Potassium, rubidium and ammonium salts of μ-(formato-κ^2^<i>O</i>:<i>O</i>')-μ-oxido-bis[oxidobis(peroxido-κ^2^<i>O</i>,<i>O</i>')molybdate(VI)]
Takehara, Masaki; Hashimoto, Masato; Acta Crystallographica Section C 69 (2013) 37–40; doi:10.1107/S0108270112049803

data_2018759
_publ_section_title
;
 Potassium, rubidium and ammonium salts of
 \m-(formato-\k^2^<i>O</i>:<i>O</i>')-\m-oxido-bis[oxidobis(peroxido-\k^2^<i>O</i>,<i>O</i>')molybdate(VI)]
;
_journal_coeditor_code           SF3186
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              37
_journal_page_last               40
_journal_paper_doi               10.1107/S0108270112049803
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'K3 [Mo2 (C H O2) O3 (O2)4]'
_chemical_formula_moiety         '3(K +), C H Mo2 O13 3-'
_chemical_formula_sum            'C H K3 Mo2 O13'
_chemical_formula_weight         530.20
_chemical_name_common            'Tripotassium formatotetraperoxidodimolybdate'
_chemical_name_systematic
;
Tripotassium \m-(formato-\k^2^<i>O</i>:<i>O</i>')-\m-oxido-
bis[oxidobis(peroxido-\k^2^<i>O</i>,<i>O</i>')molybdate(VI)]
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.147(6)
_cell_length_b                   5.985(3)
_cell_length_c                   16.320(8)
_cell_measurement_reflns_used    4262
_cell_measurement_temperature    93.0(10)
_cell_measurement_theta_max      30.0255
_cell_measurement_theta_min      3.0938
_cell_volume                     1088.8(10)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (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      93.0(10)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku SATURN724+'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9147
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    3.521
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.650
_refine_ls_abs_structure_details 'Flack (1983), with 1419 Friedel pairs'
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3067
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.3042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0401
_reflns_number_gt                3021
_reflns_number_total             3067
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3186.cif
_cod_data_source_block           I
_cod_database_code               2018759
_cod_database_fobs_code          2018759