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_7110574
_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            'C9 H21 I7 P Se'
_chemical_formula_weight         1127.49
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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            16
_cell_length_a                   50.655(3)
_cell_length_b                   15.5224(11)
_cell_length_c                   12.5356(8)
_cell_measurement_reflns_used    7012
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     9856.6(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            100493
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    10.348
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4555
_exptl_absorpt_correction_type   'multiple scans'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             7920
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.177
_refine_diff_density_min         -2.624
_refine_diff_density_rms         0.301
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_coef       0.000012(4)
_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   0.952
_refine_ls_hydrogen_treatment    'all riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         23779
_refine_ls_number_restraints     397
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                16647
_reflns_number_total             23779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903249esup1.cif
_cod_data_source_block           franca
_cod_original_cell_volume        9856.7(11)
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7110574