137(19) -0.011(15) -0.093(17) -0.045(14) C42 0.120(18) 0.120(16) 0.133(18) 0.002(14) -0.084(15) -0.038(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O11 2.054(9) . ? Ni1 O11 2.054(9) 2_666 ? Ni1 O31 2.073(8) 2_666 ? Ni1 O31 2.073(8) . ? Ni1 O21 2.099(9) . ? Ni1 O21 2.099(9) 2_666 ? S11 O11 1.526(9) . ? S11 C11 1.696(18) . ? S11 C12 1.780(15) . ? S21 O21 1.513(10) . ? S21 C21 1.747(16) . ? S21 C22 1.776(14) . ? S31 O31 1.492(9) . ? S31 C31 1.780(13) . ? S31 C32 1.778(15) . ? S41 O41 1.453(13) . ? S41 C41 1.728(17) . ? S41 C42 1.78(2) . ? 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 O11 Ni1 O11 180.0(3) . 2_666 ? O11 Ni1 O31 90.4(3) . 2_666 ? O11 Ni1 O31 89.6(3) 2_666 2_666 ? O11 Ni1 O31 89.6(3) . . ? O11 Ni1 O31 90.4(3) 2_666 . ? O31 Ni1 O31 180.0(6) 2_666 . ? O11 Ni1 O21 92.2(4) . . ? O11 Ni1 O21 87.8(4) 2_666 . ? O31 Ni1 O21 87.3(4) 2_666 . ? O31 Ni1 O21 92.7(4) . . ? O11 Ni1 O21 87.8(4) . 2_666 ? O11 Ni1 O21 92.2(4) 2_666 2_666 ? O31 Ni1 O21 92.7(4) 2_666 2_666 ? O31 Ni1 O21 87.3(4) . 2_666 ? O21 Ni1 O21 180.000(1) . 2_666 ? O11 S11 C11 104.1(8) . . ? O11 S11 C12 103.2(7) . . ? C11 S11 C12 99.4(10) . . ? O21 S21 C21 104.7(7) . . ? O21 S21 C22 105.1(6) . . ? C21 S21 C22 99.1(7) . . ? O31 S31 C31 105.0(7) . . ? O31 S31 C32 106.3(7) . . ? C31 S31 C32 98.2(8) . . ? O41 S41 C41 104.5(9) . . ? O41 S41 C42 110.7(10) . . ? C41 S41 C42 98.0(9) . . ? S11 O11 Ni1 120.3(4) . . ? S21 O21 Ni1 117.7(6) . . ? S31 O31 Ni1 119.1(5) . . ? _diffrn_measured_fraction_theta_max 0.740 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.740 _refine_diff_density_max 1.653 _refine_diff_density_min -2.181 _refine_diff_density_rms 0.183 data_hexakis(dimethylsulfoxide)nickel(II)tetrachloronickelate(II) _database_code_CSD 184729 _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis-(dimethylsulfoxide)-nickel(II) tetrachloronickelate(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 Ni O6 S6, Cl4 Ni' _chemical_formula_sum 'C12 H36 Cl4 Ni2 O6 S6' _chemical_formula_weight 727.99 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 18.950(2) _cell_length_b 18.950(2) _cell_length_c 8.5688(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3077.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3511 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'block' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 2.002 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.5409 _exptl_absorpt_correction_T_max 0.5850 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 CCD diffractometer' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ; Neglible as determined from a repetition of the first 50 frames at the end of the experiment ; _diffrn_reflns_number 18289 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3511 _reflns_number_gt 1695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998b)' _computing_cell_refinement 'Bruker SMART and SAINT (1998b)' _computing_data_reduction 'Bruker SAINT (1998b)' _computing_structure_solution 'Bruker SHELXTL (1998a)' _computing_structure_refinement 