#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/33/2013340.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2013340
loop_
_publ_author_name
'Lee, Uk'
'Joo, Hea-Chung'
'Park, Ki-Min'
'Ozeki, Tomoji'
_publ_section_title
;
 Synchrotron structure determination of an α-Keggin doubly
 PtIV-substituted silicotungstate,
 (CH₆N₃)₈[α-SiPt₂W₁₀O₄₀]·6H₂O
;
_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 α-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/[σ²(Fo²) + 65.1125P] where P = (Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
W1 0.344386(19) 0.393810(19) 0.368398(16) 0.01991(5) Uani d P 0.83 . . W
Pt1 0.344386(19) 0.393810(19) 0.368398(16) 0.01991(5) Uani d P 0.17 . . Pt
W2 0.235962(16) 0.53609(2) 0.493510(13) 0.01951(4) Uani d P 0.83 . . W
Pt2 0.235962(16) 0.53609(2) 0.493510(13) 0.01951(4) Uani d P 0.17 . . Pt
W3 0.379342(19) 0.644708(18) 0.368059(15) 0.01938(5) Uani d P 0.83 . . W
Pt3 0.379342(19) 0.644708(18) 0.368059(15) 0.01938(5) Uani d P 0.17 . . Pt
Si 0.5000 0.5000 0.5000 0.0159(5) Uani d S 1 . . Si
Ot1 0.2879(4) 0.3198(4) 0.3053(3) 0.0253(10) Uani d . 1 . . O
Ot2 0.1101(3) 0.5536(4) 0.5119(3) 0.0269(10) Uani d . 1 . . O
Ot3 0.3467(4) 0.7334(4) 0.3056(3) 0.0266(10) Uani d . 1 . . O
Oe4 0.2242(4) 0.4345(4) 0.4209(3) 0.0221(8) Uani d . 1 . . O
Oe5 0.2528(4) 0.6362(4) 0.4194(2) 0.0215(8) Uani d . 1 . . O
Oe6 0.3409(4) 0.5223(4) 0.3188(2) 0.0217(8) Uani d . 1 . . O
Oc7 0.5156(4) 0.6181(4) 0.3418(3) 0.0212(8) Uani d . 1 . . O
Oc8 0.2960(4) 0.6277(4) 0.5595(3) 0.0212(8) Uani d . 1 . . O
Oc9 0.4309(4) 0.7311(4) 0.4408(3) 0.0207(8) Uani d . 1 . . O
Od10 0.3999(3) 0.5142(3) 0.4497(2) 0.0151(7) Uani d . 1 . . O
C1 0.1961(12) 0.5002(7) 0.1541(6) 0.059(4) Uani d . 1 . . C
N1 0.1385(11) 0.5230(7) 0.0980(6) 0.068(4) Uani d . 1 . . N
H1A 0.1200 0.5842 0.0910 0.081 Uiso calc R 1 . . H
H1B 0.1203 0.4764 0.0693 0.081 Uiso calc R 1 . . H
N2 0.2231(12) 0.4051(7) 0.1638(7) 0.075(4) Uani d . 1 . . N
H2A 0.2596 0.3890 0.1995 0.090 Uiso calc R 1 . . H
H2B 0.2040 0.3596 0.1344 0.090 Uiso calc R 1 . . H
N3 0.2222(14) 0.5701(8) 0.1959(7) 0.095(6) Uani d . 1 . . N
H3A 0.2587 0.5566 0.2321 0.114 Uiso calc R 1 . . H
H3B 0.2033 0.6310 0.1880 0.114 Uiso calc R 1 . . H
C2 0.3198(13) 1.0004(10) 0.3410(9) 0.065(4) Uani d . 1 . . C
N4 0.2758(14) 0.9461(8) 0.2898(7) 0.089(5) Uani d . 1 . . N
H4A 0.2429 0.9759 0.2568 0.107 Uiso calc R 1 . . H
H4B 0.2805 0.8814 0.2901 0.107 Uiso calc R 1 . . H
N5 0.3745(12) 0.9507(9) 0.3893(6) 0.076(4) Uani d . 1 . . N
H5A 0.4064 0.9835 0.4214 0.091 Uiso calc R 1 . . H
H5B 0.3777 0.8860 0.3881 0.091 Uiso calc R 1 . . H
N6 0.3125(15) 1.0986(9) 0.3405(8) 0.100(7) Uani d . 1 . . N
H6A 0.3435 1.1337 0.3719 0.120 Uiso calc R 1 . . H
H6B 0.2768 1.1281 0.3088 0.120 Uiso calc R 1 . . H
Ow1 0.5000 0.5000 0.1949(8) 0.126(8) Uani d S 1 . . O
Ow2 0.2007(16) 0.8262(10) 0.5015(17) 0.178(8) Uani d . 1 . . O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -1.4577 1.8630
'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)'
O O 0.0032 0.0011 'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)'
C C -0.0017 0.0003
'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)'
N N -0.0027 0.0006
'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)'
Si Si 0.0025 0.0139
'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)'
Pt Pt -1.4795 2.3196
'International Tables Vol. C Table 6.1.1.4 and Sasaki (1989)'
H H 0.0000 0.0000 'International Tables Vol. C Table 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
W3 W1 W2 3_665 4_656 59.974(7) yes
W2 W1 W3 . . 60.209(8) yes
W1 W2 W3 . . 59.992(8) yes
W2 W1 W2 . 4_656 90.149(9) yes
W1 W2 W3 . 4_656 90.066(9) yes
Od10 Si Od10 4_656 . 109.63(15) yes
Od10 Si Od10 . 3_665 109.2(3) yes
W1 W3 W2 . . 59.799(8) yes
Ot1 W1 Oc8 . 4_656 101.1(2) ?
