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_2019625
_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, 2C4 H8 O'
_chemical_formula_moiety         'C64 H58 B2 P4, 2(C4 H8 O)'
_chemical_formula_sum            'C72 H74 B2 O2 P4'
_chemical_formula_weight         1116.81
_chemical_name_systematic
'2,5-[(Diphenylphosphanyl)methyl]-1,1,2,4,4,5-hexaphenyl-1,4-diphospha-2,5-diboracyclohexane tetrahydrofuran disolvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.720(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3097(6)
_cell_length_b                   13.3629(4)
_cell_length_c                   18.4243(9)
_cell_measurement_reflns_used    41292
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.8
_cell_volume                     3024.3(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.9409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+1.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                5027
_reflns_number_total             5652
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3100sup1.cif
_cod_data_source_block           Ib
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019625
_cod_database_fobs_code          2019625