# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1-La
_database_code_depnum_ccdc_archive 'CCDC 1549839'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H18 La O18 S2, 2(H2 O)'
_chemical_formula_sum            'C15 H22 La O20 S2'
_chemical_formula_weight         725.36

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'
La La -0.2871 2.4523 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8254(5)
_cell_length_b                   12.3142(8)
_cell_length_c                   12.5150(9)
_cell_angle_alpha                102.120(6)
_cell_angle_beta                 98.179(6)
_cell_angle_gamma                90.704(5)
_cell_volume                     1166.01(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3068
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      27.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             722
_exptl_absorpt_coefficient_mu    2.110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6656
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5547
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4094
_reflns_number_gt                3626
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0851P)²+3.4139P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4094
_refine_ls_number_parameters     361
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1561
_refine_ls_wR_factor_gt          0.1511
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_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
La1 La 0.76855(5) 0.20085(3) 0.44510(3) 0.01691(18) Uani 1 1 d . . .
S1 S 0.7847(3) 0.17203(15) 0.73689(15) 0.0185(4) Uani 1 1 d . . .
S2 S 0.4571(2) 0.32295(15) 0.22984(16) 0.0186(4) Uani 1 1 d . . .
O1 O 0.8468(8) 0.2209(5) 0.6527(5) 0.0281(13) Uani 1 1 d . . .
O1W O 0.4688(8) 0.1222(7) 0.4338(6) 0.0436(18) Uani 1 1 d D . .
H1W1 H 0.385(9) 0.166(7) 0.435(11) 0.065 Uiso 1 1 d D . .
H1W2 H 0.437(12) 0.062(5) 0.450(10) 0.065 Uiso 1 1 d D . .
O2W O 0.6026(9) 0.3554(6) 0.5496(6) 0.0420(17) Uani 1 1 d D . .
H2W1 H 0.602(12) 0.371(10) 0.6189(14) 0.063 Uiso 1 1 d D . .
H2W2 H 0.499(5) 0.351(11) 0.516(7) 0.063 Uiso 1 1 d D . .
O2 O 0.8890(8) 0.0811(4) 0.7608(5) 0.0253(13) Uani 1 1 d . . .
O3W O 0.9632(9) 0.3713(5) 0.5358(5) 0.0344(15) Uani 1 1 d . . .
H3W1 H 1.0556 0.3824 0.5105 0.052 Uiso 1 1 d R . .
H3W2 H 0.9734 0.4079 0.6021 0.052 Uiso 1 1 d R . .
O3 O 0.6022(8) 0.1428(5) 0.7121(5) 0.0314(14) Uani 1 1 d . . .
O4W O 0.9673(8) 0.2850(5) 0.3115(5) 0.0270(13) Uani 1 1 d . . .
H4W1 H 0.9260 0.3443 0.2961 0.040 Uiso 1 1 d R . .
H4W2 H 1.0745 0.2868 0.3068 0.040 Uiso 1 1 d R . .
O4 O 0.6131(8) 0.3886(5) 0.7774(5) 0.0306(14) Uani 1 1 d D . .
H4O H 0.555(12) 0.445(5) 0.773(9) 0.046 Uiso 1 1 d D . .
O5 O 0.7767(9) 0.6033(5) 1.1586(5) 0.0337(15) Uani 1 1 d . . .
H5O H 0.7673 0.6381 1.2208 0.051 Uiso 1 1 calc R . .
O5W O 0.2849(10) 0.2595(6) 0.6669(6) 0.057(2) Uani 1 1 d . . .
H5W1 H 0.3765 0.2253 0.6800 0.085 Uiso 1 1 d R . .
H5W2 H 0.2219 0.2208 0.6105 0.085 Uiso 1 1 d R . .
O6 O 0.9347(9) 0.4946(5) 1.2524(5) 0.0339(15) Uani 1 1 d . . .
O6W O 0.2825(10) 0.4328(7) 0.4962(8) 0.061(2) Uani 1 1 d . . .
H6W1 H 0.2819 0.3956 0.4308 0.092 Uiso 1 1 d R . .
H6W2 H 0.3144 0.4995 0.4981 0.092 Uiso 1 1 d R . .
O7 O 0.5872(8) 0.2822(5) 0.3054(5) 0.0295(14) Uani 1 1 d . . .
O8 O 0.5286(8) 0.4098(5) 0.1857(5) 0.0275(13) Uani 1 1 d . . .
O9 O 0.3027(8) 0.3551(5) 0.2782(6) 0.0353(15) Uani 1 1 d . . .
O10 O 0.2533(8) 0.1169(5) 0.2294(5) 0.0303(14) Uani 1 1 d D . .
H10O H 0.186(11) 0.062(6) 0.230(9) 0.045 Uiso 1 1 d D . .
O11 O 0.1383(11) -0.1291(6) -0.1346(6) 0.050(2) Uani 1 1 d . . .
H11O H 0.1061 -0.1774 -0.1901 0.075 Uiso 1 1 calc R . .
O12 O 0.2638(8) -0.0576(5) -0.2544(5) 0.0293(14) Uani 1 1 d . . .
O13 O 0.7766(7) 0.0077(4) 0.4842(5) 0.0264(13) Uani 1 1 d . . .
O14 O 0.9398(7) -0.1244(4) 0.5333(5) 0.0270(13) Uani 1 1 d . . .
C1 C 0.8166(10) 0.2786(6) 0.8595(6) 0.0191(16) Uani 1 1 d . . .
C2 C 0.7195(11) 0.3743(6) 0.8663(6) 0.0214(17) Uani 1 1 d . . .
C3 C 0.7365(11) 0.4503(7) 0.9655(7) 0.0242(18) Uani 1 1 d . . .
H3A H 0.6720 0.5136 0.9716 0.029 Uiso 1 1 calc R . .
C4 C 0.8494(10) 0.4336(7) 1.0575(7) 0.0219(17) Uani 1 1 d . . .
C5 C 0.9501(11) 0.3423(7) 1.0481(7) 0.0254(18) Uani 1 1 d . . .
H5A H 1.0288 0.3328 1.1081 0.031 Uiso 1 1 calc R . .
C6 C 0.9341(10) 0.2639(7) 0.9482(7) 0.0214(17) Uani 1 1 d . . .
H6A H 1.0021 0.2021 0.9415 0.026 Uiso 1 1 calc R . .
C7 C 0.8564(11) 0.5144(7) 1.1653(7) 0.0251(18) Uani 1 1 d . . .
C8 C 0.3941(9) 0.2104(6) 0.1150(6) 0.0170(15) Uani 1 1 d . . .
C9 C 0.2971(10) 0.1178(7) 0.1282(6) 0.0199(16) Uani 1 1 d . . .
C10 C 0.2469(11) 0.0345(7) 0.0375(7) 0.0254(18) Uani 1 1 d . . .
H10A H 0.1827 -0.0269 0.0447 0.030 Uiso 1 1 calc R . .
C11 C 0.2899(11) 0.0398(7) -0.0650(7) 0.0240(18) Uani 1 1 d . . .
C12 C 0.3870(11) 0.1306(7) -0.0773(7) 0.0266(19) Uani 1 1 d . . .
H12A H 0.4170 0.1340 -0.1459 0.032 Uiso 1 1 calc R . .
C13 C 0.4381(11) 0.2154(7) 0.0130(7) 0.0257(18) Uani 1 1 d . . .
H13A H 0.5027 0.2765 0.0054 0.031 Uiso 1 1 calc R . .
C14 C 0.2327(11) -0.0531(7) -0.1599(7) 0.0233(18) Uani 1 1 d . . .
C15 C 0.9178(10) -0.0331(6) 0.5053(6) 0.0169(16) 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
La1 O7 2.477(6) . ?
La1 O14 2.480(6) 2_756 ?
La1 O1W 2.500(6) . ?
La1 O13 2.526(5) . ?
La1 O3W 2.538(6) . ?
La1 O1 2.542(6) . ?
La1 O2W 2.553(7) . ?
La1 O12 2.631(6) 2_655 ?
La1 O4W 2.777(6) . ?
S1 O3 1.442(6) . ?
S1 O2 1.451(6) . ?
S1 O1 1.454(6) . ?
S1 C1 1.782(8) . ?
S2 O8 1.444(6) . ?
S2 O9 1.449(6) . ?
S2 O7 1.457(6) . ?
S2 C8 1.782(7) . ?
O1W H1W1 0.85(8) . ?
O1W H1W2 0.85(8) . ?
O2W H2W1 0.85(8) . ?
O2W H2W2 0.85(8) . ?
O3W H3W1 0.8500 . ?
O3W H3W2 0.8501 . ?
O4W H4W1 0.8499 . ?
O4W H4W2 0.8500 . ?
O4 C2 1.335(10) . ?
O4 H4O 0.85(8) . ?
O5 C7 1.279(11) . ?
O5 H5O 0.8200 . ?
O5W H5W1 0.8500 . ?
O5W H5W2 0.8500 . ?
O6 C7 1.245(11) . ?
O6W H6W1 0.8500 . ?
O6W H6W2 0.8499 . ?
O10 C9 1.361(9) . ?
O10 H10O 0.85(8) . ?
O11 C14 1.302(10) . ?
O11 H11O 0.8200 . ?
O12 C14 1.231(10) . ?
O12 La1 2.631(6) 2_655 ?
O13 C15 1.237(9) . ?
O14 C15 1.253(9) . ?
O14 La1 2.480(6) 2_756 ?
C1 C6 1.382(11) . ?
C1 C2 1.404(11) . ?
C2 C3 1.378(11) . ?
C3 C4 1.401(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.375(12) . ?
C4 C7 1.492(11) . ?
C5 C6 1.399(11) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C8 C13 1.381(11) . ?
C8 C9 1.413(11) . ?
C9 C10 1.368(11) . ?
C10 C11 1.386(12) . ?
C10 H10A 0.9300 . ?
C11 C12 1.392(12) . ?
C11 C14 1.479(11) . ?
C12 C13 1.376(11) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C15 1.551(15) 2_756 ?

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
O7 La1 O14 136.8(2) . 2_756 ?
O7 La1 O1W 74.3(2) . . ?
O14 La1 O1W 134.1(2) 2_756 . ?
O7 La1 O13 132.53(19) . . ?
O14 La1 O13 64.97(17) 2_756 . ?
O1W La1 O13 69.5(2) . . ?
O7 La1 O3W 98.1(2) . . ?
O14 La1 O3W 76.7(2) 2_756 . ?
O1W La1 O3W 141.8(2) . . ?
O13 La1 O3W 129.3(2) . . ?
O7 La1 O1 141.75(19) . . ?
O14 La1 O1 76.2(2) 2_756 . ?
O1W La1 O1 95.5(2) . . ?
O13 La1 O1 72.35(18) . . ?
O3W La1 O1 67.1(2) . . ?
O7 La1 O2W 72.7(2) . . ?
O14 La1 O2W 137.9(2) 2_756 . ?
O1W La1 O2W 73.7(3) . . ?
O13 La1 O2W 122.5(2) . . ?
O3W La1 O2W 68.3(2) . . ?
O1 La1 O2W 69.0(2) . . ?
O7 La1 O12 71.69(19) . 2_655 ?
O14 La1 O12 82.1(2) 2_756 2_655 ?
O1W La1 O12 79.1(2) . 2_655 ?
O13 La1 O12 72.19(19) . 2_655 ?
O3W La1 O12 135.06(19) . 2_655 ?
O1 La1 O12 143.72(18) . 2_655 ?
O2W La1 O12 139.8(2) . 2_655 ?
O7 La1 O4W 68.4(2) . . ?
O14 La1 O4W 71.32(18) 2_756 . ?
O1W La1 O4W 138.5(2) . . ?
O13 La1 O4W 126.51(18) . . ?
O3W La1 O4W 63.12(18) . . ?
O1 La1 O4W 125.07(18) . . ?
O2W La1 O4W 110.4(2) . . ?
O12 La1 O4W 72.69(17) 2_655 . ?
O3 S1 O2 113.2(4) . . ?
O3 S1 O1 112.6(4) . . ?
O2 S1 O1 111.6(3) . . ?
O3 S1 C1 107.1(4) . . ?
O2 S1 C1 106.3(4) . . ?
O1 S1 C1 105.4(3) . . ?
O8 S2 O9 112.7(4) . . ?
O8 S2 O7 111.4(4) . . ?
O9 S2 O7 112.5(4) . . ?
O8 S2 C8 106.0(4) . . ?
O9 S2 C8 106.9(4) . . ?
O7 S2 C8 106.9(4) . . ?
S1 O1 La1 136.0(4) . . ?
La1 O1W H1W1 119(7) . . ?
La1 O1W H1W2 129(7) . . ?
H1W1 O1W H1W2 109.4(18) . . ?
La1 O2W H2W1 126(8) . . ?
La1 O2W H2W2 108(8) . . ?
H2W1 O2W H2W2 109.7(19) . . ?
La1 O3W H3W1 119.7 . . ?
La1 O3W H3W2 128.2 . . ?
H3W1 O3W H3W2 108.0 . . ?
La1 O4W H4W1 110.6 . . ?
La1 O4W H4W2 134.3 . . ?
H4W1 O4W H4W2 107.7 . . ?
C2 O4 H4O 126(8) . . ?
C7 O5 H5O 109.5 . . ?
H5W1 O5W H5W2 108.4 . . ?
H6W1 O6W H6W2 107.9 . . ?
S2 O7 La1 170.8(4) . . ?
C9 O10 H10O 113(8) . . ?
C14 O11 H11O 109.5 . . ?
C14 O12 La1 138.8(5) . 2_655 ?
C15 O13 La1 119.3(5) . . ?
C15 O14 La1 120.8(5) . 2_756 ?
C6 C1 C2 120.9(7) . . ?
C6 C1 S1 119.0(6) . . ?
C2 C1 S1 120.1(6) . . ?
O4 C2 C3 122.1(7) . . ?
O4 C2 C1 119.4(7) . . ?
C3 C2 C1 118.5(7) . . ?
C2 C3 C4 121.0(8) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 119.8(7) . . ?
C5 C4 C7 120.8(7) . . ?
C3 C4 C7 119.4(7) . . ?
C4 C5 C6 120.0(8) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
C1 C6 C5 119.7(7) . . ?
C1 C6 H6A 120.2 . . ?
C5 C6 H6A 120.2 . . ?
O6 C7 O5 124.5(7) . . ?
O6 C7 C4 121.5(8) . . ?
O5 C7 C4 114.0(8) . . ?
C13 C8 C9 120.5(7) . . ?
C13 C8 S2 119.5(6) . . ?
C9 C8 S2 119.9(6) . . ?
O10 C9 C10 122.9(7) . . ?
O10 C9 C8 118.8(7) . . ?
C10 C9 C8 118.3(7) . . ?
C9 C10 C11 121.3(8) . . ?
C9 C10 H10A 119.4 . . ?
C11 C10 H10A 119.4 . . ?
C10 C11 C12 120.2(8) . . ?
C10 C11 C14 118.8(7) . . ?
C12 C11 C14 121.0(7) . . ?
C13 C12 C11 119.3(8) . . ?
C13 C12 H12A 120.4 . . ?
C11 C12 H12A 120.4 . . ?
C12 C13 C8 120.5(8) . . ?
C12 C13 H13A 119.8 . . ?
C8 C13 H13A 119.8 . . ?
O12 C14 O11 122.6(8) . . ?
O12 C14 C11 124.4(8) . . ?
O11 C14 C11 112.9(7) . . ?
O13 C15 O14 125.6(7) . . ?
O13 C15 C15 117.6(8) . 2_756 ?
O14 C15 C15 116.8(8) . 2_756 ?

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
O3 S1 O1 La1 -31.4(6) . . . . ?
O2 S1 O1 La1 97.2(5) . . . . ?
C1 S1 O1 La1 -147.8(5) . . . . ?
O7 La1 O1 S1 92.8(5) . . . . ?
O14 La1 O1 S1 -112.9(5) 2_756 . . . ?
O1W La1 O1 S1 21.3(5) . . . . ?
O13 La1 O1 S1 -45.1(5) . . . . ?
O3W La1 O1 S1 166.0(6) . . . . ?
O2W La1 O1 S1 91.5(5) . . . . ?
O12 La1 O1 S1 -57.8(6) 2_655 . . . ?
O4W La1 O1 S1 -167.8(4) . . . . ?
O7 La1 O13 C15 137.5(5) . . . . ?
O14 La1 O13 C15 6.0(5) 2_756 . . . ?
O1W La1 O13 C15 -179.8(6) . . . . ?
O3W La1 O13 C15 -38.8(6) . . . . ?
O1 La1 O13 C15 -76.7(6) . . . . ?
O2W La1 O13 C15 -126.3(5) . . . . ?
O12 La1 O13 C15 95.5(6) 2_655 . . . ?
O4W La1 O13 C15 44.2(6) . . . . ?
O3 S1 C1 C6 125.6(7) . . . . ?
O2 S1 C1 C6 4.2(7) . . . . ?
O1 S1 C1 C6 -114.4(6) . . . . ?
O3 S1 C1 C2 -52.5(7) . . . . ?
O2 S1 C1 C2 -173.9(6) . . . . ?
O1 S1 C1 C2 67.5(7) . . . . ?
C6 C1 C2 O4 176.8(7) . . . . ?
S1 C1 C2 O4 -5.1(11) . . . . ?
C6 C1 C2 C3 -3.8(12) . . . . ?
S1 C1 C2 C3 174.3(6) . . . . ?
O4 C2 C3 C4 -179.8(8) . . . . ?
C1 C2 C3 C4 0.8(12) . . . . ?
C2 C3 C4 C5 2.5(12) . . . . ?
C2 C3 C4 C7 -176.4(8) . . . . ?
C3 C4 C5 C6 -2.8(12) . . . . ?
C7 C4 C5 C6 176.1(7) . . . . ?
C2 C1 C6 C5 3.4(12) . . . . ?
S1 C1 C6 C5 -174.6(6) . . . . ?
C4 C5 C6 C1 -0.1(12) . . . . ?
C5 C4 C7 O6 -9.7(12) . . . . ?
C3 C4 C7 O6 169.2(8) . . . . ?
C5 C4 C7 O5 170.0(8) . . . . ?
C3 C4 C7 O5 -11.1(11) . . . . ?
O8 S2 C8 C13 7.7(7) . . . . ?
O9 S2 C8 C13 128.1(7) . . . . ?
O7 S2 C8 C13 -111.2(7) . . . . ?
O8 S2 C8 C9 -171.2(6) . . . . ?
O9 S2 C8 C9 -50.8(7) . . . . ?
O7 S2 C8 C9 69.9(7) . . . . ?
C13 C8 C9 O10 -178.7(8) . . . . ?
S2 C8 C9 O10 0.2(10) . . . . ?
C13 C8 C9 C10 -0.7(12) . . . . ?
S2 C8 C9 C10 178.2(6) . . . . ?
O10 C9 C10 C11 178.2(8) . . . . ?
C8 C9 C10 C11 0.2(12) . . . . ?
C9 C10 C11 C12 0.5(13) . . . . ?
C9 C10 C11 C14 179.7(8) . . . . ?
C10 C11 C12 C13 -0.7(13) . . . . ?
C14 C11 C12 C13 -179.9(8) . . . . ?
C11 C12 C13 C8 0.2(13) . . . . ?
C9 C8 C13 C12 0.5(12) . . . . ?
S2 C8 C13 C12 -178.4(7) . . . . ?
La1 O12 C14 O11 -11.4(14) 2_655 . . . ?
La1 O12 C14 C11 171.6(6) 2_655 . . . ?
C10 C11 C14 O12 -179.7(8) . . . . ?
C12 C11 C14 O12 -0.5(13) . . . . ?
C10 C11 C14 O11 3.0(11) . . . . ?
C12 C11 C14 O11 -177.8(8) . . . . ?
La1 O13 C15 O14 174.9(6) . . . . ?
La1 O13 C15 C15 -6.0(11) . . . 2_756 ?
La1 O14 C15 O13 174.1(6) 2_756 . . . ?
La1 O14 C15 C15 -4.9(11) 2_756 . . 2_756 ?

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
O1W H1W1 O14 0.85(8) 2.69(8) 3.281(9) 127(8) 2_656
O1W H1W2 O13 0.85(8) 2.21(6) 2.911(9) 140(8) 2_656
O2W H2W1 O4 0.85(8) 1.94(2) 2.783(9) 172(12) .
O2W H2W2 O6W 0.85(8) 1.99(7) 2.735(10) 145(11) .
O3W H3W1 O6W 0.85 1.92 2.743(10) 163.3 1_655
O3W H3W2 O6 0.85 1.99 2.814(8) 163.1 2_767
O4W H4W1 O6 0.85 2.04 2.836(9) 155.5 1_554
O4W H4W2 O9 0.85 2.07 2.867(8) 155.3 1_655
O4 H4O O8 0.85(8) 1.90(4) 2.709(8) 159(11) 2_666
O5 H5O O5W 0.82 1.78 2.574(9) 163.0 2_667
O5W H5W1 O3 0.85 2.08 2.929(10) 179.4 .
O5W H5W2 O14 0.85 2.16 3.010(9) 179.2 2_656
O6W H6W1 O9 0.85 1.90 2.724(12) 162.6 .
O6W H6W2 O2W 0.85 2.12 2.942(11) 162.2 2_666
O10 H10O O2 0.85(8) 1.88(4) 2.701(8) 161(11) 2_656
O11 H11O O4W 0.82 1.81 2.631(8) 179.1 2_655

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.879
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.203
####################################################################### 
# 
# 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_2-Nd
_database_code_depnum_ccdc_archive 'CCDC 1549840'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 Nd2 O28 S2, 2(C7 H5 O6 S), 8(H2 O)'
_chemical_formula_sum            'C30 H60 Nd2 O48 S4'
_chemical_formula_weight         1605.50