'Bruker SHELXTL (1998a)' _computing_molecular_graphics 'Bruker SHELXTL (1998a)' _computing_publication_material 'Bruker SHELXTL (1998a)' _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^)+(0.0731P)^2^+0.0000P] 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 3511 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.5000 0.5000 0.0000 0.0396(2) Uani 1 2 d S . . Ni2 Ni 0.7500 0.7500 0.5120(2) 0.1250(9) Uani 1 4 d S . . Ni3 Ni 0.2500 0.7500 0.5000 0.0556(4) Uani 1 4 d S . . Cl1 Cl 0.7500 0.7500 0.2519(3) 0.0682(8) Uani 1 4 d S . . Cl2 Cl 0.6351(2) 0.7874(3) 0.5748(5) 0.1945(19) Uani 0.75 1 d P . . Cl3 Cl 0.27034(9) 0.85094(10) 0.6310(2) 0.0932(6) Uani 1 1 d . . . S11 S 0.57906(7) 0.63310(7) 0.11423(17) 0.0540(4) Uani 1 1 d . . . S21 S 0.55349(8) 0.42361(7) 0.29470(16) 0.0576(4) Uani 1 1 d . . . S31 S 0.36833(6) 0.57089(7) 0.14032(16) 0.0490(4) Uani 1 1 d . . . O11 O 0.51338(16) 0.60677(16) 0.0331(4) 0.0503(9) Uani 1 1 d . . . O21 O 0.50765(17) 0.48421(17) 0.2387(4) 0.0508(9) Uani 1 1 d . . . O31 O 0.39184(16) 0.51420(16) 0.0253(4) 0.0475(9) Uani 1 1 d . . . C11 C 0.6333(3) 0.6649(3) -0.0391(7) 0.0716(18) Uani 1 1 d . . . H11A H 0.6524 0.6257 -0.0963 0.107 Uiso 1 1 calc R . . H11B H 0.6712 0.6923 0.0040 0.107 Uiso 1 1 calc R . . H11C H 0.6058 0.6939 -0.1078 0.107 Uiso 1 1 calc R . . C12 C 0.5529(3) 0.7154(3) 0.1960(7) 0.0709(17) Uani 1 1 d . . . H12A H 0.5223 0.7072 0.2834 0.106 Uiso 1 1 calc R . . H12B H 0.5284 0.7426 0.1186 0.106 Uiso 1 1 calc R . . H12C H 0.5939 0.7408 0.2302 0.106 Uiso 1 1 calc R . . C21 C 0.5054(4) 0.3828(3) 0.4462(8) 0.093(2) Uani 1 1 d . . . H21A H 0.4660 0.3577 0.4028 0.139 Uiso 1 1 calc R . . H21B H 0.4886 0.4182 0.5174 0.139 Uiso 1 1 calc R . . H21C H 0.5354 0.3504 0.5010 0.139 Uiso 1 1 calc R . . C22 C 0.6186(3) 0.4637(4) 0.4099(9) 0.093(2) Uani 1 1 d . . . H22A H 0.6507 0.4892 0.3441 0.140 Uiso 1 1 calc R . . H22B H 0.6439 0.4281 0.4667 0.140 Uiso 1 1 calc R . . H22C H 0.5968 0.4957 0.4821 0.140 Uiso 1 1 calc R . . C31 C 0.3337(3) 0.6387(3) 0.0181(7) 0.0688(17) Uani 1 1 d . . . H31A H 0.3717 0.6617 -0.0356 0.103 Uiso 1 1 calc R . . H31B H 0.3088 0.6725 0.0808 0.103 Uiso 1 1 calc R . . H31C H 0.3019 0.6183 -0.0566 0.103 Uiso 1 1 calc R . . C32 C 0.2875(3) 0.5396(3) 0.2197(7) 0.0711(17) Uani 1 1 d . . . H32A H 0.2969 0.5016 0.2907 0.107 Uiso 1 1 calc R . . H32B H 0.2576 0.5232 0.1369 0.107 Uiso 1 1 calc R . . H32C H 0.2644 0.5773 0.2745 0.107 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 Ni1 0.0383(5) 0.0377(5) 0.0428(5) 0.0008(4) -0.0037(4) 0.0004(4) Ni2 0.1679(14) 0.1679(14) 0.0391(11) 0.000 0.000 0.000 Ni3 0.0573(5) 0.0573(5) 0.0523(9) 0.000 0.000 0.000 Cl1 0.0781(12) 0.0781(12) 0.0483(17) 0.000 0.000 0.000 Cl2 0.205(4) 0.257(5) 0.121(3) -0.069(3) 0.064(3) -0.003(4) Cl3 0.0904(12) 0.0938(13) 0.0955(14) -0.0411(11) -0.0164(11) 0.0075(10) S11 0.0533(8) 0.0445(7) 0.0644(9) -0.0029(7) -0.0147(7) -0.0029(6) S21 0.0709(9) 0.0593(9) 0.0424(8) 0.0005(7) -0.0006(7) 0.0229(7) S31 0.0415(7) 0.0525(8) 0.0531(8) -0.0089(6) -0.0028(6) 