Synthesis, crystal structures and properties of the new compounds K<sub>7-x</sub>Ag<sub>1+x</sub>(XO<sub>4</sub>)<sub>4</sub> (X = Mo, W).
Spiridonova, Tatyana S.; Solodovnikov, Sergey F.; Savina, Aleksandra A.; Solodovnikova, Zoya A.; Stefanovich, Sergey Yu; Lazoryak, Bogdan I.; Korolkov, Iliya V.; Khaikina, Elena G.; Acta crystallographica. Section C, Structural chemistry 73 (2017) 1071–1077; doi:10.1107/S2053229617015674

data_2311947
_publ_section_title
;
 Synthesis, crystal structures and properties of the new compounds
 K<sub>7-x</sub>Ag<sub>1+x</sub>(XO<sub>4</sub>)<sub>4</sub> (X = Mo, W).
;
_journal_coeditor_code           LY3055
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              1071
_journal_page_last               1077
_journal_paper_doi               10.1107/S2053229617015674
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'K6.68 Ag1.32 Mo4 O16'
_chemical_formula_moiety         'Ag1.32 Mo4 O16, 6.68(K)'
_chemical_formula_sum            'Ag1.32 K6.68 Mo4 O16'
_chemical_formula_weight         1043.34
_chemical_name_systematic
;
Heptapotassium silver tetrakis(tetraoxomolybdate)
;
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_hydrogens   other
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.4188(2)
_cell_length_b                   12.4188(2)
_cell_length_c                   7.4338(2)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.535
_cell_measurement_theta_min      3.789
_cell_volume                     992.89(3)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2008)
;
_computing_publication_material
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker--Nonius X8 APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9592
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.535
_diffrn_reflns_theta_min         3.789
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.199
_exptl_absorpt_correction_T_max  0.455
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             969.8
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.310
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.15(8)
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+2.0336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0403
_reflns_number_gt                1178
_reflns_number_total             1189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ly3055sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        992.89(4)
_cod_database_code               2311947
_shelx_hkl_checksum              87884
_shelx_res_checksum              62149