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9284(3)
_cell_length_b                   12.3932(6)
_cell_length_c                   15.1406(7)
_cell_angle_alpha                107.264(4)
_cell_angle_beta                 96.798(3)
_cell_angle_gamma                96.614(3)
_cell_volume                     1392.83(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4063
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_T_max  0.7283
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9361
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6371
_reflns_number_gt                5594
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0244P)²+0.0568P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6371
_refine_ls_number_parameters     463
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0725
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.002
_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 0.79780(2) 0.707832(16) 0.519033(13) 0.01889(6) Uani 1 1 d . . .
S1 S 0.74099(11) 0.64634(8) 0.74904(6) 0.02233(19) Uani 1 1 d . . .
S2 S 0.56130(13) 1.13789(8) 0.76993(7) 0.0312(2) Uani 1 1 d . . .
O1 O 0.7906(3) 0.6985(2) 0.67979(17) 0.0281(6) Uani 1 1 d . . .
O1W O 1.0633(3) 0.6479(3) 0.56847(19) 0.0394(7) Uani 1 1 d D . .
H1W1 H 1.126(5) 0.601(3) 0.541(2) 0.059 Uiso 1 1 d D . .
H1W2 H 1.108(5) 0.679(4) 0.6253(11) 0.059 Uiso 1 1 d D . .
O2 O 0.5614(3) 0.5918(2) 0.72727(19) 0.0334(6) Uani 1 1 d . . .
O2W O 0.9522(4) 0.6267(3) 0.38706(19) 0.0405(7) Uani 1 1 d D . .
H2W1 H 1.0588(16) 0.649(4) 0.394(3) 0.061 Uiso 1 1 d D . .
H2W2 H 0.904(4) 0.614(4) 0.3315(13) 0.061 Uiso 1 1 d D . .
O3W O 0.6343(4) 0.8689(2) 0.5960(2) 0.0366(7) Uani 1 1 d D . .
H3W1 H 0.688(5) 0.9359(17) 0.622(2) 0.055 Uiso 1 1 d D . .
H3W2 H 0.590(5) 0.843(3) 0.635(2) 0.055 Uiso 1 1 d D . .
O3 O 0.8600(3) 0.5717(2) 0.76798(18) 0.0318(6) Uani 1 1 d . . .
O4 O 0.5633(3) 0.8510(2) 0.78170(18) 0.0282(6) Uani 1 1 d D . .
H4O H 0.529(5) 0.9150(19) 0.793(3) 0.042 Uiso 1 1 d D . .
O4W O 0.8688(4) 0.8541(2) 0.4432(2) 0.0407(7) Uani 1 1 d D . .
H4W1 H 0.894(6) 0.837(3) 0.3881(15) 0.061 Uiso 1 1 d D . .
H4W2 H 0.828(6) 0.916(2) 0.456(3) 0.061 Uiso 1 1 d D . .
O5W O 0.9974(4) 0.8796(3) 0.62988(19) 0.0382(7) Uani 1 1 d D . .
H5W1 H 1.021(5) 0.893(4) 0.6888(9) 0.057 Uiso 1 1 d D . .
H5W2 H 1.086(3) 0.899(4) 0.609(2) 0.057 Uiso 1 1 d D . .
O5 O 0.7436(4) 1.1219(2) 1.10452(19) 0.0356(7) Uani 1 1 d D . .
H5O H 0.762(6) 1.177(3) 1.1549(18) 0.053 Uiso 1 1 d D . .
O6W O 0.6029(4) 0.6469(2) 0.36133(18) 0.0324(6) Uani 1 1 d D . .
H6W1 H 0.590(5) 0.689(3) 0.328(2) 0.049 Uiso 1 1 d D . .
H6W2 H 0.552(5) 0.5794(14) 0.334(2) 0.049 Uiso 1 1 d D . .
O6 O 0.9245(4) 1.0398(3) 1.17966(19) 0.0403(7) Uani 1 1 d . . .
O7 O 0.4675(5) 1.1725(3) 0.6981(2) 0.0686(11) Uani 1 1 d . . .
O7W O 0.2756(4) 0.7503(3) 0.4221(2) 0.0452(8) Uani 1 1 d GD . .
H7W1 H 0.343(5) 0.716(4) 0.448(3) 0.068 Uiso 1 1 d D . .
H7W2 H 0.314(5) 0.764(4) 0.376(2) 0.068 Uiso 1 1 d D . .
O8W O 0.7285(4) 1.0439(3) 0.4494(3) 0.0596(9) Uani 1 1 d GD . .
H8W1 H 0.731(6) 1.104(3) 0.495(3) 0.089 Uiso 1 1 d D . .
H8W2 H 0.630(3) 1.027(4) 0.416(3) 0.089 Uiso 1 1 d D . .
O8 O 0.7185(4) 1.0988(3) 0.7429(2) 0.0577(10) Uani 1 1 d . . .
O9W O 0.9365(4) 0.8283(3) 0.2545(2) 0.0457(8) Uani 1 1 d GD . .
H9W1 H 1.0436(16) 0.849(4) 0.257(4) 0.069 Uiso 1 1 d D . .
H9W2 H 0.882(4) 0.878(3) 0.243(4) 0.069 Uiso 1 1 d D . .
O9 O 0.4557(3) 1.0544(2) 0.7986(2) 0.0365(7) Uani 1 1 d . . .
O10 O 0.7594(4) 1.3614(2) 0.7821(2) 0.0423(8) Uani 1 1 d D . .
H10O H 0.791(6) 1.4286(17) 0.782(3) 0.063 Uiso 1 1 d D . .
O10W O 1.2275(4) 0.6839(2) 0.7502(2) 0.0356(7) Uani 1 1 d GD . .
HAW H 1.324(3) 0.668(3) 0.738(3) 0.053 Uiso 1 1 d D . .
HBW H 1.164(4) 0.627(2) 0.754(3) 0.053 Uiso 1 1 d D . .
O11 O 0.8303(5) 1.6414(3) 1.1052(2) 0.0507(9) Uani 1 1 d D . .
H11O H 0.865(6) 1.694(3) 1.157(2) 0.076 Uiso 1 1 d D . .
O12 O 0.7841(4) 1.5335(3) 1.1962(2) 0.0478(8) Uani 1 1 d . . .
O13 O 0.4892(3) 0.6460(2) 0.52839(18) 0.0254(6) Uani 1 1 d . . .
O14 O 0.2847(3) 0.4984(2) 0.51336(19) 0.0278(6) Uani 1 1 d . . .
C1 C 0.7639(4) 0.7621(3) 0.8549(2) 0.0205(7) Uani 1 1 d . . .
C2 C 0.6721(4) 0.8527(3) 0.8589(2) 0.0214(7) Uani 1 1 d . . .
C3 C 0.6937(4) 0.9428(3) 0.9418(2) 0.0231(8) Uani 1 1 d . . .
H3A H 0.6326 1.0032 0.9454 0.028 Uiso 1 1 calc R . .
C4 C 0.8069(4) 0.9431(3) 1.0200(2) 0.0241(8) Uani 1 1 d . . .
C5 C 0.8985(5) 0.8529(3) 1.0152(3) 0.0260(8) Uani 1 1 d . . .
H5A H 0.9734 0.8527 1.0673 0.031 Uiso 1 1 calc R . .
C6 C 0.8773(5) 0.7635(3) 0.9323(2) 0.0249(8) Uani 1 1 d . . .
H6A H 0.9398 0.7037 0.9286 0.030 Uiso 1 1 calc R . .
C7 C 0.8317(5) 1.0390(3) 1.1092(3) 0.0262(8) Uani 1 1 d . . .
C8 C 0.6207(5) 1.2602(3) 0.8706(3) 0.0261(8) Uani 1 1 d . . .
C9 C 0.7154(5) 1.3605(3) 0.8661(3) 0.0285(8) Uani 1 1 d . . .
C10 C 0.7630(5) 1.4533(3) 0.9465(3) 0.0315(9) Uani 1 1 d . . .
H10A H 0.8253 1.5202 0.9437 0.038 Uiso 1 1 calc R . .
C11 C 0.7192(5) 1.4482(3) 1.0317(3) 0.0275(8) Uani 1 1 d . . .
C12 C 0.6222(5) 1.3499(4) 1.0356(3) 0.0337(9) Uani 1 1 d . . .
H12A H 0.5899 1.3463 1.0919 0.040 Uiso 1 1 calc R . .
C13 C 0.5735(5) 1.2566(3) 0.9547(3) 0.0330(9) Uani 1 1 d . . .
H13A H 0.5079 1.1907 0.9573 0.040 Uiso 1 1 calc R . .
C14 C 0.7793(5) 1.5441(3) 1.1195(3) 0.0307(9) Uani 1 1 d . . .
C15 C 0.4360(4) 0.5422(3) 0.5124(2) 0.0213(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 O1W 2.421(3) . ?
Nd1 O14 2.449(2) 2_666 ?
Nd1 O4W 2.465(3) . ?
Nd1 O1 2.478(2) . ?
Nd1 O2W 2.485(3) . ?
Nd1 O13 2.511(2) . ?
Nd1 O5W 2.516(3) . ?
Nd1 O6W 2.539(3) . ?
Nd1 O3W 2.568(3) . ?
S1 O1 1.454(2) . ?
S1 O3 1.457(3) . ?
S1 O2 1.459(3) . ?
S1 C1 1.779(4) . ?
S2 O7 1.442(3) . ?
S2 O8 1.448(3) . ?
S2 O9 1.454(3) . ?
S2 C8 1.771(4) . ?
O1W H1W1 0.85(3) . ?
O1W H1W2 0.85(4) . ?
O2W H2W1 0.85(4) . ?
O2W H2W2 0.85(4) . ?
O3W H3W1 0.85(4) . ?
O3W H3W2 0.85(4) . ?
O4 C2 1.361(4) . ?
O4 H4O 0.85(4) . ?
O4W H4W1 0.85(4) . ?
O4W H4W2 0.85(4) . ?
O5W H5W1 0.85(4) . ?
O5W H5W2 0.85(4) . ?
O5 C7 1.321(5) . ?
O5 H5O 0.85(4) . ?
O6W H6W1 0.85(4) . ?
O6W H6W2 0.85(4) . ?
O6 C7 1.219(5) . ?
O7W H7W1 0.85(4) . ?
O7W H7W2 0.85(4) . ?
O8W H8W1 0.85(4) . ?
O8W H8W2 0.85(4) . ?
O9W H9W1 0.85(4) . ?
O9W H9W2 0.85(4) . ?
O10 C9 1.360(4) . ?
O10 H10O 0.85(4) . ?
O10W HAW 0.85(4) . ?
O10W HBW 0.85(4) . ?
O11 C14 1.315(5) . ?
O11 H11O 0.85(4) . ?
O12 C14 1.203(5) . ?
O13 C15 1.248(4) . ?
O14 C15 1.262(4) . ?
O14 Nd1 2.449(2) 2_666 ?
C1 C6 1.385(5) . ?
C1 C2 1.398(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.397(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.390(5) . ?
C4 C7 1.485(5) . ?
C5 C6 1.382(5) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C8 C13 1.381(5) . ?
C8 C9 1.400(5) . ?
C9 C10 1.382(5) . ?
C10 C11 1.392(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.384(5) . ?
C11 C14 1.480(5) . ?
C12 C13 1.390(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C15 1.539(6) 2_666 ?

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
O1W Nd1 O14 76.75(10) . 2_666 ?
O1W Nd1 O4W 107.88(11) . . ?
O14 Nd1 O4W 142.67(9) 2_666 . ?
O1W Nd1 O1 72.82(9) . . ?
O14 Nd1 O1 79.29(9) 2_666 . ?
O4W Nd1 O1 137.96(9) . . ?
O1W Nd1 O2W 67.01(10) . . ?
O14 Nd1 O2W 77.78(10) 2_666 . ?
O4W Nd1 O2W 70.90(10) . . ?
O1 Nd1 O2W 137.19(9) . . ?
O1W Nd1 O13 132.60(10) . . ?
O14 Nd1 O13 65.24(8) 2_666 . ?
O4W Nd1 O13 119.49(9) . . ?
O1 Nd1 O13 73.20(8) . . ?
O2W Nd1 O13 126.32(9) . . ?
O1W Nd1 O5W 71.19(11) . . ?
O14 Nd1 O5W 142.23(10) 2_666 . ?
O4W Nd1 O5W 68.42(10) . . ?
O1 Nd1 O5W 72.65(9) . . ?
O2W Nd1 O5W 106.53(10) . . ?
O13 Nd1 O5W 126.68(9) . . ?
O1W Nd1 O6W 131.28(10) . . ?
O14 Nd1 O6W 76.95(9) 2_666 . ?
O4W Nd1 O6W 72.80(10) . . ?
O1 Nd1 O6W 139.30(9) . . ?
O2W Nd1 O6W 67.78(10) . . ?
O13 Nd1 O6W 66.96(9) . . ?
O5W Nd1 O6W 140.16(9) . . ?
O1W Nd1 O3W 133.71(10) . . ?
O14 Nd1 O3W 127.96(8) 2_666 . ?
O4W Nd1 O3W 76.37(10) . . ?
O1 Nd1 O3W 74.94(9) . . ?
O2W Nd1 O3W 146.12(10) . . ?
O13 Nd1 O3W 64.32(8) . . ?
O5W Nd1 O3W 68.03(10) . . ?
O6W Nd1 O3W 94.58(10) . . ?
O1 S1 O3 112.03(15) . . ?
O1 S1 O2 112.86(16) . . ?
O3 S1 O2 113.25(16) . . ?
O1 S1 C1 105.06(16) . . ?
O3 S1 C1 105.67(17) . . ?
O2 S1 C1 107.22(16) . . ?
O7 S2 O8 111.7(2) . . ?
O7 S2 O9 112.4(2) . . ?
O8 S2 O9 111.92(18) . . ?
O7 S2 C8 107.36(19) . . ?
O8 S2 C8 107.26(19) . . ?
O9 S2 C8 105.77(17) . . ?
S1 O1 Nd1 154.93(16) . . ?
Nd1 O1W H1W1 134(3) . . ?
Nd1 O1W H1W2 116(3) . . ?
H1W1 O1W H1W2 109.6(17) . . ?
Nd1 O2W H2W1 119(3) . . ?
Nd1 O2W H2W2 120(3) . . ?
H2W1 O2W H2W2 111.6(18) . . ?
Nd1 O3W H3W1 120(3) . . ?
Nd1 O3W H3W2 101(3) . . ?
H3W1 O3W H3W2 110.9(17) . . ?
C2 O4 H4O 108(3) . . ?
Nd1 O4W H4W1 122(3) . . ?
Nd1 O4W H4W2 122(3) . . ?
H4W1 O4W H4W2 110.3(17) . . ?
Nd1 O5W H5W1 125(3) . . ?
Nd1 O5W H5W2 114(3) . . ?
H5W1 O5W H5W2 109.9(17) . . ?
C7 O5 H5O 113(3) . . ?
Nd1 O6W H6W1 124(3) . . ?
Nd1 O6W H6W2 123(3) . . ?
H6W1 O6W H6W2 112.2(18) . . ?
H7W1 O7W H7W2 110.5(17) . . ?
H8W1 O8W H8W2 109.2(17) . . ?
H9W1 O9W H9W2 109.4(17) . . ?
C9 O10 H10O 112(3) . . ?
HAW O10W HBW 111.6(18) . . ?
C14 O11 H11O 111(4) . . ?
C15 O13 Nd1 119.0(2) . . ?
C15 O14 Nd1 121.9(2) . 2_666 ?
C6 C1 C2 120.2(3) . . ?
C6 C1 S1 119.5(3) . . ?
C2 C1 S1 120.2(3) . . ?
O4 C2 C3 121.3(3) . . ?
O4 C2 C1 119.5(3) . . ?
C3 C2 C1 119.1(3) . . ?
C2 C3 C4 120.3(3) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 C7 118.9(3) . . ?
C3 C4 C7 120.9(3) . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
O6 C7 O5 123.8(4) . . ?
O6 C7 C4 122.6(4) . . ?
O5 C7 C4 113.7(3) . . ?
C13 C8 C9 119.5(4) . . ?
C13 C8 S2 119.6(3) . . ?
C9 C8 S2 120.9(3) . . ?
O10 C9 C10 122.7(3) . . ?
O10 C9 C8 118.1(3) . . ?
C10 C9 C8 119.2(3) . . ?
C9 C10 C11 121.0(4) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C12 C11 C10 119.7(4) . . ?
C12 C11 C14 118.7(3) . . ?
C10 C11 C14 121.5(3) . . ?
C11 C12 C13 119.4(4) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C8 C13 C12 121.1(4) . . ?
C8 C13 H13A 119.4 . . ?
C12 C13 H13A 119.4 . . ?
O12 C14 O11 123.5(4) . . ?
O12 C14 C11 123.4(4) . . ?
O11 C14 C11 113.1(3) . . ?
O13 C15 O14 126.2(3) . . ?
O13 C15 C15 117.9(4) . 2_666 ?
O14 C15 C15 115.9(4) . 2_666 ?

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
O3 S1 O1 Nd1 87.5(4) . . . . ?
O2 S1 O1 Nd1 -41.7(4) . . . . ?
C1 S1 O1 Nd1 -158.2(3) . . . . ?
O1W Nd1 O1 S1 -99.4(4) . . . . ?
O14 Nd1 O1 S1 -20.1(4) 2_666 . . . ?
O4W Nd1 O1 S1 162.7(3) . . . . ?
O2W Nd1 O1 S1 -78.7(4) . . . . ?
O13 Nd1 O1 S1 47.0(4) . . . . ?
O5W Nd1 O1 S1 -174.6(4) . . . . ?
O6W Nd1 O1 S1 34.9(4) . . . . ?
O3W Nd1 O1 S1 114.2(4) . . . . ?
O1W Nd1 O13 C15 -40.3(3) . . . . ?
O14 Nd1 O13 C15 -0.3(2) 2_666 . . . ?
O4W Nd1 O13 C15 137.8(3) . . . . ?
O1 Nd1 O13 C15 -86.1(3) . . . . ?
O2W Nd1 O13 C15 50.7(3) . . . . ?
O5W Nd1 O13 C15 -138.2(2) . . . . ?
O6W Nd1 O13 C15 85.4(3) . . . . ?
O3W Nd1 O13 C15 -167.1(3) . . . . ?
O1 S1 C1 C6 -119.6(3) . . . . ?
O3 S1 C1 C6 -1.0(3) . . . . ?
O2 S1 C1 C6 120.1(3) . . . . ?
O1 S1 C1 C2 58.4(3) . . . . ?
O3 S1 C1 C2 177.0(3) . . . . ?
O2 S1 C1 C2 -61.9(3) . . . . ?
C6 C1 C2 O4 178.9(3) . . . . ?
S1 C1 C2 O4 0.9(4) . . . . ?
C6 C1 C2 C3 -1.2(5) . . . . ?
S1 C1 C2 C3 -179.2(3) . . . . ?
O4 C2 C3 C4 -179.6(3) . . . . ?
C1 C2 C3 C4 0.5(5) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C2 C3 C4 C7 179.9(3) . . . . ?
C3 C4 C5 C6 0.4(5) . . . . ?
C7 C4 C5 C6 -179.6(3) . . . . ?
C4 C5 C6 C1 -1.1(5) . . . . ?
C2 C1 C6 C5 1.5(5) . . . . ?
S1 C1 C6 C5 179.5(3) . . . . ?
C5 C4 C7 O6 -2.9(5) . . . . ?
C3 C4 C7 O6 177.2(3) . . . . ?
C5 C4 C7 O5 177.4(3) . . . . ?
C3 C4 C7 O5 -2.6(5) . . . . ?
O7 S2 C8 C13 124.3(3) . . . . ?
O8 S2 C8 C13 -115.6(3) . . . . ?
O9 S2 C8 C13 4.0(4) . . . . ?
O7 S2 C8 C9 -55.8(4) . . . . ?
O8 S2 C8 C9 64.3(4) . . . . ?
O9 S2 C8 C9 -176.1(3) . . . . ?
C13 C8 C9 O10 -179.7(4) . . . . ?
S2 C8 C9 O10 0.3(5) . . . . ?
C13 C8 C9 C10 1.4(6) . . . . ?
S2 C8 C9 C10 -178.5(3) . . . . ?
O10 C9 C10 C11 -178.4(4) . . . . ?
C8 C9 C10 C11 0.3(6) . . . . ?
C9 C10 C11 C12 -1.9(6) . . . . ?
C9 C10 C11 C14 175.8(4) . . . . ?
C10 C11 C12 C13 1.5(6) . . . . ?
C14 C11 C12 C13 -176.2(4) . . . . ?
C9 C8 C13 C12 -1.8(6) . . . . ?
S2 C8 C13 C12 178.1(3) . . . . ?
C11 C12 C13 C8 0.3(6) . . . . ?
C12 C11 C14 O12 17.8(6) . . . . ?
C10 C11 C14 O12 -159.9(4) . . . . ?
C12 C11 C14 O11 -163.5(4) . . . . ?
C10 C11 C14 O11 18.8(6) . . . . ?
Nd1 O13 C15 O14 -179.1(3) . . . . ?
Nd1 O13 C15 C15 -0.1(5) . . . 2_666 ?
Nd1 O14 C15 O13 -179.7(3) 2_666 . . . ?
Nd1 O14 C15 C15 1.3(5) 2_666 . . 2_666 ?

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
O1W H1W1 O14 0.85(3) 1.886(16) 2.717(3) 165(4) 1_655
O1W H1W2 O10W 0.85(4) 1.99(2) 2.784(4) 155(4) .
O2W H2W1 O7W 0.85(4) 1.93(2) 2.737(4) 160(5) 1_655
O2W H2W2 O12 0.85(4) 2.049(17) 2.866(4) 163(5) 1_544
O3W H3W1 O8 0.85(4) 2.25(2) 2.993(4) 147(3) .
O3W H3W2 O4 0.85(4) 2.23(2) 2.998(4) 151(3) .
O4 H4O O9 0.85(4) 1.866(13) 2.704(4) 171(4) .
O4W H4W1 O9W 0.85(4) 2.063(15) 2.900(4) 168(4) .
O4W H4W2 O8W 0.85(4) 1.872(16) 2.697(5) 165(4) .
O5W H5W1 O6 0.85(4) 1.890(16) 2.724(4) 166(5) 2_777
O5W H5W2 O8W 0.85(4) 1.967(12) 2.808(5) 172(4) 2_776
O5 H5O O10W 0.85(4) 1.871(15) 2.701(4) 167(5) 2_777
O6W H6W1 O7 0.85(4) 1.957(19) 2.737(4) 154(4) 2_676
O6W H6W2 O2 0.85(4) 2.090(10) 2.931(4) 176(4) 2_666
O7W H7W1 O13 0.85(4) 2.029(12) 2.867(4) 171(4) .
O7W H7W1 O6W 0.85(4) 2.66(4) 3.139(4) 117(3) .
O7W H7W2 O7 0.85(4) 2.36(2) 3.136(5) 154(4) 2_676
O7W H7W2 O10 0.85(4) 2.40(4) 2.953(4) 124(4) 2_676
O8W H8W1 O7W 0.85(4) 1.873(16) 2.717(5) 169(6) 2_676
O8W H8W2 O7 0.85(4) 2.53(4) 3.042(5) 120(4) 2_676
O8W H8W2 O3W 0.85(4) 2.60(4) 3.256(4) 135(4) 2_676
O9W H9W1 O8 0.85(4) 1.922(12) 2.772(4) 176(4) 2_776
O9W H9W2 O6 0.85(4) 2.47(3) 3.157(4) 139(3) 1_554
O10 H10O O3 0.85(4) 1.874(12) 2.715(4) 174(5) 1_565
O10W HAW O2 0.85(4) 2.203(16) 3.018(4) 164(4) 1_655
O10W HAW O4 0.85(4) 2.65(3) 3.073(4) 113(3) 1_655
O10W HBW O12 0.85(4) 2.39(3) 3.030(4) 134(3) 2_777
O10W HBW O3 0.85(4) 2.48(2) 3.157(4) 139(3) .
O11 H11O O9W 0.85(4) 1.842(15) 2.679(4) 169(5) 1_566

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_3-Tm
_database_code_depnum_ccdc_archive 'CCDC 1549848'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H5 O6 S, H14 O11 S Tm, 3(H2 O)'
_chemical_formula_sum            'C7 H25 O20 S2 Tm'
_chemical_formula_weight         662.32

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   21.5538(13)
_cell_length_b                   7.6181(5)
_cell_length_c                   12.2261(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.022(6)
_cell_angle_gamma                90.00
_cell_volume                     1970.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1971
_cell_measurement_theta_min      3.57
_cell_measurement_theta_max      28.47

