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_2018761
_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          '(NH4)3 [Mo2 (C H O2) O3 (O2)4]'
_chemical_formula_moiety         '3(H4 N +), C H Mo2 O13 3-'
_chemical_formula_sum            'C H13 Mo2 N3 O13'
_chemical_formula_weight         467.02
_chemical_name_common            'Triammonium formatotetraperoxidodimolybdate'
_chemical_name_systematic
;
Triammonium \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           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                   6.091(2)
_cell_length_b                   11.622(4)
_cell_length_c                   16.800(5)
_cell_measurement_reflns_used    4358
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.0628
_cell_measurement_theta_min      2.9922
_cell_volume                     1189.3(7)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10346
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_correction_T_min  0.8303
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.755
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0176
_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^)+(0.0207P)^2^+0.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                1704
_reflns_number_total             1779
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3186.cif
_cod_data_source_block           III
_cod_database_code               2018761
_cod_database_fobs_code          2018761