Redetermination of heptapotassium nonahydrogen bis[α-hexamolybdoplatinate(IV)] undecahydrate
Lee, Uk; Joo, Hea-Chung; Park, Ki-Min; Acta Crystallographica Section E 66 (2010) i25–; doi:10.1107/S1600536810008639

data_2225446
_publ_section_title
;
 Redetermination of heptapotassium nonahydrogen
 bis[\a-hexamolybdoplatinate(IV)] undecahydrate
;
_journal_coeditor_code           BR2139
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i25
_journal_paper_doi               10.1107/S1600536810008639
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
;
K7 [H4.5 Pt Mo6 O24]2, 11H2 O
;
_chemical_formula_moiety         '7(K +), 2(H4.5 Pt1 Mo6 O24 3.5-), 11(H2 O)'
_chemical_formula_sum            'H31 K7 Mo12 O59 Pt2'
_chemical_formula_weight         2790.39
_chemical_name_systematic
;
heptapotassium nonahydrogen \a-dodecamolybdodiplatinate(IV) undecahydrate
;
_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           SHELXL-97
_cell_angle_alpha                67.7920(10)
_cell_angle_beta                 68.5420(10)
_cell_angle_gamma                83.465(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0430(3)
_cell_length_b                   12.1512(4)
_cell_length_c                   12.4498(4)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.54
_cell_volume                     1308.58(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      148(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.999
_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  'Bruker HELIOS graded multilayer optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22108
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    8.780
_exptl_absorpt_correction_T_max  0.6209
_exptl_absorpt_correction_T_min  0.3526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296.0
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.879
_refine_diff_density_min         -2.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5699
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       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^)+(0.0236P)^2^+1.1372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                5599
_reflns_number_total             5699
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2139.cif
_cod_data_source_block           I
_cod_database_code               2225446
_cod_database_fobs_code          2225446