# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ysp4
_database_code_depnum_ccdc_archive 'CCDC 1877014'
loop_
_audit_author_name
_audit_author_address
'Ilya Yakushev'
;Kurnakov Institute of general and inorganic chemistry, RAS
Russia
;
_audit_update_record             
;
2018-11-04 deposited with the CCDC.	2019-02-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_ysp4                
;
PROBLEM: D-H Without Acceptor       O12      --H12      .     Please Check
RESPONSE: The hydrogen atom linked only with the oxygen atom of the hydroxyl group is due to the absence of a suitable acceptor atom
;
_vrf_PLAT420_ysp4_2              
;
PROBLEM: D-H Without Acceptor       O13      --H13B     .     Please Check
RESPONSE: The water molecule fixed by three hydrogen bonds (two with hydrogen atoms of inorganic layer and one with the oxygen atom of the sulfogroup); one hydrogen atom of the multiply linked water doesn't have complementary acceptor
;
# Added during the CSD deposition process: Sunday 04 November 2018 06:38 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H11 O12 S Y3, H2O'
_chemical_formula_sum            'C7 H13 O13 S Y3'
_chemical_formula_weight         603.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0050 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0140 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1510 0.1580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -1.9390 0.6320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.964(3)
_cell_length_b                   10.539(2)
_cell_length_c                   12.351(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.96(3)
_cell_angle_gamma                90
_cell_volume                     1708.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    700
_cell_measurement_theta_min      4.0
_cell_measurement_theta_max      30.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.481
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_process_details   'Scala (Evans, 2006)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.80246
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       /f
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18013
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.799
_diffrn_reflns_theta_max         30.893
_diffrn_reflns_theta_full        28.782
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3720
_reflns_number_gt                3473
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_reduction        iMosflm
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2013)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0508P)²+2.2320P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0043(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3720
_refine_ls_number_parameters     282
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.1089
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.93657(2) 0.75548(2) 0.35142(2) 0.00579(13) Uani 1 1 d . . . . .
S1 S 0.27053(5) 0.77950(7) 0.25337(7) 0.01281(19) Uani 1 1 d . . . . .
O1 O 0.21918(16) 0.6598(2) 0.20801(19) 0.0120(4) Uani 1 1 d . . . . .
C1 C 0.4024(2) 0.7464(3) 0.2961(3) 0.0146(6) Uani 1 1 d D U . . .
Y2 Y 1.04543(2) 0.58506(2) 0.14770(2) 0.00589(13) Uani 1 1 d . . . . .
O2 O 0.24948(18) 0.8778(2) 0.1668(2) 0.0230(6) Uani 1 1 d . . . . .
C2A C 0.4601(6) 0.8081(12) 0.2420(12) 0.025(2) Uani 0.59(4) 1 d D U P A 1
H2A H 0.4291 0.8669 0.1819 0.030 Uiso 0.59(4) 1 calc R U P A 1
C2B C 0.4518(8) 0.765(3) 0.2182(12) 0.031(4) Uani 0.41(4) 1 d D U P A 2
H2B H 0.4156 0.7952 0.1426 0.037 Uiso 0.41(4) 1 calc R U P A 2
Y3 Y 0.93618(2) 0.92209(2) 0.10118(2) 0.00571(13) Uani 1 1 d . . . . .
O3 O 0.25055(18) 0.8175(2) 0.3578(2) 0.0211(5) Uani 1 1 d D . . . .
C3A C 0.5650(6) 0.7840(13) 0.2759(11) 0.023(2) Uani 0.59(4) 1 d D U P A 1
H3A H 0.6053 0.8263 0.2386 0.028 Uiso 0.59(4) 1 calc R U P A 1
C3B C 0.5560(8) 0.740(3) 0.2521(12) 0.031(4) Uani 0.41(4) 1 d D U P A 2
H3B H 0.5907 0.7507 0.1985 0.038 Uiso 0.41(4) 1 calc R U P A 2
O4 O 0.76493(17) 0.6195(2) 0.49428(19) 0.0162(5) Uani 1 1 d . . . . .
C4 C 0.6099(2) 0.6985(3) 0.3637(3) 0.0128(6) Uani 1 1 d D U . . .
