#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/05/2210532.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_2210532
loop_
_publ_author_name
'Magdalena Kloskowska'
'Jarosław Chojnacki'
'Wiesław Wojnowski'
'Barbara Becker'
_publ_section_title
Tetrakis(μ₂-methanol)bis(methanol-κO)(μ₂-tri-tert-butoxysilanethiolato-κ³S:S,O)bis(tri-tert-butoxysilanethiolato-κ²S,O)tetrasodium(I)
_journal_coeditor_code           BX2025
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2476
_journal_page_last               m2478
_journal_paper_doi               10.1107/S1600536806035070
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Na4 (C12 H27 O3 S1 Si1)4 (C1 H4 O1)6]'
_chemical_formula_moiety         'C54 H132 Na4 O18 S4 Si4'
_chemical_formula_sum            'C54 H132 Na4 O18 S4 Si4'
_chemical_formula_weight         1402.16
_chemical_name_systematic
;
Tetrakis(μ₃-methanol)bis(methanol-κO)(μ₂-tri-tert-
butoxysilanethiolato-κ³S;S,O)bis(tri-tert-butoxysilanethiolato-
κ²S,O)tetrasodium(I)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                101.90(3)
_cell_angle_beta                 99.64(3)
_cell_angle_gamma                103.38(3)
_cell_formula_units_Z            1
_cell_length_a                   8.298(2)
_cell_length_b                   14.988(3)
_cell_length_c                   17.932(4)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3.5
_cell_volume                     2068.1(9)
_computing_cell_refinement       'KM-4 Software'
_computing_data_collection
'KM-4 Software (Gałdecki et al.,  1996)'
_computing_data_reduction        'KM-4 Software'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and
MERCURY (Macrae et al.,  2006)
;
_computing_publication_material  'WinGX  (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kuma KM-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7983
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        0.7
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0991P)²+0.367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                5883
_reflns_number_total             7721
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bx2025.cif
_cod_data_source_block           I
_cod_database_code               2210532
_cod_database_fobs_code          2210532
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
Si Si1 0.53647(8) 1.21023(4) 0.29777(3) 0.02378(16) Uani d . 1
Si Si2 0.27722(7) 0.76588(4) 0.19087(3) 0.02224(15) Uani d . 1
S S1 0.35219(7) 1.14608(4) 0.34831(3) 0.03003(16) Uani d . 1
S S2 0.50537(7) 0.83923(4) 0.26587(3) 0.02718(15) Uani d . 1
Na Na1 0.36575(13) 0.98569(6) 0.24666(6) 0.0367(2) Uani d . 1
Na Na2 0.43581(12) 0.89568(7) 0.41645(5) 0.0310(2) Uani d . 1
O O1 0.7265(2) 1.25378(11) 0.35334(9) 0.0301(4) Uani d . 1
O O2 0.5510(2) 1.12270(11) 0.22889(9) 0.0270(3) Uani d . 1
O O3 0.4998(2) 1.29671(11) 0.26201(10) 0.0298(4) Uani d . 1
O O4 0.21070(19) 0.84477(10) 0.15069(9) 0.0251(3) Uani d . 1
