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_2311659
_publ_section_title
;
 Synthesis and structural characterization of donor-stabilized
 disubstituted diphenyldithiophosphates of nickel(II).
;
_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         'C46 H54 N2 Ni O4 P2 S4'
_chemical_formula_sum            'C46 H54 N2 Ni O4 P2 S4'
_chemical_formula_weight         947.82
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                102.744(3)
_cell_angle_beta                 94.409(3)
_cell_angle_gamma                103.785(3)
_cell_formula_units_Z            1
_cell_length_a                   6.9327(6)
_cell_length_b                   11.2267(10)
_cell_length_c                   15.5768(14)
_cell_measurement_reflns_used    7562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.61
_cell_volume                     1137.67(18)
_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    'Sir-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21578
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6912
_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    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.694
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.694
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0800P)^2^+1.7604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                4830
_reflns_number_total             6067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5066sup1.cif
_cod_data_source_block           34ETPY_LT_0m
_cod_database_code               2311659