Triple molybdates K~3{‒~<i>x</i>}Na~1+<i>x~</i><i>M</i>~4~(MoO~4~)~6~ (<i>M</i>~= Ni, Mg, Co) and K~3+<i>x~</i>Li~1{‒~<i>x</i>}Mg~4~(MoO~4~)~6~ isotypic with II-Na~3~Fe~2~(AsO~4~)~3~ and yurmarinite: synthesis, potassium disorder, crystal chemistry and ionic conductivity
Gulyaeva, Oksana A.; Solodovnikova, Zoya A.; Solodovnikov, Sergey F.; Zolotova, Evgeniya S.; Mateyshina, Yuliya G.; Uvarov, Nikolai F.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620010677

data_2108665
_publ_section_title
;
 Triple molybdates K~3{--~<i>x</i>}Na~1+<i>x~</i><i>M</i>~4~(MoO~4~)~6~
 (<i>M</i>~= Ni, Mg, Co) and
 K~3+<i>x~</i>Li~1{--~<i>x</i>}Mg~4~(MoO~4~)~6~ isotypic with
 II-Na~3~Fe~2~(AsO~4~)~3~ and yurmarinite: synthesis, potassium disorder,
 crystal chemistry and ionic conductivity
;
_journal_coeditor_code           JE5031SUP1
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620010677
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'K2.51 Na1.49 Ni4, 6(Mo O4)'
_chemical_formula_sum            'K2.51 Mo6 Na1.49 Ni4 O24'
_chemical_formula_weight         1326.84
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.2719(2)
_cell_length_b                   14.2719(2)
_cell_length_c                   19.8063(4)
_cell_measurement_reflns_used    13749
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      2.65
_cell_measurement_theta_min      2.63
_cell_volume                     3493.80(10)
_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_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-Nonius X8 APEX CCD diffractometer'
_diffrn_measurement_method       '\ f scans, frame data integration'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13749
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.652
_diffrn_reflns_theta_min         2.635
_exptl_absorpt_coefficient_mu    6.847
_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3721
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.000093(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1106
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+12.1272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0327
_refine_ls_wR_factor_ref         0.0331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1062
_reflns_number_total             1111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            je5031sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        3493.80(14)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               2108665
_publcif_datablock.id            {b623f15d-bfee-4cc1-b923-4b87e4179b98}
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.684
_shelx_res_checksum              87086
_cod_database_fobs_code 2108665