Bis(trimethylphenylammonium) μ-oxalato-bis[oxidodiperoxidomolybdate(VI)]
Oba, Ayaka; Hashimoto, Masato; Acta Crystallographica Section E 68 (2012) m1467–; doi:10.1107/S1600536812045850

data_2236923
_publ_section_title
;
 Bis(trimethylphenylammonium) \m-oxalato-bis[oxidodiperoxidomolybdate(VI)]
;
_journal_coeditor_code           IM2410
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1467
_journal_paper_doi               10.1107/S1600536812045850
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C9 H14 N)2 [Mo2 (C2 O4) (O2)4 O2]'
_chemical_formula_moiety         '2(C9 H14 N +), C2 Mo2 O14 2-'
_chemical_formula_sum            'C20 H28 Mo2 N2 O14'
_chemical_formula_weight         712.32
_chemical_name_systematic
;
Bis(trimethylphenylammonium) \m-oxalato-bis[oxidodiperoxidomolybdate(VI)]
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.023(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.860(2)
_cell_length_b                   9.975(2)
_cell_length_c                   13.691(3)
_cell_measurement_reflns_used    5064
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.0162
_cell_measurement_theta_min      2.9085
_cell_volume                     1343.2(5)
_computing_cell_refinement       '<i>CrystalClear SM</i> (Rigaku, 2008)'
_computing_data_collection       '<i>CrystalClear SM</i> (Rigaku, 2008)'
_computing_data_reduction        '<i>CrystalClear SM</i> (Rigaku, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5174
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11791
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  0.9136
_exptl_absorpt_correction_T_min  0.8880
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(NUMABS; Higashi, 2000)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.171
_refine_diff_density_max         1.840
_refine_diff_density_min         -0.693
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.5201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                3621
_reflns_number_total             3843
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2410.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2236923
_cod_database_fobs_code          2236923