Polymorphism of 2,5-[(diphenylphosphanyl)methyl]-1,1,2,4,4,5-hexaphenyl-1,4-diphospha-2,5-diboracyclohexane
Müller, Manuela; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section C 70 (2014) –; doi:10.1107/S2053229614016684

data_2019626
_publ_section_title
;
 Polymorphism of
 2,5-[(diphenylphosphanyl)methyl]-1,1,2,4,4,5-hexaphenyl-1,4-diphospha-2,5-diboracyclohexane
;
_journal_coeditor_code           UK3100
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614016684
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C64 H58 B2 P4, C7 H8'
_chemical_formula_moiety         'C64 H58 B2 P4, C7 H8'
_chemical_formula_sum            'C71 H66 B2 P4'
_chemical_formula_weight         1064.74
_chemical_name_systematic
'2,5-[(Diphenylphosphanyl)methyl]-1,1,2,4,4,5-hexaphenyl-1,4-diphospha-2,5-diboracyclohexane toluene monosolvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 109.813(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8933(18)
_cell_length_b                   13.4283(6)
_cell_length_c                   20.2287(13)
_cell_measurement_reflns_used    15406
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.8
_cell_volume                     5850.5(7)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (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 0.984
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_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  0.0813
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50113
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         3.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         10969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0390P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                6016
_reflns_number_total             10969
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3100sup1.cif
_cod_data_source_block           Ic
_cod_original_cell_volume        5850.5(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019626
_cod_database_fobs_code          2019626