1,1,1-Tris(dimethylamino)-2-[tris(dimethylamino)phosphoranylidene]diphosphinium tetraphenylborate tetrahydrofuran monosolvate
Ellis, Bobby D.; Morasset, Erica V.; Macdonald, Charles L. B.; Acta Crystallographica Section E 70 (2014) o691–; doi:10.1107/S1600536814011258

data_2239583
_publ_section_title
;
 1,1,1-Tris(dimethylamino)-2-[tris(dimethylamino)phosphoranylidene]diphosphinium
 tetraphenylborate tetrahydrofuran monosolvate
;
_journal_coeditor_code           LH5704
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o691
_journal_paper_doi               10.1107/S1600536814011258
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C12 H36 N6 P3 +, C24 H20 B -, C4 H8 O'
_chemical_formula_moiety         'C12 H36 N6 P3 +, C24 H20 B -, C4 H8 O'
_chemical_formula_sum            'C40 H64 B N6 O P3'
_chemical_formula_weight         748.69
_chemical_name_systematic
;
1,1,1-Tris(dimethylamino)-2-[tris(dimethylamino)phosphoranylidene]diphosphinium
tetraphenylborate tetrahydrofuran monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
'from SHELXL-2012 CIF and IUCr SHELXL97-template'
_cell_angle_alpha                90
_cell_angle_beta                 98.930(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0859(17)
_cell_length_b                   11.8258(16)
_cell_length_c                   27.504(4)
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      22.84
_cell_measurement_theta_min      2.38
_cell_volume                     4204.7(10)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'WinGX (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS2012 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47616
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.283
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+2.6057P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                5621
_reflns_number_total             9592
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5704sup1.cif
_cod_data_source_block           I
_cod_database_code               2239583
_cod_database_fobs_code          2239583
_shelx_hkl_checksum              88615
_shelx_res_checksum              65615
_shelxl_version_number           .000002012