Solvent-free synthesis and crystal structure of (Ph~3~PI)I~5~, the third member in the series Ph~3~P(I~2~)~<i>n~</i> (<i>n</i> = 1, 2 and 3)
Pritchard, Robin G.; Moreland, Lee; Acta Crystallographica Section C 62 (2006) o656–o658; doi:10.1107/S0108270106039825

data_2015631
_publ_section_title
;
 Solvent-free synthesis and crystal structure of (Ph~3~PI)I~5~, the
 third member in the series Ph~3~P(I~2~)~<i>n~</i> (<i>n</i> = 1, 2 and
 3)
;
_journal_coeditor_code           BC3017
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o656
_journal_page_last               o658
_journal_paper_doi               10.1107/S0108270106039825
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C18 H15 I P + , I5 -'
_chemical_formula_moiety         'C18 H15 I P + , I5 -'
_chemical_formula_sum            'C18 H15 I6 P'
_chemical_formula_weight         1023.67
_chemical_name_systematic        'iodotriphenylphosphonium pentaiodide'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.1960(10)
_cell_angle_beta                 77.2900(10)
_cell_angle_gamma                77.6970(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4288(3)
_cell_length_b                   11.7262(4)
_cell_length_c                   12.1270(5)
_cell_measurement_reflns_used    5574
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1277.65(8)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5574
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    7.358
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.202
_refine_diff_density_min         -1.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0677P)^2^+14.7624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                3809
_reflns_number_total             5262
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bc3017.cif
_cod_data_source_block           3
_cod_original_cell_volume        1277.66(8)
_cod_original_sg_symbol_Hall     -P1
_cod_original_formula_sum        'C18 H15 I6 P1'
_cod_database_code               2015631
_cod_database_fobs_code          2015631