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    4.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4174
_exptl_absorpt_correction_T_max  0.5321
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5871
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.1049
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3459
_reflns_number_gt                2709
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.1364P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3459
_refine_ls_number_parameters     307
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0788
_refine_ls_wR_factor_ref         0.2142
_refine_ls_wR_factor_gt          0.1993
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.016
_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
Tm1 Tm 0.34891(2) 0.40849(7) 0.65882(5) 0.0202(3) Uani 1 1 d . . .
S1 S 0.15687(13) 0.6437(5) 0.3199(3) 0.0195(7) Uani 1 1 d . . .
S2 S 0.41105(14) 0.7966(4) 0.8092(3) 0.0257(7) Uani 1 1 d . . .
O1W O 0.4285(5) 0.4476(16) 0.5594(10) 0.040(3) Uani 1 1 d D . .
H1W1 H 0.427(7) 0.49(2) 0.496(7) 0.060 Uiso 1 1 d D . .
H1W2 H 0.460(5) 0.377(19) 0.573(12) 0.060 Uiso 1 1 d D . .
O1 O 0.2054(4) 0.5688(13) 0.2669(9) 0.032(2) Uani 1 1 d . . .
O2W O 0.4351(4) 0.2692(13) 0.7641(10) 0.038(3) Uani 1 1 d D . .
H2W1 H 0.467(4) 0.324(16) 0.749(15) 0.058 Uiso 1 1 d D . .
H2W2 H 0.446(6) 0.164(7) 0.782(15) 0.058 Uiso 1 1 d D . .
O2 O 0.1693(4) 0.8205(13) 0.3612(8) 0.033(2) Uani 1 1 d . . .
O3W O 0.3545(5) 0.1449(18) 0.5648(13) 0.069(4) Uani 1 1 d . . .
H3W1 H 0.3820 0.0910 0.6119 0.104 Uiso 1 1 d R . .
H3W2 H 0.3201 0.0873 0.5565 0.104 Uiso 1 1 d R . .
O3 O 0.1426(4) 0.5228(12) 0.4055(7) 0.027(2) Uani 1 1 d . . .
O4W O 0.3061(5) 0.2189(14) 0.7758(11) 0.052(3) Uani 1 1 d . . .
H4W1 H 0.2692 0.1754 0.7676 0.077 Uiso 1 1 d R . .
H4W2 H 0.3324 0.1351 0.7916 0.077 Uiso 1 1 d R . .
O4 O 0.1415(4) 0.8395(13) 0.1104(7) 0.025(2) Uani 1 1 d D . .
H4O H 0.137(7) 0.879(18) 0.044(4) 0.037 Uiso 1 1 d D . .
O5W O 0.2473(5) 0.3357(16) 0.5554(10) 0.050(3) Uani 1 1 d . . .
H5W1 H 0.2280 0.4158 0.5139 0.075 Uiso 1 1 d R . .
H5W2 H 0.2214 0.2520 0.5569 0.075 Uiso 1 1 d R . .
O5 O -0.0750(4) 0.7952(14) -0.1125(9) 0.037(3) Uani 1 1 d D . .
H5O H -0.110(4) 0.78(2) -0.158(11) 0.056 Uiso 1 1 d D . .
O6W O 0.3172(5) 0.6277(15) 0.5246(9) 0.037(3) Uani 1 1 d D . .
H6W1 H 0.330(7) 0.614(18) 0.464(7) 0.055 Uiso 1 1 d D . .
H6W2 H 0.293(6) 0.717(13) 0.519(11) 0.055 Uiso 1 1 d D . .
O6 O -0.1323(4) 0.6413(13) -0.0110(9) 0.035(2) Uani 1 1 d . . .
O7 O 0.4041(4) 0.6190(12) 0.7642(9) 0.030(2) Uani 1 1 d . . .
O7W O 0.2767(4) 0.5788(12) 0.7331(10) 0.032(2) Uani 1 1 d D . .
H7W1 H 0.2372(15) 0.567(15) 0.710(14) 0.049 Uiso 1 1 d D . .
H7W2 H 0.285(5) 0.686(5) 0.750(13) 0.049 Uiso 1 1 d D . .
O8 O 0.4402(5) 0.9092(13) 0.7374(13) 0.051(4) Uani 1 1 d . . .
O8W O 0.2498(4) -0.0815(11) 0.5592(9) 0.032(2) Uani 1 1 d . . .
H8W1 H 0.2329 -0.0812 0.6165 0.048 Uiso 1 1 d R . .
H8W2 H 0.2222 -0.1126 0.5033 0.048 Uiso 1 1 d R . .
O9 O 0.3477(4) 0.8655(12) 0.8188(8) 0.0237(19) Uani 1 1 d . . .
O9W O -0.1743(4) 0.6818(14) 0.2162(8) 0.035(2) Uani 1 1 d D . .
H9W1 H -0.166(7) 0.650(17) 0.154(6) 0.052 Uiso 1 1 d D . .
H9W2 H -0.188(7) 0.787(7) 0.211(11) 0.052 Uiso 1 1 d D . .
O10 O 0.4517(4) 0.7936(15) 0.9155(9) 0.044(3) Uani 1 1 d U . .
O10W O 0.5427(16) 0.549(6) 1.023(4) 0.28(2) Uani 1 1 d U . .
HAW H 0.5126 0.6230 1.0110 0.425 Uiso 1 1 d R . .
HBW H 0.5491 0.5186 1.0910 0.425 Uiso 1 1 d R . .
C1 C 0.0870(5) 0.6590(16) 0.2172(11) 0.021(3) Uani 1 1 d . . .
C2 C 0.0865(5) 0.7567(17) 0.1227(9) 0.019(3) Uani 1 1 d . . .
C3 C 0.0322(5) 0.7764(17) 0.0428(12) 0.026(3) Uani 1 1 d . . .
H3 H 0.0320 0.8469 -0.0193 0.031 Uiso 1 1 calc R . .
C4 C -0.0232(5) 0.6867(17) 0.0575(11) 0.023(3) Uani 1 1 d . . .
C5 C -0.0229(6) 0.5827(16) 0.1514(13) 0.027(3) Uani 1 1 d . . .
H5 H -0.0591 0.5219 0.1601 0.032 Uiso 1 1 calc R . .
C6 C 0.0318(5) 0.5709(15) 0.2317(12) 0.021(3) Uani 1 1 d . . .
H6 H 0.0321 0.5044 0.2956 0.025 Uiso 1 1 calc R . .
C7 C -0.0821(6) 0.7053(18) -0.0236(11) 0.025(3) 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
Tm1 O7 2.249(9) . ?
Tm1 O1W 2.303(9) . ?
Tm1 O2W 2.307(10) . ?
Tm1 O3W 2.328(12) . ?
Tm1 O7W 2.339(9) . ?
Tm1 O4W 2.342(10) . ?
Tm1 O6W 2.349(10) . ?
Tm1 O5W 2.375(10) . ?
S1 O2 1.446(10) . ?
S1 O1 1.448(9) . ?
S1 O3 1.470(9) . ?
S1 C1 1.770(12) . ?
S2 O10 1.422(10) . ?
S2 O8 1.453(12) . ?
S2 O7 1.457(9) . ?
S2 O9 1.488(8) . ?
O1W H1W1 0.85(7) . ?
O1W H1W2 0.85(7) . ?
O2W H2W1 0.85(7) . ?
O2W H2W2 0.85(7) . ?
O3W H3W1 0.8500 . ?
O3W H3W2 0.8500 . ?
O4W H4W1 0.8500 . ?
O4W H4W2 0.8501 . ?
O4 C2 1.376(13) . ?
O4 H4O 0.85(7) . ?
O5W H5W1 0.8500 . ?
O5W H5W2 0.8499 . ?
O5 C7 1.318(17) . ?
O5 H5O 0.85(7) . ?
O6W H6W1 0.85(7) . ?
O6W H6W2 0.85(7) . ?
O6 C7 1.223(15) . ?
O7W H7W1 0.85(7) . ?
O7W H7W2 0.85(7) . ?
O8W H8W1 0.8501 . ?
O8W H8W2 0.8500 . ?
O9W H9W1 0.85(7) . ?
O9W H9W2 0.85(7) . ?
O10W HAW 0.8500 . ?
O10W HBW 0.8500 . ?
C1 C2 1.372(17) . ?
C1 C6 1.406(16) . ?
C2 C3 1.382(16) . ?
C3 C4 1.417(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(19) . ?
C4 C7 1.461(17) . ?
C5 C6 1.386(19) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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
O7 Tm1 O1W 81.1(4) . . ?
O7 Tm1 O2W 74.2(4) . . ?
O1W Tm1 O2W 75.7(4) . . ?
O7 Tm1 O3W 145.7(4) . . ?
O1W Tm1 O3W 74.8(4) . . ?
O2W Tm1 O3W 76.5(5) . . ?
O7 Tm1 O7W 72.5(3) . . ?
O1W Tm1 O7W 138.7(4) . . ?
O2W Tm1 O7W 124.3(4) . . ?
O3W Tm1 O7W 140.5(3) . . ?
O7 Tm1 O4W 108.4(4) . . ?
O1W Tm1 O4W 145.3(4) . . ?
O2W Tm1 O4W 75.2(4) . . ?
O3W Tm1 O4W 80.4(5) . . ?
O7W Tm1 O4W 74.7(4) . . ?
O7 Tm1 O6W 86.8(4) . . ?
O1W Tm1 O6W 71.7(4) . . ?
O2W Tm1 O6W 144.3(4) . . ?
O3W Tm1 O6W 107.7(5) . . ?
O7W Tm1 O6W 75.6(4) . . ?
O4W Tm1 O6W 140.3(4) . . ?
O7 Tm1 O5W 143.5(4) . . ?
O1W Tm1 O5W 116.9(4) . . ?
O2W Tm1 O5W 138.8(4) . . ?
O3W Tm1 O5W 70.4(4) . . ?
O7W Tm1 O5W 73.9(4) . . ?
O4W Tm1 O5W 75.6(4) . . ?
O6W Tm1 O5W 71.3(4) . . ?
O2 S1 O1 115.0(6) . . ?
O2 S1 O3 112.6(6) . . ?
O1 S1 O3 109.8(6) . . ?
O2 S1 C1 105.2(6) . . ?
O1 S1 C1 107.3(6) . . ?
O3 S1 C1 106.3(6) . . ?
O10 S2 O8 107.4(8) . . ?
O10 S2 O7 109.3(6) . . ?
O8 S2 O7 110.3(7) . . ?
O10 S2 O9 110.3(6) . . ?
O8 S2 O9 110.4(6) . . ?
O7 S2 O9 109.1(5) . . ?
Tm1 O1W H1W1 129(9) . . ?
Tm1 O1W H1W2 117(10) . . ?
H1W1 O1W H1W2 109.8(19) . . ?
Tm1 O2W H2W1 104(10) . . ?
Tm1 O2W H2W2 136(10) . . ?
H2W1 O2W H2W2 109.6(19) . . ?
Tm1 O3W H3W1 100.2 . . ?
Tm1 O3W H3W2 112.2 . . ?
H3W1 O3W H3W2 108.1 . . ?
Tm1 O4W H4W1 129.6 . . ?
Tm1 O4W H4W2 106.2 . . ?
H4W1 O4W H4W2 107.6 . . ?
C2 O4 H4O 108(10) . . ?
Tm1 O5W H5W1 116.5 . . ?
Tm1 O5W H5W2 134.9 . . ?
H5W1 O5W H5W2 107.6 . . ?
C7 O5 H5O 105(10) . . ?
Tm1 O6W H6W1 115(8) . . ?
Tm1 O6W H6W2 136(9) . . ?
H6W1 O6W H6W2 109.2(18) . . ?
S2 O7 Tm1 152.0(6) . . ?
Tm1 O7W H7W1 121(10) . . ?
Tm1 O7W H7W2 120(9) . . ?
H7W1 O7W H7W2 109.6(19) . . ?
H8W1 O8W H8W2 108.6 . . ?
H9W1 O9W H9W2 109.2(18) . . ?
HAW O10W HBW 108.9 . . ?
C2 C1 C6 119.6(11) . . ?
C2 C1 S1 120.1(9) . . ?
C6 C1 S1 120.3(10) . . ?
C1 C2 O4 118.1(9) . . ?
C1 C2 C3 121.6(11) . . ?
O4 C2 C3 120.2(11) . . ?
C2 C3 C4 118.6(12) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 120.5(11) . . ?
C5 C4 C7 118.7(11) . . ?
C3 C4 C7 120.7(12) . . ?
C6 C5 C4 119.3(11) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 120.4(12) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O6 C7 O5 123.8(11) . . ?
O6 C7 C4 123.4(13) . . ?
O5 C7 C4 112.8(11) . . ?

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
O10 S2 O7 Tm1 150.7(13) . . . . ?
O8 S2 O7 Tm1 -91.5(15) . . . . ?
O9 S2 O7 Tm1 30.0(16) . . . . ?
O1W Tm1 O7 S2 113.1(15) . . . . ?
O2W Tm1 O7 S2 -169.4(15) . . . . ?
O3W Tm1 O7 S2 158.5(13) . . . . ?
O7W Tm1 O7 S2 -34.7(14) . . . . ?
O4W Tm1 O7 S2 -101.4(14) . . . . ?
O6W Tm1 O7 S2 41.1(15) . . . . ?
O5W Tm1 O7 S2 -10.9(18) . . . . ?
O2 S1 C1 C2 63.6(12) . . . . ?
O1 S1 C1 C2 -59.3(12) . . . . ?
O3 S1 C1 C2 -176.8(10) . . . . ?
O2 S1 C1 C6 -116.6(11) . . . . ?
O1 S1 C1 C6 120.5(11) . . . . ?
O3 S1 C1 C6 3.1(12) . . . . ?
C6 C1 C2 O4 -179.2(11) . . . . ?
S1 C1 C2 O4 0.6(17) . . . . ?
C6 C1 C2 C3 2(2) . . . . ?
S1 C1 C2 C3 -177.7(10) . . . . ?
C1 C2 C3 C4 -3(2) . . . . ?
O4 C2 C3 C4 178.9(11) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
C2 C3 C4 C7 179.0(12) . . . . ?
C3 C4 C5 C6 1(2) . . . . ?
C7 C4 C5 C6 -176.8(11) . . . . ?
C4 C5 C6 C1 -2(2) . . . . ?
C2 C1 C6 C5 -0.1(19) . . . . ?
S1 C1 C6 C5 -180.0(10) . . . . ?
C5 C4 C7 O6 4(2) . . . . ?
C3 C4 C7 O6 -174.5(13) . . . . ?
C5 C4 C7 O5 -175.0(12) . . . . ?
C3 C4 C7 O5 6.8(18) . . . . ?

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
O1W H1W1 O10 0.85(7) 2.02(11) 2.752(15) 144(17) 4_575
O1W H1W2 O10 0.85(7) 1.99(7) 2.800(14) 158(16) 2_646
O2W H2W1 O8 0.85(7) 2.08(6) 2.894(16) 159(15) 2_646
O2W H2W2 O8 0.85(7) 2.01(10) 2.766(16) 148(17) 1_545
O3W H3W1 O8 0.85 2.26 3.10(2) 168.9 1_545
O3W H3W1 O2W 0.85 2.41 2.870(17) 114.7 .
O3W H3W2 O8W 0.85 1.99 2.830(15) 168.3 .
O4W H4W1 O1 0.85 2.31 3.073(13) 149.0 4_566
O4W H4W1 O9W 0.85 2.36 2.961(14) 128.2 3_566
O4W H4W2 O9 0.85 2.10 2.854(14) 148.1 1_545
O4 H4O O3 0.85(7) 1.88(3) 2.721(13) 169(14) 4_575
O5W H5W1 O3 0.85 2.21 2.984(14) 151.7 .
O5W H5W2 O6 0.85 2.07 2.849(13) 151.3 2_545
O5W H5W2 O8W 0.85 2.61 3.179(15) 125.2 .
O5 H5O O9W 0.85(7) 1.88(6) 2.699(13) 161(17) 4_575
O6W H6W1 O9 0.85(7) 1.89(4) 2.720(14) 166(12) 4_575
O6W H6W2 O8W 0.85(7) 1.91(5) 2.725(13) 161(13) 1_565
O7W H7W1 O4 0.85(7) 2.30(7) 3.077(13) 152(13) 4_576
O7W H7W1 O9W 0.85(7) 2.59(13) 3.119(14) 121(12) 3_566
O7W H7W2 O9 0.85(7) 1.99(6) 2.756(13) 149(11) .
O7W H7W2 O1 0.85(7) 2.58(10) 3.161(13) 127(10) 4_576
O8W H8W1 O1 0.85 2.04 2.883(15) 171.3 4_566
O8W H8W2 O2 0.85 1.95 2.797(14) 171.0 1_545
O9W H9W1 O6 0.85(7) 2.27(5) 3.097(15) 164(14) .
O9W H9W1 O2 0.85(7) 2.51(13) 2.920(14) 110(11) 2_545
O9W H9W2 O1 0.85(7) 2.21(4) 3.039(15) 166(15) 2
O9W H9W2 O3 0.85(7) 2.60(12) 3.133(14) 122(11) 2
O10W HAW O10 0.85 2.05 2.84(4) 154.6 .
O10W HBW O7 0.85 2.14 2.93(4) 155.2 3_667
O10W HBW O2W 0.85 2.37 2.91(5) 121.2 3_667

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         5.274
_refine_diff_density_min         -4.104
_refine_diff_density_rms         0.364
####################################################################### 
# 
# 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_3-Yb
_database_code_depnum_ccdc_archive 'CCDC 1549849'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H5 O6 S, H14 O11 S Yb, 3(H2 O)'
_chemical_formula_sum            'C7 H25 O20 S2 Yb'
_chemical_formula_weight         666.43

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   21.5318(10)
_cell_length_b                   7.5936(3)
_cell_length_c                   12.2444(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.940(5)
_cell_angle_gamma                90.00
_cell_volume                     1965.61(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2579
_cell_measurement_theta_min      3.68
_cell_measurement_theta_max      29.18

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    5.069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4158
_exptl_absorpt_correction_T_max  0.4976
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7303
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4491
_reflns_number_gt                3854
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0399P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4491
_refine_ls_number_parameters     307
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.002
_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
Yb1 Yb 0.650998(12) 0.59098(3) 0.34156(2) 0.01992(10) Uani 1 1 d . . .
S1 S 0.84314(7) 0.35705(19) 0.68034(11) 0.0197(3) Uani 1 1 d . . .
S2 S 0.58917(7) 0.20316(19) 0.19119(13) 0.0244(3) Uani 1 1 d . . .
O1W O 0.5655(2) 0.7289(6) 0.2343(5) 0.0399(12) Uani 1 1 d D . .
H1W1 H 0.5297(16) 0.679(8) 0.216(7) 0.060 Uiso 1 1 d D . .
H1W2 H 0.561(3) 0.8396(18) 0.227(7) 0.060 Uiso 1 1 d D . .
O1 O 0.8306(2) 0.1801(6) 0.6380(3) 0.0307(10) Uani 1 1 d . . .
O2W O 0.5719(2) 0.5533(7) 0.4412(4) 0.0360(11) Uani 1 1 d D . .
H2W1 H 0.540(2) 0.621(7) 0.428(6) 0.054 Uiso 1 1 d D . .
H2W2 H 0.564(3) 0.465(6) 0.479(6) 0.054 Uiso 1 1 d D . .
O2 O 0.7941(2) 0.4286(5) 0.7331(4) 0.0300(10) Uani 1 1 d . . .
O3W O 0.6450(3) 0.8539(7) 0.4340(6) 0.0647(18) Uani 1 1 d . . .
H3W1 H 0.6793 0.9124 0.4427 0.097 Uiso 1 1 d R . .
H3W2 H 0.6172 0.9091 0.3880 0.097 Uiso 1 1 d R . .
O3 O 0.8572(2) 0.4770(5) 0.5944(3) 0.0254(9) Uani 1 1 d . . .
O4W O 0.7537(3) 0.6621(7) 0.4453(4) 0.0479(14) Uani 1 1 d D . .
H4W1 H 0.774(3) 0.758(6) 0.444(6) 0.072 Uiso 1 1 d D . .
H4W2 H 0.769(4) 0.605(8) 0.504(4) 0.072 Uiso 1 1 d D . .
O4 O 0.8590(2) 0.1607(6) 0.8898(3) 0.0269(9) Uani 1 1 d D . .
H4O H 0.863(4) 0.112(8) 0.953(3) 0.040 Uiso 1 1 d D . .
O5W O 0.6829(3) 0.3753(6) 0.4739(4) 0.0358(12) Uani 1 1 d D . .
H5W1 H 0.700(3) 0.281(5) 0.457(5) 0.054 Uiso 1 1 d D . .
H5W2 H 0.669(4) 0.360(8) 0.533(4) 0.054 Uiso 1 1 d D . .
O5 O 1.0756(2) 0.2027(7) 1.1122(4) 0.0343(11) Uani 1 1 d D . .
H5O H 1.1120(15) 0.200(11) 1.153(5) 0.051 Uiso 1 1 d D . .
O6W O 0.7237(2) 0.4248(5) 0.2665(4) 0.0350(12) Uani 1 1 d . . .
H6W1 H 0.7606 0.3954 0.2993 0.053 Uiso 1 1 d R . .
H6W2 H 0.7037 0.3322 0.2418 0.053 Uiso 1 1 d R . .
O6 O 1.1325(2) 0.3574(6) 1.0119(4) 0.0339(10) Uani 1 1 d . . .
O7 O 0.5961(2) 0.3802(5) 0.2367(4) 0.0308(10) Uani 1 1 d . . .
O7W O 0.6934(3) 0.7788(6) 0.2258(5) 0.0497(15) Uani 1 1 d D . .
H7W1 H 0.7288(19) 0.782(10) 0.204(7) 0.075 Uiso 1 1 d D . .
H7W2 H 0.671(3) 0.865(8) 0.198(7) 0.075 Uiso 1 1 d D . .
O8 O 0.5598(3) 0.0913(6) 0.2644(6) 0.0539(17) Uani 1 1 d . . .
O8W O 0.7495(2) 1.0791(5) 0.4410(3) 0.0310(11) Uani 1 1 d GD . .
H8W1 H 0.7662 1.0657 0.3840 0.046 Uiso 1 1 d GD . .
H8W2 H 0.7777 1.1091 0.4961 0.046 Uiso 1 1 d GD . .
O9 O 0.5483(2) 0.2096(7) 0.0817(4) 0.0462(13) Uani 1 1 d . . .
O9W O 0.8260(2) 0.6816(5) 0.2152(3) 0.0322(10) Uani 1 1 d GD . .
H9W1 H 0.8320 0.7306 0.1557 0.048 Uiso 1 1 d GD . .
H9W2 H 0.8005 0.5959 0.1991 0.048 Uiso 1 1 d GD . .
O10 O 0.6520(2) 0.1327(5) 0.1821(4) 0.0271(9) Uani 1 1 d . . .
O10W O 0.5403(6) 0.945(2) 0.5127(16) 0.253(9) Uani 1 1 d . . .
C1 C 0.9130(3) 0.3427(7) 0.7822(4) 0.0199(12) Uani 1 1 d . . .
C2 C 0.9128(3) 0.2413(7) 0.8781(4) 0.0199(12) Uani 1 1 d . . .
C3 C 0.9683(3) 0.2277(7) 0.9562(4) 0.0205(12) Uani 1 1 d . . .
H3 H 0.9690 0.1604 1.0199 0.025 Uiso 1 1 calc R . .
C4 C 1.0221(3) 0.3129(7) 0.9404(5) 0.0197(11) Uani 1 1 d . . .
C5 C 1.0225(3) 0.4159(7) 0.8474(5) 0.0259(14) Uani 1 1 d . . .
H5 H 1.0592 0.4740 0.8379 0.031 Uiso 1 1 calc R . .
C6 C 0.9677(3) 0.4308(7) 0.7691(5) 0.0221(12) Uani 1 1 d . . .
H6 H 0.9672 0.5008 0.7066 0.027 Uiso 1 1 calc R . .
C7 C 1.0823(3) 0.2957(7) 1.0242(5) 0.0229(12) 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
Yb1 O7 2.243(4) . ?
Yb1 O2W 2.294(4) . ?
Yb1 O1W 2.300(5) . ?
Yb1 O3W 2.311(5) . ?
Yb1 O5W 2.314(4) . ?
Yb1 O7W 2.317(5) . ?
Yb1 O6W 2.331(4) . ?
Yb1 O4W 2.393(5) . ?
Yb1 H3W1 2.7521 . ?
Yb1 H3W2 2.6162 . ?
Yb1 H6W2 2.6768 . ?
S1 O2 1.445(4) . ?
S1 O1 1.447(4) . ?
S1 O3 1.466(4) . ?
S1 C1 1.765(6) . ?
S2 O7 1.452(4) . ?
S2 O9 1.458(5) . ?
S2 O8 1.463(5) . ?
S2 O10 1.478(4) . ?
O1W H1W1 0.85(6) . ?
O1W H1W2 0.85(6) . ?
O2W H2W1 0.85(6) . ?
O2W H2W2 0.85(6) . ?
O3W H3W1 0.8498 . ?
O3W H3W2 0.8500 . ?
O4W H4W1 0.85(6) . ?
O4W H4W2 0.85(6) . ?
O4 C2 1.341(7) . ?
O4 H4O 0.85(5) . ?
O5W H5W1 0.85(6) . ?
O5W H5W2 0.85(6) . ?
O5 C7 1.318(7) . ?
O5 H5O 0.85(3) . ?
O6W H6W1 0.8499 . ?
O6W H6W2 0.8500 . ?
O6 C7 1.213(7) . ?
O7W H7W1 0.85(6) . ?
O7W H7W2 0.85(6) . ?
O8W H8W1 0.8502 . ?
O8W H8W2 0.8499 . ?
O9W H9W1 0.8498 . ?
O9W H9W2 0.8500 . ?
C1 C6 1.390(8) . ?
C1 C2 1.404(8) . ?
C2 C3 1.385(8) . ?
C3 C4 1.373(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(8) . ?
C4 C7 1.499(8) . ?
C5 C6 1.378(9) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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
O7 Yb1 O2W 81.46(18) . . ?
O7 Yb1 O1W 73.77(17) . . ?
O2W Yb1 O1W 76.43(17) . . ?
O7 Yb1 O3W 145.56(18) . . ?
O2W Yb1 O3W 74.4(2) . . ?
O1W Yb1 O3W 76.9(2) . . ?
O7 Yb1 O5W 87.12(18) . . ?
O2W Yb1 O5W 72.00(17) . . ?
O1W Yb1 O5W 145.14(18) . . ?
O3W Yb1 O5W 107.8(2) . . ?
O7 Yb1 O7W 108.4(2) . . ?
O2W Yb1 O7W 145.18(18) . . ?
O1W Yb1 O7W 74.7(2) . . ?
O3W Yb1 O7W 80.4(2) . . ?
O5W Yb1 O7W 139.9(2) . . ?
O7 Yb1 O6W 73.04(16) . . ?
O2W Yb1 O6W 139.85(16) . . ?
O1W Yb1 O6W 123.09(19) . . ?
O3W Yb1 O6W 139.90(17) . . ?
O5W Yb1 O6W 76.16(16) . . ?
O7W Yb1 O6W 73.72(18) . . ?
O7 Yb1 O4W 142.95(19) . . ?
O2W Yb1 O4W 116.8(2) . . ?
O1W Yb1 O4W 139.36(17) . . ?
O3W Yb1 O4W 71.1(2) . . ?
O5W Yb1 O4W 70.54(19) . . ?
O7W Yb1 O4W 75.8(2) . . ?
O6W Yb1 O4W 73.1(2) . . ?
O7 Yb1 H3W1 159.7 . . ?
O2W Yb1 H3W1 89.7 . . ?
O1W Yb1 H3W1 86.4 . . ?
O3W Yb1 H3W1 16.6 . . ?
O5W Yb1 H3W1 107.6 . . ?
O7W Yb1 H3W1 69.5 . . ?
O6W Yb1 H3W1 123.4 . . ?
O4W Yb1 H3W1 57.2 . . ?
O7 Yb1 H3W2 130.2 . . ?
O2W Yb1 H3W2 74.6 . . ?
O1W Yb1 H3W2 58.6 . . ?
O3W Yb1 H3W2 18.6 . . ?
O5W Yb1 H3W2 124.0 . . ?
O7W Yb1 H3W2 73.9 . . ?
O6W Yb1 H3W2 145.2 . . ?
O4W Yb1 H3W2 86.7 . . ?
H3W1 Yb1 H3W2 29.6 . . ?
O7 Yb1 H6W2 55.8 . . ?
O2W Yb1 H6W2 125.0 . . ?
O1W Yb1 H6W2 115.8 . . ?
O3W Yb1 H6W2 157.8 . . ?
O5W Yb1 H6W2 72.8 . . ?
O7W Yb1 H6W2 85.5 . . ?
O6W Yb1 H6W2 17.9 . . ?
O4W Yb1 H6W2 88.8 . . ?
H3W1 Yb1 H6W2 141.2 . . ?
H3W2 Yb1 H6W2 159.5 . . ?
O2 S1 O1 114.0(3) . . ?
O2 S1 O3 110.8(2) . . ?
O1 S1 O3 111.7(2) . . ?
O2 S1 C1 107.7(3) . . ?
O1 S1 C1 105.8(3) . . ?
O3 S1 C1 106.3(3) . . ?
O7 S2 O9 108.8(3) . . ?
O7 S2 O8 109.1(3) . . ?
O9 S2 O8 109.1(4) . . ?
O7 S2 O10 109.6(3) . . ?
O9 S2 O10 110.1(3) . . ?
O8 S2 O10 110.1(3) . . ?
Yb1 O1W H1W1 122(5) . . ?
Yb1 O1W H1W2 125(5) . . ?
H1W1 O1W H1W2 109.5(18) . . ?
Yb1 O2W H2W1 119(4) . . ?
Yb1 O2W H2W2 129(4) . . ?
H2W1 O2W H2W2 110.0(18) . . ?
Yb1 O3W H3W1 112.6 . . ?
Yb1 O3W H3W2 101.5 . . ?
H3W1 O3W H3W2 108.1 . . ?
Yb1 O4W H4W1 127(5) . . ?
Yb1 O4W H4W2 121(5) . . ?
H4W1 O4W H4W2 109.7(18) . . ?
C2 O4 H4O 111(5) . . ?
Yb1 O5W H5W1 121(4) . . ?
Yb1 O5W H5W2 126(4) . . ?
H5W1 O5W H5W2 109.5(18) . . ?
C7 O5 H5O 106(5) . . ?
Yb1 O6W H6W1 126.5 . . ?
Yb1 O6W H6W2 104.7 . . ?
H6W1 O6W H6W2 108.5 . . ?
S2 O7 Yb1 152.3(3) . . ?
Yb1 O7W H7W1 133(5) . . ?
Yb1 O7W H7W2 117(5) . . ?
H7W1 O7W H7W2 109.4(18) . . ?
H8W1 O8W H8W2 109.5 . . ?
H9W1 O9W H9W2 109.5 . . ?
C6 C1 C2 119.8(5) . . ?
C6 C1 S1 121.0(4) . . ?
C2 C1 S1 119.2(4) . . ?
O4 C2 C3 122.7(5) . . ?
O4 C2 C1 118.6(5) . . ?
C3 C2 C1 118.7(5) . . ?
C4 C3 C2 120.5(5) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.4(5) . . ?
C3 C4 C7 120.4(5) . . ?
C5 C4 C7 118.2(5) . . ?
C6 C5 C4 118.7(6) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 120.9(5) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O6 C7 O5 123.1(6) . . ?
O6 C7 C4 123.8(6) . . ?
O5 C7 C4 113.1(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
O9 S2 O7 Yb1 -149.0(6) . . . . ?
O8 S2 O7 Yb1 92.0(7) . . . . ?
O10 S2 O7 Yb1 -28.6(7) . . . . ?
O2W Yb1 O7 S2 -114.0(7) . . . . ?
O1W Yb1 O7 S2 167.7(7) . . . . ?
O3W Yb1 O7 S2 -159.6(6) . . . . ?
O5W Yb1 O7 S2 -41.8(7) . . . . ?
O7W Yb1 O7 S2 100.4(7) . . . . ?
O6W Yb1 O7 S2 34.6(6) . . . . ?
O4W Yb1 O7 S2 9.9(8) . . . . ?
O2 S1 C1 C6 -121.1(5) . . . . ?
O1 S1 C1 C6 116.7(5) . . . . ?
O3 S1 C1 C6 -2.2(5) . . . . ?
O2 S1 C1 C2 58.6(5) . . . . ?
O1 S1 C1 C2 -63.7(5) . . . . ?
O3 S1 C1 C2 177.4(4) . . . . ?
C6 C1 C2 O4 178.6(5) . . . . ?
S1 C1 C2 O4 -1.1(7) . . . . ?
C6 C1 C2 C3 -1.8(8) . . . . ?
S1 C1 C2 C3 178.6(4) . . . . ?
O4 C2 C3 C4 -180.0(5) . . . . ?
C1 C2 C3 C4 0.4(9) . . . . ?
C2 C3 C4 C5 0.8(9) . . . . ?
C2 C3 C4 C7 -179.0(5) . . . . ?
C3 C4 C5 C6 -0.7(9) . . . . ?
C7 C4 C5 C6 179.2(5) . . . . ?
C4 C5 C6 C1 -0.7(9) . . . . ?
C2 C1 C6 C5 2.0(8) . . . . ?
S1 C1 C6 C5 -178.4(4) . . . . ?
C3 C4 C7 O6 174.9(6) . . . . ?
C5 C4 C7 O6 -5.0(9) . . . . ?
C3 C4 C7 O5 -3.7(8) . . . . ?
C5 C4 C7 O5 176.5(5) . . . . ?

