Tetraphenylphosphonium Perchlorate
Vittal, J. J.; Dean, P. A. W.; Acta Crystallographica Section C 52 (1996) 3185–3188; doi:10.1107/S0108270196010980

data_2005820
_publ_section_title
;
 Tetraphenylphosphonium Perchlorate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              3185
_journal_page_last               3188
_journal_paper_doi               10.1107/S0108270196010980
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'C24 H20 P + , Cl O4 -'
_chemical_formula_structural     '[(C6H5)4P](ClO4)'
_chemical_formula_sum            'C24 H20 Cl O4 P'
_chemical_formula_weight         438.82
_chemical_name_common            'Tetraphenylphosphonium perchlorate'
_chemical_name_systematic
;
Tetraphenylphosphonium perchlorate
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.383(3)
_cell_length_b                   12.383(3)
_cell_length_c                   7.188(2)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      10.9
_cell_volume                     1102.2(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1246
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        1.58
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.95416
_exptl_absorpt_correction_T_min  0.94463
_exptl_absorpt_correction_type   'Siemens Gaussian'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      1.43(5)
_exptl_crystal_density_method    'floatation in CCl~4~/hexane mixture'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.249
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_hydrogen_treatment
;
All five hydrogen atoms were located and placed in calculated ideal positions
for structure-factor calculations only
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1146
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_obs          0.0491
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.8674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1236
_refine_ls_wR_factor_obs         0.0944
_reflns_number_observed          655
_reflns_number_total             1146
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1044.cif
_cod_data_source_block           JJVA
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.8674P] 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^)+(0.0343P)^2^+0.8674P] 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      I-4
_cod_original_formula_sum        'C24 H20 Cl1 O4 P1'
_cod_database_code               2005820