0.0013(6) O11 0.0412(18) 0.0409(18) 0.069(2) -0.0019(18) -0.0090(17) -0.0024(15) O21 0.054(2) 0.055(2) 0.043(2) 0.0031(17) -0.0046(17) 0.0135(16) O31 0.0446(18) 0.0420(18) 0.056(2) -0.0080(17) -0.0002(17) 0.0083(15) C11 0.053(3) 0.075(4) 0.087(5) -0.021(4) 0.014(3) -0.010(3) C12 0.079(4) 0.064(4) 0.071(4) -0.020(3) 0.002(4) -0.003(3) C21 0.116(6) 0.076(4) 0.086(5) 0.025(4) 0.026(4) 0.017(4) C22 0.071(4) 0.104(5) 0.104(6) -0.008(5) -0.036(4) 0.017(4) C31 0.073(4) 0.062(4) 0.072(4) 0.002(3) 0.008(3) 0.017(3) C32 0.055(3) 0.081(4) 0.078(4) -0.009(4) 0.017(3) -0.011(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 Ni1 O11 2.059(3) . ? Ni1 O21 2.072(3) . ? Ni1 O31 2.079(3) . ? Ni2 Cl1 2.229(3) . ? Ni2 Cl2 2.352(4) . ? Ni3 Cl3 2.2513(16) . ? S11 O11 1.511(3) . ? S11 C11 1.774(6) . ? S11 C12 1.781(5) . ? S21 O21 1.518(3) . ? S21 C22 1.753(6) . ? S21 C21 1.765(6) . ? S31 O31 1.524(3) . ? S31 C32 1.777(5) . ? S31 C31 1.783(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 O11 Ni1 O11 180.0 5_665 . ? O11 Ni1 O21 90.14(13) . 5_665 ? O11 Ni1 O21 89.86(13) . . ? O11 Ni1 O31 91.16(11) . 5_665 ? O21 Ni1 O31 90.88(13) . 5_665 ? O11 Ni1 O31 88.84(11) . . ? O21 Ni1 O31 89.12(13) . . ? O31 Ni1 O31 180.0 5_665 . ? Cl1 Ni2 Cl2 103.23(12) . . ? Cl2 Ni2 Cl2 153.5(2) 3_655 4_565 ? Cl2 Ni2 Cl2 87.00(5) . 4_565 ? Cl3 Ni3 Cl3 120.16(11) 2_565 . ? Cl3 Ni3 Cl3 104.41(5) 2_565 8_666 ? O11 S11 C11 104.4(3) . . ? O11 S11 C12 104.0(2) . . ? C11 S11 C12 98.9(3) . . ? O21 S21 C22 104.7(3) . . ? O21 S21 C21 105.6(3) . . ? C22 S21 C21 98.0(4) . . ? O31 S31 C32 105.3(2) . . ? O31 S31 C31 103.6(2) . . ? C32 S31 C31 98.5(3) . . ? S11 O11 Ni1 119.31(18) . . ? S21 O21 Ni1 117.48(19) . . ? S31 O31 Ni1 116.55(18) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.933 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.078 #===END data_bis(dimethylpropyleneurea)dibromonickel(II) _database_code_CSD 184730 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(dimethylpropylene-urea)dibromonickel(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Br2 N4 Ni O2' _chemical_formula_weight 474.88 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.021(4) _cell_length_b 8.554(5) _cell_length_c 26.606(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.968(9) _cell_angle_gamma 90.00 _cell_volume 1821.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12015 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 5.462 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.4397 _exptl_absorpt_correction_T_max 0.4946 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 diffractometer with CCD area detector ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ; Neglible as determined from a repetition of the first 50 frames at the end of the experiment ; _diffrn_reflns_number 10858 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4040 _reflns_number_gt 2270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (1998b)' _computing_cell_refinement 'Bruker SMART and SAINT (1998b)' _computing_data_reduction 'Bruker