A sulfur(II) complex of a dithioimidodiphosphinate
Ritch, Jamie S.; Chivers, Tristram; Acta Crystallographica Section C 67 (2011) o89–o91; doi:10.1107/S0108270111003064

data_2018020
_publ_section_title
;
 A sulfur(II) complex of a dithioimidodiphosphinate
;
_journal_coeditor_code           SF3147
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o89
_journal_page_last               o91
_journal_paper_doi               10.1107/S0108270111003064
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C32 H72 N2 P4 S5 , C7 H8'
_chemical_formula_moiety         'C32 H72 N2 P4 S5, C7 H8'
_chemical_formula_sum            'C39 H80 N2 P4 S5'
_chemical_formula_weight         861.23
_chemical_name_common
;
bis[<i>P</i>,<i>P</i>-di-<i>tert</i>-butyl-<i>N</i>-(di-<i>tert</i>-
butylphosphorothioyl)phosphinimidothioato-\k<i>S</i>]sulfur(II)
toluene solvate
;
_chemical_name_systematic
;
5,13-dibutyl-7,7,11,11-tetramethyl-8,9,10-trithia-6,12-diaza-5\l^5^,7\l^5^-
diphospha-11\l^5^-phospha-13\l^5^-phosphaheptadeca-6,11-diene-5,13-dithione
toluene solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 132.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.271(5)
_cell_length_b                   18.970(4)
_cell_length_c                   15.610(3)
_cell_measurement_reflns_used    19034
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.38
_cell_volume                     4840(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD area-detector'
_diffrn_measurement_method       \f
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.1095
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19034
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_correction_T_min  0.9611
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0446P)^2^+1.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                2612
_reflns_number_total             4274
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3147.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2018020
_cod_database_fobs_code          2018020