Reactivity of five- and six-coordinated solvates. A complex formation and crystallographic study of the nickel(II) bromide and iodide systems in dimethyl sulfoxide and N,N'-dimethylpropyleneurea
Bobicz, Dorota; Kristiansson, Olof; Persson, Ingmar; Journal of the Chemical Society, Dalton Transactions  (2002) 4201–4205; doi:10.1039/b204128f

data_7011790
_publ_section_title
;
 Reactivity of five- and six-coordinated solvates. A complex formation
 and crystallographic study of the nickel(II) bromide and iodide
 systems in dimethyl sulfoxide and N,N'-dimethylpropyleneurea
;
_journal_coden_ASTM              JCSDAA
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4201
_journal_page_last               4205
_journal_paper_doi               10.1039/b204128f
_journal_year                    2002
_chemical_formula_sum            'C16 H48 Cl2 Ni O8 S8'
_chemical_formula_weight         754.63
_chemical_name_systematic
; 
hexakis(dimethylsulfoxide)nickel(II) chloride
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.208(4)
_cell_angle_beta                 66.751(3)
_cell_angle_gamma                87.620(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9520(16)
_cell_length_b                   10.2209(16)
_cell_length_c                   11.0282(18)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.50
_cell_volume                     916.4(3)
_computing_cell_refinement       'Bruker SMART and SAINT (1998b)'
_computing_data_collection       'Bruker SMART (1998b)'
_computing_data_reduction        'Bruker SAINT (1998b)'
_computing_molecular_graphics    'Bruker SHELXTL (1998a)'
_computing_publication_material  'Bruker SHELXTL (1998a)'
_computing_structure_refinement  'Bruker SHELXTL (1998a)'
_computing_structure_solution    'Bruker SHELXTL (1998a)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.786
_diffrn_measured_fraction_theta_max 0.786
_diffrn_measurement_device_type
;
Bruker SMART diffractometer with CCD area detector 
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3807
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%
;
Neglible as determined from a repetition of the first 50
frames at the end of the experiment
;
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.8007
_exptl_absorpt_correction_T_min  0.6864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.074
_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_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                1895
_reflns_number_total             3140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204128f.txt
_cod_data_source_block           hexakis(dimethylsulfoxide)nickel(II)chloride
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7011790