# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 Nd2 O17 S2'
_chemical_formula_weight         806.85

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.965(3)
_cell_length_b                   6.1120(10)
_cell_length_c                   19.828(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.194(2)
_cell_angle_gamma                90.00
_cell_volume                     2255.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7673
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2426
_exptl_absorpt_correction_T_max  0.4169
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7958
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2101
_reflns_number_gt                2082
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0251P)²+14.9214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00209(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2101
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.137359(8) 1.18144(3) 0.469824(9) 0.01488(10) Uani 1 1 d . . .
S1 S 0.10879(6) 0.7643(2) 0.21905(6) 0.0383(3) Uani 1 1 d . . .
O1 O 0.23177(13) 0.3474(4) 0.43324(13) 0.0211(5) Uani 1 1 d . . .
O2 O 0.31745(13) 0.5230(4) 0.41076(14) 0.0260(5) Uani 1 1 d . . .
O3 O 0.19295(12) 0.8603(4) 0.42890(12) 0.0196(5) Uani 1 1 d . . .
O4 O 0.10797(14) 1.0398(4) 0.34369(13) 0.0272(6) Uani 1 1 d . . .
O5 O 0.04597(14) 1.2470(4) 0.52532(15) 0.0271(6) Uani 1 1 d . . .
O6 O -0.05159(13) 1.1271(4) 0.54421(14) 0.0249(5) Uani 1 1 d . . .
O7 O 0.05291(16) 1.4465(5) 0.38956(14) 0.0380(7) Uani 1 1 d . . .
H1W H 0.0387 1.5202 0.3506 0.057 Uiso 1 1 d R . .
H2W H 0.0220 1.4616 0.4095 0.057 Uiso 1 1 d R . .
O8 O 0.16447(13) 1.5279(4) 0.53562(13) 0.0250(5) Uani 1 1 d . . .
H3W H 0.1386 1.6424 0.5273 0.038 Uiso 1 1 d R . .
H4W H 0.2069 1.5682 0.5411 0.038 Uiso 1 1 d R . .
O9 O 1.0000 0.2939(7) 0.2500 0.0389(10) Uani 1 2 d S . .
H5W H 0.9640 0.2095 0.2329 0.058 Uiso 1 1 d R . .
C1 C 0.25316(17) 0.4686(5) 0.39247(17) 0.0172(6) Uani 1 1 d . . .
C2 C 0.20062(17) 0.5422(5) 0.32055(17) 0.0181(6) Uani 1 1 d . . .
C3 C 0.19145(17) 0.4196(5) 0.25134(16) 0.0160(6) Uani 1 1 d . . .
H3 H 0.2143 0.2908 0.2470 0.019 Uiso 1 1 calc R . .
C4 C 0.1423(3) 0.5373(8) 0.1960(2) 0.0411(10) Uani 1 1 d . . .
H4 H 0.1285 0.4925 0.1480 0.049 Uiso 1 1 calc R . .
C5 C 0.15823(19) 0.7278(6) 0.30892(18) 0.0208(7) Uani 1 1 d . . .
C6 C 0.15279(17) 0.8843(6) 0.36301(18) 0.0182(7) Uani 1 1 d . . .
C7 C -0.00099(17) 1.1091(5) 0.52015(18) 0.0188(7) Uani 1 1 d . . .


_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
Nd1 O8 2.443(2) . ?
Nd1 O7 2.462(3) . ?
Nd1 O1 2.469(2) 1_565 ?
Nd1 O5 2.480(2) . ?
Nd1 O6 2.494(2) 5_576 ?
Nd1 O4 2.508(2) . ?
Nd1 O3 2.528(2) . ?
Nd1 O2 2.537(3) 7_566 ?
Nd1 O1 2.631(2) 7_566 ?
Nd1 C1 2.959(3) 7_566 ?
S1 C4 1.675(5) . ?
S1 C5 1.711(3) . ?
O1 C1 1.279(4) . ?
O1 Nd1 2.469(2) 1_545 ?
O1 Nd1 2.631(2) 7_566 ?
O2 C1 1.246(4) . ?
O2 Nd1 2.537(3) 7_566 ?
O3 C6 1.270(4) . ?
O4 C6 1.266(4) . ?
O5 C7 1.237(4) . ?
O6 C7 1.268(4) . ?
O6 Nd1 2.494(2) 5_576 ?
O7 H1W 0.8499 . ?
O7 H2W 0.8500 . ?
O8 H3W 0.8499 . ?
O8 H4W 0.8502 . ?
O9 H5W 0.8500 . ?
C1 C2 1.502(4) . ?
C1 Nd1 2.959(3) 7_566 ?
C2 C5 1.384(5) . ?
C2 C3 1.515(4) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.470(5) . ?
C7 C7 1.563(7) 5_576 ?

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
O8 Nd1 O7 75.08(9) . . ?
O8 Nd1 O1 75.85(8) . 1_565 ?
O7 Nd1 O1 87.53(10) . 1_565 ?
O8 Nd1 O5 71.31(8) . . ?
O7 Nd1 O5 74.85(10) . . ?
O1 Nd1 O5 145.70(8) 1_565 . ?
O8 Nd1 O6 136.51(8) . 5_576 ?
O7 Nd1 O6 98.23(10) . 5_576 ?
O1 Nd1 O6 147.57(8) 1_565 5_576 ?
O5 Nd1 O6 65.55(8) . 5_576 ?
O8 Nd1 O4 139.34(9) . . ?
O7 Nd1 O4 73.96(9) . . ?
O1 Nd1 O4 77.11(9) 1_565 . ?
O5 Nd1 O4 123.63(9) . . ?
O6 Nd1 O4 73.98(9) 5_576 . ?
O8 Nd1 O3 143.70(8) . . ?
O7 Nd1 O3 125.51(8) . . ?
O1 Nd1 O3 75.77(8) 1_565 . ?
O5 Nd1 O3 138.28(8) . . ?
O6 Nd1 O3 74.97(8) 5_576 . ?
O4 Nd1 O3 51.94(8) . . ?
O8 Nd1 O2 89.61(9) . 7_566 ?
O7 Nd1 O2 148.96(9) . 7_566 ?
O1 Nd1 O2 115.14(8) 1_565 7_566 ?
O5 Nd1 O2 74.69(9) . 7_566 ?
O6 Nd1 O2 74.33(8) 5_576 7_566 ?
O4 Nd1 O2 129.55(9) . 7_566 ?
O3 Nd1 O2 82.41(8) . 7_566 ?
O8 Nd1 O1 72.43(8) . 7_566 ?
O7 Nd1 O1 141.59(9) . 7_566 ?
O1 Nd1 O1 65.17(9) 1_565 7_566 ?
O5 Nd1 O1 112.48(8) . 7_566 ?
O6 Nd1 O1 119.44(8) 5_576 7_566 ?
O4 Nd1 O1 121.20(8) . 7_566 ?
O3 Nd1 O1 75.36(7) . 7_566 ?
O2 Nd1 O1 50.29(7) 7_566 7_566 ?
O8 Nd1 C1 80.14(9) . 7_566 ?
O7 Nd1 C1 154.85(9) . 7_566 ?
O1 Nd1 C1 90.61(8) 1_565 7_566 ?
O5 Nd1 C1 93.28(9) . 7_566 ?
O6 Nd1 C1 96.72(9) 5_576 7_566 ?
O4 Nd1 C1 129.92(8) . 7_566 ?
O3 Nd1 C1 78.00(8) . 7_566 ?
O2 Nd1 C1 24.71(8) 7_566 7_566 ?
O1 Nd1 C1 25.58(8) 7_566 7_566 ?
C4 S1 C5 92.3(2) . . ?
C1 O1 Nd1 152.7(2) . 1_545 ?
C1 O1 Nd1 91.72(19) . 7_566 ?
Nd1 O1 Nd1 114.83(9) 1_545 7_566 ?
C1 O2 Nd1 97.0(2) . 7_566 ?
C6 O3 Nd1 93.1(2) . . ?
C6 O4 Nd1 94.2(2) . . ?
C7 O5 Nd1 120.7(2) . . ?
C7 O6 Nd1 120.1(2) . 5_576 ?
Nd1 O7 H1W 149.6 . . ?
Nd1 O7 H2W 102.4 . . ?
H1W O7 H2W 107.7 . . ?
Nd1 O8 H3W 127.5 . . ?
Nd1 O8 H4W 109.7 . . ?
H3W O8 H4W 107.1 . . ?
O2 C1 O1 121.0(3) . . ?
O2 C1 C2 119.3(3) . . ?
O1 C1 C2 119.7(3) . . ?
O2 C1 Nd1 58.31(17) . 7_566 ?
O1 C1 Nd1 62.69(17) . 7_566 ?
C2 C1 Nd1 176.7(2) . 7_566 ?
C5 C2 C1 125.4(3) . . ?
C5 C2 C3 112.8(3) . . ?
C1 C2 C3 121.8(3) . . ?
C4 C3 C2 106.3(3) . . ?
C4 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
C3 C4 S1 117.0(3) . . ?
C3 C4 H4 121.5 . . ?
S1 C4 H4 121.5 . . ?
C2 C5 C6 127.9(3) . . ?
C2 C5 S1 111.6(3) . . ?
C6 C5 S1 120.5(3) . . ?
O4 C6 O3 120.8(3) . . ?
O4 C6 C5 119.9(3) . . ?
O3 C6 C5 119.3(3) . . ?
O5 C7 O6 126.4(3) . . ?
O5 C7 C7 117.7(4) . 5_576 ?
O6 C7 C7 115.9(4) . 5_576 ?