O O5 0.12151(19) 0.72712(10) 0.23256(9) 0.0258(3) Uani d . 1
O O6 0.2748(2) 0.67304(11) 0.12471(9) 0.0271(3) Uani d . 1
C C1 0.0371(4) 0.9325(2) 0.36431(17) 0.0443(7) Uani d . 1
H H1A -0.0181 0.8951 0.3965 0.066 Uiso calc R 1
H H1B -0.0456 0.9268 0.3164 0.066 Uiso calc R 1
H H1C 0.0804 0.9992 0.3937 0.066 Uiso calc R 1
C C2 0.2417(3) 0.9401(2) 0.57091(17) 0.0432(6) Uani d . 1
H H2A 0.263 0.9652 0.6277 0.065 Uiso calc R 1
H H2B 0.1683 0.8749 0.5558 0.065 Uiso calc R 1
H H2C 0.1856 0.9796 0.5445 0.065 Uiso calc R 1
C C3 0.6683(4) 0.7390(2) 0.43424(18) 0.0545(8) Uani d . 1
H H3A 0.6524 0.7335 0.3779 0.082 Uiso calc R 1
H H3B 0.622 0.6767 0.443 0.082 Uiso calc R 1
H H3C 0.7899 0.7624 0.459 0.082 Uiso calc R 1
C C10 0.8116(3) 1.34418(17) 0.40831(14) 0.0339(6) Uani d . 1
C C11 0.8734(4) 1.41576(19) 0.36342(18) 0.0481(7) Uani d . 1
H H11A 0.9469 1.3925 0.3312 0.072 Uiso calc R 1
H H11B 0.9376 1.4765 0.4004 0.072 Uiso calc R 1
H H11C 0.7755 1.4245 0.3297 0.072 Uiso calc R 1
C C12 0.6944(4) 1.3758(2) 0.45734(18) 0.0548(8) Uani d . 1
H H12A 0.5985 1.3866 0.4237 0.082 Uiso calc R 1
H H12B 0.7568 1.4349 0.4969 0.082 Uiso calc R 1
H H12C 0.6517 1.3266 0.4833 0.082 Uiso calc R 1
C C13 0.9633(4) 1.3279(2) 0.45815(19) 0.0586(9) Uani d . 1
H H13A 0.9236 1.2859 0.4906 0.088 Uiso calc R 1
H H13B 1.0365 1.3887 0.4919 0.088 Uiso calc R 1
H H13C 1.0278 1.2984 0.4242 0.088 Uiso calc R 1
C C20 0.6783(3) 1.11954(17) 0.18231(14) 0.0327(5) Uani d . 1
C C21 0.7371(4) 1.21283(19) 0.16109(16) 0.0398(6) Uani d . 1
H H21A 0.6393 1.2271 0.1321 0.06 Uiso calc R 1
H H21B 0.82 1.2079 0.1285 0.06 Uiso calc R 1
H H21C 0.7901 1.2637 0.209 0.06 Uiso calc R 1
C C22 0.8263(4) 1.0954(2) 0.22854(17) 0.0439(7) Uani d . 1
H H22A 0.8775 1.1453 0.2772 0.066 Uiso calc R 1
H H22B 0.9118 1.0909 0.1973 0.066 Uiso calc R 1
H H22C 0.7852 1.0346 0.2408 0.066 Uiso calc R 1
C C23 0.5903(4) 1.0400(2) 0.10903(17) 0.0533(8) Uani d . 1
H H23A 0.5531 0.9803 0.1237 0.08 Uiso calc R 1
H H23B 0.6698 1.0337 0.0748 0.08 Uiso calc R 1
H H23C 0.4914 1.0546 0.0813 0.08 Uiso calc R 1
C C30 0.3505(3) 1.31012(19) 0.21777(16) 0.0370(6) Uani d . 1
C C31 0.2484(4) 1.2192(2) 0.15716(17) 0.0473(7) Uani d . 1
H H31A 0.3206 1.1977 0.1234 0.071 Uiso calc R 1
H H31B 0.1511 1.231 0.1254 0.071 Uiso calc R 1
H H31C 0.2074 1.1703 0.1836 0.071 Uiso calc R 1
C C32 0.4155(4) 1.3880(2) 0.1783(2) 0.0584(9) Uani d . 1
H H32A 0.481 1.446 0.2184 0.088 Uiso calc R 1
H H32B 0.3187 1.4005 0.1468 0.088 Uiso calc R 1
H H32C 0.4883 1.3674 0.1445 0.088 Uiso calc R 1
C C33 0.2441(4) 1.3424(2) 0.2732(2) 0.0534(8) Uani d . 1
H H33A 0.2082 1.2932 0.3002 0.08 Uiso calc R 1
H H33B 0.1436 1.3536 0.2436 0.08 Uiso calc R 1
H H33C 0.3118 1.4012 0.3118 0.08 Uiso calc R 1
C C40 0.0507(3) 0.83822(17) 0.09963(14) 0.0303(5) Uani d . 1
C C41 -0.0670(3) 0.8666(2) 0.15019(17) 0.0450(7) Uani d . 1
H H41A -0.099 0.8186 0.1788 0.067 Uiso calc R 1
