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_7110572
_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            'C27.5 H58 I6 P2 Se2'
_chemical_formula_weight         1370.00
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.193(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.687(5)
_cell_length_b                   13.955(2)
_cell_length_c                   19.383(2)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     8536(2)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device       'Stoe STADI-4'
_diffrn_measurement_method       \w-\q-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  0.0410
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_diffrn_reflns_limit_h_min       -37
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_min         3.10
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.164
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            'reddish black/metallic green'
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_description       prism
_exptl_crystal_F_000             5112
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.208
_refine_diff_density_min         -2.126
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    'all riding'
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_refine_ls_R_factor_obs          0.0519
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+243.4161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1541
_refine_ls_wR_factor_obs         0.1330
_reflns_number_observed          6593
_reflns_number_total             7530
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903249esup1.cif
_cod_data_source_block           loge
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+243.4161P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+243.4161P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8536.1(21)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C27.50 H58 I6 P2 Se2'
_cod_database_code               7110572