Synchrotron structure determination of an α-Keggin doubly Pt^IV^-substituted silicotungstate, (CH~6~N~3~)~8~[α-SiPt~2~W~10~O~40~]·6H~2~O
Lee, Uk; Joo, Hea-Chung; Park, Ki-Min; Ozeki, Tomoji; Acta Crystallographica Section C 59 (2003) m152–m155; doi:10.1107/S0108270103004517

data_2013340
_publ_section_title
;
 Synchrotron structure determination of an \a-Keggin doubly
 Pt^IV^-substituted silicotungstate,
 (CH~6~N~3~)~8~[\a-SiPt~2~W~10~O~40~]&#x00B7;6H~2~O
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m152
_journal_page_last               m155
_journal_paper_doi               10.1107/S0108270103004517
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C1 H6 N3)8 [O40 Pt2 Si1 W10], 6H2 O1'
_chemical_formula_moiety         '8C1 H6 N3 1+, O40 Pt2 Si1 W10 8-, 6H2 O1'
_chemical_formula_sum            'C8 H60 N24 O46 Pt2 Si W10'
_chemical_formula_weight         3485.57
_chemical_name_systematic
;
Octaguanidinium \a-silicodiplatinodecatungstate hexahydrate
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   13.2760(10)
_cell_length_b                   13.2760(10)
_cell_length_c                   18.9590(10)
_cell_measurement_reflns_used    12596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.80
_cell_measurement_theta_min      2.00
_cell_volume                     3341.6(4)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'DIP Xpress (MAC Science, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MAC Science DIP LABO'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3282
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42373
_diffrn_reflns_theta_full        15.80
_diffrn_reflns_theta_max         15.80
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.5548
_exptl_absorpt_correction_T_min  0.5220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(PLATON MULABS; Spek, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       truncated-tetrahedron
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.091
_refine_diff_density_min         -2.549
_refine_ls_abs_structure_details '(Flack, 1983), 3878 Friedel pairs'
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0293
_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^) + 65.1125P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                7961
_reflns_number_total             7980
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1100.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     I-4
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               2013340
_cod_database_fobs_code          2013340