Diphenyldichlorophosphonium Trichloride-Chlorine Solvate 1:1, [PPh2Cl2]+Cl3-.Cl2: An Ionic Form of Diphenyltrichlorophosphorane. Crystal Structures of [PPh2Cl2]+Cl3-.Cl2 and [(PPh2Cl2)+]2[InCl5]2-
Jan Taraba; Zdirad Zak; Inorganic Chemistry 42 (2003) 3591–3594; doi:10.1021/ic034091n

data_4313725
_publ_section_title
;
 Diphenyldichlorophosphonium Trichloride-Chlorine Solvate 1:1,
 [PPh2Cl2]+Cl3-.Cl2: An Ionic Form of Diphenyltrichlorophosphorane.
 Crystal Structures of [PPh2Cl2]+Cl3-.Cl2 and [(PPh2Cl2)+]2[InCl5]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3591
_journal_page_last               3594
_journal_paper_doi               10.1021/ic034091n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
;
[PPh~2~Cl~2~]~2~ [InCl~5~]
;
_chemical_formula_sum            'C24 H20 Cl9 In P2'
_chemical_formula_weight         804.21
_chemical_name_systematic
; 
 bis(diphenyldichlorophosphonium) pentachloroindate
;
_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                 110.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.957(2)
_cell_length_b                   21.295(4)
_cell_length_c                   13.893(3)
_cell_measurement_reflns_used    4379
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.1255
_cell_measurement_theta_min      2.1345
_cell_volume                     3041.1(12)
_computing_cell_refinement       'KUMA Crysalis RED'
_computing_data_collection       'KUMA Crysalis CCD'
_computing_data_reduction        'KUMA Crysalis RED'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.06 mm'
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_diffrn_measurement_method       omega-scan
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11228
_diffrn_reflns_theta_full        24.34
_diffrn_reflns_theta_max         24.34
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        none
_diffrn_standards_number         'after every 100 frames'
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  0.8493
_exptl_absorpt_correction_T_min  0.7288
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0206P)^2^+2.1839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0439
_reflns_number_gt                4189
_reflns_number_total             4535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034091nsi20030328_083054.cif
_cod_data_source_block           hjt40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+2.1839P] 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^)+(0.0206P)^2^+2.1839P] 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        3041.1(10)
_cod_database_code               4313725