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
O8 Nd1 O3 C6 -125.3(2) . . . . ?
O7 Nd1 O3 C6 -9.4(2) . . . . ?
O1 Nd1 O3 C6 -85.78(19) 1_565 . . . ?
O5 Nd1 O3 C6 99.1(2) . . . . ?
O6 Nd1 O3 C6 80.07(19) 5_576 . . . ?
O4 Nd1 O3 C6 -1.15(18) . . . . ?
O2 Nd1 O3 C6 155.8(2) 7_566 . . . ?
O1 Nd1 O3 C6 -153.3(2) 7_566 . . . ?
C1 Nd1 O3 C6 -179.5(2) 7_566 . . . ?
O8 Nd1 O4 C6 132.4(2) . . . . ?
O7 Nd1 O4 C6 174.2(2) . . . . ?
O1 Nd1 O4 C6 83.0(2) 1_565 . . . ?
O5 Nd1 O4 C6 -127.0(2) . . . . ?
O6 Nd1 O4 C6 -82.1(2) 5_576 . . . ?
O3 Nd1 O4 C6 1.16(18) . . . . ?
O2 Nd1 O4 C6 -29.1(2) 7_566 . . . ?
O1 Nd1 O4 C6 33.0(2) 7_566 . . . ?
C1 Nd1 O4 C6 3.3(3) 7_566 . . . ?
O8 Nd1 O5 C7 -176.5(3) . . . . ?
O7 Nd1 O5 C7 104.4(3) . . . . ?
O1 Nd1 O5 C7 166.0(2) 1_565 . . . ?
O6 Nd1 O5 C7 -2.2(3) 5_576 . . . ?
O4 Nd1 O5 C7 46.0(3) . . . . ?
O3 Nd1 O5 C7 -22.5(3) . . . . ?
O2 Nd1 O5 C7 -81.7(3) 7_566 . . . ?
O1 Nd1 O5 C7 -115.5(3) 7_566 . . . ?
C1 Nd1 O5 C7 -98.1(3) 7_566 . . . ?
Nd1 O2 C1 O1 0.9(3) 7_566 . . . ?
Nd1 O2 C1 C2 -177.5(2) 7_566 . . . ?
Nd1 O1 C1 O2 166.4(3) 1_545 . . . ?
Nd1 O1 C1 O2 -0.9(3) 7_566 . . . ?
Nd1 O1 C1 C2 -15.3(6) 1_545 . . . ?
Nd1 O1 C1 C2 177.5(3) 7_566 . . . ?
Nd1 O1 C1 Nd1 167.2(5) 1_545 . . 7_566 ?
O2 C1 C2 C5 -94.0(4) . . . . ?
O1 C1 C2 C5 87.5(4) . . . . ?
Nd1 C1 C2 C5 -135(4) 7_566 . . . ?
O2 C1 C2 C3 83.2(4) . . . . ?
O1 C1 C2 C3 -95.2(4) . . . . ?
Nd1 C1 C2 C3 42(4) 7_566 . . . ?
C5 C2 C3 C4 0.7(4) . . . . ?
C1 C2 C3 C4 -176.9(3) . . . . ?
C2 C3 C4 S1 -0.4(4) . . . . ?
C5 S1 C4 C3 0.0(4) . . . . ?
C1 C2 C5 C6 -3.0(6) . . . . ?
C3 C2 C5 C6 179.5(3) . . . . ?
C1 C2 C5 S1 176.8(3) . . . . ?
C3 C2 C5 S1 -0.7(4) . . . . ?
C4 S1 C5 C2 0.4(3) . . . . ?
C4 S1 C5 C6 -179.8(3) . . . . ?
Nd1 O4 C6 O3 -2.1(3) . . . . ?
Nd1 O4 C6 C5 177.3(3) . . . . ?
Nd1 O3 C6 O4 2.1(3) . . . . ?
Nd1 O3 C6 C5 -177.4(3) . . . . ?
C2 C5 C6 O4 -175.9(3) . . . . ?
S1 C5 C6 O4 4.4(5) . . . . ?
C2 C5 C6 O3 3.6(5) . . . . ?
S1 C5 C6 O3 -176.2(3) . . . . ?
Nd1 O5 C7 O6 -177.7(3) . . . . ?
Nd1 O5 C7 C7 1.9(5) . . . 5_576 ?
Nd1 O6 C7 O5 -178.0(3) 5_576 . . . ?
Nd1 O6 C7 C7 2.4(5) 5_576 . . 5_576 ?

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
O9 H5W O4 0.85 1.97 2.759(3) 154.7 2_645
O8 H4W O3 0.85 1.92 2.760(3) 169.6 7_576
O8 H3W O2 0.85 2.38 2.918(4) 121.4 7_576
O8 H3W O6 0.85 2.29 3.074(4) 154.1 5_586
O7 H2W O5 0.85 2.54 3.003(4) 115.7 .
O7 H1W O9 0.85 2.32 2.744(3) 111.3 1_465

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.095
_database_code_depnum_ccdc_archive 'CCDC 1020432'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
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data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 Eu2 O17 S2'
_chemical_formula_weight         822.29

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.746(6)
_cell_length_b                   6.0662(19)
_cell_length_c                   19.785(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.051(3)
_cell_angle_gamma                90.00
_cell_volume                     2211.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6608
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.25

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_absorpt_coefficient_mu    5.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1961
_exptl_absorpt_correction_T_max  0.3572
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7791
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         25.49
_reflns_number_total             2060
_reflns_number_gt                2040
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0185P)²+17.0552P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00030(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2060
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0559
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_restrained_S_all      1.268
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.137186(11) 1.18085(3) 0.470536(11) 0.01590(11) Uani 1 1 d . . .
S1 S 0.10835(9) 0.7707(3) 0.22008(8) 0.0426(3) Uani 1 1 d . . .
O1 O 0.23060(17) 0.3477(5) 0.43438(17) 0.0217(7) Uani 1 1 d . . .
O2 O 0.31758(17) 0.5198(6) 0.41228(18) 0.0270(7) Uani 1 1 d . . .
O3 O 0.19218(16) 0.8621(5) 0.43059(16) 0.0196(6) Uani 1 1 d . . .
O4 O 0.10727(17) 1.0448(6) 0.34526(17) 0.0278(7) Uani 1 1 d . . .
O5 O 0.04670(18) 1.2482(5) 0.52571(19) 0.0274(7) Uani 1 1 d . . .
O6 O -0.05174(17) 1.1261(5) 0.54466(18) 0.0262(7) Uani 1 1 d . . .
O7 O 0.0530(2) 1.4417(6) 0.39153(19) 0.0380(9) Uani 1 1 d . . .
H1W H 0.0387 1.5155 0.3525 0.057 Uiso 1 1 d R . .
H2W H 0.0220 1.4569 0.4115 0.057 Uiso 1 1 d R . .
O8 O 0.16458(17) 1.5220(5) 0.53598(17) 0.0256(7) Uani 1 1 d . . .
H3W H 0.1387 1.6365 0.5277 0.038 Uiso 1 1 d R . .
H4W H 0.2070 1.5623 0.5415 0.038 Uiso 1 1 d R . .
O9 O 1.0000 0.2996(9) 0.2500 0.0392(13) Uani 1 2 d S . .
H5W H 0.9640 0.2152 0.2329 0.059 Uiso 1 1 d R . .
C1 C 0.2522(2) 0.4675(7) 0.3935(2) 0.0172(8) Uani 1 1 d . . .
C2 C 0.1997(2) 0.5439(7) 0.3216(2) 0.0196(9) Uani 1 1 d . . .
C3 C 0.1912(2) 0.4225(7) 0.2524(2) 0.0204(9) Uani 1 1 d . . .
H3 H 0.2144 0.2927 0.2482 0.024 Uiso 1 1 calc R . .
C4 C 0.1422(3) 0.5414(11) 0.1966(3) 0.0463(15) Uani 1 1 d . . .
H4 H 0.1287 0.4968 0.1486 0.056 Uiso 1 1 calc R . .
C5 C 0.1581(3) 0.7322(8) 0.3101(2) 0.0245(10) Uani 1 1 d . . .
C6 C 0.1522(2) 0.8890(7) 0.3643(2) 0.0184(9) Uani 1 1 d . . .
C7 C -0.0010(2) 1.1092(7) 0.5202(2) 0.0196(9) Uani 1 1 d . . .


_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
Eu1 O8 2.398(3) . ?
Eu1 O7 2.418(3) . ?
Eu1 O1 2.426(3) 1_565 ?
Eu1 O5 2.440(3) . ?
Eu1 O6 2.458(3) 5_576 ?
Eu1 O4 2.474(3) . ?
Eu1 O3 2.482(3) . ?
Eu1 O2 2.484(3) 7_566 ?
Eu1 O1 2.618(3) 7_566 ?
Eu1 C1 2.932(4) 7_566 ?
Eu1 C7 3.245(4) . ?
Eu1 Eu1 4.2638(13) 7_576 ?
Eu1 H2W 2.7259 . ?
Eu1 H4W 2.7986 . ?
S1 C4 1.679(7) . ?
S1 C5 1.713(5) . ?
O1 C1 1.270(5) . ?
O1 Eu1 2.426(3) 1_545 ?
O1 Eu1 2.618(3) 7_566 ?
O2 C1 1.249(5) . ?
O2 Eu1 2.484(3) 7_566 ?
O3 C6 1.274(5) . ?
O4 C6 1.258(5) . ?
O5 C7 1.240(5) . ?
O6 C7 1.263(5) . ?
O6 Eu1 2.458(3) 5_576 ?
O7 H1W 0.8474 . ?
O7 H2W 0.8426 . ?
O8 H3W 0.8428 . ?
O8 H4W 0.8411 . ?
O9 H5W 0.8427 . ?
C1 C2 1.501(6) . ?
C1 Eu1 2.932(4) 7_566 ?
C2 C5 1.378(6) . ?
C2 C3 1.509(6) . ?
C3 C4 1.382(8) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.469(6) . ?
C7 C7 1.555(9) 5_576 ?