O5 O 0.76939(18) 0.7324(2) 0.3434(2) 0.0200(5) Uani 1 1 d . . . . .
C5A C 0.5510(9) 0.6401(14) 0.4192(12) 0.021(3) Uani 0.59(4) 1 d D U P A 1
H5A H 0.5823 0.5843 0.4818 0.025 Uiso 0.59(4) 1 calc R U P A 1
C5B C 0.5558(13) 0.670(2) 0.4358(14) 0.023(4) Uani 0.41(4) 1 d D U P A 2
H5B H 0.5897 0.6327 0.5088 0.027 Uiso 0.41(4) 1 calc R U P A 2
O6 O 0.91146(16) 0.7046(2) 0.16360(17) 0.0075(4) Uani 1 1 d D . . . .
H6 H 0.8533(19) 0.677(5) 0.1232(17) 0.054(17) Uiso 1 1 d DR . . . .
C6A C 0.4466(8) 0.6617(15) 0.3845(16) 0.021(3) Uani 0.59(4) 1 d D U P A 1
H6A H 0.4061 0.6189 0.4212 0.026 Uiso 0.59(4) 1 calc R U P A 1
C6B C 0.4521(11) 0.697(2) 0.4022(19) 0.021(3) Uani 0.41(4) 1 d D U P A 2
H6B H 0.4160 0.6799 0.4533 0.026 Uiso 0.41(4) 1 calc R U P A 2
O7 O 1.07801(16) 0.63428(19) 0.34872(18) 0.0077(4) Uani 1 1 d D . . . .
H7 H 1.1216(14) 0.690(2) 0.359(5) 0.08(2) Uiso 1 1 d DR . . . .
C7 C 0.7236(2) 0.6808(3) 0.4037(3) 0.0119(6) Uani 1 1 d . . . . .
O8 O 1.08317(17) 0.43469(19) 0.03316(19) 0.0081(4) Uani 1 1 d D . . . .
H8 H 1.1437(16) 0.428(3) 0.032(3) 0.030(14) Uiso 1 1 d DR . . . .
O9 O 1.03794(16) 0.77156(19) 0.04885(17) 0.0066(4) Uani 1 1 d D . . . .
H9 H 1.0852(12) 0.818(2) 0.048(3) 0.029(12) Uiso 1 1 d DR . . . .
O10 O 1.03533(17) 0.91165(17) 0.3002(2) 0.0075(4) Uani 1 1 d D . . . .
H10 H 1.0999(15) 0.909(3) 0.322(4) 0.040(16) Uiso 1 1 d DR . . . .
O11 O 1.07878(16) 1.0429(2) 0.09495(18) 0.0075(4) Uani 1 1 d . . . . .
H11 H 1.133(4) 1.007(3) 0.134(4) 0.056(17) Uiso 1 1 d R . . . .
O12 O 0.85179(17) 0.92602(17) 0.23416(19) 0.0075(4) Uani 1 1 d D . . . .
H12 H 0.7875(17) 0.937(6) 0.2093(8) 0.07(2) Uiso 1 1 d DR . . . .
O13 O 0.2718(2) 1.0565(3) 0.4717(3) 0.0352(7) Uani 1 1 d D . . . .
H13A H 0.280(4) 0.979(3) 0.447(4) 0.053 Uiso 1 1 d D U . . .
H13B H 0.325(3) 1.057(5) 0.535(3) 0.053 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O6 2.288(2) . ?
Y1 O5 2.315(2) . ?
Y1 O12 2.358(2) . ?
Y1 O7 2.362(2) . ?
Y1 O11 2.367(2) 2_745 ?
Y1 O10 2.368(2) . ?
Y1 O9 2.382(2) 4_576 ?
Y1 O8 2.438(2) 2_755 ?
Y1 Y2 3.4821(8) 2_755 ?
Y1 Y3 3.5531(7) . ?
Y1 Y3 3.6098(7) 4_576 ?
Y1 Y2 3.8052(8) . ?
S1 O2 1.445(3) . ?
S1 O1 1.465(2) . ?
S1 O3 1.466(3) . ?
