2,4-Bis(diphenylphosphanyl)-1,1,2,3,3,4-hexaphenyl-1,3-diphospha-2,4-diboracyclobutane tetrahydrofuran sesquisolvate
Peulecke, Normen; Müller, Bernd H.; Spannenberg, Anke; Rosenthal, Uwe; Acta Crystallographica Section E 68 (2012) o1125–; doi:10.1107/S1600536812011361

data_2234480
_publ_section_title
;
 2,4-Bis(diphenylphosphanyl)-1,1,2,3,3,4-hexaphenyl-1,3-diphospha-2,4-diboracyclobutane
 tetrahydrofuran sesquisolvate
;
_journal_coeditor_code           YK2048
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1125
_journal_paper_doi               10.1107/S1600536812011361
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C60 H50 B2 P4, 1.5C4 H8 O'
_chemical_formula_moiety         'C60 H50 B2 P4, 1.5(C4 H8 O)'
_chemical_formula_sum            'C66 H62 B2 O1.5 P4'
_chemical_formula_weight         1024.66
_chemical_name_systematic
;
2,4-Bis(diphenylphosphanyl)-1,1,2,3,3,4-hexaphenyl-
1,3-diphospha-2,4-diboracyclobutane tetrahydrofuran sesquisolvate
;
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2421(4)
_cell_length_b                   11.6938(2)
_cell_length_c                   24.9769(5)
_cell_measurement_reflns_used    6569
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      1.62
_cell_volume                     5620.13(19)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS II'
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            91233
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9267
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6705
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                4392
_reflns_number_total             6705
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yk2048.cif
_cod_data_source_block           I
_cod_database_code               2234480
_cod_database_fobs_code          2234480