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
O8 Eu1 O7 75.73(12) . . ?
O8 Eu1 O1 75.60(11) . 1_565 ?
O7 Eu1 O1 87.45(13) . 1_565 ?
O8 Eu1 O5 70.92(11) . . ?
O7 Eu1 O5 74.66(13) . . ?
O1 Eu1 O5 144.94(11) 1_565 . ?
O8 Eu1 O6 137.04(10) . 5_576 ?
O7 Eu1 O6 97.72(13) . 5_576 ?
O1 Eu1 O6 147.27(10) 1_565 5_576 ?
O5 Eu1 O6 66.47(11) . 5_576 ?
O8 Eu1 O4 139.05(11) . . ?
O7 Eu1 O4 73.10(11) . . ?
O1 Eu1 O4 77.11(11) 1_565 . ?
O5 Eu1 O4 123.67(11) . . ?
O6 Eu1 O4 73.64(11) 5_576 . ?
O8 Eu1 O3 143.59(10) . . ?
O7 Eu1 O3 125.60(11) . . ?
O1 Eu1 O3 76.41(10) 1_565 . ?
O5 Eu1 O3 138.38(11) . . ?
O6 Eu1 O3 74.36(10) 5_576 . ?
O4 Eu1 O3 52.80(10) . . ?
O8 Eu1 O2 89.04(11) . 7_566 ?
O7 Eu1 O2 149.05(12) . 7_566 ?
O1 Eu1 O2 115.03(10) 1_565 7_566 ?
O5 Eu1 O2 74.93(12) . 7_566 ?
O6 Eu1 O2 75.15(11) 5_576 7_566 ?
O4 Eu1 O2 130.40(11) . 7_566 ?
O3 Eu1 O2 82.16(11) . 7_566 ?
O8 Eu1 O1 72.29(10) . 7_566 ?
O7 Eu1 O1 141.67(12) . 7_566 ?
O1 Eu1 O1 64.66(12) 1_565 7_566 ?
O5 Eu1 O1 113.02(11) . 7_566 ?
O6 Eu1 O1 120.09(11) 5_576 7_566 ?
O4 Eu1 O1 121.02(10) . 7_566 ?
O3 Eu1 O1 74.92(10) . 7_566 ?
O2 Eu1 O1 50.61(10) 7_566 7_566 ?
O8 Eu1 C1 79.64(11) . 7_566 ?
O7 Eu1 C1 155.06(12) . 7_566 ?
O1 Eu1 C1 90.23(11) 1_565 7_566 ?
O5 Eu1 C1 93.70(12) . 7_566 ?
O6 Eu1 C1 97.58(12) 5_576 7_566 ?
O4 Eu1 C1 130.39(11) . 7_566 ?
O3 Eu1 C1 77.65(11) . 7_566 ?
O2 Eu1 C1 24.94(11) 7_566 7_566 ?
O1 Eu1 C1 25.67(10) 7_566 7_566 ?
O8 Eu1 C7 90.19(11) . . ?
O7 Eu1 C7 79.96(13) . . ?
O1 Eu1 C7 163.02(11) 1_565 . ?
O5 Eu1 C7 19.30(11) . . ?
O6 Eu1 C7 47.19(10) 5_576 . ?
O4 Eu1 C7 109.55(11) . . ?
O3 Eu1 C7 120.26(11) . . ?
O2 Eu1 C7 73.21(11) 7_566 . ?
O1 Eu1 C7 120.23(10) 7_566 . ?
C1 Eu1 C7 96.38(11) 7_566 . ?
O8 Eu1 Eu1 70.83(7) . 7_576 ?
O7 Eu1 Eu1 117.16(10) . 7_576 ?
O1 Eu1 Eu1 33.71(7) 1_565 7_576 ?
O5 Eu1 Eu1 134.90(8) . 7_576 ?
O6 Eu1 Eu1 141.86(8) 5_576 7_576 ?
O4 Eu1 Eu1 100.93(8) . 7_576 ?
O3 Eu1 Eu1 72.94(7) . 7_576 ?
O2 Eu1 Eu1 81.44(7) 7_566 7_576 ?
O1 Eu1 Eu1 30.95(7) 7_566 7_576 ?
C1 Eu1 Eu1 56.55(8) 7_566 7_576 ?
C7 Eu1 Eu1 148.58(8) . 7_576 ?
O8 Eu1 H2W 72.1 . . ?
O7 Eu1 H2W 17.6 . . ?
O1 Eu1 H2W 102.9 1_565 . ?
O5 Eu1 H2W 57.1 . . ?
O6 Eu1 H2W 89.0 5_576 . ?
O4 Eu1 H2W 85.0 . . ?
O3 Eu1 H2W 137.3 . . ?
O2 Eu1 H2W 131.8 7_566 . ?
O1 Eu1 H2W 144.2 7_566 . ?
C1 Eu1 H2W 144.5 7_566 . ?
C7 Eu1 H2W 63.2 . . ?
Eu1 Eu1 H2W 128.7 7_576 . ?
O8 Eu1 H4W 16.4 . . ?
O7 Eu1 H4W 83.3 . . ?
O1 Eu1 H4W 60.9 1_565 . ?
O5 Eu1 H4W 86.9 . . ?
O6 Eu1 H4W 151.7 5_576 . ?
O4 Eu1 H4W 132.5 . . ?
O3 Eu1 H4W 127.6 . . ?
O2 Eu1 H4W 89.4 7_566 . ?
O1 Eu1 H4W 60.7 7_566 . ?
C1 Eu1 H4W 73.9 7_566 . ?
C7 Eu1 H4W 106.0 . . ?
Eu1 Eu1 H4W 54.7 7_576 . ?
H2W Eu1 H4W 83.8 . . ?
C4 S1 C5 92.2(3) . . ?
C1 O1 Eu1 153.1(3) . 1_545 ?
C1 O1 Eu1 91.1(2) . 7_566 ?
Eu1 O1 Eu1 115.34(12) 1_545 7_566 ?
C1 O2 Eu1 98.0(3) . 7_566 ?
C6 O3 Eu1 92.7(2) . . ?
C6 O4 Eu1 93.5(3) . . ?
C7 O5 Eu1 120.2(3) . . ?
C7 O6 Eu1 119.7(3) . 5_576 ?
Eu1 O7 H1W 149.4 . . ?
Eu1 O7 H2W 102.4 . . ?
H1W O7 H2W 108.0 . . ?
Eu1 O8 H3W 127.1 . . ?
Eu1 O8 H4W 109.9 . . ?
H3W O8 H4W 107.0 . . ?
O2 C1 O1 120.3(4) . . ?
O2 C1 C2 119.5(4) . . ?
O1 C1 C2 120.3(4) . . ?
O2 C1 Eu1 57.0(2) . 7_566 ?
O1 C1 Eu1 63.3(2) . 7_566 ?
C2 C1 Eu1 176.0(3) . 7_566 ?
C5 C2 C1 125.5(4) . . ?
C5 C2 C3 112.9(4) . . ?
C1 C2 C3 121.5(4) . . ?
C4 C3 C2 106.8(4) . . ?
C4 C3 H3 126.6 . . ?
C2 C3 H3 126.6 . . ?
C3 C4 S1 116.4(4) . . ?
C3 C4 H4 121.8 . . ?
S1 C4 H4 121.8 . . ?
C2 C5 C6 127.9(4) . . ?
C2 C5 S1 111.7(3) . . ?
C6 C5 S1 120.3(3) . . ?
O4 C6 O3 120.9(4) . . ?
O4 C6 C5 120.0(4) . . ?
O3 C6 C5 119.1(4) . . ?
O5 C7 O6 126.4(4) . . ?
O5 C7 C7 117.7(5) . 5_576 ?
O6 C7 C7 115.9(5) . 5_576 ?
O5 C7 Eu1 40.5(2) . . ?
O6 C7 Eu1 166.9(3) . . ?
C7 C7 Eu1 77.2(3) 5_576 . ?