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
O1W H1W1 O8 0.85(6) 2.10(4) 2.896(8) 157(8) 2_655
O1W H1W2 O8 0.85(6) 1.97(3) 2.783(7) 161(8) 1_565
O2W H2W1 O9 0.85(6) 2.00(3) 2.812(7) 160(6) 2_655
O2W H2W2 O9 0.85(6) 1.902(17) 2.745(6) 172(8) 4_566
O3W H3W1 O8W 0.85 1.98 2.814(7) 168.9 .
O3W H3W2 O8 0.85 2.24 3.079(9) 168.5 1_565
O3W H3W2 O1W 0.85 2.42 2.867(8) 113.5 .
O4W H4W1 O6 0.85(6) 2.13(5) 2.827(7) 139(7) 2_756
O4W H4W1 O8W 0.85(6) 2.49(6) 3.168(6) 138(8) .
O4W H4W2 O3 0.85(6) 2.23(6) 2.955(7) 144(8) .
O4 H4O O3 0.85(5) 1.885(18) 2.722(5) 170(8) 4_566
O5W H5W1 O8W 0.85(6) 1.894(17) 2.738(6) 171(8) 1_545
O5W H5W2 O10 0.85(6) 1.92(2) 2.755(6) 166(8) 4_566
O5 H5O O9W 0.85(3) 1.9(2) 2.7(3) 159(13) 2_746
O6W H6W1 O4 0.85 2.24 3.086(6) 175.6 4_565
O6W H6W2 O10 0.85 1.94 2.787(6) 175.4 .
O7W H7W1 O9W 0.85(6) 2.21(4) 2.975(7) 150(7) .
O7W H7W1 O2 0.85(6) 2.59(8) 3.093(7) 119(7) 4_575
O7W H7W2 O10 0.85(6) 2.08(5) 2.851(7) 151(9) 1_565
O8W H8W1 O2 0.85 2.05 2.886(6) 168.5 4_575
O8W H8W2 O1 0.85 1.96 2.803(6) 169.9 1_565
O9W H9W1 O6 0.85 2.42 3.092(6) 137.0 3_766
O9W H9W1 O3 0.85 2.44 3.120(6) 137.9 4_575
O9W H9W2 O1 0.85 2.36 2.912(6) 123.3 4_565
O9W H9W2 O6W 0.85 2.37 3.095(6) 143.3 .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.185
####################################################################### 
# 
# 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_3-Er
_database_code_depnum_ccdc_archive 'CCDC 1549847'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H5 O6 S, Er H14 O11 S, 3(H2 O)'
_chemical_formula_sum            'C7 H25 Er O20 S2'
_chemical_formula_weight         660.65

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   21.6150(9)
_cell_length_b                   7.6224(3)
_cell_length_c                   12.2659(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.123(5)
_cell_angle_gamma                90.00
_cell_volume                     1982.95(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2355
_cell_measurement_theta_min      3.87
_cell_measurement_theta_max      29.30

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1308
_exptl_absorpt_coefficient_mu    4.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4349
_exptl_absorpt_correction_T_max  0.5491
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6978
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4530
_reflns_number_gt                3750
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0326P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4530
_refine_ls_number_parameters     325
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.039
_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
Er1 Er 0.651043(11) 0.59262(3) 0.34044(2) 0.01891(9) Uani 1 1 d . . .
S1 S 0.84330(6) 0.35671(18) 0.67930(11) 0.0189(3) Uani 1 1 d . . .
S2 S 0.58910(6) 0.20379(18) 0.18999(12) 0.0235(3) Uani 1 1 d . . .
O1 O 0.79455(18) 0.4294(5) 0.7324(3) 0.0298(10) Uani 1 1 d . . .
O1W O 0.7538(2) 0.6645(7) 0.4452(4) 0.0443(12) Uani 1 1 d D . .
H1W1 H 0.775(3) 0.758(5) 0.442(6) 0.066 Uiso 1 1 d D . .
H1W2 H 0.774(3) 0.597(7) 0.495(5) 0.066 Uiso 1 1 d D . .
O2 O 0.83065(19) 0.1799(5) 0.6379(3) 0.0308(9) Uani 1 1 d . . .
O2W O 0.6927(2) 0.7824(6) 0.2222(5) 0.0480(14) Uani 1 1 d D . .
H2W1 H 0.7294(15) 0.776(9) 0.207(6) 0.072 Uiso 1 1 d D . .
H2W2 H 0.674(3) 0.873(7) 0.191(6) 0.072 Uiso 1 1 d D . .
O3 O 0.85727(18) 0.4763(5) 0.5933(3) 0.0251(9) Uani 1 1 d . . .
O3W O 0.72376(19) 0.4237(6) 0.2651(4) 0.0363(11) Uani 1 1 d D . .
H3W1 H 0.7631(7) 0.435(8) 0.271(5) 0.054 Uiso 1 1 d D . .
H3W2 H 0.709(2) 0.345(7) 0.219(5) 0.054 Uiso 1 1 d D . .
O4W O 0.6829(2) 0.3739(6) 0.4731(4) 0.0336(10) Uani 1 1 d D . .
H4W1 H 0.670(3) 0.361(7) 0.534(3) 0.050 Uiso 1 1 d D . .
H4W2 H 0.704(3) 0.283(5) 0.461(5) 0.050 Uiso 1 1 d D . .
O4 O 0.85888(17) 0.1620(6) 0.8892(3) 0.0256(9) Uani 1 1 d D . .
H4O H 0.867(3) 0.107(7) 0.950(3) 0.038 Uiso 1 1 d D . .
O5 O 1.07572(18) 0.2034(6) 1.1116(3) 0.0332(10) Uani 1 1 d D . .
H5O H 1.1093(18) 0.193(10) 1.160(4) 0.050 Uiso 1 1 d D . .
O5W O 0.6457(2) 0.8591(7) 0.4324(6) 0.0666(19) Uani 1 1 d D . .
H5W1 H 0.676(2) 0.930(8) 0.449(8) 0.100 Uiso 1 1 d D . .
H5W2 H 0.613(2) 0.915(9) 0.404(8) 0.100 Uiso 1 1 d D . .
O6 O 1.13218(18) 0.3583(6) 1.0124(4) 0.0335(10) Uani 1 1 d . . .
O6W O 0.57214(19) 0.5551(6) 0.4418(4) 0.0351(11) Uani 1 1 d D . .
H6W1 H 0.571(3) 0.467(6) 0.484(5) 0.053 Uiso 1 1 d D . .
H6W2 H 0.5349(11) 0.592(8) 0.419(5) 0.053 Uiso 1 1 d D . .
O7 O 0.59522(18) 0.3817(5) 0.2347(4) 0.0293(10) Uani 1 1 d . . .
O7W O 0.5640(2) 0.7302(6) 0.2331(4) 0.0392(11) Uani 1 1 d D . .
H7W1 H 0.559(3) 0.8408(18) 0.237(6) 0.059 Uiso 1 1 d D . .
H7W2 H 0.5279(14) 0.682(7) 0.212(6) 0.059 Uiso 1 1 d D . .
O8 O 0.65215(18) 0.1343(5) 0.1817(4) 0.0297(10) Uani 1 1 d . . .
O8W O 0.8260(2) -0.1836(6) 0.7153(4) 0.0324(10) Uani 1 1 d D . .
H8W1 H 0.832(3) -0.076(2) 0.702(4) 0.049 Uiso 1 1 d D . .
H8W2 H 0.821(3) -0.243(6) 0.656(3) 0.049 Uiso 1 1 d D . .
O9 O 0.5487(2) 0.2080(6) 0.0802(4) 0.0460(12) Uani 1 1 d . . .
O9W O 0.75011(18) 0.4199(5) 0.9395(3) 0.0299(9) Uani 1 1 d . . .
H9W1 H 0.7671 0.4197 0.8825 0.045 Uiso 1 1 d R . .
H9W2 H 0.7776 0.3891 0.9955 0.045 Uiso 1 1 d R . .
O10 O 0.5599(2) 0.0916(6) 0.2640(5) 0.0515(14) Uani 1 1 d . . .
O10W O 0.5393(6) 0.955(2) 0.5026(16) 0.315(11) Uani 1 1 d . . .
HAW H 0.5543 1.0412 0.5428 0.473 Uiso 1 1 d R . .
HBW H 0.5393 0.8668 0.5454 0.473 Uiso 1 1 d R . .
C1 C 0.9130(2) 0.3425(7) 0.7816(4) 0.0158(10) Uani 1 1 d . . .
C2 C 0.9131(2) 0.2423(7) 0.8768(4) 0.0187(11) Uani 1 1 d . . .
C3 C 0.9681(2) 0.2268(7) 0.9554(4) 0.0202(11) Uani 1 1 d . . .
H3 H 0.9687 0.1585 1.0184 0.024 Uiso 1 1 calc R . .
C4 C 1.0226(2) 0.3134(7) 0.9403(4) 0.0193(11) Uani 1 1 d . . .
C5 C 1.0222(2) 0.4171(7) 0.8472(5) 0.0213(12) Uani 1 1 d . . .
H5A H 1.0584 0.4768 0.8383 0.026 Uiso 1 1 calc R . .
C6 C 0.9677(3) 0.4309(7) 0.7680(5) 0.0223(12) Uani 1 1 d . . .
H6 H 0.9673 0.4995 0.7052 0.027 Uiso 1 1 calc R . .
C7 C 1.0824(2) 0.2940(7) 1.0239(5) 0.0220(12) 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
Er1 O7 2.262(4) . ?
Er1 O6W 2.314(4) . ?
Er1 O7W 2.328(4) . ?
Er1 O5W 2.337(5) . ?
Er1 O4W 2.338(4) . ?
Er1 O2W 2.348(4) . ?
Er1 O3W 2.354(4) . ?
Er1 O1W 2.405(4) . ?
S1 O2 1.448(4) . ?
S1 O1 1.451(4) . ?
S1 O3 1.469(4) . ?
S1 C1 1.769(5) . ?
S2 O9 1.457(5) . ?
S2 O7 1.459(4) . ?
S2 O10 1.475(5) . ?
S2 O8 1.484(4) . ?
O1W H1W1 0.85(6) . ?
O1W H1W2 0.85(6) . ?
O2W H2W1 0.85(6) . ?
O2W H2W2 0.85(6) . ?
O3W H3W1 0.85(6) . ?
O3W H3W2 0.85(6) . ?
O4W H4W1 0.85(6) . ?
O4W H4W2 0.85(6) . ?
O4 C2 1.357(6) . ?
O4 H4O 0.85(5) . ?
O5 C7 1.310(7) . ?
O5 H5O 0.85(6) . ?
O5W H5W1 0.85(6) . ?
O5W H5W2 0.85(6) . ?
O6 C7 1.215(6) . ?
O6W H6W1 0.85(6) . ?
O6W H6W2 0.85(6) . ?
O7W H7W1 0.85(6) . ?
O7W H7W2 0.85(6) . ?
O8W H8W1 0.85(6) . ?
O8W H8W2 0.85(6) . ?
O9W H9W1 0.8500 . ?
O9W H9W2 0.8500 . ?
O10W HAW 0.8499 . ?
O10W HBW 0.8500 . ?
C1 C2 1.395(7) . ?
C1 C6 1.398(7) . ?
C2 C3 1.383(7) . ?
C3 C4 1.393(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(7) . ?
C4 C7 1.494(7) . ?
C5 C6 1.379(8) . ?
C5 H5A 0.9300 . ?
C6 H6 0.9300 . ?

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
O7 Er1 O6W 81.55(16) . . ?
O7 Er1 O7W 73.28(16) . . ?
O6W Er1 O7W 76.13(16) . . ?
O7 Er1 O5W 145.48(17) . . ?
O6W Er1 O5W 74.83(19) . . ?
O7W Er1 O5W 76.8(2) . . ?
O7 Er1 O4W 86.85(16) . . ?
O6W Er1 O4W 71.75(15) . . ?
O7W Er1 O4W 144.30(15) . . ?
O5W Er1 O4W 108.6(2) . . ?
O7 Er1 O2W 108.04(18) . . ?
O6W Er1 O2W 144.94(16) . . ?
O7W Er1 O2W 74.80(17) . . ?
O5W Er1 O2W 79.8(2) . . ?
O4W Er1 O2W 140.57(17) . . ?
O7 Er1 O3W 73.08(15) . . ?
O6W Er1 O3W 139.49(16) . . ?
O7W Er1 O3W 123.54(18) . . ?
O5W Er1 O3W 139.77(16) . . ?
O4W Er1 O3W 75.74(16) . . ?
O2W Er1 O3W 74.32(17) . . ?
O7 Er1 O1W 143.48(16) . . ?
O6W Er1 O1W 116.21(18) . . ?
O7W Er1 O1W 139.66(16) . . ?
O5W Er1 O1W 70.75(19) . . ?
O4W Er1 O1W 70.91(17) . . ?
O2W Er1 O1W 76.40(19) . . ?
O3W Er1 O1W 73.54(18) . . ?
O2 S1 O1 114.1(2) . . ?
O2 S1 O3 112.1(2) . . ?
O1 S1 O3 110.7(2) . . ?
O2 S1 C1 105.6(2) . . ?
O1 S1 C1 107.4(2) . . ?
O3 S1 C1 106.4(2) . . ?
O9 S2 O7 108.8(3) . . ?
O9 S2 O10 109.3(3) . . ?
O7 S2 O10 109.0(3) . . ?
O9 S2 O8 109.9(3) . . ?
O7 S2 O8 109.9(2) . . ?
O10 S2 O8 110.0(3) . . ?
Er1 O1W H1W1 128(4) . . ?
Er1 O1W H1W2 123(4) . . ?
H1W1 O1W H1W2 109.1(18) . . ?
Er1 O2W H2W1 126(4) . . ?
Er1 O2W H2W2 124(4) . . ?
H2W1 O2W H2W2 109.6(18) . . ?
Er1 O3W H3W1 131(4) . . ?
Er1 O3W H3W2 117(4) . . ?
H3W1 O3W H3W2 111.3(18) . . ?
Er1 O4W H4W1 126(4) . . ?
Er1 O4W H4W2 123(4) . . ?
H4W1 O4W H4W2 109.4(18) . . ?
C2 O4 H4O 107(4) . . ?
C7 O5 H5O 114(5) . . ?
Er1 O5W H5W1 124(6) . . ?
Er1 O5W H5W2 111(6) . . ?
H5W1 O5W H5W2 109.6(18) . . ?
Er1 O6W H6W1 123(4) . . ?
Er1 O6W H6W2 122(4) . . ?
H6W1 O6W H6W2 109.2(18) . . ?
S2 O7 Er1 151.1(3) . . ?
Er1 O7W H7W1 121(5) . . ?
Er1 O7W H7W2 125(4) . . ?
H7W1 O7W H7W2 108.8(18) . . ?
H8W1 O8W H8W2 110.0(18) . . ?
H9W1 O9W H9W2 108.6 . . ?
HAW O10W HBW 107.4 . . ?
C2 C1 C6 119.9(5) . . ?
C2 C1 S1 119.4(4) . . ?
C6 C1 S1 120.7(4) . . ?
O4 C2 C3 121.9(5) . . ?
O4 C2 C1 118.6(5) . . ?
C3 C2 C1 119.5(5) . . ?
C2 C3 C4 120.1(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 C7 119.2(5) . . ?
C3 C4 C7 120.3(5) . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C1 120.4(5) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O6 C7 O5 123.3(5) . . ?
O6 C7 C4 123.3(5) . . ?
O5 C7 C4 113.4(4) . . ?

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
O9 S2 O7 Er1 -148.7(5) . . . . ?
O10 S2 O7 Er1 92.3(6) . . . . ?
O8 S2 O7 Er1 -28.4(6) . . . . ?
O6W Er1 O7 S2 -113.8(6) . . . . ?
O7W Er1 O7 S2 168.2(6) . . . . ?
O5W Er1 O7 S2 -160.8(5) . . . . ?
O4W Er1 O7 S2 -41.8(5) . . . . ?
O2W Er1 O7 S2 100.9(5) . . . . ?
O3W Er1 O7 S2 34.2(5) . . . . ?
O1W Er1 O7 S2 9.5(7) . . . . ?
O2 S1 C1 C2 -63.2(4) . . . . ?
O1 S1 C1 C2 58.9(5) . . . . ?
O3 S1 C1 C2 177.5(4) . . . . ?
O2 S1 C1 C6 117.0(4) . . . . ?
O1 S1 C1 C6 -120.8(4) . . . . ?
O3 S1 C1 C6 -2.3(5) . . . . ?
C6 C1 C2 O4 178.1(5) . . . . ?
S1 C1 C2 O4 -1.6(7) . . . . ?
C6 C1 C2 C3 -2.1(8) . . . . ?
S1 C1 C2 C3 178.1(4) . . . . ?
O4 C2 C3 C4 -179.1(5) . . . . ?
C1 C2 C3 C4 1.2(8) . . . . ?
C2 C3 C4 C5 0.6(8) . . . . ?
C2 C3 C4 C7 -178.8(5) . . . . ?
C3 C4 C5 C6 -1.5(8) . . . . ?
C7 C4 C5 C6 177.9(5) . . . . ?
C4 C5 C6 C1 0.6(8) . . . . ?
C2 C1 C6 C5 1.3(8) . . . . ?
S1 C1 C6 C5 -179.0(4) . . . . ?
C5 C4 C7 O6 -3.6(8) . . . . ?
C3 C4 C7 O6 175.8(5) . . . . ?
C5 C4 C7 O5 175.4(5) . . . . ?
C3 C4 C7 O5 -5.2(7) . . . . ?

