Crystal structure of pentapotassium dihydrogen nonavanadato(V)platinate(IV) nonahydrate
Joo, Hea-Chung; Lee, Uk; Acta Crystallographica Section E 71 (2015) 647–649; doi:10.1107/S2056989015009135

data_2240744
_publ_section_title
;
 Crystal structure of pentapotassium dihydrogen
 nonavanadato(V)platinate(IV) nonahydrate
;
_journal_coeditor_code           VN2093
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              647
_journal_page_last               649
_journal_paper_doi               10.1107/S2056989015009135
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'K5 [H2 Pt V9 O28], 9H2 O'
_chemical_formula_moiety         'H2 O28 Pt V9, 9(H2 O), 5(K)'
_chemical_formula_structural     'Pt H2 V9 O28, 98(H2 O), K5'
_chemical_formula_sum            'H20 K5 O37 Pt V9'
_chemical_formula_weight         1461.21
_chemical_name_systematic
;
Pentapotassium dihydrogen nonavanadato(V)platinate(IV) nonahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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           SHELXL-2014/7
_cell_angle_alpha                103.734(5)
_cell_angle_beta                 106.193(6)
_cell_angle_gamma                92.480(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1663(7)
_cell_length_b                   12.8350(7)
_cell_length_c                   13.615(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.50
_cell_measurement_theta_min      9.55
_cell_volume                     1645.8(3)
_computing_cell_refinement
;
<i>STADI4</i> (Stoe & Cie, 1996)
;
_computing_data_collection
;
<i>STADI4</i> (Stoe & Cie, 1996)
;
_computing_data_reduction
;
<i>X-RED</i> (Stoe & Cie, 1996)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows </i> (Farrugia, 2012) and
<i>DIAMOND</i> (Brandenburg, 1998)
;
_computing_publication_material
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2014</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe Stadi4'
_diffrn_measurement_method       '\w/2-\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6797
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.485
_diffrn_reflns_theta_min         1.613
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.421
_exptl_absorpt_correction_T_max  0.3778
_exptl_absorpt_correction_T_min  0.3010
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>X-SHAPE</i>; Stoe & Cie,1996)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.949
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.463
_refine_ls_extinction_coef       0.00505(13)
_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   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         6797
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0277P)^2^+4.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                6242
_reflns_number_total             6797
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            vn2093sup1.cf
_cod_data_source_block           I
_cod_database_code               2240744
_shelx_hkl_checksum              8152
_shelx_res_checksum              24635
_cod_database_fobs_code 2240744