Double salt crystal structure of nonasodium dihydrogen nonavanadoplatinate(IV) trihydrogen nonavanadoplatinate(IV) tetracontahydrate: stepwise-protonated nonavanadoplatinate(IV)
Joo, Hea-Chung; Park, Ki-Min; Lee, Uk; Acta Crystallographica Section E 71 (2015) 786–790; doi:10.1107/S2056989015010956

data_2240838
_publ_section_title
;
 Double salt crystal structure of nonasodium dihydrogen
 nonavanadoplatinate(IV) trihydrogen nonavanadoplatinate(IV)
 tetracontahydrate: stepwise-protonated nonavanadoplatinate(IV)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              786
_journal_page_last               790
_journal_paper_doi               10.1107/S2056989015010956
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'Na9 [H2 Pt V9 O28] [H3 Pt V9 O28], 40H2 O'
_chemical_formula_moiety         'H2 O28 Pt V9, H3 O28 Pt V9, 40(H2 O), 9(Na)'
_chemical_formula_structural
'(H2 Pt V9 O28), (H3 Pt V9 O28), 40(H2O), 9(Na)'
_chemical_formula_sum            'H42.5 Na4.5 O48 Pt V9'
_chemical_formula_weight         1567.84
_chemical_name_systematic
;Nonasodium dihydrogen nonavanadoplatinate(IV)
trihydrogen nonavanadoplatinate(IV) tetracontahydrate
;
_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
_cell_angle_alpha                93.7600(10)
_cell_angle_beta                 98.4490(10)
_cell_angle_gamma                113.3180(10)
_cell_formula_units_Z            4
_cell_length_a                   12.7060(10)
_cell_length_b                   12.8750(10)
_cell_length_c                   28.319(2)
_cell_measurement_reflns_used    7031
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.51
_cell_volume                     4168.9(5)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 1997)
;
_computing_data_collection
;
<i>SMART</i> (Bruker, 1997)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 1997)
;
_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>SHELXL2014</i> (Sheldrick, 2015)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker SMART CCD '
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            37312
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_min         1.739
_exptl_absorpt_coefficient_mu    5.441
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 1997)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.498
_exptl_crystal_description       block
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.987
_refine_diff_density_min         -2.146
_refine_ls_extinction_coef       0.00027(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   1.050
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         19046
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0047P)^2^+66.1402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                13416
_reflns_number_total             19046
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2554sup1.cf
_cod_data_source_block           I
_cod_original_formula_sum        'H42.50 Na4.50 O48 Pt V9'
_cod_database_code               2240838
_cod_database_fobs_code          2240838
_shelx_hkl_checksum              46680
_shelx_res_checksum              29066