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
O1W H1W1 O6 0.85(6) 2.12(4) 2.834(6) 142(6) 2_756
O1W H1W1 O9W 0.85(6) 2.52(5) 3.169(6) 134(6) 4_575
O1W H1W2 O3 0.85(6) 2.17(3) 2.965(6) 155(6) .
O2W H2W1 O8W 0.85(6) 2.19(2) 2.995(6) 158(6) 4_565
O2W H2W1 O1 0.85(6) 2.64(7) 3.095(6) 115(6) 4_575
O2W H2W2 O8 0.85(6) 2.05(4) 2.835(6) 154(8) 1_565
O3W H3W1 O4 0.85(6) 2.41(5) 3.092(6) 139(6) 4_565
O3W H3W2 O8 0.85(6) 2.02(3) 2.774(6) 148(6) .
O4W H4W1 O8 0.85(6) 1.925(17) 2.766(6) 169(7) 4_566
O4W H4W2 O9W 0.85(6) 1.892(12) 2.743(6) 178(5) 4_565
O4 H4O O3 0.85(5) 1.91(2) 2.722(5) 159(6) 4_566
O5 H5O O8W 0.85(6) 1.862(17) 2.701(6) 170(7) 3_757
O5W H5W1 O9W 0.85(6) 1.98(3) 2.803(6) 163(9) 4_575
O5W H5W2 O10W 0.85(6) 2.19(9) 2.708(12) 119(8) .
O5W H5W2 O10 0.85(6) 2.30(5) 3.060(9) 149(9) 1_565
O6W H6W1 O9 0.85(6) 1.903(19) 2.738(6) 166(5) 4_566
O6W H6W2 O9 0.85(6) 2.01(3) 2.824(6) 160(7) 2_655
O7W H7W1 O10 0.85(6) 1.941(15) 2.785(7) 171(7) 1_565
O7W H7W2 O10 0.85(6) 2.09(3) 2.885(6) 154(7) 2_655
O8W H8W1 O2 0.85(6) 2.105(19) 2.937(6) 167(6) .
O8W H8W2 O3 0.85(6) 2.45(4) 3.132(6) 137(5) 1_545
O8W H8W2 O6 0.85(6) 2.58(5) 3.113(6) 122(4) 2_746
O9W H9W1 O1 0.85 2.04 2.885(5) 171.3 .
O9W H9W2 O2 0.85 1.97 2.810(6) 171.2 4_566
O10W HAW O9 0.85 1.98 2.736(15) 148.5 4_576
O10W HAW O7 0.85 2.42 3.130(17) 141.2 4_576
O10W HBW O7W 0.85 2.38 3.11(2) 144.6 4_576

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.549
_refine_diff_density_rms         0.172
####################################################################### 
# 
# 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_3-Y
_database_code_depnum_ccdc_archive 'CCDC 1549851'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H5 O6 S, H14 O11 S Y, 3(H2 O)'
_chemical_formula_sum            'C7 H25 O20 S2 Y'
_chemical_formula_weight         582.30

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   21.6467(7)
_cell_length_b                   7.6433(3)
_cell_length_c                   12.2972(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.007(4)
_cell_angle_gamma                90.00
_cell_volume                     1997.17(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1541
_cell_measurement_theta_min      3.85
_cell_measurement_theta_max      28.76

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    3.227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5240
_exptl_absorpt_correction_T_max  0.5792
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7218
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4559
_reflns_number_gt                3435
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0518P)²+0.9096P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4559
_refine_ls_number_parameters     319
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1233
_refine_ls_wR_factor_gt          0.1119
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.031
_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
Y1 Y 0.65110(2) 1.59291(5) 1.34024(3) 0.02103(13) Uani 1 1 d . . .
S1 S 0.84356(5) 1.14325(14) 1.17958(8) 0.0210(2) Uani 1 1 d . . .
S2 S 0.58909(5) 1.20361(14) 1.18936(10) 0.0264(3) Uani 1 1 d . . .
O1 O 0.79493(15) 1.0713(4) 1.2324(3) 0.0317(8) Uani 1 1 d . . .
O1W O 0.56377(17) 1.7330(4) 1.2332(3) 0.0407(9) Uani 1 1 d D . .
H1W1 H 0.556(2) 1.841(2) 1.240(5) 0.061 Uiso 1 1 d D . .
H1W2 H 0.5297(13) 1.676(5) 1.214(5) 0.061 Uiso 1 1 d D . .
O2W O 0.57203(17) 1.5556(5) 1.4420(3) 0.0387(9) Uani 1 1 d D . .
H2W1 H 0.565(2) 1.467(5) 1.480(4) 0.058 Uiso 1 1 d D . .
H2W2 H 0.5368(12) 1.605(6) 1.417(4) 0.058 Uiso 1 1 d D . .
O2 O 0.83096(16) 1.3201(4) 1.1382(3) 0.0335(8) Uani 1 1 d . . .
O3 O 0.85760(15) 1.0245(4) 1.0936(2) 0.0289(7) Uani 1 1 d . . .
O3W O 0.6456(2) 1.8607(5) 1.4324(5) 0.0714(15) Uani 1 1 d D . .
H3W1 H 0.6094(14) 1.895(8) 1.402(7) 0.107 Uiso 1 1 d D . .
H3W2 H 0.671(2) 1.946(6) 1.444(6) 0.107 Uiso 1 1 d D . .
O4 O 0.85900(15) 1.3389(4) 1.3885(2) 0.0289(7) Uani 1 1 d D . .
H4O H 0.865(3) 1.380(6) 1.4536(17) 0.043 Uiso 1 1 d D . .
O4W O 0.75429(19) 1.6645(5) 1.4455(3) 0.0482(10) Uani 1 1 d D . .
H4W1 H 0.781(2) 1.748(5) 1.446(4) 0.072 Uiso 1 1 d D . .
H4W2 H 0.766(3) 1.603(6) 1.504(3) 0.072 Uiso 1 1 d D . .
O5W O 0.68310(18) 1.3738(4) 1.4730(3) 0.0364(8) Uani 1 1 d D . .
H5W1 H 0.704(2) 1.282(4) 1.462(4) 0.055 Uiso 1 1 d D . .
H5W2 H 0.671(3) 1.364(6) 1.535(2) 0.055 Uiso 1 1 d D . .
O5 O 1.07549(16) 1.2964(5) 1.6113(3) 0.0364(8) Uani 1 1 d D . .
H5O H 1.1099(14) 1.304(7) 1.657(4) 0.055 Uiso 1 1 d D . .
O6W O 0.72431(17) 1.4249(4) 1.2637(3) 0.0399(9) Uani 1 1 d . . .
H6W1 H 0.7609 1.3955 1.2969 0.060 Uiso 1 1 d R . .
H6W2 H 0.7042 1.3328 1.2398 0.060 Uiso 1 1 d R . .
O6 O 1.13178(16) 1.1420(4) 1.5119(3) 0.0366(8) Uani 1 1 d . . .
O7 O 0.59555(16) 1.3809(4) 1.2345(3) 0.0319(8) Uani 1 1 d . . .
O7W O 0.69296(19) 1.7833(4) 1.2216(3) 0.0526(11) Uani 1 1 d . . .
H7W1 H 0.6843 1.8906 1.2082 0.079 Uiso 1 1 d R . .
H7W2 H 0.7313 1.7662 1.2179 0.079 Uiso 1 1 d R . .
O8 O 0.5600(2) 1.0925(4) 1.2632(4) 0.0549(11) Uani 1 1 d . . .
O8W O 0.75017(16) 1.0805(4) 1.4396(3) 0.0327(8) Uani 1 1 d D . .
H8W1 H 0.7770(17) 1.110(7) 1.496(2) 0.049 Uiso 1 1 d D . .
H8W2 H 0.767(2) 1.082(7) 1.382(2) 0.049 Uiso 1 1 d D . .
O9W O 1.17334(17) 1.3159(4) 1.7837(3) 0.0340(8) Uani 1 1 d D . .
H9W1 H 1.169(3) 1.254(5) 1.839(2) 0.051 Uiso 1 1 d D . .
H9W2 H 1.178(3) 1.4219(19) 1.802(3) 0.051 Uiso 1 1 d D . .
O9 O 0.54879(19) 1.2089(5) 1.0801(3) 0.0511(11) Uani 1 1 d . . .
O10 O 0.65219(16) 1.1349(4) 1.1819(3) 0.0326(8) Uani 1 1 d . . .
O10W O 0.4591(5) 1.4519(16) 0.9996(12) 0.294(8) Uani 1 1 d . . .
HAW H 0.4443 1.5375 0.9586 0.441 Uiso 1 1 d R . .
HBW H 0.4597 1.3637 0.9577 0.441 Uiso 1 1 d R . .
C1 C 0.9135(2) 1.1570(5) 1.2816(3) 0.0191(9) Uani 1 1 d . . .
C2 C 0.9134(2) 1.2585(5) 1.3768(3) 0.0191(9) Uani 1 1 d . . .
C3 C 0.9685(2) 1.2718(5) 1.4557(3) 0.0225(9) Uani 1 1 d . . .
H3 H 0.9690 1.3380 1.5193 0.027 Uiso 1 1 calc R . .
C4 C 1.0226(2) 1.1872(5) 1.4402(3) 0.0212(9) Uani 1 1 d . . .
C5 C 1.0225(2) 1.0840(6) 1.3479(4) 0.0255(10) Uani 1 1 d . . .
H5 H 1.0588 1.0248 1.3390 0.031 Uiso 1 1 calc R . .
C6 C 0.9672(2) 1.0696(5) 1.2677(4) 0.0239(10) Uani 1 1 d . . .
H6 H 0.9667 1.0010 1.2051 0.029 Uiso 1 1 calc R . .
C7 C 1.0823(2) 1.2044(5) 1.5239(4) 0.0232(10) 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
Y1 O7 2.272(3) . ?
Y1 O2W 2.322(3) . ?
Y1 O1W 2.345(3) . ?
Y1 O5W 2.349(3) . ?
Y1 O3W 2.353(4) . ?
Y1 O7W 2.360(3) . ?
Y1 O6W 2.370(3) . ?
Y1 O4W 2.421(4) . ?
S1 O1 1.447(3) . ?
S1 O2 1.452(3) . ?
S1 O3 1.468(3) . ?
S1 C1 1.776(4) . ?
S2 O9 1.456(4) . ?
S2 O7 1.461(3) . ?
S2 O8 1.470(4) . ?
S2 O10 1.483(3) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2W H2W1 0.85(5) . ?
O2W H2W2 0.85(5) . ?
O3W H3W1 0.85(5) . ?
O3W H3W2 0.85(5) . ?
O4 C2 1.361(5) . ?
O4 H4O 0.85(4) . ?
O4W H4W1 0.85(5) . ?
O4W H4W2 0.85(5) . ?
O5W H5W1 0.85(5) . ?
O5W H5W2 0.85(5) . ?
O5 C7 1.316(5) . ?
O5 H5O 0.85(4) . ?
O6W H6W1 0.8500 . ?
O6W H6W2 0.8500 . ?
O6 C7 1.207(5) . ?
O7W H7W1 0.8501 . ?
O7W H7W2 0.8500 . ?
O8W H8W1 0.85(5) . ?
O8W H8W2 0.85(5) . ?
O9W H9W1 0.85(5) . ?
O9W H9W2 0.85(5) . ?
O10W HAW 0.8500 . ?
O10W HBW 0.8499 . ?
C1 C6 1.378(6) . ?
C1 C2 1.404(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.382(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(6) . ?
C4 C7 1.496(6) . ?
C5 C6 1.403(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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
O7 Y1 O2W 81.76(14) . . ?
O7 Y1 O1W 73.90(12) . . ?
O2W Y1 O1W 76.14(13) . . ?
O7 Y1 O5W 86.72(13) . . ?
O2W Y1 O5W 71.82(12) . . ?
O1W Y1 O5W 144.54(13) . . ?
O7 Y1 O3W 145.66(14) . . ?
O2W Y1 O3W 74.77(16) . . ?
O1W Y1 O3W 76.34(16) . . ?
O5W Y1 O3W 108.71(17) . . ?
O7 Y1 O7W 108.04(13) . . ?
O2W Y1 O7W 144.89(12) . . ?
O1W Y1 O7W 74.64(14) . . ?
O5W Y1 O7W 140.53(14) . . ?
O3W Y1 O7W 79.75(16) . . ?
O7 Y1 O6W 72.98(12) . . ?
O2W Y1 O6W 139.88(12) . . ?
O1W Y1 O6W 123.57(14) . . ?
O5W Y1 O6W 76.03(12) . . ?
O3W Y1 O6W 139.61(14) . . ?
O7W Y1 O6W 73.98(12) . . ?
O7 Y1 O4W 143.17(13) . . ?
O2W Y1 O4W 116.07(15) . . ?
O1W Y1 O4W 139.41(13) . . ?
O5W Y1 O4W 70.73(13) . . ?
O3W Y1 O4W 70.87(16) . . ?
O7W Y1 O4W 76.54(14) . . ?
O6W Y1 O4W 73.50(14) . . ?
O1 S1 O2 114.0(2) . . ?
O1 S1 O3 110.90(19) . . ?
O2 S1 O3 111.94(19) . . ?
O1 S1 C1 107.50(19) . . ?
O2 S1 C1 105.69(19) . . ?
O3 S1 C1 106.23(19) . . ?
O9 S2 O7 108.8(2) . . ?
O9 S2 O8 109.5(3) . . ?
O7 S2 O8 108.8(2) . . ?
O9 S2 O10 110.5(2) . . ?
O7 S2 O10 109.25(19) . . ?
O8 S2 O10 110.0(2) . . ?
Y1 O1W H1W1 123(3) . . ?
Y1 O1W H1W2 119(3) . . ?
H1W1 O1W H1W2 109.5(18) . . ?
Y1 O2W H2W1 128(3) . . ?
Y1 O2W H2W2 117(3) . . ?
H2W1 O2W H2W2 108.7(17) . . ?
Y1 O3W H3W1 101(5) . . ?
Y1 O3W H3W2 131(5) . . ?
H3W1 O3W H3W2 110.7(19) . . ?
C2 O4 H4O 106(4) . . ?
Y1 O4W H4W1 136(3) . . ?
Y1 O4W H4W2 115(4) . . ?
H4W1 O4W H4W2 108.1(17) . . ?
Y1 O5W H5W1 125(3) . . ?
Y1 O5W H5W2 126(3) . . ?
H5W1 O5W H5W2 108.7(17) . . ?
C7 O5 H5O 111(4) . . ?
Y1 O6W H6W1 125.9 . . ?
Y1 O6W H6W2 104.4 . . ?
H6W1 O6W H6W2 108.5 . . ?
S2 O7 Y1 151.7(2) . . ?
Y1 O7W H7W1 128.2 . . ?
Y1 O7W H7W2 115.6 . . ?
H7W1 O7W H7W2 108.6 . . ?
H8W1 O8W H8W2 110.4(18) . . ?
H9W1 O9W H9W2 110.5(18) . . ?
HAW O10W HBW 107.4 . . ?
C6 C1 C2 120.4(4) . . ?
C6 C1 S1 120.6(3) . . ?
C2 C1 S1 119.0(3) . . ?
O4 C2 C3 122.5(4) . . ?
O4 C2 C1 118.5(4) . . ?
C3 C2 C1 119.0(4) . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.8(4) . . ?
C3 C4 C7 120.5(4) . . ?
C5 C4 C7 118.7(4) . . ?
C4 C5 C6 119.3(4) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C5 120.1(4) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O6 C7 O5 123.5(4) . . ?
O6 C7 C4 123.4(4) . . ?
O5 C7 C4 113.1(4) . . ?

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
O9 S2 O7 Y1 -148.6(4) . . . . ?
O8 S2 O7 Y1 92.2(5) . . . . ?
O10 S2 O7 Y1 -27.9(5) . . . . ?
O2W Y1 O7 S2 -113.9(5) . . . . ?
O1W Y1 O7 S2 168.2(5) . . . . ?
O5W Y1 O7 S2 -41.8(5) . . . . ?
O3W Y1 O7 S2 -160.9(4) . . . . ?
O7W Y1 O7 S2 100.8(5) . . . . ?
O6W Y1 O7 S2 34.6(5) . . . . ?
O4W Y1 O7 S2 9.3(6) . . . . ?
O1 S1 C1 C6 120.8(4) . . . . ?
O2 S1 C1 C6 -117.0(4) . . . . ?
O3 S1 C1 C6 2.1(4) . . . . ?
O1 S1 C1 C2 -59.2(4) . . . . ?
O2 S1 C1 C2 62.9(4) . . . . ?
O3 S1 C1 C2 -178.0(3) . . . . ?
C6 C1 C2 O4 -178.4(4) . . . . ?
S1 C1 C2 O4 1.7(5) . . . . ?
C6 C1 C2 C3 1.1(6) . . . . ?
S1 C1 C2 C3 -178.9(3) . . . . ?
O4 C2 C3 C4 179.8(4) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C3 C4 C5 -1.8(6) . . . . ?
C2 C3 C4 C7 178.7(4) . . . . ?
C3 C4 C5 C6 1.8(6) . . . . ?
C7 C4 C5 C6 -178.7(4) . . . . ?
C2 C1 C6 C5 -1.1(6) . . . . ?
S1 C1 C6 C5 178.8(3) . . . . ?
C4 C5 C6 C1 -0.3(6) . . . . ?
C3 C4 C7 O6 -175.6(4) . . . . ?
C5 C4 C7 O6 4.9(7) . . . . ?
C3 C4 C7 O5 3.6(6) . . . . ?
C5 C4 C7 O5 -175.9(4) . . . . ?

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
O1W H1W1 O8 0.85(5) 1.945(15) 2.776(5) 165(5) 1_565
O1W H1W2 O8 0.85(5) 2.11(3) 2.894(6) 153(5) 2_657
O2W H2W1 O9 0.85(5) 1.903(14) 2.748(5) 172(6) 4_586
O2W H2W2 O9 0.85(5) 2.02(2) 2.831(5) 158(5) 2_657
O3W H3W1 O10W 0.85(5) 2.13(8) 2.655(12) 120(7) 2_657
O3W H3W1 O8 0.85(5) 2.38(5) 3.071(7) 140(7) 1_565
O3W H3W1 O1W 0.85(5) 2.45(7) 2.904(6) 114(6) .
O3W H3W2 O8W 0.85(5) 2.01(3) 2.806(6) 157(7) 1_565
O4 H4O O3 0.85(4) 1.906(17) 2.736(4) 166(5) 4_586
O4W H4W1 O6 0.85(5) 2.05(3) 2.837(5) 153(5) 3_788
O4W H4W1 O8W 0.85(5) 2.62(5) 3.181(5) 124(5) 1_565
O4W H4W2 O3 0.85(5) 2.29(4) 2.975(5) 138(5) 4_586
O5W H5W1 O8W 0.85(5) 1.887(11) 2.744(5) 179(6) .
O5W H5W2 O10 0.85(5) 1.931(13) 2.777(5) 173(6) 4_586
O5 H5O O9W 0.85(4) 1.869(18) 2.699(4) 166(6) .
O6W H6W1 O4 0.85 2.25 3.095(5) 175.7 .
O6W H6W2 O10 0.85 1.94 2.786(5) 175.3 .
O7W H7W1 O10 0.85 2.00 2.841(5) 171.9 1_565
O7W H7W2 O9W 0.85 2.16 3.005(5) 171.6 3_788
O8W H8W1 O2 0.85(5) 1.980(11) 2.823(4) 173(4) 4_586
O8W H8W2 O1 0.85(5) 2.054(12) 2.895(5) 172(4) .
O9W H9W1 O3 0.85(5) 2.40(2) 3.144(5) 148(4) 3_778
O9W H9W1 O6 0.85(5) 2.54(4) 3.123(5) 127(4) 4_586
O9W H9W2 O2 0.85(5) 2.129(19) 2.951(4) 165(5) 3_788
O10W HAW O9 0.85 2.01 2.765(11) 147.8 3_687
O10W HAW O7 0.85 2.45 3.165(13) 142.5 3_687
O10W HBW O1W 0.85 2.42 3.146(16) 143.6 3_687

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.110
####################################################################### 
# 
# 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_3-Lu
_database_code_depnum_ccdc_archive 'CCDC 1549850'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H5 O6 S, H14 Lu O11 S, 3(H2 O)'
_chemical_formula_sum            'C7 H25 Lu O20 S2'
_chemical_formula_weight         668.36

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   21.5768(6)
_cell_length_b                   7.5992(2)
_cell_length_c                   12.2880(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.920(3)
_cell_angle_gamma                90.00
_cell_volume                     1978.35(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2223
_cell_measurement_theta_min      3.66
_cell_measurement_theta_max      29.37