S1 C1 1.769(3) . ?
O1 Y2 2.414(2) 1_455 ?
C1 C6B 1.36(2) . ?
C1 C2A 1.374(8) . ?
C1 C2B 1.376(11) . ?
C1 C6A 1.382(16) . ?
Y2 O9 2.297(2) . ?
Y2 O8 2.302(2) . ?
Y2 O6 2.319(2) . ?
Y2 O8 2.349(2) 3_765 ?
Y2 O10 2.350(2) 2_745 ?
Y2 O12 2.360(2) 2_745 ?
Y2 O1 2.414(2) 1_655 ?
Y2 O7 2.423(2) . ?
Y2 Y3 3.4774(7) 2_745 ?
Y2 Y1 3.4822(8) 2_745 ?
Y2 Y3 3.8309(7) . ?
C2A C3A 1.402(8) . ?
C2A H2A 0.9500 . ?
C2B C3B 1.396(11) . ?
C2B H2B 0.9500 . ?
Y3 O12 2.326(2) . ?
Y3 O4 2.345(2) 4_575 ?
Y3 O7 2.347(2) 2_755 ?
Y3 O9 2.362(2) . ?
Y3 O10 2.377(2) . ?
Y3 O11 2.387(2) . ?
Y3 O11 2.388(2) 3_775 ?
Y3 O6 2.480(2) . ?
Y3 Y2 3.4774(7) 2_755 ?
Y3 Y1 3.6098(7) 4_575 ?
C3A C4 1.385(8) . ?
C3A H3A 0.9500 . ?
C3B C4 1.396(10) . ?
C3B H3B 0.9500 . ?
O4 C7 1.250(4) . ?
O4 Y3 2.345(2) 4_576 ?
C4 C5A 1.382(8) . ?
C4 C5B 1.382(10) . ?
C4 C7 1.505(4) . ?
O5 C7 1.259(4) . ?
C5A C6A 1.392(9) . ?
C5A H5A 0.9500 . ?
C5B C6B 1.391(12) . ?
C5B H5B 0.9500 . ?
O6 H6 0.85(2) . ?
C6A H6A 0.9500 . ?
C6B H6B 0.9500 . ?
O7 Y3 2.347(2) 2_745 ?
O7 H7 0.82(2) . ?
O8 Y2 2.349(2) 3_765 ?
O8 Y1 2.438(2) 2_745 ?
O8 H8 0.85(2) . ?
O9 Y1 2.382(2) 4_575 ?
O9 H9 0.824(19) . ?
O10 Y2 2.350(2) 2_755 ?
O10 H10 0.85(2) . ?
O11 Y1 2.367(2) 2_755 ?
O11 Y3 2.388(2) 3_775 ?
O11 H11 0.84(6) . ?
O12 Y2 2.360(2) 2_755 ?
O12 H12 0.85(2) . ?
O13 H13A 0.896(17) . ?
O13 H13B 0.87(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Y1 O5 97.38(9) . . ?
O6 Y1 O12 71.64(8) . . ?
O5 Y1 O12 76.48(8) . . ?
O6 Y1 O7 72.44(8) . . ?
O5 Y1 O7 141.11(8) . . ?
O12 Y1 O7 130.58(8) . . ?
O6 Y1 O11 93.70(8) . 2_745 ?
O5 Y1 O11 74.11(8) . 2_745 ?
O12 Y1 O11 144.99(7) . 2_745 ?
O7 Y1 O11 69.40(7) . 2_745 ?
O6 Y1 O10 78.10(8) . . ?
O5 Y1 O10 137.07(8) . . ?
O12 Y1 O10 61.45(7) . . ?
O7 Y1 O10 78.82(7) . . ?
O11 Y1 O10 148.16(8) 2_745 . ?
O6 Y1 O9 147.30(7) . 4_576 ?
O5 Y1 O9 105.63(9) . 4_576 ?
O12 Y1 O9 135.92(7) . 4_576 ?
O7 Y1 O9 75.06(7) . 4_576 ?
O11 Y1 O9 71.29(7) 2_745 4_576 ?
O10 Y1 O9 99.20(8) . 4_576 ?
