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_2007040
_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          '(C36 H30 N P2)[Mo O Br4]'
_chemical_formula_sum            'C36 H30 Br4 Mo N O P2'
_chemical_formula_weight         970.13
_chemical_name_systematic
;
bis(triphenylphoshine)iminium tetrabromooxomolybdate(V)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 131.137(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.960(3)
_cell_length_b                   9.1643(8)
_cell_length_c                   18.488(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      10.7
_cell_volume                     3567.8(8)
_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       'omega 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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3211
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.967
_exptl_absorpt_correction_T_max  0.107
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'Brownish yellow'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
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_refine_diff_density_min         -0.523
_refine_ls_extinction_coef       0.00013(6)
_refine_ls_extinction_method     'SHELXL (Sheldrick, 1993)'
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_refine_ls_goodness_of_fit_obs   1.150
_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.150
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_obs          .0291
_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^)+(0.0316P)^2^+8.5059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0697
_refine_ls_wR_factor_obs         .0651
_reflns_number_observed          2624
_reflns_number_total             3142
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ta1139.cif
_cod_data_source_block           UM118
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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^)+(0.0316P)^2^+8.5059P] 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^)+(0.0316P)^2^+8.5059P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3567.8(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2007040