Tetraphenylphosphonium Hexatungstate(VI) Acetonitrile Solvate
Parvez, Masood; Boorman, P. Michael; Langdon, Naomi; Acta Crystallographica Section C 54 (1998) 608–609; doi:10.1107/S0108270197016946

data_2007223
_publ_section_title
;
 Tetraphenylphosphonium Hexatungstate(VI) Acetonitrile Solvate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              608
_journal_page_last               609
_journal_paper_doi               10.1107/S0108270197016946
_journal_volume                  54
_journal_year                    1998
_chemical_formula_analytical     'C52 H40 D6 N2 O19 P2 W6 '
_chemical_formula_iupac          '(C24 H20 P)2 [W6 O19],  2C2 D3 N'
_chemical_formula_structural     '(W6 O19), (C24 H20 P)2, 2(C2 D3 N) '
_chemical_formula_sum            'C52 H40 D6 N2 O19 P2 W6'
_chemical_formula_weight         2174.04
_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'
_cell_angle_alpha                90
_cell_angle_beta                 101.126(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.102(3)
_cell_length_b                   11.570(2)
_cell_length_c                   19.345(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2877.4(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1994)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      170
_diffrn_measurement_device       'Rigaku AFC-6S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_av_sigmaI/netI    0.110
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5095
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        1.05
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.07
_exptl_absorpt_correction_T_max  0.114
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type
' psi-scan (3 reflections) (North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3992.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.93
_refine_ls_extinction_coef       8.0(5)x10^-8^
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.22
_refine_ls_goodness_of_fit_obs   1.31
_refine_ls_hydrogen_treatment
'H atoms geometrically idealized with C-H 0.95 \%A'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.122
_refine_ls_R_factor_obs          .035
_refine_ls_shift/esd_max         0.024
_refine_ls_shift/esd_mean        0.0031
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(Fo)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.028
_refine_ls_wR_factor_obs         .022
_reflns_number_observed          2765
_reflns_number_total             5095
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            fg1378.cif
_cod_data_source_block           Hexatungstate
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/\s^2^(Fo)' 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)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2877.3(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C52 H40 D6 N2 O19 P2 W6 '
_cod_database_code               2007223