Two mononuclear tetraphenylphosphonium oxochromium complexes: (PPh~4~)[Cr^V^O~3~(H~2~O)] and (PPh~4~)[Cr^VI^O~3~(OH)]
Alok K. Mukherjee; Anuradha Mukhopadhaya; Monika Mukherjee; Siddhartha Ray; Acta Crystallographica Section C 50 (1994) 1401–1404; doi:10.1107/S0108270194003148

data_2010033
_publ_section_title
;
 Two mononuclear tetraphenylphosphonium oxochromium complexes:
 (PPh~4~)[Cr^V^O~3~(H~2~O)] and (PPh~4~)[Cr^VI^O~3~(OH)]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1401
_journal_page_last               1404
_journal_paper_doi               10.1107/S0108270194003148
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C24 H22 Cr O4 P'
_chemical_formula_weight         457.41
_chemical_name_systematic
;
 Tetraphenyl Phosphonium Aquatrioxo Chromate(V) .
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.250(3)
_cell_length_b                   12.250(3)
_cell_length_c                   7.309(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     1096.8(5)
_computing_cell_refinement       'Enraf-Nonius CAD-4 Software'
_computing_data_collection
'Enraf-Nonius CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'Enraf-nonius CAD-4 Software'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX-76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD 4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            304
_diffrn_reflns_theta_max         68.90
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.281
_exptl_absorpt_correction_T_max  .856
_exptl_absorpt_correction_T_min  .685
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             474
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.246
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(9)
_refine_ls_extinction_coef       0.0000(15)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.239
_refine_ls_goodness_of_fit_obs   1.239
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         296
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.481
_refine_ls_restrained_S_obs      1.224
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_obs          0.0765
_refine_ls_shift/esd_max         0.443
_refine_ls_shift/esd_mean        0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(Fo^2^) + (0.1311P)^2^ + 0.5169P]
where P = (Fo^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.2259
_refine_ls_wR_factor_obs         0.1841
_reflns_number_observed          296
_reflns_number_total             304
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            he1008.cif
_cod_data_source_block           PPh4CrO3H2O
_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 
;
_cod_original_formula_sum        'C24 H22 Cr1 O4 P1'
_cod_database_code               2010033