Double salt crystal structure of hexasodium hemiundecahydrogen <i>{α</i>}-hexamolybdoplatinate(IV) heminonahydrogen <i>{α</i>}-hexamolybdoplatinate(IV) nonacosahydrate: dihydrogen disordered-mixture double salt
Joo, Hea-Chung; Park, Ki-Min; Lee, Uk; Acta Crystallographica Section E 71 (2015) 1250–1254; doi:10.1107/S2056989015017703

data_2241163
_publ_section_title
;
 Double salt crystal structure of hexasodium hemiundecahydrogen
 <i>{\a</i>}-hexamolybdoplatinate(IV) heminonahydrogen
 <i>{\a</i>}-hexamolybdoplatinate(IV) nonacosahydrate: dihydrogen
 disordered-mixture double salt
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1250
_journal_page_last               1254
_journal_paper_doi               10.1107/S2056989015017703
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'H6 Mo6 O24 Pt, 14.5(H2 O), 3(Na)'
_chemical_formula_sum            'H34 Mo6 Na3 O38.5 Pt'
_chemical_formula_weight         1489.92
_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                72.825(2)
_cell_angle_beta                 75.522(2)
_cell_angle_gamma                89.168(2)
_cell_formula_units_Z            4
_cell_length_a                   14.0384(6)
_cell_length_b                   15.7969(6)
_cell_length_c                   16.7235(6)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.24
_cell_volume                     3423.7(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>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2014/7</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graphite multilayer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58415
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.352
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.358
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.891
_exptl_crystal_description       Block
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.665
_exptl_crystal_size_mid          0.441
_exptl_crystal_size_min          0.222
_refine_diff_density_max         1.730
_refine_diff_density_min         -2.247
_refine_ls_extinction_coef       0.00097(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick 2014
;
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         14940
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+5.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                12688
_reflns_number_total             14940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7461sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2023-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'H6 Mo6 O24 Pt, H4 Mo6 O24 Pt, 29(H2 O), 6(Na)'
_cod_original_formula_sum        'H68 Mo12 Na6 O77 Pt2 '
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2979.85
_cod_database_code               2241163
_cod_database_fobs_code          2241163
_shelx_hkl_checksum              49887
_shelx_res_checksum              7878