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
O8 Eu1 O3 C6 -125.4(3) . . . . ?
O7 Eu1 O3 C6 -8.0(3) . . . . ?
O1 Eu1 O3 C6 -84.7(2) 1_565 . . . ?
O5 Eu1 O3 C6 100.4(3) . . . . ?
O6 Eu1 O3 C6 80.4(2) 5_576 . . . ?
O4 Eu1 O3 C6 -0.7(2) . . . . ?
O2 Eu1 O3 C6 157.1(3) 7_566 . . . ?
O1 Eu1 O3 C6 -151.7(3) 7_566 . . . ?
C1 Eu1 O3 C6 -178.0(3) 7_566 . . . ?
C7 Eu1 O3 C6 91.8(3) . . . . ?
Eu1 Eu1 O3 C6 -119.5(2) 7_576 . . . ?
O8 Eu1 O4 C6 132.6(3) . . . . ?
O7 Eu1 O4 C6 174.6(3) . . . . ?
O1 Eu1 O4 C6 83.3(3) 1_565 . . . ?
O5 Eu1 O4 C6 -127.7(3) . . . . ?
O6 Eu1 O4 C6 -81.8(3) 5_576 . . . ?
O3 Eu1 O4 C6 0.7(2) . . . . ?
O2 Eu1 O4 C6 -28.7(3) 7_566 . . . ?
O1 Eu1 O4 C6 33.9(3) 7_566 . . . ?
C1 Eu1 O4 C6 4.2(3) 7_566 . . . ?
C7 Eu1 O4 C6 -113.0(3) . . . . ?
Eu1 Eu1 O4 C6 59.3(3) 7_576 . . . ?
O8 Eu1 O5 C7 -176.4(4) . . . . ?
O7 Eu1 O5 C7 103.7(4) . . . . ?
O1 Eu1 O5 C7 165.5(3) 1_565 . . . ?
O6 Eu1 O5 C7 -2.1(3) 5_576 . . . ?
O4 Eu1 O5 C7 46.7(4) . . . . ?
O3 Eu1 O5 C7 -23.2(4) . . . . ?
O2 Eu1 O5 C7 -82.2(3) 7_566 . . . ?
O1 Eu1 O5 C7 -116.2(3) 7_566 . . . ?
C1 Eu1 O5 C7 -98.7(4) 7_566 . . . ?
Eu1 Eu1 O5 C7 -143.1(3) 7_576 . . . ?
Eu1 O2 C1 O1 1.2(4) 7_566 . . . ?
Eu1 O2 C1 C2 -177.7(3) 7_566 . . . ?
Eu1 O1 C1 O2 168.2(4) 1_545 . . . ?
Eu1 O1 C1 O2 -1.1(4) 7_566 . . . ?
Eu1 O1 C1 C2 -12.9(9) 1_545 . . . ?
Eu1 O1 C1 C2 177.8(3) 7_566 . . . ?
Eu1 O1 C1 Eu1 169.3(6) 1_545 . . 7_566 ?
O2 C1 C2 C5 -93.6(6) . . . . ?
O1 C1 C2 C5 87.6(6) . . . . ?
Eu1 C1 C2 C5 -122(4) 7_566 . . . ?
O2 C1 C2 C3 82.6(5) . . . . ?
O1 C1 C2 C3 -96.3(5) . . . . ?
Eu1 C1 C2 C3 54(4) 7_566 . . . ?
C5 C2 C3 C4 -0.2(6) . . . . ?
C1 C2 C3 C4 -176.8(4) . . . . ?
C2 C3 C4 S1 -0.2(6) . . . . ?
C5 S1 C4 C3 0.4(5) . . . . ?
C1 C2 C5 C6 -4.2(8) . . . . ?
C3 C2 C5 C6 179.4(4) . . . . ?
C1 C2 C5 S1 176.9(3) . . . . ?
C3 C2 C5 S1 0.5(5) . . . . ?
C4 S1 C5 C2 -0.5(4) . . . . ?
C4 S1 C5 C6 -179.5(4) . . . . ?
Eu1 O4 C6 O3 -1.3(4) . . . . ?
Eu1 O4 C6 C5 177.5(4) . . . . ?
Eu1 O3 C6 O4 1.3(4) . . . . ?
Eu1 O3 C6 C5 -177.5(4) . . . . ?
C2 C5 C6 O4 -174.6(5) . . . . ?
S1 C5 C6 O4 4.3(6) . . . . ?
C2 C5 C6 O3 4.3(7) . . . . ?
S1 C5 C6 O3 -176.9(3) . . . . ?
Eu1 O5 C7 O6 -178.2(3) . . . . ?
Eu1 O5 C7 C7 2.1(7) . . . 5_576 ?
Eu1 O6 C7 O5 -178.0(4) 5_576 . . . ?
Eu1 O6 C7 C7 1.6(6) 5_576 . . 5_576 ?
Eu1 O6 C7 Eu1 176.9(12) 5_576 . . . ?
O8 Eu1 C7 O5 3.4(4) . . . . ?
O7 Eu1 C7 O5 -72.1(4) . . . . ?
O1 Eu1 C7 O5 -29.4(6) 1_565 . . . ?
O6 Eu1 C7 O5 177.4(4) 5_576 . . . ?
O4 Eu1 C7 O5 -140.0(3) . . . . ?
O3 Eu1 C7 O5 162.4(3) . . . . ?
O2 Eu1 C7 O5 92.3(4) 7_566 . . . ?
O1 Eu1 C7 O5 72.9(4) 7_566 . . . ?
C1 Eu1 C7 O5 83.0(4) 7_566 . . . ?
Eu1 Eu1 C7 O5 54.7(4) 7_576 . . . ?
O8 Eu1 C7 O6 9.6(14) . . . . ?
O7 Eu1 C7 O6 -65.9(14) . . . . ?
O1 Eu1 C7 O6 -23.2(16) 1_565 . . . ?
O5 Eu1 C7 O6 6.2(12) . . . . ?
O6 Eu1 C7 O6 -176.4(14) 5_576 . . . ?
O4 Eu1 C7 O6 -133.8(14) . . . . ?
O3 Eu1 C7 O6 168.6(13) . . . . ?
O2 Eu1 C7 O6 98.5(14) 7_566 . . . ?
O1 Eu1 C7 O6 79.1(14) 7_566 . . . ?
C1 Eu1 C7 O6 89.2(14) 7_566 . . . ?
Eu1 Eu1 C7 O6 60.9(14) 7_576 . . . ?
O8 Eu1 C7 C7 -174.7(3) . . . 5_576 ?
O7 Eu1 C7 C7 109.8(3) . . . 5_576 ?
O1 Eu1 C7 C7 152.5(3) 1_565 . . 5_576 ?
O5 Eu1 C7 C7 -178.1(6) . . . 5_576 ?
O6 Eu1 C7 C7 -0.7(3) 5_576 . . 5_576 ?
O4 Eu1 C7 C7 41.9(3) . . . 5_576 ?
O3 Eu1 C7 C7 -15.7(4) . . . 5_576 ?
O2 Eu1 C7 C7 -85.8(3) 7_566 . . 5_576 ?
O1 Eu1 C7 C7 -105.2(3) 7_566 . . 5_576 ?
C1 Eu1 C7 C7 -95.1(3) 7_566 . . 5_576 ?
Eu1 Eu1 C7 C7 -123.4(3) 7_576 . . 5_576 ?

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
O9 H5W O4 0.84 1.97 2.750(4) 153.6 2_645
O8 H4W O3 0.84 1.92 2.754(4) 170.9 7_576
O8 H3W O2 0.84 2.40 2.939(5) 122.3 7_576
O8 H3W O6 0.84 2.30 3.084(5) 154.3 5_586
O7 H2W O5 0.84 2.48 2.946(5) 115.6 .
O7 H1W O9 0.85 2.30 2.752(4) 113.5 1_465

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.109
_database_code_depnum_ccdc_archive 'CCDC 1020433'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 Gd2 O17 S2'
_chemical_formula_weight         832.87

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.671(4)
_cell_length_b                   6.0556(13)
_cell_length_c                   19.793(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.098(2)
_cell_angle_gamma                90.00
_cell_volume                     2199.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6792
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.16

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    6.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1837
_exptl_absorpt_correction_T_max  0.3400
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7618
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         25.49
_reflns_number_total             2042
_reflns_number_gt                2017
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0251P)²+14.9214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00126(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2042
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0528
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.137133(9) 1.18107(3) 0.470411(9) 0.01390(10) Uani 1 1 d . . .
S1 S 0.10845(7) 0.7709(2) 0.22011(6) 0.0372(3) Uani 1 1 d . . .
O1 O 0.23088(15) 0.3459(4) 0.43468(15) 0.0199(6) Uani 1 1 d . . .
O2 O 0.31831(15) 0.5196(5) 0.41264(15) 0.0241(6) Uani 1 1 d . . .
O3 O 0.19227(14) 0.8622(4) 0.43086(14) 0.0180(6) Uani 1 1 d . . .
O4 O 0.10717(16) 1.0455(5) 0.34558(15) 0.0252(6) Uani 1 1 d . . .
O5 O 0.04674(16) 1.2493(5) 0.52537(17) 0.0253(6) Uani 1 1 d . . .
O6 O -0.05205(15) 1.1262(5) 0.54471(16) 0.0234(6) Uani 1 1 d . . .
O7 O 0.05317(18) 1.4399(6) 0.39174(16) 0.0363(8) Uani 1 1 d . . .
H1W H 0.0389 1.5137 0.3528 0.054 Uiso 1 1 d R . .
H2W H 0.0222 1.4551 0.4117 0.054 Uiso 1 1 d R . .
O8 O 0.16466(15) 1.5215(4) 0.53578(15) 0.0220(6) Uani 1 1 d . . .
H3W H 0.1388 1.6360 0.5275 0.033 Uiso 1 1 d R . .
H4W H 0.2071 1.5617 0.5413 0.033 Uiso 1 1 d R . .
O9 O 1.0000 0.3019(8) 0.2500 0.0359(11) Uani 1 2 d S . .
H5W H 0.9640 0.2175 0.2329 0.054 Uiso 1 1 d R . .
C1 C 0.2527(2) 0.4676(6) 0.3938(2) 0.0161(7) Uani 1 1 d . . .
C2 C 0.2003(2) 0.5434(6) 0.3217(2) 0.0174(8) Uani 1 1 d . . .
C3 C 0.19157(19) 0.4209(6) 0.25212(18) 0.0139(7) Uani 1 1 d . . .
H3 H 0.2148 0.2910 0.2477 0.017 Uiso 1 1 calc R . .
C4 C 0.1419(3) 0.5419(9) 0.1965(3) 0.0402(12) Uani 1 1 d . . .
H4 H 0.1280 0.4977 0.1484 0.048 Uiso 1 1 calc R . .
C5 C 0.1579(2) 0.7316(7) 0.3103(2) 0.0203(8) Uani 1 1 d . . .
C6 C 0.1519(2) 0.8884(6) 0.3646(2) 0.0166(8) Uani 1 1 d . . .
C7 C -0.0012(2) 1.1090(6) 0.5202(2) 0.0173(8) Uani 1 1 d . . .


_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
Gd1 O8 2.390(3) . ?
Gd1 O1 2.416(3) 1_565 ?
Gd1 O7 2.400(3) . ?
Gd1 O5 2.431(3) . ?
Gd1 O6 2.448(3) 5_576 ?
Gd1 O4 2.465(3) . ?
Gd1 O3 2.476(3) . ?
Gd1 O2 2.478(3) 7_566 ?
Gd1 O1 2.605(3) 7_566 ?
Gd1 C1 2.921(4) 7_566 ?
S1 C4 1.672(6) . ?
S1 C5 1.715(4) . ?
O1 C1 1.277(5) . ?
O1 Gd1 2.416(3) 1_545 ?
O1 Gd1 2.605(3) 7_566 ?
O2 C1 1.247(5) . ?
O2 Gd1 2.478(3) 7_566 ?
O3 C6 1.275(5) . ?
O4 C6 1.258(5) . ?
O5 C7 1.246(5) . ?
O6 C7 1.263(5) . ?
O6 Gd1 2.448(3) 5_576 ?
O7 H1W 0.8470 . ?
O7 H2W 0.8408 . ?
O8 H3W 0.8407 . ?
O8 H4W 0.8379 . ?
O9 H5W 0.8401 . ?
C1 C2 1.501(5) . ?
C1 Gd1 2.921(4) 7_566 ?
C2 C5 1.383(6) . ?
C2 C3 1.518(5) . ?
C3 C4 1.389(6) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.470(5) . ?
C7 C7 1.553(8) 5_576 ?

