Crystal structure of potassium sodium heptahydrogen hexamolybdocobaltate(III) octahydrate: an extra-protonated <i>B</i>-series Anderson-type heteropolyoxidometalate
Park, Ki-Min; Joo, Hea-Chung; Lee, Uk; Acta Crystallographica Section E 71 (2015) 1032–1035; doi:10.1107/S2056989015014784

data_2241008
_publ_section_title
;
 Crystal structure of potassium sodium heptahydrogen
 hexamolybdocobaltate(III) octahydrate: an extra-protonated
 <i>B</i>-series Anderson-type heteropolyoxidometalate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1032
_journal_page_last               1035
_journal_paper_doi               10.1107/S2056989015014784
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'K Na [Co Mo6 O17 (O H)7], 8H2 O'
_chemical_formula_moiety         'K +, Na +, Co H7 Mo6 O24 2-, 8(H2 O)'
_chemical_formula_structural     'Co H7 Mo6 O24, 8(H2 O), K, Na'
_chemical_formula_sum            'Co H23 K Mo6 Na O32'
_chemical_formula_weight         1231.84
_chemical_name_systematic
;Sodium potassium
hexa-\m~3~-hydroxido-\m~2~-hydroxido-heptadecaoxidocobaltate(II)hexamolybdate(VI)
octahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.6660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9758(5)
_cell_length_b                   20.7702(9)
_cell_length_c                   12.7906(6)
_cell_measurement_reflns_used    5031
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.47
_cell_volume                     2874.5(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2009)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2009)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012),
PLATON (Spek, 2009) and
DIAMOND (Brandenburg, 1998)
;
_computing_publication_material
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.272
_diffrn_reflns_theta_min         1.889
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2009)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.846
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.020
_refine_diff_density_min         -1.064
_refine_ls_extinction_coef       0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6701
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+12.1333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                4416
_reflns_number_total             6701
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2252sup1.cf
_cod_data_source_block           I
_cod_database_code               2241008
_shelx_estimated_absorpt_t_min   0.552
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              12582
_cod_database_fobs_code 2241008