O6 Y1 O8 139.96(7) . 2_755 ?
O5 Y1 O8 78.05(8) . 2_755 ?
O12 Y1 O8 68.61(7) . 2_755 ?
O7 Y1 O8 133.57(7) . 2_755 ?
O11 Y1 O8 122.04(7) 2_745 2_755 ?
O10 Y1 O8 79.06(7) . 2_755 ?
O9 Y1 O8 68.92(7) 4_576 2_755 ?
O6 Y1 Y2 102.88(5) . 2_755 ?
O5 Y1 Y2 100.11(6) . 2_755 ?
O12 Y1 Y2 42.45(5) . 2_755 ?
O7 Y1 Y2 118.67(5) . 2_755 ?
O11 Y1 Y2 163.08(5) 2_745 2_755 ?
O10 Y1 Y2 42.23(5) . 2_755 ?
O9 Y1 Y2 95.69(5) 4_576 2_755 ?
O8 Y1 Y2 41.23(5) 2_755 2_755 ?
O6 Y1 Y3 43.93(5) . . ?
O5 Y1 Y3 108.21(7) . . ?
O12 Y1 Y3 40.32(5) . . ?
O7 Y1 Y3 90.45(6) . . ?
O11 Y1 Y3 137.55(5) 2_745 . ?
O10 Y1 Y3 41.60(6) . . ?
O9 Y1 Y3 140.67(5) 4_576 . ?
O8 Y1 Y3 99.15(5) 2_755 . ?
Y2 Y1 Y3 59.235(10) 2_755 . ?
O6 Y1 Y3 134.45(5) . 4_576 ?
O5 Y1 Y3 71.73(7) . 4_576 ?
O12 Y1 Y3 140.64(6) . 4_576 ?
O7 Y1 Y3 88.68(5) . 4_576 ?
O11 Y1 Y3 40.83(5) 2_745 4_576 ?
O10 Y1 Y3 139.43(6) . 4_576 ?
O9 Y1 Y3 40.26(5) 4_576 4_576 ?
O8 Y1 Y3 82.44(5) 2_755 4_576 ?
Y2 Y1 Y3 122.385(12) 2_755 4_576 ?
Y3 Y1 Y3 178.379(9) . 4_576 ?
O6 Y1 Y2 34.57(5) . . ?
O5 Y1 Y2 123.13(7) . . ?
O12 Y1 Y2 100.59(6) . . ?
O7 Y1 Y2 37.87(5) . . ?
O11 Y1 Y2 80.39(5) 2_745 . ?
O10 Y1 Y2 75.57(5) . . ?
O9 Y1 Y2 112.86(5) 4_576 . ?
O8 Y1 Y2 154.52(5) 2_755 . ?
Y2 Y1 Y2 115.353(12) 2_755 . ?
Y3 Y1 Y2 62.637(16) . . ?
Y3 Y1 Y2 115.970(17) 4_576 . ?
O2 S1 O1 112.66(15) . . ?
O2 S1 O3 113.79(16) . . ?
O1 S1 O3 110.90(14) . . ?
O2 S1 C1 106.86(15) . . ?
O1 S1 C1 105.54(14) . . ?
O3 S1 C1 106.46(15) . . ?
S1 O1 Y2 135.08(13) . 1_455 ?
C6B C1 C2B 121.1(7) . . ?
C2A C1 C6A 120.9(5) . . ?
C6B C1 S1 120.0(5) . . ?
C2A C1 S1 119.1(4) . . ?
C2B C1 S1 118.8(5) . . ?
C6A C1 S1 120.1(4) . . ?
O9 Y2 O8 103.93(7) . . ?
O9 Y2 O6 71.86(8) . . ?
O8 Y2 O6 141.87(8) . . ?
O9 Y2 O8 71.89(7) . 3_765 ?
O8 Y2 O8 67.40(9) . 3_765 ?
O6 Y2 O8 75.62(8) . 3_765 ?
O9 Y2 O10 150.68(7) . 2_745 ?
O8 Y2 O10 82.23(7) . 2_745 ?
O6 Y2 O10 85.57(7) . 2_745 ?
O8 Y2 O10 84.78(8) 3_765 2_745 ?