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
O8 Gd1 O1 75.76(9) . 1_565 ?
O8 Gd1 O7 75.92(11) . . ?
O1 Gd1 O7 87.69(11) 1_565 . ?
O8 Gd1 O5 70.78(9) . . ?
O1 Gd1 O5 145.01(9) 1_565 . ?
O7 Gd1 O5 74.68(11) . . ?
O8 Gd1 O6 137.18(9) . 5_576 ?
O1 Gd1 O6 147.00(9) 1_565 5_576 ?
O7 Gd1 O6 97.85(12) . 5_576 ?
O5 Gd1 O6 66.78(9) . 5_576 ?
O8 Gd1 O4 139.08(10) . . ?
O1 Gd1 O4 77.08(10) 1_565 . ?
O7 Gd1 O4 72.95(10) . . ?
O5 Gd1 O4 123.75(10) . . ?
O6 Gd1 O4 73.63(10) 5_576 . ?
O8 Gd1 O3 143.54(9) . . ?
O1 Gd1 O3 76.24(9) 1_565 . ?
O7 Gd1 O3 125.58(10) . . ?
O5 Gd1 O3 138.45(10) . . ?
O6 Gd1 O3 74.14(9) 5_576 . ?
O4 Gd1 O3 52.93(9) . . ?
O8 Gd1 O2 88.98(10) . 7_566 ?
O1 Gd1 O2 115.18(9) 1_565 7_566 ?
O7 Gd1 O2 148.84(10) . 7_566 ?
O5 Gd1 O2 74.64(10) . 7_566 ?
O6 Gd1 O2 74.81(10) 5_576 7_566 ?
O4 Gd1 O2 130.50(10) . 7_566 ?
O3 Gd1 O2 82.25(9) . 7_566 ?
O8 Gd1 O1 72.00(9) . 7_566 ?
O1 Gd1 O1 64.49(11) 1_565 7_566 ?
O7 Gd1 O1 141.58(11) . 7_566 ?
O5 Gd1 O1 112.81(10) . 7_566 ?
O6 Gd1 O1 120.05(9) 5_576 7_566 ?
O4 Gd1 O1 121.23(9) . 7_566 ?
O3 Gd1 O1 75.09(9) . 7_566 ?
O2 Gd1 O1 50.96(9) 7_566 7_566 ?
O8 Gd1 C1 79.59(10) . 7_566 ?
O1 Gd1 C1 90.29(10) 1_565 7_566 ?
O7 Gd1 C1 155.17(11) . 7_566 ?
O5 Gd1 C1 93.47(11) . 7_566 ?
O6 Gd1 C1 97.26(10) 5_576 7_566 ?
O4 Gd1 C1 130.53(10) . 7_566 ?
O3 Gd1 C1 77.66(9) . 7_566 ?
O2 Gd1 C1 25.03(10) 7_566 7_566 ?
O1 Gd1 C1 25.93(9) 7_566 7_566 ?
C4 S1 C5 92.5(2) . . ?
C1 O1 Gd1 152.9(3) . 1_545 ?
C1 O1 Gd1 91.0(2) . 7_566 ?
Gd1 O1 Gd1 115.51(11) 1_545 7_566 ?
C1 O2 Gd1 97.8(2) . 7_566 ?
C6 O3 Gd1 92.7(2) . . ?
C6 O4 Gd1 93.6(2) . . ?
C7 O5 Gd1 120.1(2) . . ?
C7 O6 Gd1 119.4(2) . 5_576 ?
Gd1 O7 H1W 149.3 . . ?
Gd1 O7 H2W 102.3 . . ?
H1W O7 H2W 108.1 . . ?
Gd1 O8 H3W 127.0 . . ?
Gd1 O8 H4W 110.0 . . ?
H3W O8 H4W 106.9 . . ?
O2 C1 O1 120.3(3) . . ?
O2 C1 C2 119.3(3) . . ?
O1 C1 C2 120.4(3) . . ?
O2 C1 Gd1 57.21(19) . 7_566 ?
O1 C1 Gd1 63.1(2) . 7_566 ?
C2 C1 Gd1 175.9(3) . 7_566 ?
C5 C2 C1 125.1(3) . . ?
C5 C2 C3 113.0(3) . . ?
C1 C2 C3 121.9(3) . . ?
C4 C3 C2 106.2(3) . . ?
C4 C3 H3 126.9 . . ?
C2 C3 H3 126.9 . . ?
C3 C4 S1 116.8(3) . . ?
C3 C4 H4 121.6 . . ?
S1 C4 H4 121.6 . . ?
C2 C5 C6 128.0(4) . . ?
C2 C5 S1 111.5(3) . . ?
C6 C5 S1 120.5(3) . . ?
O4 C6 O3 120.8(3) . . ?
O4 C6 C5 120.1(3) . . ?
O3 C6 C5 119.2(3) . . ?
O5 C7 O6 126.4(4) . . ?
O5 C7 C7 117.3(4) . 5_576 ?
O6 C7 C7 116.3(4) . 5_576 ?

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
O8 Gd1 O3 C6 -125.9(2) . . . . ?
O1 Gd1 O3 C6 -85.1(2) 1_565 . . . ?
O7 Gd1 O3 C6 -8.2(3) . . . . ?
O5 Gd1 O3 C6 100.3(2) . . . . ?
O6 Gd1 O3 C6 80.2(2) 5_576 . . . ?
O4 Gd1 O3 C6 -1.1(2) . . . . ?
O2 Gd1 O3 C6 156.5(2) 7_566 . . . ?
O1 Gd1 O3 C6 -151.9(2) 7_566 . . . ?
C1 Gd1 O3 C6 -178.5(2) 7_566 . . . ?
O8 Gd1 O4 C6 132.9(2) . . . . ?
O1 Gd1 O4 C6 83.5(2) 1_565 . . . ?
O7 Gd1 O4 C6 175.0(3) . . . . ?
O5 Gd1 O4 C6 -127.5(2) . . . . ?
O6 Gd1 O4 C6 -81.2(2) 5_576 . . . ?
O3 Gd1 O4 C6 1.1(2) . . . . ?
O2 Gd1 O4 C6 -28.8(3) 7_566 . . . ?
O1 Gd1 O4 C6 34.4(3) 7_566 . . . ?
C1 Gd1 O4 C6 4.4(3) 7_566 . . . ?
O8 Gd1 O5 C7 -176.0(3) . . . . ?
O1 Gd1 O5 C7 166.3(3) 1_565 . . . ?
O7 Gd1 O5 C7 103.9(3) . . . . ?
O6 Gd1 O5 C7 -1.8(3) 5_576 . . . ?
O4 Gd1 O5 C7 47.2(3) . . . . ?
O3 Gd1 O5 C7 -23.0(4) . . . . ?
O2 Gd1 O5 C7 -81.6(3) 7_566 . . . ?
O1 Gd1 O5 C7 -116.1(3) 7_566 . . . ?
C1 Gd1 O5 C7 -98.3(3) 7_566 . . . ?
Gd1 O2 C1 O1 0.6(4) 7_566 . . . ?
Gd1 O2 C1 C2 -177.4(3) 7_566 . . . ?
Gd1 O1 C1 O2 167.5(4) 1_545 . . . ?
Gd1 O1 C1 O2 -0.6(4) 7_566 . . . ?
Gd1 O1 C1 C2 -14.5(8) 1_545 . . . ?
Gd1 O1 C1 C2 177.4(3) 7_566 . . . ?
Gd1 O1 C1 Gd1 168.1(6) 1_545 . . 7_566 ?
O2 C1 C2 C5 -94.7(5) . . . . ?
O1 C1 C2 C5 87.3(5) . . . . ?
Gd1 C1 C2 C5 -126(3) 7_566 . . . ?
O2 C1 C2 C3 82.4(5) . . . . ?
O1 C1 C2 C3 -95.6(4) . . . . ?
Gd1 C1 C2 C3 51(4) 7_566 . . . ?
C5 C2 C3 C4 0.3(5) . . . . ?
C1 C2 C3 C4 -177.1(4) . . . . ?
C2 C3 C4 S1 0.0(5) . . . . ?
C5 S1 C4 C3 -0.3(4) . . . . ?
C1 C2 C5 C6 -3.2(7) . . . . ?
C3 C2 C5 C6 179.4(4) . . . . ?
C1 C2 C5 S1 176.8(3) . . . . ?
C3 C2 C5 S1 -0.6(4) . . . . ?
C4 S1 C5 C2 0.5(4) . . . . ?
C4 S1 C5 C6 -179.5(4) . . . . ?
Gd1 O4 C6 O3 -1.9(4) . . . . ?
Gd1 O4 C6 C5 177.8(3) . . . . ?
Gd1 O3 C6 O4 1.9(4) . . . . ?
Gd1 O3 C6 C5 -177.8(3) . . . . ?
C2 C5 C6 O4 -175.8(4) . . . . ?
S1 C5 C6 O4 4.2(5) . . . . ?
C2 C5 C6 O3 4.0(6) . . . . ?
S1 C5 C6 O3 -176.1(3) . . . . ?
Gd1 O5 C7 O6 -178.3(3) . . . . ?
Gd1 O5 C7 C7 1.8(6) . . . 5_576 ?
Gd1 O6 C7 O5 -178.3(3) 5_576 . . . ?
Gd1 O6 C7 C7 1.7(5) 5_576 . . 5_576 ?