H H41B -0.1695 0.8717 0.117 0.067 Uiso calc R 1
H H41C -0.0089 0.9281 0.1875 0.067 Uiso calc R 1
C C42 -0.0298(3) 0.73908(18) 0.04606(15) 0.0374(6) Uani d . 1
H H42A 0.0469 0.7228 0.0127 0.056 Uiso calc R 1
H H42B -0.1381 0.7372 0.0132 0.056 Uiso calc R 1
H H42C -0.0498 0.6933 0.0777 0.056 Uiso calc R 1
C C43 0.0948(4) 0.9098(2) 0.05193(17) 0.0491(7) Uani d . 1
H H43A 0.1466 0.9732 0.0873 0.074 Uiso calc R 1
H H43B -0.009 0.9099 0.0166 0.074 Uiso calc R 1
H H43C 0.1751 0.8924 0.0212 0.074 Uiso calc R 1
C C50 0.0705(3) 0.64053(16) 0.25804(14) 0.0304(5) Uani d . 1
C C51 -0.0495(4) 0.6605(2) 0.31068(18) 0.0486(7) Uani d . 1
H H51A 0.0139 0.7102 0.358 0.073 Uiso calc R 1
H H51B -0.1001 0.6026 0.3252 0.073 Uiso calc R 1
H H51C -0.1397 0.6816 0.2828 0.073 Uiso calc R 1
C C52 -0.0238(4) 0.55871(18) 0.18731(16) 0.0432(7) Uani d . 1
H H52A -0.1198 0.5747 0.1585 0.065 Uiso calc R 1
H H52B -0.0661 0.5016 0.2047 0.065 Uiso calc R 1
H H52C 0.0536 0.547 0.1531 0.065 Uiso calc R 1
C C53 0.2242(4) 0.6198(2) 0.30164(17) 0.0440(7) Uani d . 1
H H53A 0.3005 0.6093 0.2666 0.066 Uiso calc R 1
H H53B 0.1876 0.563 0.3202 0.066 Uiso calc R 1
H H53C 0.2843 0.6739 0.3465 0.066 Uiso calc R 1
C C60 0.3905(3) 0.65625(17) 0.07526(14) 0.0325(5) Uani d . 1
C C61 0.5391(3) 0.63416(19) 0.12255(17) 0.0409(6) Uani d . 1
H H61A 0.5989 0.6888 0.1669 0.061 Uiso calc R 1
H H61B 0.6174 0.6207 0.0893 0.061 Uiso calc R 1
H H61C 0.4968 0.5788 0.142 0.061 Uiso calc R 1
C C62 0.4518(4) 0.7420(2) 0.04459(16) 0.0411(6) Uani d . 1
H H62A 0.3547 0.7535 0.0124 0.062 Uiso calc R 1
H H62B 0.5336 0.7303 0.0128 0.062 Uiso calc R 1
H H62C 0.5066 0.7977 0.0887 0.062 Uiso calc R 1
C C63 0.2891(4) 0.5709(2) 0.00865(18) 0.0552(8) Uani d . 1
H H63A 0.2459 0.5172 0.03 0.083 Uiso calc R 1
H H63B 0.3626 0.5539 -0.0262 0.083 Uiso calc R 1
H H63C 0.1934 0.5864 -0.0208 0.083 Uiso calc R 1
O O10 0.3990(2) 0.94111(13) 0.54874(10) 0.0346(4) Uani d . 1
O O11 0.1739(2) 0.89821(14) 0.34444(12) 0.0436(5) Uani d . 1
O O12 0.5828(3) 0.80317(16) 0.46715(12) 0.0486(5) Uani d . 1
H H10D 0.451(5) 0.917(3) 0.574(2) 0.072(12) Uiso d . 1
H H11D 0.137(4) 0.847(2) 0.3104(19) 0.049(9) Uiso d . 1
H H12D 0.595(4) 0.813(3) 0.514(2) 0.064(11) Uiso d . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 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
O1 Si1 O3 . . 104.47(9) ?
O1 Si1 O2 . . 105.05(9) ?
O3 Si1 O2 . . 111.15(9) ?
O1 Si1 S1 . . 116.00(7) ?
O3 Si1 S1 . . 115.87(7) ?
O2 Si1 S1 . . 103.90(7) ?
O1 Si1 Na1 . . 120.12(7) ?
O3 Si1 Na1 . . 133.03(7) ?
O2 Si1 Na1 . . 46.10(6) ?
S1 Si1 Na1 . . 57.97(4) ?
O6 Si2 O5 . . 104.09(9) ?
O6 Si2 O4 . . 111.37(8) ?
O5 Si2 O4 . . 102.44(8) ?
O6 Si2 S2 . . 117.11(7) ?
O5 Si2 S2 . . 115.49(7) ?
O4 Si2 S2 . . 105.49(7) ?
O6 Si2 Na1 . . 148.12(7) ?
O5 Si2 Na1 . . 104.62(7) ?
O4 Si2 Na1 . . 48.45(6) ?
S2 Si2 Na1 . . 60.75(4) ?
Si1 S1 Na1 . . 82.51(4) yes
Si2 S2 Na1 . . 79.07(4) ?
