1,2-Bis(diphenylphosphino)benzene and two related mono-methiodides, [<i>o</i>-C~6~H~4~(P<i>R</i>~2~)(P<i>R</i>~2~Me)]I (<i>R</i> = Ph or Me)
Levason, William; Reid, Gillian; Webster, Michael; Acta Crystallographica Section C 62 (2006) o438–o440; doi:10.1107/S0108270106015915

data_2015411
_publ_section_title
;
 1,2-Bis(diphenylphosphino)benzene and two related mono-methiodides,
 [<i>o</i>-C~6~H~4~(P<i>R</i>~2~)(P<i>R</i>~2~Me)]I (<i>R</i> = Ph or
 Me)
;
_journal_coeditor_code           FA3012
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o438
_journal_page_last               o440
_journal_paper_doi               10.1107/S0108270106015915
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C31 H27 P2 +, I -'
_chemical_formula_moiety         'C31 H27 P2 +, I -'
_chemical_formula_sum            'C31 H27 I P2'
_chemical_formula_weight         588.37
_chemical_name_common
'o-phenylenebis(diphenylphosphine) monomethiodide'
_chemical_name_systematic
;
[2-(diphenylphosphino)phenyl]methyldiphenylphosphonium iodide
;
_space_group_IT_number           2
_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 + hand edit'
_cell_angle_alpha                69.536(3)
_cell_angle_beta                 67.260(3)
_cell_angle_gamma                70.847(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3323(5)
_cell_length_b                   11.8412(10)
_cell_length_c                   12.7828(10)
_cell_measurement_reflns_used    26612
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1317.22(17)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20101
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.952
_refine_diff_density_min         -1.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0360P)^2^+0.2511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                5063
_reflns_number_total             5956
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3012.cif
_cod_data_source_block           II
_cod_original_cell_volume        1317.22(16)
_cod_database_code               2015411