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
O9 H5W O4 0.84 1.97 2.750(4) 153.4 2_645
O8 H4W O3 0.84 1.91 2.741(4) 170.9 7_576
O8 H3W O2 0.84 2.40 2.938(4) 122.7 7_576
O8 H3W O6 0.84 2.30 3.075(4) 154.3 5_586
O7 H2W O5 0.84 2.46 2.930(5) 115.9 .
O7 H1W O9 0.85 2.29 2.748(3) 114.1 1_465

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.112
_database_code_depnum_ccdc_archive 'CCDC 1020434'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 O17 S2 Tb2'
_chemical_formula_weight         836.21

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.621(3)
_cell_length_b                   6.0421(9)
_cell_length_c                   19.795(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.0900(10)
_cell_angle_gamma                90.00
_cell_volume                     2189.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8253
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.17

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    6.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1703
_exptl_absorpt_correction_T_max  0.3210
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7571
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         25.49
_reflns_number_total             2033
_reflns_number_gt                2028
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0193P)²+26.2459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00113(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2033
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0580
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.155
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.136880(11) 1.18107(3) 0.470511(11) 0.01407(11) Uani 1 1 d . . .
S1 S 0.10837(9) 0.7736(3) 0.22043(8) 0.0386(4) Uani 1 1 d . . .
O1 O 0.22997(18) 0.3461(5) 0.43480(18) 0.0203(7) Uani 1 1 d . . .
O2 O 0.31828(18) 0.5176(6) 0.41358(18) 0.0244(7) Uani 1 1 d . . .
O3 O 0.19170(17) 0.8636(5) 0.43136(17) 0.0175(7) Uani 1 1 d . . .
O4 O 0.10649(19) 1.0477(6) 0.34599(18) 0.0257(8) Uani 1 1 d . . .
O5 O 0.04693(19) 1.2495(6) 0.5255(2) 0.0248(8) Uani 1 1 d . . .
O6 O -0.05185(18) 1.1258(6) 0.54490(19) 0.0236(7) Uani 1 1 d . . .
O7 O 0.0531(2) 1.4394(7) 0.3924(2) 0.0358(9) Uani 1 1 d . . .
H1W H 0.0388 1.5131 0.3534 0.054 Uiso 1 1 d R . .
H2W H 0.0221 1.4546 0.4123 0.054 Uiso 1 1 d R . .
O8 O 0.16458(18) 1.5189(5) 0.53593(18) 0.0223(7) Uani 1 1 d . . .
H3W H 0.1387 1.6334 0.5276 0.034 Uiso 1 1 d R . .
H4W H 0.2070 1.5591 0.5414 0.034 Uiso 1 1 d R . .
O9 O 1.0000 0.3049(9) 0.2500 0.0358(13) Uani 1 2 d S . .
H5W H 0.9640 0.2205 0.2329 0.054 Uiso 1 1 d R . .
C1 C 0.2523(2) 0.4672(7) 0.3943(2) 0.0162(9) Uani 1 1 d . . .
C2 C 0.1999(2) 0.5445(8) 0.3220(2) 0.0167(9) Uani 1 1 d . . .
C3 C 0.1915(2) 0.4228(7) 0.2523(2) 0.0144(9) Uani 1 1 d . . .
H3 H 0.2148 0.2928 0.2477 0.017 Uiso 1 1 calc R . .
C4 C 0.1420(4) 0.5445(12) 0.1969(3) 0.0416(15) Uani 1 1 d . . .
H4 H 0.1281 0.5006 0.1488 0.050 Uiso 1 1 calc R . .
C5 C 0.1579(3) 0.7337(8) 0.3107(3) 0.0212(10) Uani 1 1 d . . .
C6 C 0.1516(2) 0.8905(8) 0.3650(2) 0.0167(9) Uani 1 1 d . . .
C7 C -0.0010(2) 1.1089(8) 0.5204(2) 0.0169(9) Uani 1 1 d . . .


_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
Tb1 O8 2.373(3) . ?
Tb1 O7 2.388(4) . ?
Tb1 O1 2.400(3) 1_565 ?
Tb1 O5 2.419(3) . ?
Tb1 O6 2.439(3) 5_576 ?
Tb1 O4 2.454(3) . ?
Tb1 O2 2.455(3) 7_566 ?
Tb1 O3 2.457(3) . ?
Tb1 O1 2.616(3) 7_566 ?
Tb1 C1 2.916(4) 7_566 ?
S1 C4 1.670(7) . ?
S1 C5 1.716(5) . ?
O1 C1 1.274(5) . ?
O1 Tb1 2.400(3) 1_545 ?
O1 Tb1 2.616(3) 7_566 ?
O2 C1 1.248(6) . ?
O2 Tb1 2.455(3) 7_566 ?
O3 C6 1.275(5) . ?
O4 C6 1.260(6) . ?
O5 C7 1.244(6) . ?
O6 C7 1.261(5) . ?
O6 Tb1 2.439(3) 5_576 ?
O7 H1W 0.8466 . ?
O7 H2W 0.8394 . ?
O8 H3W 0.8387 . ?
O8 H4W 0.8357 . ?
O9 H5W 0.8382 . ?
C1 C2 1.505(6) . ?
C1 Tb1 2.916(4) 7_566 ?
C2 C5 1.380(7) . ?
C2 C3 1.520(6) . ?
C3 C4 1.386(8) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.472(7) . ?
C7 C7 1.552(9) 5_576 ?

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
O8 Tb1 O7 76.13(13) . . ?
O8 Tb1 O1 75.77(11) . 1_565 ?
O7 Tb1 O1 87.57(13) . 1_565 ?
O8 Tb1 O5 70.64(11) . . ?
O7 Tb1 O5 74.67(14) . . ?
O1 Tb1 O5 144.82(11) 1_565 . ?
O8 Tb1 O6 137.24(11) . 5_576 ?
O7 Tb1 O6 97.77(14) . 5_576 ?
O1 Tb1 O6 146.92(11) 1_565 5_576 ?
O5 Tb1 O6 67.00(11) . 5_576 ?
O8 Tb1 O4 139.08(12) . . ?
O7 Tb1 O4 72.70(12) . . ?
O1 Tb1 O4 77.07(12) 1_565 . ?
O5 Tb1 O4 123.71(12) . . ?
O6 Tb1 O4 73.54(12) 5_576 . ?
O8 Tb1 O2 88.62(12) . 7_566 ?
O7 Tb1 O2 148.93(13) . 7_566 ?
O1 Tb1 O2 115.06(11) 1_565 7_566 ?
O5 Tb1 O2 74.77(12) . 7_566 ?
O6 Tb1 O2 75.17(12) 5_576 7_566 ?
O4 Tb1 O2 130.84(12) . 7_566 ?
O8 Tb1 O3 143.45(11) . . ?
O7 Tb1 O3 125.72(12) . . ?
O1 Tb1 O3 76.44(11) 1_565 . ?
O5 Tb1 O3 138.44(11) . . ?
O6 Tb1 O3 74.00(11) 5_576 . ?
O4 Tb1 O3 53.31(11) . . ?
O2 Tb1 O3 82.10(11) 7_566 . ?
O8 Tb1 O1 71.90(11) . 7_566 ?
O7 Tb1 O1 141.50(13) . 7_566 ?
O1 Tb1 O1 64.36(13) 1_565 7_566 ?
O5 Tb1 O1 112.99(11) . 7_566 ?
O6 Tb1 O1 120.25(11) 5_576 7_566 ?
O4 Tb1 O1 121.21(11) . 7_566 ?
O2 Tb1 O1 50.94(10) 7_566 7_566 ?
O3 Tb1 O1 74.89(10) . 7_566 ?
O8 Tb1 C1 79.32(12) . 7_566 ?
O7 Tb1 C1 155.14(13) . 7_566 ?
O1 Tb1 C1 90.16(12) 1_565 7_566 ?
O5 Tb1 C1 93.63(13) . 7_566 ?
O6 Tb1 C1 97.57(13) 5_576 7_566 ?
O4 Tb1 C1 130.71(12) . 7_566 ?
O2 Tb1 C1 25.03(12) 7_566 7_566 ?
O3 Tb1 C1 77.48(11) . 7_566 ?
O1 Tb1 C1 25.91(11) 7_566 7_566 ?
C4 S1 C5 92.4(3) . . ?
C1 O1 Tb1 153.5(3) . 1_545 ?
C1 O1 Tb1 90.3(3) . 7_566 ?
Tb1 O1 Tb1 115.64(13) 1_545 7_566 ?
C1 O2 Tb1 98.6(3) . 7_566 ?
C6 O3 Tb1 92.7(3) . . ?
C6 O4 Tb1 93.2(3) . . ?
C7 O5 Tb1 120.0(3) . . ?
C7 O6 Tb1 119.4(3) . 5_576 ?
Tb1 O7 H1W 149.2 . . ?
Tb1 O7 H2W 102.3 . . ?
H1W O7 H2W 108.3 . . ?
Tb1 O8 H3W 126.8 . . ?
Tb1 O8 H4W 110.1 . . ?
H3W O8 H4W 106.9 . . ?
O2 C1 O1 120.1(4) . . ?
O2 C1 C2 119.5(4) . . ?
O1 C1 C2 120.3(4) . . ?
O2 C1 Tb1 56.4(2) . 7_566 ?
O1 C1 Tb1 63.8(2) . 7_566 ?
C2 C1 Tb1 175.4(3) . 7_566 ?
C5 C2 C1 125.2(4) . . ?
C5 C2 C3 112.9(4) . . ?
C1 C2 C3 121.8(4) . . ?
C4 C3 C2 106.2(4) . . ?
C4 C3 H3 126.9 . . ?
C2 C3 H3 126.9 . . ?
C3 C4 S1 117.0(4) . . ?
C3 C4 H4 121.5 . . ?
S1 C4 H4 121.5 . . ?
C2 C5 C6 128.1(4) . . ?
C2 C5 S1 111.5(4) . . ?
C6 C5 S1 120.3(4) . . ?
O4 C6 O3 120.7(4) . . ?
O4 C6 C5 120.1(4) . . ?
O3 C6 C5 119.1(4) . . ?
O5 C7 O6 126.4(4) . . ?
O5 C7 C7 117.5(5) . 5_576 ?
O6 C7 C7 116.2(5) . 5_576 ?

