Crystal structure of the Anderson-type heteropolyoxometalate; K~2~[H~7~Cr^III^Mo~6~O~24~]·8H~2~O: a redetermination revealing the position of the extra H atom in the polyanion
Joo, Hea-Chung; Park, Ki-Min; Lee, Uk; Acta Crystallographica Section E 71 (2015) 157–160; doi:10.1107/S2056989015000390

data_2240399
_publ_section_title
;
 Crystal structure of the Anderson-type heteropolyoxometalate;
 K~2~[H~7~Cr^III^Mo~6~O~24~]&#x00B7;8H~2~O: a redetermination revealing
 the position of the extra H atom in the polyanion
;
_journal_coeditor_code           BR2242
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              157
_journal_page_last               160
_journal_paper_doi               10.1107/S2056989015000390
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'K2 [H7 Cr Mo6 O24], 8H2 O'
_chemical_formula_structural     '2(K +), Cr H7 Mo6 O24 2-, 8(H2 O)'
_chemical_formula_sum            'Cr H23 K2 Mo6 O32'
_chemical_formula_weight         1241.02
_chemical_name_systematic
;
Dipotassium heptahydrogen hexamolybdochromate(III) octahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form.cif (version 2.0)'
_cell_angle_alpha                99.2960(10)
_cell_angle_beta                 94.4690(10)
_cell_angle_gamma                99.2830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4588(2)
_cell_length_b                   10.8553(2)
_cell_length_c                   12.6287(3)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    446(2)
_cell_measurement_theta_max      33.51
_cell_measurement_theta_min      2.51
_cell_volume                     1388.44(5)
_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>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      446(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graphite multilayer'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23489
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    3.419
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.673
_refine_ls_extinction_coef       0.00391(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6028
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+6.3059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                5893
_reflns_number_total             6028
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2242sup1.cf
_cod_data_source_block           I
_cod_database_code               2240399
_cod_database_fobs_code          2240399