SAINT (1998b)' _computing_structure_solution 'Bruker SHELXTL (1998a)' _computing_structure_refinement 'Bruker SHELXTL (1998a)' _computing_molecular_graphics 'Bruker SHELXTL (1998a)' _computing_publication_material 'Bruker SHELXTL (1998a)' _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^)+(0.0435P)^2^+0.0000P] 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 0.0148(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4040 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.855 _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 Ni1 Ni 0.32159(6) 0.30566(6) 0.379279(16) 0.04380(17) Uani 1 1 d . . . Br1 Br 0.30971(7) 0.03328(5) 0.394608(18) 0.0727(2) Uani 1 1 d . . . Br2 Br 0.55953(6) 0.44759(6) 0.356903(17) 0.06453(18) Uani 1 1 d . . . O1 O 0.2393(3) 0.3913(3) 0.44062(9) 0.0506(7) Uani 1 1 d . . . O11 O 0.1575(3) 0.3645(3) 0.32502(9) 0.0529(7) Uani 1 1 d . . . N1 N 0.3096(4) 0.2679(4) 0.51442(11) 0.0493(9) Uani 1 1 d . . . N2 N 0.0337(4) 0.2915(4) 0.48497(11) 0.0478(8) Uani 1 1 d . . . N11 N 0.1817(4) 0.5831(4) 0.27794(12) 0.0542(9) Uani 1 1 d . . . N12 N 0.2410(4) 0.3387(4) 0.24591(11) 0.0471(8) Uani 1 1 d . . . C1 C 0.1953(5) 0.3167(4) 0.47901(13) 0.0419(9) Uani 1 1 d . . . C2 C -0.0303(6) 0.2264(6) 0.52998(15) 0.0609(12) Uani 1 1 d . . . H2A H -0.0802 0.1253 0.5221 0.073 Uiso 1 1 calc R . . H2B H -0.1172 0.2943 0.5412 0.073 Uiso 1 1 calc R . . C3 C 0.1009(7) 0.2080(8) 0.57093(19) 0.097(2) Uani 1 1 d . . . H1A H 0.1068 0.3037 0.5905 0.116 Uiso 1 1 calc R . . H1B H 0.0675 0.1250 0.5930 0.116 Uiso 1 1 calc R . . C4 C 0.2643(6) 0.1733(6) 0.55609(17) 0.0743(15) Uani 1 1 d . . . H3A H 0.2694 0.0639 0.5467 0.089 Uiso 1 1 calc R . . H3B H 0.3447 0.1902 0.5845 0.089 Uiso 1 1 calc R . . C5 C -0.0913(6) 0.3271(5) 0.44383(16) 0.0658(13) Uani 1 1 d . . . H7A H -0.2006 0.3021 0.4541 0.099 Uiso 1 1 calc R . . H7B H -0.0689 0.2663 0.4147 0.099 Uiso 1 1 calc R . . H7C H -0.0863 0.4363 0.4357 0.099 Uiso 1 1 calc R . . C6 C 0.4884(5) 0.2829(6) 0.50835(17) 0.0694(14) Uani 1 1 d . . . H6A H 0.5501 0.2416 0.5376 0.104 Uiso 1 1 calc R . . H6B H 0.5161 0.3912 0.5044 0.104 Uiso 1 1 calc R . . H6C H 0.5166 0.2257 0.4791 0.104 Uiso 1 1 calc R . . C11 C 0.1945(5) 0.4292(5) 0.28395(14) 0.0444(10) Uani 1 1 d . . . C12 C 0.3036(6) 0.4051(6) 0.20135(15) 0.0661(13) Uani 1 1 d . . . H12A H 0.2865 0.3323 0.1735 0.079 Uiso 1 1 calc R . . H12B H 0.4227 0.4243 0.2070 0.079 Uiso 1 1 calc R . . C13 C 0.2148(7) 0.5555(6) 0.18848(17) 0.0753(15) Uani 1 1 d . . . H13A H 0.2647 0.6045 0.1603 0.090 Uiso 1 1 calc R . . H13B H 0.0985 0.5339 0.1784 0.090 Uiso 1 1 calc R . . C14 C 0.2247(6) 0.6648(5) 0.23242(18) 0.0690(14) Uani 1 1 d . . . H14A H 0.3370 0.7068 0.2373 0.083 Uiso 1 1 calc R . . H14B H 0.1483 0.7514 0.2257 0.083 Uiso 1 1 calc R . . C15 C 0.2620(6) 0.1719(5) 0.25376(17) 0.0657(13) Uani 1 1 d . . . H15A H 0.2948 0.1241 0.2233 0.099 Uiso 1 1 calc R . . H15B H 0.1583 0.1273 0.2628 0.099 Uiso 1 1 calc R . . H15C H 0.3467 0.1539 0.2804 0.099 Uiso 1 1 calc R . . C16 C 0.1519(8) 0.6791(6) 0.32144(19) 