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
O8 Tb1 O3 C6 -126.0(3) . . . . ?
O7 Tb1 O3 C6 -7.7(3) . . . . ?
O1 Tb1 O3 C6 -84.5(3) 1_565 . . . ?
O5 Tb1 O3 C6 101.0(3) . . . . ?
O6 Tb1 O3 C6 80.4(3) 5_576 . . . ?
O4 Tb1 O3 C6 -0.7(2) . . . . ?
O2 Tb1 O3 C6 157.2(3) 7_566 . . . ?
O1 Tb1 O3 C6 -151.2(3) 7_566 . . . ?
C1 Tb1 O3 C6 -177.8(3) 7_566 . . . ?
O8 Tb1 O4 C6 132.8(3) . . . . ?
O7 Tb1 O4 C6 174.8(3) . . . . ?
O1 Tb1 O4 C6 83.3(3) 1_565 . . . ?
O5 Tb1 O4 C6 -127.9(3) . . . . ?
O6 Tb1 O4 C6 -81.3(3) 5_576 . . . ?
O2 Tb1 O4 C6 -28.8(3) 7_566 . . . ?
O3 Tb1 O4 C6 0.7(2) . . . . ?
O1 Tb1 O4 C6 34.5(3) 7_566 . . . ?
C1 Tb1 O4 C6 4.5(3) 7_566 . . . ?
O8 Tb1 O5 C7 -175.7(4) . . . . ?
O7 Tb1 O5 C7 103.9(4) . . . . ?
O1 Tb1 O5 C7 166.2(3) 1_565 . . . ?
O6 Tb1 O5 C7 -1.7(3) 5_576 . . . ?
O4 Tb1 O5 C7 47.5(4) . . . . ?
O2 Tb1 O5 C7 -81.7(4) 7_566 . . . ?
O3 Tb1 O5 C7 -23.2(4) . . . . ?
O1 Tb1 O5 C7 -116.2(3) 7_566 . . . ?
C1 Tb1 O5 C7 -98.4(4) 7_566 . . . ?
Tb1 O2 C1 O1 0.7(5) 7_566 . . . ?
Tb1 O2 C1 C2 -177.5(3) 7_566 . . . ?
Tb1 O1 C1 O2 168.0(4) 1_545 . . . ?
Tb1 O1 C1 O2 -0.6(4) 7_566 . . . ?
Tb1 O1 C1 C2 -13.9(9) 1_545 . . . ?
Tb1 O1 C1 C2 177.5(4) 7_566 . . . ?
Tb1 O1 C1 Tb1 168.6(7) 1_545 . . 7_566 ?
O2 C1 C2 C5 -94.6(6) . . . . ?
O1 C1 C2 C5 87.3(6) . . . . ?
Tb1 C1 C2 C5 -122(4) 7_566 . . . ?
O2 C1 C2 C3 82.1(6) . . . . ?
O1 C1 C2 C3 -96.1(5) . . . . ?
Tb1 C1 C2 C3 55(4) 7_566 . . . ?
C5 C2 C3 C4 -0.2(6) . . . . ?
C1 C2 C3 C4 -177.2(5) . . . . ?
C2 C3 C4 S1 0.2(6) . . . . ?
C5 S1 C4 C3 -0.2(5) . . . . ?
C1 C2 C5 C6 -3.7(8) . . . . ?
C3 C2 C5 C6 179.3(4) . . . . ?
C1 C2 C5 S1 177.0(4) . . . . ?
C3 C2 C5 S1 0.1(5) . . . . ?
C4 S1 C5 C2 0.1(4) . . . . ?
C4 S1 C5 C6 -179.3(4) . . . . ?
Tb1 O4 C6 O3 -1.3(4) . . . . ?
Tb1 O4 C6 C5 177.9(4) . . . . ?
Tb1 O3 C6 O4 1.3(4) . . . . ?
Tb1 O3 C6 C5 -177.9(4) . . . . ?
C2 C5 C6 O4 -174.9(5) . . . . ?
S1 C5 C6 O4 4.3(6) . . . . ?
C2 C5 C6 O3 4.3(8) . . . . ?
S1 C5 C6 O3 -176.5(3) . . . . ?
Tb1 O5 C7 O6 -178.3(4) . . . . ?
Tb1 O5 C7 C7 1.4(7) . . . 5_576 ?
Tb1 O6 C7 O5 -178.5(4) 5_576 . . . ?
Tb1 O6 C7 C7 1.8(6) 5_576 . . 5_576 ?

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
O9 H5W O4 0.84 1.97 2.745(5) 153.0 2_645
O8 H4W O3 0.84 1.92 2.750(5) 171.4 7_576
O8 H3W O2 0.84 2.41 2.952(5) 123.0 7_576
O8 H3W O6 0.84 2.31 3.085(5) 154.4 5_586
O7 H2W O5 0.84 2.45 2.916(6) 115.8 .
O7 H1W O9 0.85 2.29 2.753(4) 114.9 1_465

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.119
_database_code_depnum_ccdc_archive 'CCDC 1020435'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 Ho2 O17 S2'
_chemical_formula_weight         848.23

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.489(5)
_cell_length_b                   6.0107(16)
_cell_length_c                   19.762(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.257(2)
_cell_angle_gamma                90.00
_cell_volume                     2157.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5613
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.21

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    7.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1475
_exptl_absorpt_correction_T_max  0.2870
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6495
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2008
_reflns_number_gt                1976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0220P)²+16.6440P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00043(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2008
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0533
_refine_ls_wR_factor_gt          0.0531
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_restrained_S_all      1.166
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.136604(10) 1.18113(3) 0.470600(10) 0.01359(10) Uani 1 1 d . . .
S1 S 0.10814(8) 0.7766(3) 0.22083(7) 0.0373(3) Uani 1 1 d . . .
O1 O 0.22941(17) 0.3454(5) 0.43523(17) 0.0198(7) Uani 1 1 d . . .
O2 O 0.31856(16) 0.5161(6) 0.41465(17) 0.0233(7) Uani 1 1 d . . .
O3 O 0.19154(16) 0.8649(5) 0.43227(16) 0.0170(6) Uani 1 1 d . . .
O4 O 0.10594(17) 1.0499(6) 0.34679(17) 0.0247(7) Uani 1 1 d . . .
O5 O 0.04701(18) 1.2511(5) 0.52538(19) 0.0245(7) Uani 1 1 d . . .
O6 O -0.05212(17) 1.1253(5) 0.54520(18) 0.0236(7) Uani 1 1 d . . .
O7 O 0.0532(2) 1.4375(6) 0.39329(18) 0.0348(9) Uani 1 1 d . . .
H1W H 0.0389 1.5112 0.3543 0.052 Uiso 1 1 d R . .
H2W H 0.0222 1.4527 0.4132 0.052 Uiso 1 1 d R . .
O8 O 0.16491(16) 1.5167(5) 0.53589(17) 0.0214(7) Uani 1 1 d . . .
H3W H 0.1390 1.6312 0.5276 0.032 Uiso 1 1 d R . .
H4W H 0.2073 1.5570 0.5414 0.032 Uiso 1 1 d R . .
O9 O 1.0000 0.3099(9) 0.2500 0.0350(13) Uani 1 2 d S . .
H5W H 0.9640 0.2255 0.2329 0.052 Uiso 1 1 d R . .
C1 C 0.2520(2) 0.4665(7) 0.3947(2) 0.0150(8) Uani 1 1 d . . .
C2 C 0.1999(2) 0.5447(7) 0.3226(2) 0.0164(8) Uani 1 1 d . . .
C3 C 0.1917(2) 0.4231(7) 0.2525(2) 0.0115(8) Uani 1 1 d . . .
H3 H 0.2152 0.2924 0.2479 0.014 Uiso 1 1 calc R . .
C4 C 0.1419(3) 0.5468(11) 0.1968(3) 0.0386(13) Uani 1 1 d . . .
H4 H 0.1281 0.5038 0.1485 0.046 Uiso 1 1 calc R . .
C5 C 0.1573(2) 0.7349(8) 0.3112(2) 0.0194(9) Uani 1 1 d . . .
C6 C 0.1510(2) 0.8915(7) 0.3655(2) 0.0158(8) Uani 1 1 d . . .
C7 C -0.0010(2) 1.1091(7) 0.5203(2) 0.0170(9) Uani 1 1 d . . .


_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
Ho1 O8 2.350(3) . ?
Ho1 O7 2.356(3) . ?
Ho1 O1 2.377(3) 1_565 ?
Ho1 O5 2.402(3) . ?
Ho1 O6 2.414(3) 5_576 ?
Ho1 O2 2.424(3) 7_566 ?
Ho1 O4 2.430(3) . ?
Ho1 O3 2.433(3) . ?
Ho1 O1 2.605(3) 7_566 ?
Ho1 C1 2.898(4) 7_566 ?
S1 C4 1.671(6) . ?
S1 C5 1.712(4) . ?
O1 C1 1.272(5) . ?
O1 Ho1 2.377(3) 1_545 ?
O1 Ho1 2.605(3) 7_566 ?
O2 C1 1.248(5) . ?
O2 Ho1 2.424(3) 7_566 ?
O3 C6 1.278(5) . ?
O4 C6 1.256(5) . ?
O5 C7 1.244(5) . ?
O6 C7 1.264(5) . ?
O6 Ho1 2.414(3) 5_576 ?
O7 H1W 0.8437 . ?
O7 H2W 0.8360 . ?
O8 H3W 0.8336 . ?
O8 H4W 0.8298 . ?
O9 H5W 0.8324 . ?
C1 C2 1.495(6) . ?
C1 Ho1 2.898(4) 7_566 ?
C2 C5 1.382(6) . ?
C2 C3 1.522(6) . ?
C3 C4 1.389(7) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.466(6) . ?
C7 C7 1.546(9) 5_576 ?

