Bis(tetraphenylphosphonium) bis(1-carboxybenzene-2,3-diolato-κ^2^<i>O</i>,<i>O</i>')-<i>cis</i>-dioxomolybdate(VI)
Litos, Charalambos; Karaliota, Alexandra; Parsons, Simon; Acta Crystallographica Section E 62 (2006) m928–m930; doi:10.1107/S1600536806010907

data_2208684
_publ_section_title
;Bis(tetraphenylphosphonium)
 bis(1-carboxybenzene-2,3-diolato-\k^2^<i>O</i>,<i>O</i>')-<i>cis</i>-dioxomolybdate(VI)
;
_journal_coeditor_code           OB2002
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m928
_journal_page_last               m930
_journal_paper_doi               10.1107/S1600536806010907
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C24 H20 P)2 [Mo O2 (C7 H4 O4)2]'
_chemical_formula_moiety         '2(C24 H20 P), C14 H8 Mo O10'
_chemical_formula_sum            'C62 H48 Mo O10 P2'
_chemical_formula_weight         1110.88
_chemical_name_systematic
;
Bis(tetraphenylphosphonium)
(cis-dioxo)bis(1-carboxybenzene-2,3-diolate-O,O')molybdenum(VI)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3595(3)
_cell_length_b                   16.9998(4)
_cell_length_c                   45.5887(13)
_cell_measurement_reflns_used    8839
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2
_cell_volume                     10353.6(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Sheldrick, 1997)'
_computing_publication_material
'XCIF (Sheldrick, 1993) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens <i>et al.</i>,  1996)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART Apex CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            122211
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.504
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         15149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0315P)^2^+9.6314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                11301
_reflns_number_total             15149
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob2002.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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:

'_atom_sites_solution_hydrogens' value 'geom/difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               2208684