Ot1 W1 Oc7 . 3_665 101.0(2) ?
Oc8 W1 Oc7 4_656 3_665 86.8(2) ?
Ot1 W1 Oe6 . . 98.9(2) ?
Oc8 W1 Oe6 4_656 . 160.0(2) ?
Oc7 W1 Oe6 3_665 . 88.2(2) ?
Ot1 W1 Oe4 . . 99.0(2) ?
Oc8 W1 Oe4 4_656 . 89.0(2) ?
Oc7 W1 Oe4 3_665 . 160.0(2) ?
Oe6 W1 Oe4 . . 89.1(2) ?
Ot1 W1 Od10 . . 170.3(2) ?
Oc8 W1 Od10 4_656 . 86.13(18) ?
Oc7 W1 Od10 3_665 . 85.67(18) ?
Oe6 W1 Od10 . . 74.18(17) ?
Oe4 W1 Od10 . . 74.55(17) ?
W3 W1 W2 . 4_656 120.118(10) ?
Ot2 W2 Oc8 . . 100.7(2) ?
Ot2 W2 Oc9 . 4_656 100.8(2) ?
Oc8 W2 Oc9 . 4_656 86.8(2) ?
Ot2 W2 Oe4 . . 99.2(2) ?
Oc8 W2 Oe4 . . 160.1(2) ?
Oc9 W2 Oe4 4_656 . 88.4(2) ?
Ot2 W2 Oe5 . . 99.5(2) ?
Oc8 W2 Oe5 . . 89.5(2) ?
Oc9 W2 Oe5 4_656 . 159.7(2) ?
Oe4 W2 Oe5 . . 88.4(2) ?
Ot2 W2 Od10 . . 171.0(2) ?
Oc8 W2 Od10 . . 85.67(18) ?
Oc9 W2 Od10 4_656 . 85.87(18) ?
Oe4 W2 Od10 . . 74.71(17) ?
Oe5 W2 Od10 . . 73.92(17) ?
W3 W2 W3 . 4_656 119.912(10) ?
Ot3 W3 Oc7 . . 100.7(2) ?
Ot3 W3 Oc9 . . 100.1(2) ?
Oc7 W3 Oc9 . . 87.7(2) ?
Ot3 W3 Oe6 . . 100.1(2) ?
Oc7 W3 Oe6 . . 88.2(2) ?
Oc9 W3 Oe6 . . 159.8(2) ?
Ot3 W3 Oe5 . . 99.5(2) ?
Oc7 W3 Oe5 . . 159.8(2) ?
Oc9 W3 Oe5 . . 89.0(2) ?
Oe6 W3 Oe5 . . 88.0(2) ?
Ot3 W3 Od10 . . 171.5(2) ?
Oc7 W3 Od10 . . 85.67(18) ?
Oc9 W3 Od10 . . 85.73(18) ?
Oe6 W3 Od10 . . 74.26(17) ?
Oe5 W3 Od10 . . 74.18(17) ?
W2 Oe4 W1 . . 119.3(2) ?
W3 Oe5 W2 . . 120.0(2) ?
W3 Oe5 Ow2 . . 113.8(5) ?
W2 Oe5 Ow2 . . 99.8(6) ?
W3 Oe6 W1 . . 119.6(2) ?
W3 Oe6 Ow1 . . 105.0(2) ?
W1 Oe6 Ow1 . . 105.1(2) ?
W3 Oc7 W1 . 3_665 149.2(3) ?
W3 Oc7 Ow1 . . 104.81(18) ?
W1 Oc7 Ow1 3_665 . 104.42(18) ?
W2 Oc8 W1 . 2_566 150.1(3) ?
W2 Oc8 Ow2 . . 97.9(4) ?
W1 Oc8 Ow2 2_566 . 111.2(4) ?
W3 Oc9 W2 . 2_566 149.4(3) ?
W1 Od10 W3 . . 91.92(14) ?
W1 Od10 W2 . . 91.46(14) ?
W3 Od10 W2 . . 91.94(14) ?
