Tetraphenylphosphonium octahydrotriborate
Beckett, Michael A.; Horton, Peter N.; Hursthouse, Michael B.; Pszolla, Christian; Acta Crystallographica Section E 66 (2010) o833–; doi:10.1107/S1600536810008263

data_2225633
_publ_section_title
;
 Tetraphenylphosphonium octahydrotriborate
;
_journal_coeditor_code           LH2986
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o833
_journal_paper_doi               10.1107/S1600536810008263
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C24 H20 P +, B3 H8 -'
_chemical_formula_moiety         'C24 H20 P +, H8 B3 -'
_chemical_formula_sum            'C24 H28 B3 P'
_chemical_formula_weight         379.86
_chemical_name_systematic
;
Tetraphenylphosphonium octahydrotriborate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.995(4)
_cell_angle_beta                 79.779(6)
_cell_angle_gamma                79.780(5)
_cell_formula_units_Z            5
_cell_length_a                   7.0314(5)
_cell_length_b                   19.820(2)
_cell_length_c                   19.832(2)
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2676.8(4)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.776
_diffrn_measured_fraction_theta_max 0.776
_diffrn_measurement_device_type
'Bruker--Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15011
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.9454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.520
_refine_ls_abs_structure_details 'Flack (1983), 3867 Friedel pairs'
_refine_ls_abs_structure_Flack   0.07(9)
_refine_ls_extinction_coef       0.0055(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         13369
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0656P)^2^+2.9193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                10251
_reflns_number_total             13369
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2986.cif
_cod_data_source_block           I
_cod_database_code               2225633
_cod_database_fobs_code          2225633