O9 Y2 O12 147.57(7) . 2_745 ?
O8 Y2 O12 70.89(8) . 2_745 ?
O6 Y2 O12 132.18(7) . 2_745 ?
O8 Y2 O12 129.13(7) 3_765 2_745 ?
O10 Y2 O12 61.69(7) 2_745 2_745 ?
O9 Y2 O1 75.14(7) . 1_655 ?
O8 Y2 O1 89.85(8) . 1_655 ?
O6 Y2 O1 123.49(7) . 1_655 ?
O8 Y2 O1 133.14(8) 3_765 1_655 ?
O10 Y2 O1 134.02(8) 2_745 1_655 ?
O12 Y2 O1 72.89(7) 2_745 1_655 ?
O9 Y2 O7 108.67(7) . . ?
O8 Y2 O7 140.80(7) . . ?
O6 Y2 O7 70.83(8) . . ?
O8 Y2 O7 143.96(7) 3_765 . ?
O10 Y2 O7 79.96(8) 2_745 . ?
O12 Y2 O7 69.92(7) 2_745 . ?
O1 Y2 O7 78.27(8) 1_655 . ?
O9 Y2 Y3 150.78(5) . 2_745 ?
O8 Y2 Y3 104.21(6) . 2_745 ?
O6 Y2 Y3 90.50(6) . 2_745 ?
O8 Y2 Y3 127.16(6) 3_765 2_745 ?
O10 Y2 Y3 42.93(6) 2_745 2_745 ?
O12 Y2 Y3 41.72(5) 2_745 2_745 ?
O1 Y2 Y3 97.21(6) 1_655 2_745 ?
O7 Y2 Y3 42.34(5) . 2_745 ?
O9 Y2 Y1 147.69(5) . 2_745 ?
O8 Y2 Y1 44.26(5) . 2_745 ?
O6 Y2 Y1 126.95(5) . 2_745 ?
O8 Y2 Y1 86.88(5) 3_765 2_745 ?
O10 Y2 Y1 42.63(5) 2_745 2_745 ?
O12 Y2 Y1 42.40(5) 2_745 2_745 ?
O1 Y2 Y1 105.10(5) 1_655 2_745 ?
O7 Y2 Y1 102.84(5) . 2_745 ?
Y3 Y2 Y1 61.399(10) 2_745 2_745 ?
O9 Y2 Y1 89.52(5) . . ?
O8 Y2 Y1 163.38(5) . . ?
O6 Y2 Y1 34.06(5) . . ?
O8 Y2 Y1 108.81(5) 3_765 . ?
O10 Y2 Y1 81.29(6) 2_745 . ?
O12 Y2 Y1 102.85(6) 2_745 . ?
O1 Y2 Y1 103.20(6) 1_655 . ?
O7 Y2 Y1 36.77(5) . . ?
Y3 Y2 Y1 64.396(16) 2_745 . ?
Y1 Y2 Y1 120.893(11) 2_745 . ?
O9 Y2 Y3 35.26(5) . . ?
O8 Y2 Y3 135.16(5) . . ?
O6 Y2 Y3 38.51(5) . . ?
O8 Y2 Y3 78.67(5) 3_765 . ?
O10 Y2 Y3 123.95(5) 2_745 . ?
O12 Y2 Y3 151.44(5) 2_745 . ?
O1 Y2 Y3 92.91(5) 1_655 . ?
O7 Y2 Y3 83.17(5) . . ?
Y3 Y2 Y3 119.742(14) 2_745 . ?
Y1 Y2 Y3 161.792(12) 2_745 . ?
Y1 Y2 Y3 55.459(10) . . ?
C1 C2A C3A 119.7(6) . . ?
C1 C2A H2A 120.2 . . ?
C3A C2A H2A 120.2 . . ?
C1 C2B C3B 118.8(9) . . ?
C1 C2B H2B 120.6 . . ?
C3B C2B H2B 120.6 . . ?
O12 Y3 O4 74.68(8) . 4_575 ?
O12 Y3 O7 71.82(7) . 2_755 ?
O4 Y3 O7 99.49(8) 4_575 2_755 ?
