Two Tetrahalooxomolybdate(V) Structures, [Ph~3~PNPPh~3~][MoOBr~4~] and [PPh~4~][MoOI~4~(H~2~ O)]
Fettinger, James C.; Mattamana, Sundeep P.; Poli, Rinaldo; Acta Crystallographica Section C 54 (1998) 184–187; doi:10.1107/S0108270197010718

data_2007041
_publ_section_title
;
 Two Tetrahalooxomolybdate(V) Structures, [Ph~3~PNPPh~3~][MoOBr~4~] and
 [PPh~4~][MoOI~4~(H~2~ O)]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              184
_journal_page_last               187
_journal_paper_doi               10.1107/S0108270197010718
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C24 H20 P)[Mo O I4 (H2 O)]'
_chemical_formula_sum            'C24 H22 I4 Mo O2 P'
_chemical_formula_weight         976.93
_chemical_name_systematic
;
tetraphenylphosphonium aquotetraiodooxomolybdate(V)
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                   13.258(2)
_cell_length_b                   13.258(2)
_cell_length_c                   7.8926(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      9.3
_cell_volume                     1387.3(4)
_computing_cell_refinement       EXPRESS
_computing_data_collection       'EXPRESS (Enraf-Nonius, 19??)'
_computing_data_reduction
'XCAD-4 (Harms, 19??), SHELXTL (Siemens, 19??)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q 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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1335
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.000
_exptl_absorpt_correction_T_max  0.5618
_exptl_absorpt_correction_T_min  0.4769
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'Dark Brown'
_exptl_crystal_density_diffrn    2.339
_exptl_crystal_description       Block
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.548
_refine_diff_density_min         -1.458
_refine_ls_extinction_coef       0.0002(3)
_refine_ls_extinction_method     'SHELXL (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.195
_refine_ls_goodness_of_fit_obs   1.254
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1225
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.194
_refine_ls_restrained_S_obs      1.252
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_obs          .0551
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0482P)^2^+17.3173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1266
_refine_ls_wR_factor_obs         .1212
_reflns_number_observed          1031
_reflns_number_total             1225
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ta1139.cif
_cod_data_source_block           UM233
_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^)+(0.0482P)^2^+17.3173P] 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^)+(0.0482P)^2^+17.3173P] 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      'P 4/n'
_cod_database_code               2007041