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    5.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4325
_exptl_absorpt_correction_T_max  0.5688
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7067
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4522
_reflns_number_gt                3796
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0357P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4522
_refine_ls_number_parameters     319
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.028
_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
Lu1 Lu 1.348952(11) 0.09011(3) 1.157871(19) 0.01939(9) Uani 1 1 d . . .
S1 S 1.15688(7) 0.64334(19) 1.31940(11) 0.0191(3) Uani 1 1 d . . .
S2 S 1.41096(7) -0.2972(2) 1.30830(12) 0.0244(3) Uani 1 1 d . . .
O1 O 1.1431(2) 0.5228(5) 1.4049(3) 0.0262(9) Uani 1 1 d . . .
O1W O 1.3066(3) 0.2786(6) 1.2733(5) 0.0468(14) Uani 1 1 d D . .
H1W1 H 1.328(3) 0.368(7) 1.299(6) 0.070 Uiso 1 1 d D . .
H1W2 H 1.2712(18) 0.279(9) 1.294(6) 0.070 Uiso 1 1 d D . .
O2W O 1.2774(2) -0.0778(6) 1.2333(4) 0.0358(11) Uani 1 1 d D . .
H2W1 H 1.284(3) -0.180(4) 1.260(6) 0.054 Uiso 1 1 d D . .
H2W2 H 1.2384(9) -0.054(8) 1.223(6) 0.054 Uiso 1 1 d D . .
O2 O 1.1695(2) 0.8203(5) 1.3604(3) 0.0309(10) Uani 1 1 d . . .
O3 O 1.2054(2) 0.5713(6) 1.2660(3) 0.0308(10) Uani 1 1 d . . .
O3W O 1.2466(2) 0.1627(7) 1.0553(4) 0.0457(13) Uani 1 1 d D . .
H3W1 H 1.226(3) 0.258(6) 1.057(6) 0.069 Uiso 1 1 d D . .
H3W2 H 1.230(3) 0.102(8) 1.000(4) 0.069 Uiso 1 1 d D . .
O4W O 1.3176(2) -0.1242(6) 1.0258(4) 0.0339(11) Uani 1 1 d D . .
H4W1 H 1.329(3) -0.126(8) 0.963(3) 0.051 Uiso 1 1 d D . .
H4W2 H 1.287(2) -0.194(8) 1.026(5) 0.051 Uiso 1 1 d D . .
O4 O 1.14149(19) 0.8395(6) 1.1099(3) 0.0270(9) Uani 1 1 d D . .
H4O H 1.143(3) 0.881(8) 1.046(2) 0.041 Uiso 1 1 d D . .
O5 O 0.9241(2) 0.7968(6) 0.8874(3) 0.0353(11) Uani 1 1 d D . .
H5O H 0.8887(17) 0.807(11) 0.844(5) 0.053 Uiso 1 1 d D . .
O5W O 1.3544(3) 0.3530(7) 1.0645(5) 0.0667(19) Uani 1 1 d . . .
H5W1 H 1.3820 0.4078 1.1106 0.100 Uiso 1 1 d R . .
H5W2 H 1.3201 0.4110 1.0562 0.100 Uiso 1 1 d R . .
O6W O 1.4278(2) 0.0529(6) 1.0579(4) 0.0355(11) Uani 1 1 d D . .
H6W1 H 1.433(3) -0.039(6) 1.021(5) 0.053 Uiso 1 1 d D . .
H6W2 H 1.460(2) 0.070(8) 1.108(4) 0.053 Uiso 1 1 d D . .
O6 O 0.8672(2) 0.6421(6) 0.9882(4) 0.0343(11) Uani 1 1 d . . .
O7W O 1.4346(2) 0.2285(6) 1.2643(4) 0.0383(11) Uani 1 1 d D . .
H7W1 H 1.4680(19) 0.170(7) 1.289(6) 0.057 Uiso 1 1 d D . .
H7W2 H 1.443(3) 0.338(2) 1.271(6) 0.057 Uiso 1 1 d D . .
O7 O 1.4043(2) -0.1199(5) 1.2628(4) 0.0292(10) Uani 1 1 d . . .
O8 O 1.4407(3) -0.4088(6) 1.2351(5) 0.0511(15) Uani 1 1 d . . .
O8W O 1.4576(6) 0.051(2) 1.4894(15) 0.278(10) Uani 1 1 d . . .
H8W2 H 1.4511 0.0185 1.4220 0.417 Uiso 1 1 d R . .
H8W1 H 1.4882 0.1232 1.5005 0.417 Uiso 1 1 d R . .
O9W O 1.2504(2) 0.9206(6) 1.5591(4) 0.0305(10) Uani 1 1 d D . .
H9W1 H 1.2188(18) 0.914(9) 1.506(3) 0.046 Uiso 1 1 d D . .
H9W2 H 1.238(3) 0.913(9) 1.620(2) 0.046 Uiso 1 1 d D . .
O9 O 1.4513(2) -0.2913(7) 1.4178(4) 0.0480(13) Uani 1 1 d . . .
O10 O 1.34799(19) -0.3679(5) 1.3173(3) 0.0280(10) Uani 1 1 d . . .
O10W O 1.1751(2) 0.1814(6) 1.2847(3) 0.0319(10) Uani 1 1 d . . .
HAW H 1.1659 0.1283 1.3405 0.048 Uiso 1 1 d R . .
HBW H 1.1705 0.2910 1.2943 0.048 Uiso 1 1 d R . .
C1 C 1.0872(3) 0.6582(7) 1.2176(4) 0.0180(11) Uani 1 1 d . . .
C2 C 1.0869(3) 0.7582(7) 1.1221(4) 0.0172(11) Uani 1 1 d . . .
C3 C 1.0321(3) 0.7717(7) 1.0441(4) 0.0205(12) Uani 1 1 d . . .
H3A H 1.0321 0.8381 0.9805 0.025 Uiso 1 1 calc R . .
C4 C 0.9771(3) 0.6885(7) 1.0585(4) 0.0185(11) Uani 1 1 d . . .
C5 C 0.9774(3) 0.5861(7) 1.1519(5) 0.0238(13) Uani 1 1 d . . .
H5A H 0.9409 0.5282 1.1618 0.029 Uiso 1 1 calc R . .
C6 C 1.0325(3) 0.5705(8) 1.2309(5) 0.0243(13) Uani 1 1 d . . .
H6A H 1.0328 0.5008 1.2932 0.029 Uiso 1 1 calc R . .
C7 C 0.9178(3) 0.7054(7) 0.9761(5) 0.0226(12) 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
Lu1 O7 2.247(4) . ?
Lu1 O6W 2.297(4) . ?
Lu1 O7W 2.306(5) . ?
Lu1 O4W 2.308(4) . ?
Lu1 O5W 2.318(5) . ?
Lu1 O1W 2.321(4) . ?
Lu1 O2W 2.326(4) . ?
Lu1 O3W 2.391(5) . ?
S1 O2 1.444(4) . ?
S1 O3 1.445(4) . ?
S1 O1 1.467(4) . ?
S1 C1 1.768(5) . ?
S2 O7 1.456(4) . ?
S2 O9 1.459(5) . ?
S2 O8 1.470(5) . ?
S2 O10 1.484(4) . ?
O1W H1W1 0.85(6) . ?
O1W H1W2 0.85(6) . ?
O2W H2W1 0.85(6) . ?
O2W H2W2 0.85(6) . ?
O3W H3W1 0.85(6) . ?
O3W H3W2 0.85(6) . ?
O4W H4W1 0.85(6) . ?
O4W H4W2 0.85(6) . ?
O4 C2 1.365(6) . ?
O4 H4O 0.85(6) . ?
O5 C7 1.321(7) . ?
O5 H5O 0.85(6) . ?
O5W H5W1 0.8501 . ?
O5W H5W2 0.8498 . ?
O6W H6W1 0.85(6) . ?
O6W H6W2 0.85(6) . ?
O6 C7 1.226(7) . ?
O7W H7W1 0.85(6) . ?
O7W H7W2 0.85(6) . ?
O8W H8W2 0.8501 . ?
O8W H8W1 0.8500 . ?
O9W H9W1 0.85(6) . ?
O9W H9W2 0.85(6) . ?
O10W HAW 0.8500 . ?
O10W HBW 0.8500 . ?
C1 C6 1.392(8) . ?
C1 C2 1.397(7) . ?
C2 C3 1.376(7) . ?
C3 C4 1.387(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.386(8) . ?
C4 C7 1.479(7) . ?
C5 C6 1.391(8) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?

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
O7 Lu1 O6W 81.55(17) . . ?
O7 Lu1 O7W 73.56(16) . . ?
O6W Lu1 O7W 76.38(17) . . ?
O7 Lu1 O4W 87.44(18) . . ?
O6W Lu1 O4W 71.66(16) . . ?
O7W Lu1 O4W 144.83(17) . . ?
O7 Lu1 O5W 145.59(18) . . ?
O6W Lu1 O5W 74.30(19) . . ?
O7W Lu1 O5W 77.2(2) . . ?
O4W Lu1 O5W 107.2(2) . . ?
O7 Lu1 O1W 108.38(19) . . ?
O6W Lu1 O1W 145.06(17) . . ?
O7W Lu1 O1W 74.79(19) . . ?
O4W Lu1 O1W 140.19(19) . . ?
O5W Lu1 O1W 80.39(19) . . ?
O7 Lu1 O2W 72.67(16) . . ?
O6W Lu1 O2W 139.48(17) . . ?
O7W Lu1 O2W 123.02(18) . . ?
O4W Lu1 O2W 76.40(17) . . ?
O5W Lu1 O2W 140.31(17) . . ?
O1W Lu1 O2W 74.19(18) . . ?
O7 Lu1 O3W 143.44(18) . . ?
O6W Lu1 O3W 116.77(19) . . ?
O7W Lu1 O3W 139.02(17) . . ?
O4W Lu1 O3W 70.96(18) . . ?
O5W Lu1 O3W 70.6(2) . . ?
O1W Lu1 O3W 75.4(2) . . ?
O2W Lu1 O3W 73.74(19) . . ?
O2 S1 O3 113.9(3) . . ?
O2 S1 O1 112.5(2) . . ?
O3 S1 O1 110.6(3) . . ?
O2 S1 C1 105.5(3) . . ?
O3 S1 C1 107.2(3) . . ?
O1 S1 C1 106.6(3) . . ?
O7 S2 O9 108.9(3) . . ?
O7 S2 O8 108.8(3) . . ?
O9 S2 O8 109.2(4) . . ?
O7 S2 O10 109.7(3) . . ?
O9 S2 O10 109.7(3) . . ?
O8 S2 O10 110.4(3) . . ?
Lu1 O1W H1W1 119(5) . . ?
Lu1 O1W H1W2 132(5) . . ?
H1W1 O1W H1W2 109.2(18) . . ?
Lu1 O2W H2W1 125(4) . . ?
Lu1 O2W H2W2 123(4) . . ?
H2W1 O2W H2W2 110.7(18) . . ?
Lu1 O3W H3W1 128(5) . . ?
Lu1 O3W H3W2 121(5) . . ?
H3W1 O3W H3W2 109.4(18) . . ?
Lu1 O4W H4W1 124(4) . . ?
Lu1 O4W H4W2 124(4) . . ?
H4W1 O4W H4W2 110.0(18) . . ?
C2 O4 H4O 117(5) . . ?
C7 O5 H5O 110(5) . . ?
Lu1 O5W H5W1 100.7 . . ?
Lu1 O5W H5W2 112.4 . . ?
H5W1 O5W H5W2 108.1 . . ?
Lu1 O6W H6W1 125(5) . . ?
Lu1 O6W H6W2 101(5) . . ?
H6W1 O6W H6W2 109.8(18) . . ?
Lu1 O7W H7W1 120(4) . . ?
Lu1 O7W H7W2 129(4) . . ?
H7W1 O7W H7W2 108.9(18) . . ?
S2 O7 Lu1 151.8(3) . . ?
H8W2 O8W H8W1 108.9 . . ?
H9W1 O9W H9W2 109.6(18) . . ?
HAW O10W HBW 107.6 . . ?
C6 C1 C2 119.3(5) . . ?
C6 C1 S1 120.9(4) . . ?
C2 C1 S1 119.9(4) . . ?
O4 C2 C3 122.3(5) . . ?
O4 C2 C1 118.1(5) . . ?
C3 C2 C1 119.6(5) . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 C7 118.9(5) . . ?
C3 C4 C7 121.6(5) . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C5 C6 C1 120.7(5) . . ?
C5 C6 H6A 119.7 . . ?
C1 C6 H6A 119.7 . . ?
O6 C7 O5 122.7(5) . . ?
O6 C7 C4 123.8(5) . . ?
O5 C7 C4 113.5(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
O9 S2 O7 Lu1 -148.4(6) . . . . ?
O8 S2 O7 Lu1 92.6(6) . . . . ?
O10 S2 O7 Lu1 -28.3(7) . . . . ?
O6W Lu1 O7 S2 -114.1(6) . . . . ?
O7W Lu1 O7 S2 167.7(6) . . . . ?
O4W Lu1 O7 S2 -42.3(6) . . . . ?
O5W Lu1 O7 S2 -159.6(5) . . . . ?
O1W Lu1 O7 S2 100.4(6) . . . . ?
O2W Lu1 O7 S2 34.2(6) . . . . ?
O3W Lu1 O7 S2 10.2(8) . . . . ?
O2 S1 C1 C6 -117.1(5) . . . . ?
O3 S1 C1 C6 121.2(5) . . . . ?
O1 S1 C1 C6 2.7(5) . . . . ?
O2 S1 C1 C2 63.3(5) . . . . ?
O3 S1 C1 C2 -58.4(5) . . . . ?
O1 S1 C1 C2 -176.9(4) . . . . ?
C6 C1 C2 O4 -178.5(5) . . . . ?
S1 C1 C2 O4 1.1(7) . . . . ?
C6 C1 C2 C3 1.5(8) . . . . ?
S1 C1 C2 C3 -178.8(4) . . . . ?
O4 C2 C3 C4 -179.7(5) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
C2 C3 C4 C5 -1.5(8) . . . . ?
C2 C3 C4 C7 178.8(5) . . . . ?
C3 C4 C5 C6 1.1(8) . . . . ?
C7 C4 C5 C6 -179.2(5) . . . . ?
C4 C5 C6 C1 0.7(9) . . . . ?
C2 C1 C6 C5 -2.0(8) . . . . ?
S1 C1 C6 C5 178.4(4) . . . . ?
C5 C4 C7 O6 4.4(8) . . . . ?
C3 C4 C7 O6 -175.9(6) . . . . ?
C5 C4 C7 O5 -176.0(5) . . . . ?
C3 C4 C7 O5 3.8(8) . . . . ?

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
O1W H1W1 O10 0.85(6) 2.05(4) 2.850(6) 156(8) 1_565
O1W H1W2 O10W 0.85(6) 2.18(3) 2.962(7) 151(6) .
O1W H1W2 O3 0.85(6) 2.62(7) 3.107(7) 117(6) .
O2W H2W1 O10 0.85(6) 2.01(3) 2.765(6) 148(6) .
O2W H2W1 O3 0.85(6) 2.56(5) 3.149(6) 128(5) 1_545
O2W H2W2 O4 0.85(6) 2.42(5) 3.100(6) 138(6) 1_545
O2W H2W2 O10W 0.85(6) 2.46(5) 3.112(6) 135(6) .
O2W H2W2 O2 0.85(6) 2.63(6) 3.136(6) 120(5) 1_545
O3W H3W1 O6 0.85(6) 2.12(5) 2.831(7) 141(6) 3_767
O3W H3W1 O9W 0.85(6) 2.50(5) 3.168(7) 136(7) 4_575
O3W H3W2 O1 0.85(6) 2.21(5) 2.970(6) 148(8) 4_565
O4W H4W1 O10 0.85(6) 1.916(13) 2.764(6) 176(6) 4
O4W H4W2 O9W 0.85(6) 1.97(4) 2.750(6) 153(7) 4_565
O4 H4O O1 0.85(6) 1.883(12) 2.733(5) 178(7) 4_575
O5 H5O O10W 0.85(6) 1.89(2) 2.715(6) 163(7) 3_767
O5W H5W1 O8 0.85 2.27 3.108(9) 169.1 1_565
O5W H5W1 O7W 0.85 2.43 2.884(8) 114.2 .
O5W H5W2 O9W 0.85 1.98 2.817(7) 168.3 4_575
O6W H6W1 O9 0.85(6) 1.90(2) 2.739(6) 167(7) 4
O6W H6W2 O9 0.85(6) 2.25(6) 2.828(7) 125(6) 2_857
O6W H6W2 O7W 0.85(6) 2.42(6) 2.846(6) 112(5) .
O7W H7W1 O8 0.85(6) 2.13(5) 2.884(7) 147(7) 2_857
O7W H7W2 O8 0.85(6) 1.97(3) 2.786(7) 159(6) 1_565
O8W H8W2 O7 0.85 2.28 3.090(16) 159.0 .
O8W H8W2 O7W 0.85 2.48 3.03(2) 123.2 .
O8W H8W1 O9 0.85 1.96 2.766(15) 157.7 3_858
O9W H9W1 O2 0.85(6) 2.03(3) 2.824(6) 155(6) .
O9W H9W1 O6 0.85(6) 2.55(6) 3.009(6) 115(5) 2_757
O9W H9W2 O3 0.85(6) 2.045(15) 2.889(6) 173(7) 4_576
O10W HAW O6 0.85 2.35 3.110(6) 149.0 2_747
O10W HAW O2 0.85 2.35 2.907(6) 123.2 1_545
O10W HBW O3 0.85 2.31 3.053(6) 146.4 .
O10W HBW O1 0.85 2.37 3.127(6) 149.1 .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.594
_refine_diff_density_min         -2.614
_refine_diff_density_rms         0.188
####################################################################### 
# 
# 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_3-Ho
_database_code_depnum_ccdc_archive 'CCDC 1549846'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H5 O6 S, H14 Ho O11 S, 3(H2 O)'
_chemical_formula_sum            'C7 H25 Ho O20 S2'
_chemical_formula_weight         658.32

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   21.6475(8)
_cell_length_b                   7.6506(3)
_cell_length_c                   12.2817(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.053(4)
_cell_angle_gamma                90.00
_cell_volume                     1996.31(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2212
_cell_measurement_theta_min      3.93
_cell_measurement_theta_max      29.42

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    4.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4976
_exptl_absorpt_correction_T_max  0.5863
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7344
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4553
_reflns_number_gt                3861
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0377P)²+0.4804P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4553
_refine_ls_number_parameters     325
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0885
_refine_ls_wR_factor_gt          0.0809
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_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 0.651079(10) 0.40660(3) 0.839803(18) 0.01996(8) Uani 1 1 d . . .
S1 S 0.84352(6) 0.85656(17) 0.67905(9) 0.0195(2) Uani 1 1 d . . .
S2 S 0.58909(6) 0.79601(17) 0.68924(11) 0.0260(3) Uani 1 1 d . . .
O1 O 0.79453(18) 0.9280(5) 0.7319(3) 0.0310(9) Uani 1 1 d . . .
O1W O 0.7546(2) 0.3355(6) 0.9456(4) 0.0488(12) Uani 1 1 d D . .
H1W1 H 0.770(3) 0.233(4) 0.946(5) 0.073 Uiso 1 1 d D . .
H1W2 H 0.773(3) 0.389(7) 1.004(4) 0.073 Uiso 1 1 d D . .
O2W O 0.6831(2) 0.6269(5) 0.9727(3) 0.0366(10) Uani 1 1 d D . .
H2W1 H 0.672(3) 0.642(7) 1.035(3) 0.055 Uiso 1 1 d D . .
H2W2 H 0.707(2) 0.711(5) 0.961(4) 0.055 Uiso 1 1 d D . .
O2 O 0.83073(18) 0.6809(5) 0.6374(3) 0.0325(9) Uani 1 1 d . . .
O3 O 0.85731(17) 0.9753(5) 0.5932(3) 0.0274(8) Uani 1 1 d . . .
O3W O 0.6451(3) 0.1378(6) 0.9328(5) 0.0709(17) Uani 1 1 d D . .
H3W1 H 0.676(2) 0.067(8) 0.946(7) 0.106 Uiso 1 1 d D . .
H3W2 H 0.615(3) 0.092(9) 0.888(7) 0.106 Uiso 1 1 d D . .
O4 O 0.85907(16) 0.6605(5) 0.8883(3) 0.0262(8) Uani 1 1 d D . .
H4O H 0.858(3) 0.626(7) 0.9534(19) 0.039 Uiso 1 1 d D . .
O4W O 0.57195(18) 0.4436(6) 0.9429(4) 0.0372(10) Uani 1 1 d D . .
H4W1 H 0.565(2) 0.538(5) 0.976(5) 0.056 Uiso 1 1 d D . .
H4W2 H 0.5368(13) 0.393(6) 0.920(5) 0.056 Uiso 1 1 d D . .
O5W O 0.56338(19) 0.2670(5) 0.7328(4) 0.0397(10) Uani 1 1 d D . .
H5W1 H 0.5298(15) 0.327(6) 0.716(6) 0.060 Uiso 1 1 d D . .
H5W2 H 0.554(3) 0.159(2) 0.731(6) 0.060 Uiso 1 1 d D . .
O5 O 1.07544(18) 0.7034(5) 1.1111(3) 0.0348(9) Uani 1 1 d D . .
H5O H 1.1122(13) 0.695(9) 1.150(5) 0.052 Uiso 1 1 d D . .
O6W O 0.72388(19) 0.5755(5) 0.7639(4) 0.0389(10) Uani 1 1 d D . .
H6W1 H 0.7634(6) 0.568(8) 0.783(5) 0.058 Uiso 1 1 d D . .
H6W2 H 0.713(2) 0.660(6) 0.721(4) 0.058 Uiso 1 1 d D . .
O6 O 1.13202(17) 0.8583(5) 1.0116(3) 0.0352(9) Uani 1 1 d . . .
O7 O 0.59523(17) 0.6187(4) 0.7341(3) 0.0303(9) Uani 1 1 d . . .
O7W O 0.6931(2) 0.2160(6) 0.7210(4) 0.0516(12) Uani 1 1 d D . .
H7W1 H 0.7271(18) 0.228(9) 0.696(5) 0.077 Uiso 1 1 d D . .
H7W2 H 0.674(3) 0.124(6) 0.693(6) 0.077 Uiso 1 1 d D . .
O8W O 0.75047(18) 0.9189(5) 0.9393(3) 0.0317(9) Uani 1 1 d D . .
H8W1 H 0.764(2) 0.928(8) 0.879(2) 0.048 Uiso 1 1 d D . .
H8W2 H 0.7807(17) 0.893(8) 0.992(3) 0.048 Uiso 1 1 d D . .
O8 O 0.5600(2) 0.9071(5) 0.7636(4) 0.0516(13) Uani 1 1 d . . .
O9 O 0.5486(2) 0.7909(6) 0.5796(3) 0.0472(12) Uani 1 1 d . . .
O9W O 0.82668(17) 0.3156(5) 0.7159(3) 0.0340(9) Uani 1 1 d . . .
H9W1 H 0.8385 0.2864 0.6563 0.051 Uiso 1 1 d R . .
H9W2 H 0.8233 0.4263 0.7159 0.051 Uiso 1 1 d R . .
O10 O 0.65183(17) 0.8644(5) 0.6814(3) 0.0308(9) Uani 1 1 d . . .
O10W O 0.4610(5) 0.550(2) 0.4955(15) 0.307(10) Uani 1 1 d . . .
HAW H 0.4433 0.4932 0.4385 0.460 Uiso 1 1 d R . .
HBW H 0.4522 0.5010 0.5528 0.460 Uiso 1 1 d R . .
C1 C 0.9134(2) 0.8428(6) 0.7811(4) 0.0177(9) Uani 1 1 d . . .
C2 C 0.9132(2) 0.7415(6) 0.8767(4) 0.0193(10) Uani 1 1 d . . .
C3 C 0.9685(2) 0.7271(7) 0.9559(4) 0.0240(11) Uani 1 1 d . . .
H3 H 0.9689 0.6601 1.0192 0.029 Uiso 1 1 calc R . .
C4 C 1.0228(2) 0.8125(6) 0.9407(4) 0.0199(10) Uani 1 1 d . . .
C5 C 1.0228(2) 0.9159(6) 0.8470(4) 0.0247(11) Uani 1 1 d . . .
H5 H 1.0591 0.9746 0.8379 0.030 Uiso 1 1 calc R . .
C6 C 0.9680(2) 0.9302(6) 0.7673(4) 0.0228(11) Uani 1 1 d . . .
H6 H 0.9676 0.9983 0.7044 0.027 Uiso 1 1 calc R . .
C7 C 1.0823(2) 0.7958(6) 1.0247(4) 0.0243(11) 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 O7 2.275(3) . ?
Ho1 O4W 2.335(4) . ?
Ho1 O5W 2.348(4) . ?
Ho1 O2W 2.356(4) . ?
Ho1 O6W 2.363(4) . ?
Ho1 O7W 2.365(4) . ?
Ho1 O3W 2.368(5) . ?
Ho1 O1W 2.426(4) . ?
S1 O2 1.446(4) . ?
S1 O1 1.452(4) . ?
S1 O3 1.465(4) . ?
S1 C1 1.773(5) . ?
S2 O9 1.460(4) . ?
S2 O7 1.461(3) . ?
S2 O8 1.474(5) . ?
S2 O10 1.476(4) . ?
O1W H1W1 0.85(6) . ?
O1W H1W2 0.85(6) . ?
O2W H2W1 0.85(6) . ?
O2W H2W2 0.85(6) . ?
O3W H3W1 0.85(6) . ?
O3W H3W2 0.85(6) . ?
O4 C2 1.357(6) . ?
O4 H4O 0.85(6) . ?
O4W H4W1 0.85(6) . ?
O4W H4W2 0.85(6) . ?
O5W H5W1 0.85(6) . ?
O5W H5W2 0.85(6) . ?
O5 C7 1.307(6) . ?
O5 H5O 0.85(6) . ?
O6W H6W1 0.85(6) . ?
O6W H6W2 0.85(6) . ?
O6 C7 1.217(6) . ?
O7W H7W1 0.85(6) . ?
O7W H7W2 0.85(6) . ?
O8W H8W1 0.85(6) . ?
O8W H8W2 0.85(6) . ?
O9W H9W1 0.8501 . ?
O9W H9W2 0.8500 . ?
O10W HAW 0.8500 . ?
O10W HBW 0.8500 . ?
C1 C6 1.396(7) . ?
C1 C2 1.407(6) . ?
C2 C3 1.394(6) . ?
C3 C4 1.390(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(7) . ?
C4 C7 1.492(6) . ?
C5 C6 1.391(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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
O7 Ho1 O4W 81.84(16) . . ?
O7 Ho1 O5W 73.80(14) . . ?
O4W Ho1 O5W 76.12(14) . . ?
O7 Ho1 O2W 86.50(15) . . ?
O4W Ho1 O2W 71.73(14) . . ?
O5W Ho1 O2W 144.29(15) . . ?
O7 Ho1 O6W 72.95(13) . . ?
O4W Ho1 O6W 139.62(15) . . ?
O5W Ho1 O6W 123.84(16) . . ?
O2W Ho1 O6W 75.65(15) . . ?
O7 Ho1 O7W 108.23(17) . . ?
O4W Ho1 O7W 144.93(15) . . ?
O5W Ho1 O7W 74.90(16) . . ?
O2W Ho1 O7W 140.51(16) . . ?
O6W Ho1 O7W 74.31(16) . . ?
O7 Ho1 O3W 145.31(16) . . ?
O4W Ho1 O3W 74.34(18) . . ?
O5W Ho1 O3W 76.22(18) . . ?
O2W Ho1 O3W 108.84(19) . . ?
O6W Ho1 O3W 140.11(16) . . ?
O7W Ho1 O3W 79.93(19) . . ?
O7 Ho1 O1W 143.17(15) . . ?
O4W Ho1 O1W 115.79(17) . . ?
O5W Ho1 O1W 139.65(15) . . ?
O2W Ho1 O1W 70.76(16) . . ?
O6W Ho1 O1W 73.53(16) . . ?
O7W Ho1 O1W 76.55(18) . . ?
O3W Ho1 O1W 71.17(18) . . ?
O2 S1 O1 113.7(2) . . ?
O2 S1 O3 112.0(2) . . ?
O1 S1 O3 110.8(2) . . ?
O2 S1 C1 105.9(2) . . ?
O1 S1 C1 107.6(2) . . ?
O3 S1 C1 106.4(2) . . ?
O9 S2 O7 108.6(2) . . ?
O9 S2 O8 109.6(3) . . ?
O7 S2 O8 108.7(3) . . ?
O9 S2 O10 110.3(2) . . ?
O7 S2 O10 109.6(2) . . ?
O8 S2 O10 110.1(2) . . ?
Ho1 O1W H1W1 122(4) . . ?
Ho1 O1W H1W2 125(4) . . ?
H1W1 O1W H1W2 108.6(17) . . ?
Ho1 O2W H2W1 129(4) . . ?
Ho1 O2W H2W2 122(3) . . ?
H2W1 O2W H2W2 108.9(18) . . ?
Ho1 O3W H3W1 122(6) . . ?
Ho1 O3W H3W2 99(6) . . ?
H3W1 O3W H3W2 110.0(18) . . ?
C2 O4 H4O 115(4) . . ?
Ho1 O4W H4W1 124(4) . . ?
Ho1 O4W H4W2 118(4) . . ?
H4W1 O4W H4W2 108.9(18) . . ?
Ho1 O5W H5W1 117(4) . . ?
Ho1 O5W H5W2 128(4) . . ?
H5W1 O5W H5W2 109.4(18) . . ?
C7 O5 H5O 105(5) . . ?
Ho1 O6W H6W1 125(4) . . ?
Ho1 O6W H6W2 123(4) . . ?
H6W1 O6W H6W2 111.1(18) . . ?
S2 O7 Ho1 151.3(2) . . ?
Ho1 O7W H7W1 128(4) . . ?
Ho1 O7W H7W2 123(4) . . ?
H7W1 O7W H7W2 109.1(18) . . ?
H8W1 O8W H8W2 109.8(18) . . ?
H9W1 O9W H9W2 107.6 . . ?
HAW O10W HBW 108.7 . . ?
C6 C1 C2 120.2(4) . . ?
C6 C1 S1 120.8(4) . . ?
C2 C1 S1 119.0(4) . . ?
O4 C2 C3 122.2(4) . . ?
O4 C2 C1 118.7(4) . . ?
C3 C2 C1 119.1(4) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 C7 120.5(4) . . ?
C5 C4 C7 118.8(5) . . ?
C6 C5 C4 119.3(5) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.3(5) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O6 C7 O5 124.1(5) . . ?
O6 C7 C4 122.9(5) . . ?
O5 C7 C4 113.0(4) . . ?