O12 Y3 O9 134.61(7) . . ?
O4 Y3 O9 108.27(8) 4_575 . ?
O7 Y3 O9 145.58(7) 2_755 . ?
O12 Y3 O10 61.77(8) . . ?
O4 Y3 O10 134.09(8) 4_575 . ?
O7 Y3 O10 80.97(7) 2_755 . ?
O9 Y3 O10 93.41(7) . . ?
O12 Y3 O11 129.99(7) . . ?
O4 Y3 O11 141.56(8) 4_575 . ?
O7 Y3 O11 69.31(8) 2_755 . ?
O9 Y3 O11 76.29(7) . . ?
O10 Y3 O11 81.96(8) . . ?
O12 Y3 O11 145.45(8) . 3_775 ?
O4 Y3 O11 74.84(8) 4_575 3_775 ?
O7 Y3 O11 97.72(7) 2_755 3_775 ?
O9 Y3 O11 71.26(7) . 3_775 ?
O10 Y3 O11 151.02(8) . 3_775 ?
O11 Y3 O11 70.73(9) . 3_775 ?
O12 Y3 O6 68.84(7) . . ?
O4 Y3 O6 77.22(8) 4_575 . ?
O7 Y3 O6 139.96(7) 2_755 . ?
O9 Y3 O6 67.97(7) . . ?
O10 Y3 O6 74.30(6) . . ?
O11 Y3 O6 135.17(7) . . ?
O11 Y3 O6 119.01(7) 3_775 . ?
O12 Y3 Y2 42.46(5) . 2_755 ?
O4 Y3 Y2 110.19(6) 4_575 2_755 ?
O7 Y3 Y2 44.05(5) 2_755 2_755 ?
O9 Y3 Y2 135.04(5) . 2_755 ?
O10 Y3 Y2 42.33(5) . 2_755 ?
O11 Y3 Y2 87.53(6) . 2_755 ?
O11 Y3 Y2 141.51(5) 3_775 2_755 ?
O6 Y3 Y2 98.92(5) . 2_755 ?
O12 Y3 Y1 40.99(5) . . ?
O4 Y3 Y1 95.50(6) 4_575 . ?
O7 Y3 Y1 102.51(5) 2_755 . ?
O9 Y3 Y1 94.80(5) . . ?
O10 Y3 Y1 41.41(5) . . ?
O11 Y3 Y1 122.55(6) . . ?
O11 Y3 Y1 158.81(5) 3_775 . ?
O6 Y3 Y1 39.81(5) . . ?
Y2 Y3 Y1 59.366(16) 2_755 . ?
O12 Y3 Y1 139.61(5) . 4_575 ?
O4 Y3 Y1 73.78(6) 4_575 4_575 ?
O7 Y3 Y1 138.10(5) 2_755 4_575 ?
O9 Y3 Y1 40.67(5) . 4_575 ?
O10 Y3 Y1 133.60(5) . 4_575 ?
O11 Y3 Y1 90.25(6) . 4_575 ?
O11 Y3 Y1 40.39(5) 3_775 4_575 ?
O6 Y3 Y1 80.06(5) . 4_575 ?
Y2 Y3 Y1 175.652(10) 2_755 4_575 ?
Y1 Y3 Y1 119.157(15) . 4_575 ?
O12 Y3 Y2 100.51(5) . . ?
O4 Y3 Y2 100.87(6) 4_575 . ?
O7 Y3 Y2 155.39(5) 2_755 . ?
O9 Y3 Y2 34.15(5) . . ?
O10 Y3 Y2 74.95(5) . . ?
O11 Y3 Y2 101.86(5) . . ?
O11 Y3 Y2 100.83(5) 3_775 . ?
O6 Y3 Y2 35.60(5) . . ?
Y2 Y3 Y2 114.820(17) 2_755 . ?
Y1 Y3 Y2 61.904(14) . . ?
Y1 Y3 Y2 62.017(16) 4_575 . ?
C4 C3A C2A 119.9(6) . . ?
C4 C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C2B C3B C4 120.7(9) . . ?
C2B C3B H3B 119.6 . . ?
C4 C3B H3B 119.6 . . ?
