Tribenzylphosphane and its hydrochloride salt, tribenzylphosphonium hydrogen dichloride–tribenzylphosphane (1/1)
Levason, William; Pugh, David; Reid, Gillian; Acta Crystallographica Section C 69 (2013) 560–564; doi:10.1107/S0108270113010226

data_2019018
_publ_section_title
;
 Tribenzylphosphane and its hydrochloride salt, tribenzylphosphonium
 hydrogen dichloride--tribenzylphosphane (1/1)
;
_journal_coeditor_code           YF3030
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              560
_journal_page_last               564
_journal_paper_doi               10.1107/S0108270113010226
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C42 H43 P2 +, H Cl2 -'
_chemical_formula_moiety         'C42 H43 P2 +, H Cl2 -'
_chemical_formula_sum            'C42 H44 Cl2 P2'
_chemical_formula_weight         681.61
_chemical_name_systematic
;
Tribenzylphosphonium hydrogen dichloride--tribenzylphosphane (1/1)
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.941(5)
_cell_length_b                   13.941(5)
_cell_length_c                   15.693(7)
_cell_measurement_reflns_used    2232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.1
_cell_volume                     2641.3(18)
_computing_cell_refinement
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2011)
;
_computing_data_collection
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2011)
;
_computing_data_reduction
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2011)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material
;
PLATON (Spek, 2009), WinGX (Farrugia, 2012), enCIFer (Allen
<i>et al.</i>, 2004),
publCIF (Westrip, 2010) and Mercury (Macrae <i>et al.</i>,
2006).
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2521
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_correction_T_min  0.9819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>CrystalClear-SM Expert</i>; Rigaku, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.571
_refine_ls_abs_structure_details 'Flack (1983), 325 Friedel pairs'
_refine_ls_abs_structure_Flack   0.34(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                1414
_reflns_number_total             1664
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yf3030.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2019018
_cod_database_fobs_code          2019018