Si2 S2 Na2 . . 106.66(4) ?
Na1 S2 Na2 . . 79.44(4) ?
O4 Na1 O2 . . 127.76(7) yes
O4 Na1 S1 . . 146.61(6) yes
O2 Na1 S1 . . 69.40(5) yes
O4 Na1 S2 . . 69.88(5) yes
O2 Na1 S2 . . 116.42(6) yes
S1 Na1 S2 . . 133.13(4) yes
O4 Na1 O11 . . 82.81(7) yes
O2 Na1 O11 . . 148.80(7) yes
S1 Na1 O11 . . 81.10(5) yes
S2 Na1 O11 . . 76.74(5) yes
O4 Na1 Si2 . . 31.64(4) ?
O2 Na1 Si2 . . 139.58(6) ?
S1 Na1 Si2 . . 150.31(4) ?
S2 Na1 Si2 . . 40.18(3) ?
O11 Na1 Si2 . . 69.21(5) ?
O4 Na1 Si1 . . 150.96(6) ?
O2 Na1 Si1 . . 29.96(4) ?
S1 Na1 Si1 . . 39.52(3) ?
S2 Na1 Si1 . . 130.07(4) ?
O11 Na1 Si1 . . 119.52(6) ?
Si2 Na1 Si1 . . 167.56(4) ?
O4 Na1 Na2 . . 100.77(5) ?
O2 Na1 Na2 . . 124.00(6) ?
S1 Na1 Na2 . . 85.56(4) ?
S2 Na1 Na2 . . 51.39(3) ?
O11 Na1 Na2 . . 40.72(5) ?
Si2 Na1 Na2 . . 72.02(4) ?
Si1 Na1 Na2 . . 108.27(4) ?
O12 Na2 O11 . . 144.91(9) yes
O12 Na2 O10 . 2_676 111.68(9) yes
O11 Na2 O10 . 2_676 103.36(8) yes
O12 Na2 O10 . . 83.08(8) yes
O11 Na2 O10 . . 100.85(8) yes
O10 Na2 O10 2_676 . 81.23(8) yes
O12 Na2 S2 . . 92.68(6) yes
O11 Na2 S2 . . 83.93(6) yes
O10 Na2 S2 2_676 . 98.31(6) yes
O10 Na2 S2 . . 175.19(6) yes
O12 Na2 C2 . 2_676 95.08(9) ?
O11 Na2 C2 . 2_676 118.33(9) ?
O10 Na2 C2 2_676 2_676 25.84(7) ?
O10 Na2 C2 . 2_676 98.65(8) ?
S2 Na2 C2 . 2_676 79.39(7) ?
O12 Na2 Na1 . . 140.83(7) ?
O11 Na2 Na1 . . 52.94(6) ?
O10 Na2 Na1 2_676 . 72.30(6) ?
O10 Na2 Na1 . . 134.56(6) ?
S2 Na2 Na1 . . 49.16(3) ?
C2 Na2 Na1 2_676 . 72.17(7) ?
O12 Na2 Na2 . 2_676 99.38(7) ?
O11 Na2 Na2 . 2_676 106.02(7) ?
O10 Na2 Na2 2_676 2_676 40.77(5) ?
O10 Na2 Na2 . 2_676 40.46(5) ?
S2 Na2 Na2 . 2_676 138.87(5) ?
C2 Na2 Na2 2_676 2_676 60.56(7) ?
Na1 Na2 Na2 . 2_676 105.30(4) ?
C10 O1 Si1 . . 132.77(16) ?
C20 O2 Si1 . . 129.96(14) ?
C20 O2 Na1 . . 123.89(13) ?
Si1 O2 Na1 . . 103.95(8) ?
C30 O3 Si1 . . 133.23(15) ?
C40 O4 Si2 . . 131.46(14) ?
C40 O4 Na1 . . 121.66(13) ?
Si2 O4 Na1 . . 99.92(8) ?
C50 O5 Si2 . . 131.83(15) ?
C60 O6 Si2 . . 131.83(14) ?
O11 C1 H1A . . 109.5 ?
O11 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
O11 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O10 C2 H2A . . 109.5 ?
O10 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
O10 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
O12 C3 H3A . . 109.5 ?
O12 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
O12 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
O1 C10 C12 . . 110.6(2) ?
O1 C10 C13 . . 105.1(2) ?
C12 C10 C13 . . 111.3(3) ?
O1 C10 C11 . . 108.8(2) ?