C7 O4 Y3 132.2(2) . 4_576 ?
C5A C4 C3A 119.5(6) . . ?
C5B C4 C3B 118.3(8) . . ?
C5A C4 C7 121.4(6) . . ?
C5B C4 C7 120.6(8) . . ?
C3A C4 C7 118.8(4) . . ?
C3B C4 C7 121.0(5) . . ?
C7 O5 Y1 136.8(2) . . ?
C4 C5A C6A 120.8(8) . . ?
C4 C5A H5A 119.6 . . ?
C6A C5A H5A 119.6 . . ?
C4 C5B C6B 120.4(12) . . ?
C4 C5B H5B 119.8 . . ?
C6B C5B H5B 119.8 . . ?
Y1 O6 Y2 111.37(9) . . ?
Y1 O6 Y3 96.26(7) . . ?
Y2 O6 Y3 105.89(8) . . ?
Y1 O6 H6 117.5 . . ?
Y2 O6 H6 113.6 . . ?
Y3 O6 H6 110.2 . . ?
C1 C6A C5A 119.1(9) . . ?
C1 C6A H6A 120.4 . . ?
C5A C6A H6A 120.4 . . ?
C1 C6B C5B 120.1(12) . . ?
C1 C6B H6B 120.0 . . ?
C5B C6B H6B 120.0 . . ?
Y3 O7 Y1 111.43(9) 2_745 . ?
Y3 O7 Y2 93.61(7) 2_745 . ?
Y1 O7 Y2 105.36(8) . . ?
Y3 O7 H7 139.7 2_745 . ?
Y1 O7 H7 100.7 . . ?
Y2 O7 H7 100.8 . . ?
O4 C7 O5 125.5(3) . . ?
O4 C7 C4 118.1(3) . . ?
O5 C7 C4 116.4(3) . . ?
Y2 O8 Y2 112.60(9) . 3_765 ?
Y2 O8 Y1 94.51(8) . 2_745 ?
Y2 O8 Y1 106.56(8) 3_765 2_745 ?
Y2 O8 H8 119.9 . . ?
Y2 O8 H8 114.9 3_765 . ?
Y1 O8 H8 104.8 2_745 . ?
Y2 O9 Y3 110.59(9) . . ?
Y2 O9 Y1 110.18(8) . 4_575 ?
Y3 O9 Y1 99.07(8) . 4_575 ?
Y2 O9 H9 128.5 . . ?
Y3 O9 H9 99.3 . . ?
Y1 O9 H9 105.0 4_575 . ?
Y2 O10 Y1 95.15(9) 2_755 . ?
Y2 O10 Y3 94.74(8) 2_755 . ?
Y1 O10 Y3 96.99(8) . . ?
Y2 O10 H10 119.7 2_755 . ?
Y1 O10 H10 122.9 . . ?
Y3 O10 H10 120.9 . . ?
Y1 O11 Y3 109.85(9) 2_755 . ?
Y1 O11 Y3 98.79(8) 2_755 3_775 ?
Y3 O11 Y3 109.27(9) . 3_775 ?
Y1 O11 H11 114.5 2_755 . ?
Y3 O11 H11 109.9 . . ?
Y3 O11 H11 114.0 3_775 . ?
Y3 O12 Y1 98.68(8) . . ?
Y3 O12 Y2 95.83(8) . 2_755 ?
Y1 O12 Y2 95.15(8) . 2_755 ?
Y3 O12 H12 118.3 . . ?
Y1 O12 H12 124.9 . . ?
Y2 O12 H12 117.9 2_755 . ?
H13A O13 H13B 98(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 O1 Y2 -72.5(2) . . . 1_455 ?
O3 S1 O1 Y2 56.4(2) . . . 1_455 ?
C1 S1 O1 Y2 171.29(17) . . . 1_455 ?
O2 S1 C1 C6B 155.0(12) . . . . ?
O1 S1 C1 C6B -84.8(12) . . . . ?
O3 S1 C1 C6B 33.1(12) . . . . ?
O2 S1 C1 C2A -3.0(8) . . . . ?
O1 S1 C1 C2A 117.1(8) . . . . ?