0.0918(18) Uani 1 1 d . . . H16A H 0.1446 0.7869 0.3115 0.138 Uiso 1 1 calc R . . H16B H 0.2423 0.6661 0.3467 0.138 Uiso 1 1 calc R . . H16C H 0.0491 0.6478 0.3349 0.138 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 Ni1 0.0423(3) 0.0549(3) 0.0345(3) 0.0056(2) 0.0048(2) -0.0005(3) Br1 0.0966(4) 0.0524(3) 0.0688(3) 0.0071(2) 0.0027(3) -0.0006(3) Br2 0.0440(3) 0.0866(4) 0.0634(3) 0.0163(2) 0.0064(2) -0.0116(3) O1 0.0568(19) 0.0575(16) 0.0385(14) 0.0064(13) 0.0116(13) 0.0047(15) O11 0.0362(17) 0.083(2) 0.0391(15) 0.0032(14) 0.0001(12) 0.0056(15) N1 0.035(2) 0.070(2) 0.0429(18) 0.0083(17) 0.0010(15) 0.0044(18) N2 0.034(2) 0.067(2) 0.0420(18) 0.0051(16) 0.0014(15) 0.0048(18) N11 0.055(2) 0.056(2) 0.049(2) -0.0055(18) -0.0119(17) 0.0128(19) N12 0.046(2) 0.058(2) 0.0378(18) -0.0043(15) 0.0004(15) 0.0027(17) C1 0.049(3) 0.045(2) 0.032(2) -0.0024(17) 0.0032(18) 0.003(2) C2 0.047(3) 0.080(3) 0.057(3) 0.013(2) 0.008(2) -0.007(3) C3 0.076(4) 0.152(6) 0.065(3) 0.051(3) 0.022(3) 0.028(4) C4 0.060(3) 0.101(4) 0.062(3) 0.031(3) 0.000(2) 0.003(3) C5 0.050(3) 0.080(3) 0.066(3) 0.011(2) -0.013(2) 0.009(3) C6 0.040(3) 0.099(4) 0.068(3) 0.005(3) 0.002(2) -0.011(3) C11 0.028(2) 0.067(3) 0.037(2) -0.006(2) -0.0075(17) 0.002(2) C12 0.068(3) 0.089(4) 0.042(2) -0.004(2) 0.009(2) -0.002(3) C13 0.083(4) 0.093(4) 0.049(3) 0.020(3) -0.001(2) -0.016(3) C14 0.060(3) 0.062(3) 0.082(4) 0.010(3) -0.010(3) -0.002(3) C15 0.065(3) 0.066(3) 0.065(3) -0.012(2) 0.001(2) 0.008(3) C16 0.107(5) 0.084(4) 0.080(4) -0.022(3) -0.020(3) 0.029(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 Ni1 O1 1.946(3) . ? Ni1 O11 1.951(3) . ? Ni1 Br1 2.3684(14) . ? Ni1 Br2 2.3724(11) . ? O1 C1 1.274(4) . ? O11 C11 1.278(4) . ? N1 C1 1.335(5) . ? N1 C4 1.440(5) . ? N1 C6 1.460(5) . ? N2 C1 1.335(5) . ? N2 C2 1.447(5) . ? N2 C5 1.464(5) . ? N11 C11 1.330(5) . ? N11 C16 1.452(6) . ? N11 C14 1.460(6) . ? N12 C11 1.347(5) . ? N12 C12 1.436(5) . ? N12 C15 1.450(5) . ? C2 C3 1.470(7) . ? C3 C4 1.426(7) . ? C12 C13 1.498(6) . ? C13 C14 1.495(6) . ? 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 Ni1 O11 105.83(12) . . ? O1 Ni1 Br1 101.88(8) . . ? O11 Ni1 Br1 110.37(9) . . ? O1 Ni1 Br2 110.09(9) . . ? O11 Ni1 Br2 101.27(9) . . ? Br1 Ni1 Br2 126.11(3) . . ? C1 O1 Ni1 127.8(2) . . ? C11 O11 Ni1 124.0(2) . . ? C1 N1 C4 121.4(4) . . ? C1 N1 C6 121.8(3) . . ? C4 N1 C6 115.9(3) . . ? C1 N2 C2 124.3(3) . . ? C1 N2 C5 119.9(3) . . ? C2 N2 C5 115.8(4) . . ? C11 N11 C16 118.7(4) . . ? C11 N11 C14 123.6(4) . . ? C16 N11 C14 116.9(4) . . ? C11 N12 C12 121.6(4) . . ? C11 N12 C15 119.5(3) . . ? C12 N12 C15 117.7(3) . . ? O1 C1 N2 120.1(3) . . ? O1 C1 N1 120.5(4) . . ? N2 C1 N1 119.4(3) . . ? N2 C2 C3 112.2(4) . . ? C4 C3 C2 116.2(4) . . ? C3 C4 N1 112.5(4) . . ? O11 C11 N11 120.7(4) . . ? O11 C11 N12 119.1(4) . . ? N11 C11 N12 120.1(4) . . ? N12 C12 C13 109.9(4) . . ? C14 C13 C12 111.1(4) . . ? N11 C14 C13 110.3(4) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.571 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.088 #===END