Synthesis and structural characterization of donor-stabilized disubstituted diphenyldithiophosphates of nickel(II).
Kumar, Sandeep; Khajuria, Ruchi; Jassal, Amanpreet Kaur; Hundal, Geeta; Hundal, Maninder S.; Pandey, Sushil K.; Acta crystallographica Section B, Structural science, crystal engineering and materials 70 (2014) 761–767; doi:10.1107/S2052520614014966

data_2311657
_publ_section_title
;
 Synthesis and structural characterization of donor-stabilized
 disubstituted diphenyldithiophosphates of nickel(II).
;
_journal_coeditor_code           BP5066
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              761
_journal_page_last               767
_journal_paper_doi               10.1107/S2052520614014966
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C42 H46 N2 Ni O4 P2 S4'
_chemical_formula_sum            'C42 H46 N2 Ni O4 P2 S4'
_chemical_formula_weight         891.72
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7905(3)
_cell_length_b                   14.4443(4)
_cell_length_c                   12.8825(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.71
_cell_measurement_theta_min      2.16
_cell_volume                     2117.26(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33731
_diffrn_reflns_theta_full        34.22
_diffrn_reflns_theta_max         34.22
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0527P)^2^+0.3611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                6366
_reflns_number_total             8779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5066sup1.cif
_cod_data_source_block           Py_JAMMU_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2311657