The reaction of some tertiary phosphines with two mole equivalents of diiodine to produce the iodophosphonium triiodides [R3PI]I3; influence of R in causing subtle variations in solid state structures
Cross, Wendy I.; Godfrey, Stephen M.; McAuliffe, Charles A.; Pritchard, Robin G.; Sheffield, Joanne M.; Thompson, Graeme M.; Journal of the Chemical Society, Dalton Transactions  (1999) 2795–; doi:10.1039/a903974k

data_7027556
_publ_section_title
;
 The reaction of some tertiary phosphines with two mole equivalents of
 diiodine to produce the iodophosphonium triiodides [R3PI]I3; influence of
 R in causing subtle variations in solid state structures
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2795
_journal_paper_doi               10.1039/a903974k
_journal_year                    1999
_chemical_formula_sum            'C9 H21 I4 P'
_chemical_formula_weight         667.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   15.072(5)
_cell_length_b                   11.309(7)
_cell_length_c                   31.994(13)
_cell_measurement_temperature    203(2)
_cell_volume                     5446(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            9830
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    6.929
_exptl_absorpt_correction_T_max  0.3379
_exptl_absorpt_correction_T_min  0.2303
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.873
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         9438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+179.7100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.2186
_reflns_number_gt                6335
_reflns_number_total             9438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903974ksup1.cif
_cod_data_source_block           t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+179.7100P] 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^)+(0.1112P)^2^+179.7100P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7027556