N3 C1 N2 . . 122.5(10) ?
N3 C1 N1 . . 118.9(9) ?
N2 C1 N1 . . 118.6(9) ?
N6 C2 N5 . . 122.3(13) ?
N6 C2 N4 . . 119.9(13) ?
N5 C2 N4 . . 117.7(11) ?
Oe6 Ow1 Oe6 3_665 . 84.5(4) ?
Oe6 Ow1 Oc7 3_665 . 50.1(2) ?
Oe6 Ow1 Oc7 . . 49.7(2) ?
Oe6 Ow1 Oc7 3_665 3_665 49.7(2) ?
Oe6 Ow1 Oc7 . 3_665 50.1(2) ?
Oc7 Ow1 Oc7 . 3_665 59.2(3) ?
Oe5 Ow2 Oc8 . . 52.4(2) ?
C1 N1 H1A . . 120.0 ?
C1 N1 H1B . . 120.0 ?
H1A N1 H1B . . 120.0 ?
C1 N2 H2A . . 120.0 ?
C1 N2 H2B . . 120.0 ?
H2A N2 H2B . . 120.0 ?
C1 N3 H3A . . 120.0 ?
C1 N3 H3B . . 120.0 ?
H3A N3 H3B . . 120.0 ?
C2 N4 H4A . . 120.0 ?
C2 N4 H4B . . 120.0 ?
H4A N4 H4B . . 120.0 ?
C2 N5 H5A . . 120.0 ?
C2 N5 H5B . . 120.0 ?
H5A N5 H5B . . 120.0 ?
C2 N6 H6A . . 120.0 ?
C2 N6 H6B . . 120.0 ?
H6A N6 H6B . . 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 W2 . 3.3565(4) yes
W1 W3 . 3.3631(4) yes
W2 W3 . 3.3704(4) yes
W1 W2 4_656 3.7100(4) yes
W1 W3 3_665 3.7033(4) yes
W2 W3 4_656 3.7051(4) yes
W1 Ot1 . 1.721(5) yes
W1 Oc8 4_656 1.921(5) yes
W1 Oc7 3_665 1.932(5) yes
W1 Oe6 . 1.948(5) yes
W1 Oe4 . 1.956(5) yes
W1 Od10 . 2.339(4) yes
W2 Ot2 . 1.722(4) yes
W2 Oc8 . 1.919(5) yes
W2 Oc9 4_656 1.922(5) yes
W2 Oe4 . 1.934(5) yes
W2 Oe5 . 1.948(5) yes
W2 Od10 . 2.348(4) yes
W3 Ot3 . 1.725(5) yes
W3 Oc7 . 1.910(5) yes
W3 Oc9 . 1.920(5) yes
W3 Oe6 . 1.943(5) yes
W3 Oe5 . 1.945(5) yes
W3 Od10 . 2.339(4) yes
Si Od10 . 1.646(4) yes
C1 N3 . 1.268(13) yes
C1 N2 . 1.324(13) yes
C1 N1 . 1.344(12) yes
C2 N6 . 1.308(17) yes
C2 N5 . 1.342(18) yes
C2 N4 . 1.342(17) yes
Ow1 Oe6 3_665 3.174(13) yes
Ow1 Oc7 . 3.204(14) yes
Ow1 Oe6 . 3.174(13) yes
Ow1 Oe6 . 3.174(13) yes
Ow2 Oe5 . 3.043(17) yes
Ow2 Oc8 . 3.123(19) yes
N5 Ot2 2_566 3.132(13) yes
N1 H1A . 0.8600 ?
N1 H1B . 0.8600 ?
N2 H2A . 0.8600 ?
N2 H2B . 0.8600 ?
N3 H3A . 0.8600 ?
N3 H3B . 0.8600 ?
N4 H4A . 0.8600 ?
N4 H4B . 0.8600 ?
N5 H5A . 0.8600 ?
N5 H5B . 0.8600 ?
N6 H6A . 0.8600 ?
N6 H6B . 0.8600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1B Ot2 6_455 0.86 2.11 2.957(10) 166.1
N1 H1A Oe4 8 0.86 2.01 2.864(10) 174.9
N2 H2A Ot1 . 0.86 2.24 3.036(12) 154.5
N2 H2B Oe5 6_455 0.86 2.02 2.865(12) 167.9
N3 H3B Ot1 8 0.86 2.11 2.945(11) 163.8
N3 H3A Oe6 . 0.86 2.02 2.884(11) 178.1
N4 H4B Ot1 8 0.86 2.57 3.045(13) 116.2
N4 H4B Ot3 . 0.86 2.17 2.991(12) 158.8
N5 H5A Ot2 4_666 0.86 2.17 2.984(12) 157.8
N6 H6B Ot1 1_565 0.86 2.55 3.029(13) 116.2
N6 H6B Ot3 6_465 0.86 2.27 3.050(14) 151.1
