Hydrogen bis[tris(4-fluorophenyl)phosphane oxide] triiodide
Haghjoo, Farhad; Barnes, Nicholas A.; Pritchard, Robin; Godfrey, Stephen M.; Ratcliffe, Shane; Acta Crystallographica Section C 68 (2012) o216–o219; doi:10.1107/S0108270112020112

data_2018490
_publ_section_title
;
 Hydrogen bis[tris(4-fluorophenyl)phosphane oxide] triiodide
;
_journal_coeditor_code           EG3082
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o216
_journal_page_last               o219
_journal_paper_doi               10.1107/S0108270112020112
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C36 H25 F6 O2 P2 + , I3 -'
_chemical_formula_moiety         'C36 H25 F6 O2 P2 +, I3 -'
_chemical_formula_sum            'C36 H25 F6 I3 O2 P2'
_chemical_formula_weight         1046
_chemical_name_systematic
;
\m-hydrogen-bis[tris(4-fluorophenyl)phosphane oxide] triiodide
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2153(4)
_cell_length_b                   15.9752(6)
_cell_length_c                   18.5695(6)
_cell_measurement_reflns_used    3916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3710.8(2)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'HKL DENZO and SCALEPACK (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF08 (Beurskens <i>et al.</i>, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14255
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    2.675
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            purple--brown
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.034
_refine_diff_density_min         -1.601
_refine_ls_abs_structure_details 'Flack (1983), with 1024 Friedel pairs'
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5376
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0392P)^2^+81.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                4363
_reflns_number_total             5376
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3082.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2018490
_cod_database_fobs_code          2018490