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
O9 S2 O7 Ho1 148.4(5) . . . . ?
O8 S2 O7 Ho1 -92.5(6) . . . . ?
O10 S2 O7 Ho1 27.8(6) . . . . ?
O4W Ho1 O7 S2 114.0(5) . . . . ?
O5W Ho1 O7 S2 -168.1(6) . . . . ?
O2W Ho1 O7 S2 42.0(5) . . . . ?
O6W Ho1 O7 S2 -34.0(5) . . . . ?
O7W Ho1 O7 S2 -100.5(5) . . . . ?
O3W Ho1 O7 S2 160.7(5) . . . . ?
O1W Ho1 O7 S2 -8.8(7) . . . . ?
O2 S1 C1 C6 116.7(4) . . . . ?
O1 S1 C1 C6 -121.4(4) . . . . ?
O3 S1 C1 C6 -2.6(4) . . . . ?
O2 S1 C1 C2 -63.0(4) . . . . ?
O1 S1 C1 C2 58.9(4) . . . . ?
O3 S1 C1 C2 177.7(4) . . . . ?
C6 C1 C2 O4 179.0(4) . . . . ?
S1 C1 C2 O4 -1.3(6) . . . . ?
C6 C1 C2 C3 -1.2(7) . . . . ?
S1 C1 C2 C3 178.5(4) . . . . ?
O4 C2 C3 C4 -179.9(4) . . . . ?
C1 C2 C3 C4 0.2(7) . . . . ?
C2 C3 C4 C5 1.0(7) . . . . ?
C2 C3 C4 C7 -179.3(4) . . . . ?
C3 C4 C5 C6 -1.3(7) . . . . ?
C7 C4 C5 C6 179.0(4) . . . . ?
C4 C5 C6 C1 0.3(7) . . . . ?
C2 C1 C6 C5 0.9(7) . . . . ?
S1 C1 C6 C5 -178.8(4) . . . . ?
C3 C4 C7 O6 174.9(5) . . . . ?
C5 C4 C7 O6 -5.4(7) . . . . ?
C3 C4 C7 O5 -3.1(7) . . . . ?
C5 C4 C7 O5 176.6(5) . . . . ?

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
O1W H1W1 O6 0.85(6) 2.20(5) 2.829(6) 130(6) 3_767
O1W H1W1 O8W 0.85(6) 2.44(4) 3.189(6) 148(6) 1_545
O1W H1W2 O3 0.85(6) 2.20(5) 2.964(6) 148(8) 4_576
O2W H2W1 O10 0.85(6) 1.931(15) 2.775(6) 170(6) 4_576
O2W H2W2 O8W 0.85(6) 1.894(15) 2.741(5) 172(6) .
O3W H3W1 O8W 0.85(6) 1.99(3) 2.818(6) 165(9) 1_545
O3W H3W2 O8 0.85(6) 2.25(3) 3.059(8) 161(7) 1_545
O3W H3W2 O5W 0.85(6) 2.42(8) 2.911(7) 118(7) .
O4 H4O O3 0.85(6) 1.885(13) 2.730(5) 174(6) 4_576
O4W H4W1 O9 0.85(6) 1.91(2) 2.742(5) 165(7) 4_576
O4W H4W2 O9 0.85(6) 2.01(3) 2.825(6) 160(6) 2_646
O5W H5W1 O8 0.85(6) 2.10(3) 2.887(6) 154(6) 2_646
O5W H5W2 O8 0.85(6) 1.97(2) 2.782(6) 161(5) 1_545
O5 H5O O9W 0.85(6) 1.91(3) 2.702(5) 155(6) 3_767
O6W H6W1 O4 0.85(6) 2.33(3) 3.099(5) 151(6) .
O6W H6W1 O9W 0.85(6) 2.59(6) 3.124(6) 122(5) .
O6W H6W1 O2 0.85(6) 2.65(5) 3.129(6) 117(4) .
O6W H6W2 O10 0.85(6) 2.05(4) 2.782(5) 145(6) .
O7W H7W1 O9W 0.85(6) 2.23(3) 3.003(6) 152(6) .
O7W H7W2 O10 0.85(6) 2.04(3) 2.846(6) 157(7) 1_545
O8W H8W1 O1 0.85(6) 2.040(13) 2.887(5) 175(6) .
O8W H8W2 O2 0.85(6) 1.987(17) 2.811(5) 163(5) 4_576
O9W H9W1 O6 0.85 2.34 3.109(6) 151.1 2_746
O9W H9W1 O3 0.85 2.56 3.141(5) 126.6 1_545
O9W H9W2 O2 0.85 2.19 2.963(5) 150.6 .
O9W H9W2 O6W 0.85 2.60 3.124(6) 120.8 .
O10W HAW O9 0.85 2.20 2.760(15) 123.8 3_666
O10W HAW O7 0.85 2.29 3.128(15) 168.5 3_666
O10W HBW O8 0.85 2.43 3.27(2) 168.6 2_646

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.316
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.158
####################################################################### 
# 
# 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_4-Er
_database_code_depnum_ccdc_archive 'CCDC 1549852'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H9 Er O9 S, H2 O'
_chemical_formula_sum            'C7 H11 Er O10 S'
_chemical_formula_weight         454.48

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.8891(3)
_cell_length_b                   9.3172(3)
_cell_length_c                   12.0758(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.687(3)
_cell_angle_gamma                90.00
_cell_volume                     1224.63(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1870
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    7.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3183
_exptl_absorpt_correction_T_max  0.3975
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4329
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2793
_reflns_number_gt                2277
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0311P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2793
_refine_ls_number_parameters     196
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.014
_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
Er1 Er -0.02811(3) 0.31617(4) 0.93771(2) 0.01330(11) Uani 1 1 d . . .
S1 S 0.25597(15) 0.2406(2) 1.07032(13) 0.0166(4) Uani 1 1 d . . .
O1 O 0.1377(4) 0.1930(6) 1.0234(4) 0.0276(13) Uani 1 1 d . . .
O1W O -0.0895(5) 0.1679(6) 1.0808(4) 0.0283(13) Uani 1 1 d D . .
H1W1 H -0.042(5) 0.104(6) 1.110(6) 0.042 Uiso 1 1 d D . .
H1W2 H -0.164(2) 0.146(8) 1.095(6) 0.042 Uiso 1 1 d D . .
O2 O 0.2440(5) 0.3136(6) 1.1758(4) 0.0297(14) Uani 1 1 d . . .
O2W O -0.2397(5) 0.2655(7) 0.8999(4) 0.0271(13) Uani 1 1 d D . .
H2W1 H -0.269(7) 0.202(6) 0.943(4) 0.041 Uiso 1 1 d D . .
H2W2 H -0.254(7) 0.241(8) 0.8330(18) 0.041 Uiso 1 1 d D . .
O3 O 0.3434(4) 0.1237(6) 1.0781(4) 0.0211(11) Uani 1 1 d . . .
O3W O -0.0873(5) 0.4654(7) 0.7897(4) 0.0281(13) Uani 1 1 d D . .
H3W1 H -0.099(6) 0.436(8) 0.724(3) 0.042 Uiso 1 1 d D . .
H3W2 H -0.144(5) 0.524(7) 0.807(5) 0.042 Uiso 1 1 d D . .
O4 O 0.1171(4) 0.4902(6) 0.9726(3) 0.0145(10) Uani 1 1 d . . .
O4W O 0.3324(6) 0.8952(8) 0.9213(5) 0.0435(17) Uani 1 1 d D . .
H4W1 H 0.345(9) 0.984(3) 0.934(6) 0.065 Uiso 1 1 d D . .
H4W2 H 0.357(8) 0.873(8) 0.857(4) 0.065 Uiso 1 1 d D . .
O5 O 0.4018(5) 0.7698(6) 0.7190(4) 0.0228(12) Uani 1 1 d . . .
O6 O 0.5203(4) 0.5957(6) 0.6603(4) 0.0207(11) Uani 1 1 d . . .
C1 C 0.3102(6) 0.3645(9) 0.9747(5) 0.0168(15) Uani 1 1 d . . .
C2 C 0.2331(5) 0.4752(8) 0.9358(5) 0.0130(14) Uani 1 1 d . . .
C3 C 0.2776(6) 0.5652(8) 0.8548(5) 0.0153(14) Uani 1 1 d . . .
H3 H 0.2290 0.6401 0.8276 0.018 Uiso 1 1 calc R . .
C4 C 0.3943(6) 0.5445(8) 0.8139(5) 0.0162(14) Uani 1 1 d . . .
C5 C 0.4687(6) 0.4334(9) 0.8528(6) 0.0211(16) Uani 1 1 d . . .
H5 H 0.5461 0.4197 0.8241 0.025 Uiso 1 1 calc R . .
C6 C 0.4276(7) 0.3441(9) 0.9338(5) 0.0231(18) Uani 1 1 d . . .
H6 H 0.4774 0.2704 0.9613 0.028 Uiso 1 1 calc R . .
C7 C 0.4417(6) 0.6412(9) 0.7268(5) 0.0185(16) 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
Er1 O4 2.296(5) . ?
Er1 O1W 2.326(5) . ?
Er1 O4 2.330(5) 3_567 ?
Er1 O3W 2.340(5) . ?
Er1 O1 2.353(5) . ?
Er1 O6 2.373(5) 2_546 ?
Er1 O2W 2.383(5) . ?
Er1 O5 2.412(5) 2_546 ?
Er1 C7 2.757(7) 2_546 ?
Er1 Er1 3.7841(6) 3_567 ?
S1 O3 1.448(5) . ?
S1 O2 1.453(5) . ?
S1 O1 1.461(5) . ?
S1 C1 1.749(7) . ?
O1W H1W1 0.85(8) . ?
O1W H1W2 0.85(8) . ?
O2W H2W1 0.85(8) . ?
O2W H2W2 0.85(8) . ?
O3W H3W1 0.85(8) . ?
O3W H3W2 0.85(8) . ?
O4 C2 1.358(7) . ?
O4 Er1 2.330(5) 3_567 ?
O4W H4W1 0.85(8) . ?
O4W H4W2 0.85(8) . ?
O5 C7 1.277(9) . ?
O5 Er1 2.412(5) 2_556 ?
O6 C7 1.264(8) . ?
O6 Er1 2.373(5) 2_556 ?
C1 C6 1.397(9) . ?
C1 C2 1.403(10) . ?
C2 C3 1.386(9) . ?
C3 C4 1.390(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(10) . ?
C4 C7 1.488(9) . ?
C5 C6 1.369(10) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 Er1 2.757(7) 2_556 ?

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
O4 Er1 O1W 119.65(18) . . ?
O4 Er1 O4 70.22(16) . 3_567 ?
O1W Er1 O4 88.97(18) . 3_567 ?
O4 Er1 O3W 83.88(18) . . ?
O1W Er1 O3W 147.31(19) . . ?
O4 Er1 O3W 77.62(17) 3_567 . ?
O4 Er1 O1 75.41(18) . . ?
O1W Er1 O1 67.49(18) . . ?
O4 Er1 O1 119.84(18) 3_567 . ?
O3W Er1 O1 144.72(18) . . ?
O4 Er1 O6 131.93(15) . 2_546 ?
O1W Er1 O6 82.64(19) . 2_546 ?
O4 Er1 O6 157.42(16) 3_567 2_546 ?
O3W Er1 O6 98.42(18) . 2_546 ?
O1 Er1 O6 76.06(18) . 2_546 ?
O4 Er1 O2W 146.32(19) . . ?
O1W Er1 O2W 74.17(19) . . ?
O4 Er1 O2W 80.16(18) 3_567 . ?
O3W Er1 O2W 74.2(2) . . ?
O1 Er1 O2W 135.5(2) . . ?
O6 Er1 O2W 77.40(18) 2_546 . ?
O4 Er1 O5 82.24(16) . 2_546 ?
O1W Er1 O5 131.3(2) . 2_546 ?
O4 Er1 O5 139.33(17) 3_567 2_546 ?
O3W Er1 O5 70.00(18) . 2_546 ?
O1 Er1 O5 79.02(18) . 2_546 ?
O6 Er1 O5 54.80(17) 2_546 2_546 ?
O2W Er1 O5 112.65(17) . 2_546 ?
O4 Er1 C7 107.59(18) . 2_546 ?
O1W Er1 C7 107.2(2) . 2_546 ?
O4 Er1 C7 161.50(18) 3_567 2_546 ?
O3W Er1 C7 83.9(2) . 2_546 ?
O1 Er1 C7 75.80(19) . 2_546 ?
O6 Er1 C7 27.23(19) 2_546 2_546 ?
O2W Er1 C7 95.37(19) . 2_546 ?
O5 Er1 C7 27.6(2) 2_546 2_546 ?
O4 Er1 Er1 35.41(11) . 3_567 ?
O1W Er1 Er1 106.80(15) . 3_567 ?
O4 Er1 Er1 34.81(11) 3_567 3_567 ?
O3W Er1 Er1 78.66(14) . 3_567 ?
O1 Er1 Er1 98.83(14) . 3_567 ?
O6 Er1 Er1 166.89(11) 2_546 3_567 ?
O2W Er1 Er1 113.55(15) . 3_567 ?
O5 Er1 Er1 112.64(13) 2_546 3_567 ?
C7 Er1 Er1 140.10(16) 2_546 3_567 ?
O3 S1 O2 111.8(3) . . ?
O3 S1 O1 111.6(3) . . ?
O2 S1 O1 112.4(3) . . ?
O3 S1 C1 107.8(3) . . ?
O2 S1 C1 108.1(4) . . ?
O1 S1 C1 104.8(3) . . ?
S1 O1 Er1 132.8(3) . . ?
Er1 O1W H1W1 122(5) . . ?
Er1 O1W H1W2 126(5) . . ?
H1W1 O1W H1W2 108.6(18) . . ?
Er1 O2W H2W1 113(6) . . ?
Er1 O2W H2W2 112(5) . . ?
H2W1 O2W H2W2 109.5(18) . . ?
Er1 O3W H3W1 123(6) . . ?
Er1 O3W H3W2 112(5) . . ?
H3W1 O3W H3W2 110.2(18) . . ?
C2 O4 Er1 120.6(4) . . ?
C2 O4 Er1 129.4(4) . 3_567 ?
Er1 O4 Er1 109.78(16) . 3_567 ?
H4W1 O4W H4W2 110.0(18) . . ?
C7 O5 Er1 91.4(4) . 2_556 ?
C7 O6 Er1 93.6(5) . 2_556 ?
C6 C1 C2 121.8(6) . . ?
C6 C1 S1 118.3(6) . . ?
C2 C1 S1 119.7(5) . . ?
O4 C2 C3 121.1(6) . . ?
O4 C2 C1 121.3(6) . . ?
C3 C2 C1 117.5(6) . . ?
C2 C3 C4 120.6(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 120.9(6) . . ?
C5 C4 C7 118.6(6) . . ?
C3 C4 C7 120.5(6) . . ?
C6 C5 C4 119.7(6) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 119.4(7) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
O6 C7 O5 120.2(7) . . ?
O6 C7 C4 120.1(7) . . ?
O5 C7 C4 119.7(6) . . ?
O6 C7 Er1 59.2(4) . 2_556 ?
O5 C7 Er1 61.0(4) . 2_556 ?
C4 C7 Er1 178.8(5) . 2_556 ?

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
O3 S1 O1 Er1 -159.7(3) . . . . ?
O2 S1 O1 Er1 73.8(5) . . . . ?
C1 S1 O1 Er1 -43.4(5) . . . . ?
O4 Er1 O1 S1 3.0(4) . . . . ?
O1W Er1 O1 S1 -128.4(5) . . . . ?
O4 Er1 O1 S1 -53.5(5) 3_567 . . . ?
O3W Er1 O1 S1 59.0(6) . . . . ?
O6 Er1 O1 S1 143.9(4) 2_546 . . . ?
O2W Er1 O1 S1 -161.1(3) . . . . ?
O5 Er1 O1 S1 87.7(4) 2_546 . . . ?
C7 Er1 O1 S1 115.8(4) 2_546 . . . ?
Er1 Er1 O1 S1 -23.8(4) 3_567 . . . ?
O1W Er1 O4 C2 107.1(4) . . . . ?
O4 Er1 O4 C2 -176.0(5) 3_567 . . . ?
O3W Er1 O4 C2 -96.9(4) . . . . ?
O1 Er1 O4 C2 54.2(4) . . . . ?
O6 Er1 O4 C2 -1.1(5) 2_546 . . . ?
O2W Er1 O4 C2 -146.1(4) . . . . ?
O5 Er1 O4 C2 -26.4(4) 2_546 . . . ?
C7 Er1 O4 C2 -15.4(5) 2_546 . . . ?
Er1 Er1 O4 C2 -176.0(5) 3_567 . . . ?
O1W Er1 O4 Er1 -76.9(2) . . . 3_567 ?
O4 Er1 O4 Er1 0.0 3_567 . . 3_567 ?
O3W Er1 O4 Er1 79.0(2) . . . 3_567 ?
O1 Er1 O4 Er1 -129.8(2) . . . 3_567 ?
O6 Er1 O4 Er1 174.85(16) 2_546 . . 3_567 ?
O2W Er1 O4 Er1 29.9(3) . . . 3_567 ?
O5 Er1 O4 Er1 149.6(2) 2_546 . . 3_567 ?
C7 Er1 O4 Er1 160.59(19) 2_546 . . 3_567 ?
O3 S1 C1 C6 -7.5(7) . . . . ?
O2 S1 C1 C6 113.5(6) . . . . ?
O1 S1 C1 C6 -126.5(6) . . . . ?
O3 S1 C1 C2 168.4(5) . . . . ?
O2 S1 C1 C2 -70.7(6) . . . . ?
O1 S1 C1 C2 49.4(6) . . . . ?
Er1 O4 C2 C3 113.0(6) . . . . ?
Er1 O4 C2 C3 -62.1(8) 3_567 . . . ?
Er1 O4 C2 C1 -64.2(7) . . . . ?
Er1 O4 C2 C1 120.7(6) 3_567 . . . ?
C6 C1 C2 O4 177.0(7) . . . . ?
S1 C1 C2 O4 1.3(9) . . . . ?
C6 C1 C2 C3 -0.3(10) . . . . ?
S1 C1 C2 C3 -176.0(5) . . . . ?
O4 C2 C3 C4 -176.9(6) . . . . ?
C1 C2 C3 C4 0.4(10) . . . . ?
C2 C3 C4 C5 0.2(11) . . . . ?
C2 C3 C4 C7 179.9(6) . . . . ?
C3 C4 C5 C6 -1.0(11) . . . . ?
C7 C4 C5 C6 179.3(7) . . . . ?
C4 C5 C6 C1 1.1(11) . . . . ?
C2 C1 C6 C5 -0.5(11) . . . . ?
S1 C1 C6 C5 175.2(6) . . . . ?
Er1 O6 C7 O5 -0.5(7) 2_556 . . . ?
Er1 O6 C7 C4 178.9(5) 2_556 . . . ?
Er1 O5 C7 O6 0.5(7) 2_556 . . . ?
Er1 O5 C7 C4 -178.9(5) 2_556 . . . ?
C5 C4 C7 O6 27.3(10) . . . . ?
C3 C4 C7 O6 -152.5(7) . . . . ?
C5 C4 C7 O5 -153.3(7) . . . . ?
C3 C4 C7 O5 26.9(10) . . . . ?

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
O1W H1W1 O6 0.85(8) 2.07(3) 2.884(8) 159(7) 4_566
O1W H1W2 O4W 0.85(8) 1.88(3) 2.709(8) 162(7) 3_567
O2W H2W1 O4W 0.85(8) 2.02(2) 2.837(8) 162(7) 3_567
O2W H2W2 O2 0.85(8) 1.965(17) 2.806(7) 171(8) 4_565
O3W H3W1 O3 0.85(8) 1.933(18) 2.771(7) 170(6) 4_565
O3W H3W2 O2 0.85(8) 1.88(3) 2.713(8) 165(9) 3_567
O4W H4W1 O3 0.85(8) 2.18(5) 2.849(8) 136(7) 1_565
O4W H4W2 O5 0.85(8) 2.00(2) 2.830(8) 165(8) .

