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_7011793
_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            'C12 H24 Br2 N4 Ni O2'
_chemical_formula_weight         474.88
_chemical_name_systematic
; 
bis(dimethylpropylene-urea)dibromonickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.968(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.021(4)
_cell_length_b                   8.554(5)
_cell_length_c                   26.606(14)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.50
_cell_volume                     1821.1(17)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10858
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%
;
Neglible as determined from a repetition of the first 50
frames at the end of the experiment
;
_exptl_absorpt_coefficient_mu    5.462
_exptl_absorpt_correction_T_max  0.4946
_exptl_absorpt_correction_T_min  0.4397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.088
_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_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                2270
_reflns_number_total             4040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204128f.txt
_cod_data_source_block           bis(dimethylpropyleneurea)dibromonickel(II)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1821.1(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011793