C12 C10 C11 . . 111.4(2) ?
C13 C10 C11 . . 109.4(2) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C10 C13 H13A . . 109.5 ?
C10 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C10 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
O2 C20 C21 . . 111.3(2) ?
O2 C20 C23 . . 105.2(2) ?
C21 C20 C23 . . 110.5(2) ?
O2 C20 C22 . . 108.29(19) ?
C21 C20 C22 . . 111.2(2) ?
C23 C20 C22 . . 110.2(2) ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C20 C22 H22A . . 109.5 ?
C20 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C20 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C20 C23 H23A . . 109.5 ?
C20 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C20 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
O3 C30 C33 . . 109.0(2) ?
O3 C30 C31 . . 110.8(2) ?
C33 C30 C31 . . 110.5(2) ?
O3 C30 C32 . . 105.4(2) ?
C33 C30 C32 . . 110.3(2) ?
C31 C30 C32 . . 110.7(2) ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C30 C33 H33A . . 109.5 ?
C30 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C30 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
O4 C40 C41 . . 108.17(19) ?
O4 C40 C42 . . 111.91(19) ?
C41 C40 C42 . . 110.8(2) ?
O4 C40 C43 . . 105.25(19) ?
C41 C40 C43 . . 110.1(2) ?
C42 C40 C43 . . 110.5(2) ?
C40 C41 H41A . . 109.5 ?
C40 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
C40 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
C40 C42 H42A . . 109.5 ?
C40 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C40 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
C40 C43 H43A . . 109.5 ?
C40 C43 H43B . . 109.5 ?
H43A C43 H43B . . 109.5 ?
C40 C43 H43C . . 109.5 ?
H43A C43 H43C . . 109.5 ?
H43B C43 H43C . . 109.5 ?
O5 C50 C53 . . 110.39(19) ?
O5 C50 C52 . . 109.36(18) ?
C53 C50 C52 . . 110.8(2) ?
O5 C50 C51 . . 104.70(19) ?
C53 C50 C51 . . 111.6(2) ?
C52 C50 C51 . . 109.9(2) ?
C50 C51 H51A . . 109.5 ?
C50 C51 H51B . . 109.5 ?
H51A C51 H51B . . 109.5 ?
C50 C51 H51C . . 109.5 ?
H51A C51 H51C . . 109.5 ?
H51B C51 H51C . . 109.5 ?
C50 C52 H52A . . 109.5 ?
C50 C52 H52B . . 109.5 ?
H52A C52 H52B . . 109.5 ?
C50 C52 H52C . . 109.5 ?
H52A C52 H52C . . 109.5 ?
H52B C52 H52C . . 109.5 ?
C50 C53 H53A . . 109.5 ?
C50 C53 H53B . . 109.5 ?
H53A C53 H53B . . 109.5 ?
C50 C53 H53C . . 109.5 ?
H53A C53 H53C . . 109.5 ?
H53B C53 H53C . . 109.5 ?
O6 C60 C62 . . 110.6(2) ?
O6 C60 C61 . . 108.4(2) ?
C62 C60 C61 . . 110.7(2) ?
O6 C60 C63 . . 105.3(2) ?
C62 C60 C63 . . 110.8(2) ?
C61 C60 C63 . . 110.8(2) ?
C60 C61 H61A . . 109.5 ?
C60 C61 H61B . . 109.5 ?
H61A C61 H61B . . 109.5 ?
C60 C61 H61C . . 109.5 ?
H61A C61 H61C . . 109.5 ?
H61B C61 H61C . . 109.5 ?
C60 C62 H62A . . 109.5 ?
C60 C62 H62B . . 109.5 ?
H62A C62 H62B . . 109.5 ?
C60 C62 H62C . . 109.5 ?
H62A C62 H62C . . 109.5 ?
H62B C62 H62C . . 109.5 ?
C60 C63 H63A . . 109.5 ?
C60 C63 H63B . . 109.5 ?
H63A C63 H63B . . 109.5 ?
C60 C63 H63C . . 109.5 ?
H63A C63 H63C . . 109.5 ?
H63B C63 H63C . . 109.5 ?
C2 O10 Na2 . 2_676 106.76(16) ?
C2 O10 Na2 . . 126.00(16) ?
Na2 O10 Na2 2_676 . 98.77(8) ?
C2 O10 H10D . . 110(3) ?
Na2 O10 H10D 2_676 . 105(3) ?
Na2 O10 H10D . . 108(3) ?
C1 O11 Na2 . . 134.03(17) ?