O3 S1 C1 C2A -125.0(8) . . . . ?
O2 S1 C1 C2B -28.4(13) . . . . ?
O1 S1 C1 C2B 91.7(13) . . . . ?
O3 S1 C1 C2B -150.4(13) . . . . ?
O2 S1 C1 C6A 175.4(9) . . . . ?
O1 S1 C1 C6A -64.4(9) . . . . ?
O3 S1 C1 C6A 53.5(9) . . . . ?
C6B C1 C2A C3A 20.6(11) . . . . ?
C2B C1 C2A C3A -85.1(17) . . . . ?
C6A C1 C2A C3A 0.8(10) . . . . ?
S1 C1 C2A C3A 179.2(5) . . . . ?
C6B C1 C2B C3B -3.9(13) . . . . ?
C2A C1 C2B C3B 82.9(17) . . . . ?
C6A C1 C2B C3B -23.5(12) . . . . ?
S1 C1 C2B C3B 179.7(7) . . . . ?
C1 C2A C3A C4 -0.2(10) . . . . ?
C1 C2B C3B C4 -1.4(13) . . . . ?
C2A C3A C4 C5A -1.6(11) . . . . ?
C2A C3A C4 C5B -18.8(12) . . . . ?
C2A C3A C4 C3B 82.0(16) . . . . ?
C2A C3A C4 C7 -176.0(5) . . . . ?
C2B C3B C4 C5A 23.8(14) . . . . ?
C2B C3B C4 C5B 6.9(17) . . . . ?
C2B C3B C4 C3A -84.0(18) . . . . ?
C2B C3B C4 C7 -175.1(7) . . . . ?
C5B C4 C5A C6A 85(4) . . . . ?
C3A C4 C5A C6A 2.8(15) . . . . ?
C3B C4 C5A C6A -21.9(16) . . . . ?
C7 C4 C5A C6A 177.1(8) . . . . ?
C5A C4 C5B C6B -88(5) . . . . ?
C3A C4 C5B C6B 17.9(19) . . . . ?
C3B C4 C5B C6B -7(2) . . . . ?
C7 C4 C5B C6B 174.7(12) . . . . ?
C6B C1 C6A C5A -83(3) . . . . ?
C2A C1 C6A C5A 0.5(13) . . . . ?
C2B C1 C6A C5A 25.4(13) . . . . ?
S1 C1 C6A C5A -178.0(8) . . . . ?
C4 C5A C6A C1 -2.3(16) . . . . ?
C2A C1 C6B C5B -21.7(17) . . . . ?
C2B C1 C6B C5B 3.4(18) . . . . ?
C6A C1 C6B C5B 84(3) . . . . ?
S1 C1 C6B C5B 179.9(12) . . . . ?
C4 C5B C6B C1 2(2) . . . . ?
Y3 O4 C7 O5 3.7(5) 4_576 . . . ?
Y3 O4 C7 C4 -174.5(2) 4_576 . . . ?
Y1 O5 C7 O4 -1.5(5) . . . . ?
Y1 O5 C7 C4 176.8(2) . . . . ?
C5A C4 C7 O4 -5.5(10) . . . . ?
C5B C4 C7 O4 12.6(13) . . . . ?
C3A C4 C7 O4 168.8(8) . . . . ?
C3B C4 C7 O4 -165.3(14) . . . . ?
C5A C4 C7 O5 176.1(9) . . . . ?
C5B C4 C7 O5 -165.8(13) . . . . ?
C3A C4 C7 O5 -9.6(9) . . . . ?
C3B C4 C7 O5 16.3(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13A O3 0.896(17) 1.990(17) 2.850(4) 161(5) .
O6 H6 O13 0.85 2.15 2.976(4) 164.1 2_645
O7 H7 O3 0.82 2.25 3.060(3) 166.7 1_655
O10 H10 O3 0.85 2.22 3.010(3) 155.5 1_655
O11 H11 O2 0.84 2.05 2.838(3) 155.7 1_655
O8 H8 O13 0.85 2.17 2.982(4) 159.6 4_675

_refine_diff_density_max         1.646
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.211

_shelxl_version_number           2013-4

