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_7011792
_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_moiety         'C12 H36 Ni O6 S6, Cl4 Ni'
_chemical_formula_sum            'C12 H36 Cl4 Ni2 O6 S6'
_chemical_formula_weight         727.99
_chemical_name_systematic
; 
hexakis-(dimethylsulfoxide)-nickel(II) tetrachloronickelate(II)
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.950(2)
_cell_length_b                   18.950(2)
_cell_length_c                   8.5688(15)
_cell_measurement_reflns_used    3511
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.52
_cell_volume                     3077.1(7)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18289
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%
;
Neglible as determined from a repetition of the first 50 frames
at the end of the experiment
;
_exptl_absorpt_coefficient_mu    2.002
_exptl_absorpt_correction_T_max  0.5850
_exptl_absorpt_correction_T_min  0.5409
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                1695
_reflns_number_total             3511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204128f.txt
_cod_data_source_block
hexakis(dimethylsulfoxide)nickel(II)tetrachloronickelate(II)
_cod_original_cell_volume        3077.0(8)
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7011792