Coordination and oxidation of phosphine selenides with iodine: from cation pairs [(R3PSe)2I+]2 to (iodoseleno)phosphonium ions [R3PSeI]+ existing as guests in polyiodide matrices
Seppälä, Emma; Ruthe, Frank; Jeske, Jörg; du Mont, Wolf-W.; Jones, Peter G.; Chemical Communications  (1999) 1471–; doi:10.1039/a903249e

data_7110573
_publ_section_title
;
 Coordination and oxidation of phosphine selenides with iodine: from
 cation pairs [(R3PSe)2I+]2 to (iodoseleno)phosphonium ions [R3PSeI]+
 existing as guests in polyiodide matrices
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1471
_journal_paper_doi               10.1039/a903249e
_journal_year                    1999
_chemical_formula_sum            'C11 H25 I7 P Se'
_chemical_formula_weight         1155.54
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6693(10)
_cell_length_b                   16.4329(12)
_cell_length_c                   25.2272(18)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     5252.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43866
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    9.714
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   'multiple scans'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.743
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_coef       0.000315(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         15312
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0380
_reflns_number_gt                12864
_reflns_number_total             15312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903249esup1.cif
_cod_data_source_block           finiki
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7110573