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_7011791
_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 Br2 Ni O8 S8'
_chemical_formula_weight         843.55
_chemical_name_systematic
; 
hexakis(dimethylsulfoxide)nickel(II) bromide
;
_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                63.608(12)
_cell_angle_beta                 67.713(8)
_cell_angle_gamma                87.889(9)
_cell_formula_units_Z            1
_cell_length_a                   9.900(5)
_cell_length_b                   10.380(6)
_cell_length_c                   11.295(6)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.50
_cell_volume                     949.8(9)
_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 0.740
_diffrn_measured_fraction_theta_max 0.740
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.1482
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3516
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%
;
Approximately 20 % as determined from a repetition of the first 50
frames at the end of the experiment
;
_exptl_absorpt_coefficient_mu    3.085
_exptl_absorpt_correction_T_max  0.5248
_exptl_absorpt_correction_T_min  0.3870
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.653
_refine_diff_density_min         -2.181
_refine_diff_density_rms         0.183
_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_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.440
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.440
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.1100
_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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2355
_refine_ls_wR_factor_ref         0.2433
_reflns_number_gt                1346
_reflns_number_total             3076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204128f.txt
_cod_data_source_block           hexakis(dimethylsulfoxide)nickel(II)bromide
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011791