C1 O11 Na1 . . 118.50(17) ?
Na2 O11 Na1 . . 86.34(7) ?
C1 O11 H11D . . 110(2) ?
Na2 O11 H11D . . 106(2) ?
Na1 O11 H11D . . 92(2) ?
C3 O12 Na2 . . 132.85(18) ?
C3 O12 H12D . . 115(3) ?
Na2 O12 H12D . . 112(3) ?
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
Si1 O1 . 1.6234(18) ?
Si1 O3 . 1.6261(17) ?
Si1 O2 . 1.6480(17) ?
Si1 S1 . 2.0559(10) yes
Si1 Na1 . 3.2029(15) ?
Si2 O6 . 1.6254(17) ?
Si2 O5 . 1.6496(16) ?
Si2 O4 . 1.6559(16) ?
Si2 S2 . 2.0434(13) yes
Si2 Na1 . 3.1095(14) ?
S1 Na1 . 2.7386(15) yes
S2 Na1 . 2.7632(13) yes
S2 Na2 . 2.8542(13) yes
Na1 O4 . 2.362(2) yes
Na1 O2 . 2.3778(19) yes
Na1 O11 . 2.871(2) yes
Na1 Na2 . 3.5906(16) yes
Na2 O12 . 2.273(2) yes
Na2 O11 . 2.347(2) yes
Na2 O10 2_676 2.405(2) yes
Na2 O10 . 2.420(2) yes
Na2 C2 2_676 3.129(3) ?
Na2 Na2 2_676 3.663(2) yes
O1 C10 . 1.442(3) ?
O2 C20 . 1.455(3) ?
O3 C30 . 1.434(3) ?
O4 C40 . 1.451(3) ?
O5 C50 . 1.459(3) ?
O6 C60 . 1.441(3) ?
C1 O11 . 1.418(3) ?
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?
C2 O10 . 1.424(3) ?
C2 H2A . 0.98 ?
C2 H2B . 0.98 ?
C2 H2C . 0.98 ?
C3 O12 . 1.414(3) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C10 C12 . 1.507(4) ?
C10 C13 . 1.516(4) ?
C10 C11 . 1.517(4) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C20 C21 . 1.518(3) ?
C20 C23 . 1.520(4) ?
C20 C22 . 1.522(4) ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?
C30 C33 . 1.515(4) ?
C30 C31 . 1.517(4) ?
C30 C32 . 1.526(4) ?
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
C32 H32A . 0.98 ?
C32 H32B . 0.98 ?
C32 H32C . 0.98 ?
C33 H33A . 0.98 ?
C33 H33B . 0.98 ?
C33 H33C . 0.98 ?
C40 C41 . 1.513(4) ?
C40 C42 . 1.521(3) ?
C40 C43 . 1.522(3) ?
C41 H41A . 0.98 ?
C41 H41B . 0.98 ?
C41 H41C . 0.98 ?
C42 H42A . 0.98 ?
C42 H42B . 0.98 ?
C42 H42C . 0.98 ?
C43 H43A . 0.98 ?
C43 H43B . 0.98 ?
C43 H43C . 0.98 ?
C50 C53 . 1.511(4) ?
C50 C52 . 1.519(4) ?
C50 C51 . 1.519(4) ?
C51 H51A . 0.98 ?
C51 H51B . 0.98 ?
C51 H51C . 0.98 ?
C52 H52A . 0.98 ?
C52 H52B . 0.98 ?
C52 H52C . 0.98 ?
C53 H53A . 0.98 ?
C53 H53B . 0.98 ?
C53 H53C . 0.98 ?
C60 C62 . 1.515(4) ?
C60 C61 . 1.518(4) ?
C60 C63 . 1.519(4) ?
C61 H61A . 0.98 ?
C61 H61B . 0.98 ?
C61 H61C . 0.98 ?
C62 H62A . 0.98 ?
C62 H62B . 0.98 ?
C62 H62C . 0.98 ?
C63 H63A . 0.98 ?
C63 H63B . 0.98 ?
C63 H63C . 0.98 ?
O10 H10D . 0.78(4) ?
O11 H11D . 0.83(3) ?
O12 H12D . 0.81(4) ?
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
O10 H10D S1 2_676 0.78(4) 2.44(4) 3.216(2) 172(4)
O11 H11D O5 . 0.83(3) 1.99(3) 2.803(3) 163(3)
O12 H12D S1 2_676 0.81(4) 2.35(4) 3.161(2) 175(4)
