Redetermination of bis(<i>O</i>,<i>O</i>'-dicyclohexyl phosphorodithioato)nickel(II)
Murat Taş; Mehtap Yaĝan; Hümeyra Batı; Beki̇r Batı; Orhan Büyükgüngör; Acta Crystallographica Section E 61 (2005) m1684–m1685; doi:10.1107/S1600536805023895

data_2206737
_publ_section_title
;
 Redetermination of bis(<i>O</i>,<i>O</i>'-dicyclohexyl
 phosphorodithioato)nickel(II)
;
_journal_coeditor_code           LH6464
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1684
_journal_page_last               m1685
_journal_paper_doi               10.1107/S1600536805023895
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni (C12 H22 O2 P S2)2]'
_chemical_formula_moiety         'C24 H44 Ni O4 P2 S4'
_chemical_formula_sum            'C24 H44 Ni O4 P2 S4'
_chemical_formula_weight         645.50
_chemical_name_systematic
;
bis(O,O'-dicyclohexyl phosphorodithioato)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'STOE X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.764(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7991(6)
_cell_length_b                   9.3550(5)
_cell_length_c                   14.2138(8)
_cell_measurement_reflns_used    21951
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.12
_cell_volume                     1558.01(15)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'rotation method; \w? \f? 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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20380
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.9320
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal-shaped plate'
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0384P)^2^+0.2064P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                2749
_reflns_number_total             3706
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6464.cif
_cod_data_source_block           I
_cod_original_cell_volume        1558.01(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206737
_cod_database_fobs_code          2206737