Phase change in tetraphenylphosphonium perchlorate
Batten, Stuart R.; Harris, Alexander R.; Murray, Keith S.; Acta Crystallographica Section C 56 (2000) 1394–1395; doi:10.1107/S0108270100011562

data_2011580
_publ_section_title
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 Phase change in tetraphenylphosphonium perchlorate
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_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1394
_journal_page_last               1395
_journal_paper_doi               10.1107/S0108270100011562
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C24 H20 P +, Cl O4 -'
_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            8
_cell_length_a                   17.0481(4)
_cell_length_b                   17.0481(4)
_cell_length_c                   13.7568(3)
_cell_measurement_reflns_used    11973
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      1.69
_cell_volume                     3998.24(16)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full .993
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0260
_diffrn_reflns_av_sigmaI/netI    .0402
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11969
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    .301
_exptl_absorpt_correction_T_max  .9542
_exptl_absorpt_correction_T_min  .9134
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Siemens, 1994)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .15
_refine_diff_density_max         .266
_refine_diff_density_min         -.355
_refine_ls_abs_structure_details 'Flack (1983), 2804 Friedel pairs'
_refine_ls_abs_structure_Flack   .03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          .0495
_refine_ls_R_factor_gt           .0381
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0486P)^2^+1.5872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1037
_reflns_number_gt                5030
_reflns_number_total             5981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ta1294.cif
_cod_data_source_block           I
_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:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2011580
_cod_database_fobs_code          2011580