1,1,4,4-Tetrabenzyl-1,4-diphosphinane-1,4-diium dibromide deuterochloroform disolvate
Fild, Manfred; Krüger, Oana N.; Silaghi-Dumitrescu, Ioan; Thöne, Carsten; Acta Crystallographica Section E 63 (2007) o4525–o4525; doi:10.1107/S1600536807052932

data_2216469
_publ_section_title
;
 1,1,4,4-Tetrabenzyl-1,4-diphosphinane-1,4-diium dibromide
 deuterochloroform disolvate
;
_journal_coeditor_code           HB2582
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4525
_journal_page_last               o4525
_journal_paper_doi               10.1107/S1600536807052932
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C32 H36 P2 2+, 2Br -, 2C D Cl3'
_chemical_formula_moiety         'C32 H36 P2 2+, 2Br -, 2C D Cl3'
_chemical_formula_sum            'C34 H36 Br2 Cl6 D2 P2'
_chemical_formula_weight         883.08
_chemical_name_systematic
;
1,1,4,4-Tetrabenzyl-1,4-diphosphinane-1,4-diium dibromide deuterochloroform
disolvate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.350(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2692(10)
_cell_length_b                   17.5649(10)
_cell_length_c                   13.9110(8)
_cell_measurement_reflns_used    8675
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.38
_cell_measurement_theta_min      2.32
_cell_volume                     3676.7(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XP (Siemens, 2000)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       \w
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37985
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0419P)^2^+6.1465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                4684
_reflns_number_total             5373
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2582.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2216469
_cod_database_fobs_code          2216469