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_7027557
_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            'C18 H42 I4 N3 P'
_chemical_formula_weight         839.11
_chemical_name_systematic
; 
 ? 
;
_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                 94.02(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.913(3)
_cell_length_b                   9.7437(15)
_cell_length_c                   35.602(8)
_cell_measurement_temperature    203(2)
_cell_volume                     5852.6(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1238
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            10630
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    4.322
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         10630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1768
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          1.113
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.0355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                4857
_reflns_number_total             10630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903974ksup1.cif
_cod_data_source_block           gt4b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7027557