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
O8 Ho1 O7 76.35(12) . . ?
O8 Ho1 O1 75.68(11) . 1_565 ?
O7 Ho1 O1 87.56(13) . 1_565 ?
O8 Ho1 O5 70.52(11) . . ?
O7 Ho1 O5 74.58(13) . . ?
O1 Ho1 O5 144.55(11) 1_565 . ?
O8 Ho1 O6 137.68(11) . 5_576 ?
O7 Ho1 O6 97.88(13) . 5_576 ?
O1 Ho1 O6 146.59(11) 1_565 5_576 ?
O5 Ho1 O6 67.59(11) . 5_576 ?
O8 Ho1 O2 88.44(11) . 7_566 ?
O7 Ho1 O2 148.93(12) . 7_566 ?
O1 Ho1 O2 115.06(10) 1_565 7_566 ?
O5 Ho1 O2 74.83(11) . 7_566 ?
O6 Ho1 O2 75.26(11) 5_576 7_566 ?
O8 Ho1 O4 138.98(11) . . ?
O7 Ho1 O4 72.51(11) . . ?
O1 Ho1 O4 76.96(11) 1_565 . ?
O5 Ho1 O4 123.86(11) . . ?
O6 Ho1 O4 73.44(12) 5_576 . ?
O2 Ho1 O4 131.07(11) 7_566 . ?
O8 Ho1 O3 143.06(10) . . ?
O7 Ho1 O3 125.95(11) . . ?
O1 Ho1 O3 76.43(10) 1_565 . ?
O5 Ho1 O3 138.68(11) . . ?
O6 Ho1 O3 73.75(10) 5_576 . ?
O2 Ho1 O3 81.91(11) 7_566 . ?
O4 Ho1 O3 53.73(10) . . ?
O8 Ho1 O1 71.66(10) . 7_566 ?
O7 Ho1 O1 141.34(12) . 7_566 ?
O1 Ho1 O1 64.09(12) 1_565 7_566 ?
O5 Ho1 O1 113.14(11) . 7_566 ?
O6 Ho1 O1 120.38(10) 5_576 7_566 ?
O2 Ho1 O1 51.21(10) 7_566 7_566 ?
O4 Ho1 O1 121.09(10) . 7_566 ?
O3 Ho1 O1 74.59(10) . 7_566 ?
O8 Ho1 C1 79.04(11) . 7_566 ?
O7 Ho1 C1 155.10(12) . 7_566 ?
O1 Ho1 C1 90.03(11) 1_565 7_566 ?
O5 Ho1 C1 93.72(12) . 7_566 ?
O6 Ho1 C1 97.71(12) 5_576 7_566 ?
O2 Ho1 C1 25.16(11) 7_566 7_566 ?
O4 Ho1 C1 130.87(11) . 7_566 ?
O3 Ho1 C1 77.23(11) . 7_566 ?
O1 Ho1 C1 26.04(10) 7_566 7_566 ?
C4 S1 C5 92.6(3) . . ?
C1 O1 Ho1 153.6(3) . 1_545 ?
C1 O1 Ho1 90.0(2) . 7_566 ?
Ho1 O1 Ho1 115.91(12) 1_545 7_566 ?
C1 O2 Ho1 99.2(3) . 7_566 ?
C6 O3 Ho1 92.7(2) . . ?
C6 O4 Ho1 93.4(3) . . ?
C7 O5 Ho1 119.5(3) . . ?
C7 O6 Ho1 119.2(3) . 5_576 ?
Ho1 O7 H1W 149.0 . . ?
Ho1 O7 H2W 102.2 . . ?
H1W O7 H2W 108.5 . . ?
Ho1 O8 H3W 126.6 . . ?
Ho1 O8 H4W 110.3 . . ?
H3W O8 H4W 106.8 . . ?
O2 C1 O1 119.7(4) . . ?
O2 C1 C2 119.6(4) . . ?
O1 C1 C2 120.7(4) . . ?
O2 C1 Ho1 55.7(2) . 7_566 ?
O1 C1 Ho1 64.0(2) . 7_566 ?
C2 C1 Ho1 174.8(3) . 7_566 ?
C5 C2 C1 125.1(4) . . ?
C5 C2 C3 113.0(4) . . ?
C1 C2 C3 121.8(4) . . ?
C4 C3 C2 106.0(4) . . ?
C4 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
C3 C4 S1 116.8(4) . . ?
C3 C4 H4 121.6 . . ?
S1 C4 H4 121.6 . . ?
C2 C5 C6 128.1(4) . . ?
C2 C5 S1 111.5(3) . . ?
C6 C5 S1 120.4(3) . . ?
O4 C6 O3 120.2(4) . . ?
O4 C6 C5 120.4(4) . . ?
O3 C6 C5 119.4(4) . . ?
O5 C7 O6 126.3(4) . . ?
O5 C7 C7 117.6(5) . 5_576 ?
O6 C7 C7 116.1(5) . 5_576 ?

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
O8 Ho1 O3 C6 -126.4(3) . . . . ?
O7 Ho1 O3 C6 -7.8(3) . . . . ?
O1 Ho1 O3 C6 -84.5(2) 1_565 . . . ?
O5 Ho1 O3 C6 101.4(3) . . . . ?
O6 Ho1 O3 C6 80.2(2) 5_576 . . . ?
O2 Ho1 O3 C6 157.2(2) 7_566 . . . ?
O4 Ho1 O3 C6 -0.9(2) . . . . ?
O1 Ho1 O3 C6 -150.9(3) 7_566 . . . ?
C1 Ho1 O3 C6 -177.7(3) 7_566 . . . ?
O8 Ho1 O4 C6 132.7(2) . . . . ?
O7 Ho1 O4 C6 175.1(3) . . . . ?
O1 Ho1 O4 C6 83.5(3) 1_565 . . . ?
O5 Ho1 O4 C6 -128.1(3) . . . . ?
O6 Ho1 O4 C6 -80.8(3) 5_576 . . . ?
O2 Ho1 O4 C6 -28.5(3) 7_566 . . . ?
O3 Ho1 O4 C6 0.9(2) . . . . ?
O1 Ho1 O4 C6 35.1(3) 7_566 . . . ?
C1 Ho1 O4 C6 5.0(3) 7_566 . . . ?
O8 Ho1 O5 C7 -175.2(4) . . . . ?
O7 Ho1 O5 C7 104.1(3) . . . . ?
O1 Ho1 O5 C7 166.5(3) 1_565 . . . ?
O6 Ho1 O5 C7 -1.4(3) 5_576 . . . ?
O2 Ho1 O5 C7 -81.4(3) 7_566 . . . ?
O4 Ho1 O5 C7 48.2(4) . . . . ?
O3 Ho1 O5 C7 -23.3(4) . . . . ?
O1 Ho1 O5 C7 -116.1(3) 7_566 . . . ?
C1 Ho1 O5 C7 -98.2(3) 7_566 . . . ?
Ho1 O2 C1 O1 0.8(4) 7_566 . . . ?
Ho1 O2 C1 C2 -177.5(3) 7_566 . . . ?
Ho1 O1 C1 O2 168.1(4) 1_545 . . . ?
Ho1 O1 C1 O2 -0.8(4) 7_566 . . . ?
Ho1 O1 C1 C2 -13.5(9) 1_545 . . . ?
Ho1 O1 C1 C2 177.5(3) 7_566 . . . ?
Ho1 O1 C1 Ho1 168.9(6) 1_545 . . 7_566 ?
O2 C1 C2 C5 -95.1(5) . . . . ?
O1 C1 C2 C5 86.6(6) . . . . ?
Ho1 C1 C2 C5 -119(3) 7_566 . . . ?
O2 C1 C2 C3 81.9(5) . . . . ?
O1 C1 C2 C3 -96.4(5) . . . . ?
Ho1 C1 C2 C3 58(3) 7_566 . . . ?
C5 C2 C3 C4 0.1(5) . . . . ?
C1 C2 C3 C4 -177.3(4) . . . . ?
C2 C3 C4 S1 0.2(5) . . . . ?
C5 S1 C4 C3 -0.3(5) . . . . ?
C1 C2 C5 C6 -3.2(7) . . . . ?
C3 C2 C5 C6 179.6(4) . . . . ?
C1 C2 C5 S1 177.0(3) . . . . ?
C3 C2 C5 S1 -0.3(5) . . . . ?
C4 S1 C5 C2 0.3(4) . . . . ?
C4 S1 C5 C6 -179.6(4) . . . . ?
Ho1 O4 C6 O3 -1.6(4) . . . . ?
Ho1 O4 C6 C5 178.1(4) . . . . ?
Ho1 O3 C6 O4 1.6(4) . . . . ?
Ho1 O3 C6 C5 -178.1(4) . . . . ?
C2 C5 C6 O4 -175.3(4) . . . . ?
S1 C5 C6 O4 4.6(6) . . . . ?
C2 C5 C6 O3 4.4(7) . . . . ?
S1 C5 C6 O3 -175.8(3) . . . . ?
Ho1 O5 C7 O6 -178.7(3) . . . . ?
Ho1 O5 C7 C7 1.2(6) . . . 5_576 ?
Ho1 O6 C7 O5 -178.7(3) 5_576 . . . ?
Ho1 O6 C7 C7 1.4(6) 5_576 . . 5_576 ?

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
O9 H5W O4 0.83 1.97 2.739(4) 152.4 2_645
O8 H4W O3 0.83 1.91 2.730(4) 171.9 7_576
O8 H3W O2 0.83 2.41 2.953(5) 123.7 7_576
O8 H3W O6 0.83 2.30 3.078(5) 154.5 5_586
O7 H2W O5 0.84 2.42 2.883(5) 116.1 .
O7 H1W O9 0.84 2.27 2.748(4) 116.1 1_465

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.124
_database_code_depnum_ccdc_archive 'CCDC 1020436'