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.592
_refine_diff_density_min         -2.127
_refine_diff_density_rms         0.235
####################################################################### 
# 
# 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_4-Tm
_database_code_depnum_ccdc_archive 'CCDC 1549853'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H9 O9 S Tm, H2 O'
_chemical_formula_sum            'C7 H11 O10 S Tm'
_chemical_formula_weight         456.15

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.8795(3)
_cell_length_b                   9.3023(2)
_cell_length_c                   12.0554(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.715(2)
_cell_angle_gamma                90.00
_cell_volume                     1219.52(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1985
_cell_measurement_theta_min      3.37
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            'yellow green'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    7.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3021
_exptl_absorpt_correction_T_max  0.3995
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4452
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2784
_reflns_number_gt                2331
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0073P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2784
_refine_ls_number_parameters     196
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0547
_refine_ls_wR_factor_gt          0.0507
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_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
Tm1 Tm 1.02781(2) 0.68331(2) 0.06202(2) 0.01295(7) Uani 1 1 d . . .
S1 S 0.74356(13) 0.75919(14) -0.07065(11) 0.0166(3) Uani 1 1 d . . .
O1W O 1.0897(4) 0.8296(4) -0.0812(4) 0.0274(10) Uani 1 1 d D . .
H1W1 H 1.037(3) 0.895(4) -0.096(5) 0.041 Uiso 1 1 d D . .
H1W2 H 1.1615(18) 0.864(5) -0.087(6) 0.041 Uiso 1 1 d D . .
O1 O 0.8627(4) 0.8059(4) -0.0237(3) 0.0270(10) Uani 1 1 d . . .
O2 O 0.7560(4) 0.6868(4) -0.1761(3) 0.0301(11) Uani 1 1 d . . .
O2W O 1.2389(4) 0.7340(4) 0.0998(3) 0.0270(10) Uani 1 1 d D . .
H2W1 H 1.261(5) 0.753(6) 0.1657(15) 0.040 Uiso 1 1 d D . .
H2W2 H 1.274(5) 0.789(5) 0.055(3) 0.040 Uiso 1 1 d D . .
O3 O 0.6555(4) 0.8769(4) -0.0774(3) 0.0213(9) Uani 1 1 d . . .
O3W O 1.0874(4) 0.5347(4) 0.2096(3) 0.0253(10) Uani 1 1 d D . .
H3W1 H 1.143(4) 0.475(5) 0.193(4) 0.038 Uiso 1 1 d D . .
H3W2 H 1.100(5) 0.567(5) 0.275(2) 0.038 Uiso 1 1 d D . .
O4 O 0.8831(3) 0.5084(4) 0.0275(3) 0.0143(8) Uani 1 1 d . . .
O4W O 0.6667(5) 0.1036(5) 0.0780(4) 0.0414(13) Uani 1 1 d D . .
H4W1 H 0.640(7) 0.129(6) 0.141(3) 0.062 Uiso 1 1 d D . .
H4W2 H 0.654(7) 0.015(2) 0.068(5) 0.062 Uiso 1 1 d D . .
O5 O 0.5977(4) 0.2300(4) 0.2822(3) 0.0216(9) Uani 1 1 d . . .
O6 O 0.4807(4) 0.4038(4) 0.3409(3) 0.0216(9) Uani 1 1 d . . .
C1 C 0.6894(5) 0.6359(5) 0.0259(5) 0.0160(12) Uani 1 1 d . . .
C2 C 0.7672(5) 0.5241(5) 0.0646(4) 0.0134(11) Uani 1 1 d . . .
C3 C 0.7217(5) 0.4353(5) 0.1465(4) 0.0140(12) Uani 1 1 d . . .
H3 H 0.7708 0.3614 0.1750 0.017 Uiso 1 1 calc R . .
C4 C 0.6056(5) 0.4541(5) 0.1865(5) 0.0152(12) Uani 1 1 d . . .
C5 C 0.5301(5) 0.5636(6) 0.1476(5) 0.0232(14) Uani 1 1 d . . .
H5 H 0.4521 0.5761 0.1756 0.028 Uiso 1 1 calc R . .
C6 C 0.5729(5) 0.6548(5) 0.0659(5) 0.0182(13) Uani 1 1 d . . .
H6 H 0.5230 0.7285 0.0382 0.022 Uiso 1 1 calc R . .
C7 C 0.5586(5) 0.3580(6) 0.2746(5) 0.0172(12) 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
Tm1 O4 2.294(3) . ?
Tm1 O4 2.312(3) 3_765 ?
Tm1 O1W 2.315(4) . ?
Tm1 O3W 2.330(4) . ?
Tm1 O1 2.342(4) . ?
Tm1 O6 2.365(3) 2_655 ?
Tm1 O2W 2.375(4) . ?
Tm1 O5 2.395(4) 2_655 ?
Tm1 C7 2.741(5) 2_655 ?
Tm1 Tm1 3.7656(4) 3_765 ?
S1 O2 1.448(4) . ?
S1 O3 1.455(4) . ?
S1 O1 1.465(4) . ?
S1 C1 1.749(5) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2W H2W1 0.85(5) . ?
O2W H2W2 0.85(5) . ?
O3W H3W1 0.85(5) . ?
O3W H3W2 0.85(5) . ?
O4 C2 1.358(6) . ?
O4 Tm1 2.312(3) 3_765 ?
O4W H4W1 0.85(5) . ?
O4W H4W2 0.85(5) . ?
O5 C7 1.266(6) . ?
O5 Tm1 2.395(4) 2_645 ?
O6 C7 1.257(6) . ?
O6 Tm1 2.365(3) 2_645 ?
C1 C6 1.381(7) . ?
C1 C2 1.412(7) . ?
C2 C3 1.390(7) . ?
C3 C4 1.376(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(7) . ?
C4 C7 1.491(7) . ?
C5 C6 1.390(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 Tm1 2.741(5) 2_645 ?

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
O4 Tm1 O4 70.34(14) . 3_765 ?
O4 Tm1 O1W 119.67(14) . . ?
O4 Tm1 O1W 88.28(13) 3_765 . ?
O4 Tm1 O3W 83.77(14) . . ?
O4 Tm1 O3W 77.75(13) 3_765 . ?
O1W Tm1 O3W 146.96(16) . . ?
O4 Tm1 O1 75.64(13) . . ?
O4 Tm1 O1 119.78(14) 3_765 . ?
O1W Tm1 O1 67.71(14) . . ?
O3W Tm1 O1 144.90(15) . . ?
O4 Tm1 O6 131.94(13) . 2_655 ?
O4 Tm1 O6 157.37(13) 3_765 2_655 ?
O1W Tm1 O6 82.86(14) . 2_655 ?
O3W Tm1 O6 98.68(13) . 2_655 ?
O1 Tm1 O6 75.82(14) . 2_655 ?
O4 Tm1 O2W 146.13(13) . . ?
O4 Tm1 O2W 79.98(14) 3_765 . ?
O1W Tm1 O2W 74.06(15) . . ?
O3W Tm1 O2W 74.10(16) . . ?
O1 Tm1 O2W 135.43(14) . . ?
O6 Tm1 O2W 77.57(14) 2_655 . ?
O4 Tm1 O5 82.34(12) . 2_655 ?
O4 Tm1 O5 139.72(12) 3_765 2_655 ?
O1W Tm1 O5 131.59(13) . 2_655 ?
O3W Tm1 O5 70.18(14) . 2_655 ?
O1 Tm1 O5 79.03(14) . 2_655 ?
O6 Tm1 O5 54.75(12) 2_655 2_655 ?
O2W Tm1 O5 112.60(14) . 2_655 ?
O4 Tm1 C7 107.61(15) . 2_655 ?
O4 Tm1 C7 161.81(14) 3_765 2_655 ?
O1W Tm1 C7 107.53(15) . 2_655 ?
O3W Tm1 C7 84.07(15) . 2_655 ?
O1 Tm1 C7 75.71(15) . 2_655 ?
O6 Tm1 C7 27.25(14) 2_655 2_655 ?
O2W Tm1 C7 95.45(15) . 2_655 ?
O5 Tm1 C7 27.50(13) 2_655 2_655 ?
O4 Tm1 Tm1 35.33(8) . 3_765 ?
O4 Tm1 Tm1 35.01(9) 3_765 3_765 ?
O1W Tm1 Tm1 106.45(11) . 3_765 ?
O3W Tm1 Tm1 78.67(10) . 3_765 ?
O1 Tm1 Tm1 98.85(9) . 3_765 ?
O6 Tm1 Tm1 166.89(9) 2_655 3_765 ?
O2W Tm1 Tm1 113.52(10) . 3_765 ?
O5 Tm1 Tm1 112.78(8) 2_655 3_765 ?
C7 Tm1 Tm1 140.15(12) 2_655 3_765 ?
O2 S1 O3 112.3(2) . . ?
O2 S1 O1 111.8(3) . . ?
O3 S1 O1 111.8(2) . . ?
O2 S1 C1 108.7(2) . . ?
O3 S1 C1 107.2(2) . . ?
O1 S1 C1 104.5(3) . . ?
Tm1 O1W H1W1 112(4) . . ?
Tm1 O1W H1W2 125(4) . . ?
H1W1 O1W H1W2 109.5(17) . . ?
S1 O1 Tm1 133.2(2) . . ?
Tm1 O2W H2W1 118(4) . . ?
Tm1 O2W H2W2 116(4) . . ?
H2W1 O2W H2W2 111.1(18) . . ?
Tm1 O3W H3W1 113(4) . . ?
Tm1 O3W H3W2 122(4) . . ?
H3W1 O3W H3W2 110.2(18) . . ?
C2 O4 Tm1 120.2(3) . . ?
C2 O4 Tm1 130.0(3) . 3_765 ?
Tm1 O4 Tm1 109.66(14) . 3_765 ?
H4W1 O4W H4W2 110.0(18) . . ?
C7 O5 Tm1 91.6(3) . 2_645 ?
C7 O6 Tm1 93.3(3) . 2_645 ?
C6 C1 C2 121.7(5) . . ?
C6 C1 S1 118.7(4) . . ?
C2 C1 S1 119.5(4) . . ?
O4 C2 C3 121.6(5) . . ?
O4 C2 C1 121.6(5) . . ?
C3 C2 C1 116.7(5) . . ?
C4 C3 C2 121.5(5) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 121.2(5) . . ?
C3 C4 C7 120.7(5) . . ?
C5 C4 C7 118.1(5) . . ?
C4 C5 C6 118.8(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C5 120.0(5) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
O6 C7 O5 120.3(5) . . ?
O6 C7 C4 120.1(5) . . ?
O5 C7 C4 119.6(5) . . ?
O6 C7 Tm1 59.5(3) . 2_645 ?
O5 C7 Tm1 60.9(3) . 2_645 ?
C4 C7 Tm1 179.5(4) . 2_645 ?

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 Tm1 -74.2(4) . . . . ?
O3 S1 O1 Tm1 158.9(3) . . . . ?
C1 S1 O1 Tm1 43.3(4) . . . . ?
O4 Tm1 O1 S1 -2.7(3) . . . . ?
O4 Tm1 O1 S1 54.2(4) 3_765 . . . ?
O1W Tm1 O1 S1 128.4(4) . . . . ?
O3W Tm1 O1 S1 -58.7(5) . . . . ?
O6 Tm1 O1 S1 -143.6(4) 2_655 . . . ?
O2W Tm1 O1 S1 161.4(3) . . . . ?
O5 Tm1 O1 S1 -87.5(3) 2_655 . . . ?
C7 Tm1 O1 S1 -115.5(4) 2_655 . . . ?
Tm1 Tm1 O1 S1 24.2(3) 3_765 . . . ?
O4 Tm1 O4 C2 176.3(5) 3_765 . . . ?
O1W Tm1 O4 C2 -107.6(4) . . . . ?
O3W Tm1 O4 C2 97.1(4) . . . . ?
O1 Tm1 O4 C2 -54.2(4) . . . . ?
O6 Tm1 O4 C2 1.0(4) 2_655 . . . ?
O2W Tm1 O4 C2 146.0(4) . . . . ?
O5 Tm1 O4 C2 26.4(4) 2_655 . . . ?
C7 Tm1 O4 C2 15.4(4) 2_655 . . . ?
Tm1 Tm1 O4 C2 176.3(5) 3_765 . . . ?
O4 Tm1 O4 Tm1 0.0 3_765 . . 3_765 ?
O1W Tm1 O4 Tm1 76.09(19) . . . 3_765 ?
O3W Tm1 O4 Tm1 -79.18(16) . . . 3_765 ?
O1 Tm1 O4 Tm1 129.48(18) . . . 3_765 ?
O6 Tm1 O4 Tm1 -175.27(14) 2_655 . . 3_765 ?
O2W Tm1 O4 Tm1 -30.3(3) . . . 3_765 ?
O5 Tm1 O4 Tm1 -149.94(17) 2_655 . . 3_765 ?
C7 Tm1 O4 Tm1 -160.92(15) 2_655 . . 3_765 ?
O2 S1 C1 C6 -112.9(5) . . . . ?
O3 S1 C1 C6 8.8(5) . . . . ?
O1 S1 C1 C6 127.6(5) . . . . ?
O2 S1 C1 C2 70.1(5) . . . . ?
O3 S1 C1 C2 -168.3(4) . . . . ?
O1 S1 C1 C2 -49.5(5) . . . . ?
Tm1 O4 C2 C3 -112.9(4) . . . . ?
Tm1 O4 C2 C3 62.5(7) 3_765 . . . ?
Tm1 O4 C2 C1 63.9(6) . . . . ?
Tm1 O4 C2 C1 -120.6(5) 3_765 . . . ?
C6 C1 C2 O4 -178.0(5) . . . . ?
S1 C1 C2 O4 -1.0(7) . . . . ?
C6 C1 C2 C3 -1.0(8) . . . . ?
S1 C1 C2 C3 175.9(4) . . . . ?
O4 C2 C3 C4 178.0(5) . . . . ?
C1 C2 C3 C4 1.0(8) . . . . ?
C2 C3 C4 C5 -0.8(8) . . . . ?
C2 C3 C4 C7 -179.8(5) . . . . ?
C3 C4 C5 C6 0.6(9) . . . . ?
C7 C4 C5 C6 179.6(5) . . . . ?
C2 C1 C6 C5 0.9(9) . . . . ?
S1 C1 C6 C5 -176.1(4) . . . . ?
C4 C5 C6 C1 -0.6(9) . . . . ?
Tm1 O6 C7 O5 0.4(5) 2_645 . . . ?
Tm1 O6 C7 C4 -179.6(4) 2_645 . . . ?
Tm1 O5 C7 O6 -0.4(5) 2_645 . . . ?
Tm1 O5 C7 C4 179.6(4) 2_645 . . . ?
C3 C4 C7 O6 151.4(5) . . . . ?
C5 C4 C7 O6 -27.6(8) . . . . ?
C3 C4 C7 O5 -28.6(8) . . . . ?
C5 C4 C7 O5 152.4(5) . . . . ?

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
O1W H1W1 O6 0.85(5) 2.10(3) 2.893(5) 154(5) 4_675
O1W H1W2 O4W 0.85(5) 1.892(16) 2.721(6) 165(5) 3_765
O2W H2W1 O2 0.85(5) 1.99(2) 2.801(6) 161(6) 4_676
O2W H2W2 O4W 0.85(5) 2.010(14) 2.840(6) 167(5) 3_765
O3W H3W1 O2 0.85(5) 1.880(17) 2.712(5) 167(6) 3_765
O3W H3W2 O3 0.85(5) 1.935(15) 2.776(5) 170(5) 4_676
O4W H4W1 O5 0.85(5) 2.016(15) 2.849(6) 167(5) .
O4W H4W2 O3 0.85(5) 2.17(4) 2.821(6) 134(5) 1_545

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.190
####################################################################### 
# 
# 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_6-Nd
_database_code_depnum_ccdc_archive 'CCDC 1549868'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 N2 Nd O7 S'
_chemical_formula_sum            'C19 H13 N2 Nd O7 S'
_chemical_formula_weight         557.61

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.9718(3)
_cell_length_b                   8.51291(18)
_cell_length_c                   18.0845(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0039(19)
_cell_angle_gamma                90.00
_cell_volume                     1795.82(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3117
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_T_max  0.6405
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6427
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4097
_reflns_number_gt                3498
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0285P)²+1.2142P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4097
_refine_ls_number_parameters     277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0721
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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 0.880633(16) 0.53909(2) 0.199935(10) 0.01638(7) Uani 1 1 d . . .
S1 S 0.81906(8) 0.12710(11) 0.17108(5) 0.0199(2) Uani 1 1 d . . .
O1 O 0.7699(2) 0.2814(3) 0.18045(15) 0.0256(6) Uani 1 1 d . . .
O1W O 0.8456(3) 0.7704(3) 0.27871(17) 0.0295(6) Uani 1 1 d D . .
H1W1 H 0.811(3) 0.846(3) 0.252(2) 0.044 Uiso 1 1 d D . .
H1W2 H 0.904(3) 0.809(4) 0.310(2) 0.044 Uiso 1 1 d D . .
O2 O 0.7372(3) 0.0003(3) 0.16697(16) 0.0297(7) Uani 1 1 d . . .
O3 O 0.9226(2) 0.0985(3) 0.23021(15) 0.0280(6) Uani 1 1 d . . .
O4 O 0.9601(2) 0.3796(3) 0.12242(14) 0.0232(6) Uani 1 1 d . . .
O5 O 0.9036(2) 0.0828(3) -0.18167(15) 0.0286(6) Uani 1 1 d . . .
O6 O 1.0369(2) 0.2604(3) -0.13375(14) 0.0251(6) Uani 1 1 d . . .
N1 N 0.7287(3) 0.6059(4) 0.07333(18) 0.0254(7) Uani 1 1 d . . .
N2 N 0.6615(3) 0.5680(4) 0.20564(19) 0.0252(7) Uani 1 1 d . . .
C1 C 0.8597(3) 0.1368(4) 0.0835(2) 0.0198(8) Uani 1 1 d . . .
C2 C 0.9242(3) 0.2695(4) 0.0701(2) 0.0195(8) Uani 1 1 d . . .
C3 C 0.9500(3) 0.2781(4) -0.0014(2) 0.0199(8) Uani 1 1 d . . .
H3 H 0.9898 0.3650 -0.0132 0.024 Uiso 1 1 calc R . .
C4 C 0.9178(3) 0.1608(4) -0.05564(19) 0.0179(7) Uani 1 1 d . . .
C5 C 0.8550(3) 0.0324(4) -0.0400(2) 0.0194(8) Uani 1 1 d . . .
H5 H 0.8329 -0.0462 -0.0760 0.023 Uiso 1 1 calc R . .
C6 C 0.8258(3) 0.0230(4) 0.0295(2) 0.0205(8) Uani 1 1 d . . .
H6 H 0.7826 -0.0616 0.0398 0.025 Uiso 1 1 calc R . .
C7 C 0.9557(3) 0.1708(4) -0.1298(2) 0.0186(8) Uani 1 1 d . . .
C8 C 0.7582(4) 0.6167(6) 0.0071(2) 0.0378(11) Uani 1 1 d . . .
H8 H 0.8324 0.5881 0.0050 0.045 Uiso 1 1 calc R . .
C9 C 0.6850(5) 0.6682(6) -0.0595(3) 0.0465(13) Uani 1 1 d . . .
H9 H 0.7096 0.6735 -0.1047 0.056 Uiso 1 1 calc R . .
C10 C 0.5774(5) 0.7100(6) -0.0569(3) 0.0535(15) Uani 1 1 d . . .
H10 H 0.5274 0.7459 -0.1006 0.064 Uiso 1 1 calc R . .
C11 C 0.5401(4) 0.7000(5) 0.0108(3) 0.0417(12) Uani 1 1 d . . .
C12 C 0.4275(5) 0.7381(7) 0.0169(4) 0.0622(17) Uani 1 1 d . . .
H12 H 0.3761 0.7797 -0.0248 0.075 Uiso 1 1 calc R . .
C13 C 0.3939(4) 0.7155(7) 0.0812(4) 0.0610(17) Uani 1 1 d . . .
H13 H 0.3191 0.7412 0.0832 0.073 Uiso 1 1 calc R . .
C14 C 0.4689(4) 0.6531(6) 0.1474(3) 0.0428(12) Uani 1 1 d . . .
C15 C 0.4366(4) 0.6164(7) 0.2144(3) 0.0519(14) Uani 1 1 d . . .
H15 H 0.3618 0.6360 0.2184 0.062 Uiso 1 1 calc R . .
C16 C 0.5112(5) 0.5532(6) 0.2735(3) 0.0464(13) Uani 1 1 d . . .
H16 H 0.4882 0.5238 0.3173 0.056 Uiso 1 1 calc R . .
C17 C 0.6255(4) 0.5329(5) 0.2671(3) 0.0363(11) Uani 1 1 d . . .
H17 H 0.6782 0.4926 0.3086 0.044 Uiso 1 1 calc R . .
C18 C 0.5842(3) 0.6238(5) 0.1446(2) 0.0281(9) Uani 1 1 d . . .
C19 C 0.6195(3) 0.6446(5) 0.0757(2) 0.0277(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
Nd1 O4 2.305(3) . ?
Nd1 O5 2.339(3) 4_566 ?
Nd1 O6 2.419(3) 3_765 ?
Nd1 O3 2.462(3) 2_755 ?
Nd1 O1W 2.520(3) . ?
Nd1 O1 2.546(3) . ?
Nd1 N1 2.646(3) . ?
Nd1 N2 2.660(3) . ?
S1 O2 1.449(3) . ?
S1 O3 1.464(3) . ?
S1 O1 1.464(3) . ?
S1 C1 1.760(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O3 Nd1 2.462(3) 2_745 ?
O4 C2 1.332(4) . ?
O5 C7 1.252(4) . ?
O5 Nd1 2.339(3) 4_565 ?
O6 C7 1.250(4) . ?
O6 Nd1 2.419(3) 3_765 ?
N1 C8 1.326(5) . ?
N1 C19 1.359(5) . ?
N2 C17 1.314(6) . ?
N2 C18 1.357(5) . ?
C1 C6 1.371(5) . ?
C1 C2 1.419(5) . ?
C2 C3 1.398(5) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(5) . ?
C4 C7 1.512(5) . ?
C5 C6 1.381(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.392(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.347(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(8) . ?
C10 H10 0.9300 . ?
C11 C19 1.415(6) . ?
C11 C12 1.415(8) . ?
C12 C13 1.326(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.428(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(7) . ?
C14 C18 1.415(6) . ?
C15 C16 1.341(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.410(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.414(6) . ?

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
O4 Nd1 O5 108.41(10) . 4_566 ?
O4 Nd1 O6 81.06(9) . 3_765 ?
O5 Nd1 O6 142.07(10) 4_566 3_765 ?
O4 Nd1 O3 87.43(9) . 2_755 ?
O5 Nd1 O3 73.72(10) 4_566 2_755 ?
O6 Nd1 O3 70.05(9) 3_765 2_755 ?
O4 Nd1 O1W 161.43(9) . . ?
O5 Nd1 O1W 80.17(10) 4_566 . ?
O6 Nd1 O1W 82.35(9) 3_765 . ?
O3 Nd1 O1W 79.11(10) 2_755 . ?
O4 Nd1 O1 71.42(9) . . ?
O5 Nd1 O1 72.23(9) 4_566 . ?
O6 Nd1 O1 142.85(9) 3_765 . ?
O3 Nd1 O1 131.01(9) 2_755 . ?
O1W Nd1 O1 127.14(9) . . ?
O4 Nd1 N1 84.12(10) . . ?
O5 Nd1 N1 143.51(10) 4_566 . ?
O6 Nd1 N1 72.41(10) 3_765 . ?
O3 Nd1 N1 142.36(10) 2_755 . ?
O1W Nd1 N1 98.74(10) . . ?
O1 Nd1 N1 80.24(9) . . ?
O4 Nd1 N2 128.58(9) . . ?
O5 Nd1 N2 85.38(10) 4_566 . ?
O6 Nd1 N2 118.02(10) 3_765 . ?
O3 Nd1 N2 143.05(10) 2_755 . ?
O1W Nd1 N2 67.34(10) . . ?
O1 Nd1 N2 66.30(9) . . ?
N1 Nd1 N2 61.43(10) . . ?
O2 S1 O3 111.45(17) . . ?
O2 S1 O1 112.92(17) . . ?
O3 S1 O1 111.14(17) . . ?
O2 S1 C1 108.05(18) . . ?
O3 S1 C1 107.74(17) . . ?
O1 S1 C1 105.16(17) . . ?
S1 O1 Nd1 125.36(15) . . ?
Nd1 O1W H1W1 113(3) . . ?
Nd1 O1W H1W2 117(3) . . ?
H1W1 O1W H1W2 107.7(16) . . ?
S1 O3 Nd1 164.61(17) . 2_745 ?
C2 O4 Nd1 137.3(2) . . ?
C7 O5 Nd1 152.6(3) . 4_565 ?
C7 O6 Nd1 150.2(2) . 3_765 ?
C8 N1 C19 117.7(4) . . ?
C8 N1 Nd1 121.7(3) . . ?
C19 N1 Nd1 120.3(3) . . ?
C17 N2 C18 118.3(4) . . ?
C17 N2 Nd1 121.7(3) . . ?
C18 N2 Nd1 120.0(3) . . ?
C6 C1 C2 121.7(3) . . ?
C6 C1 S1 120.7(3) . . ?
C2 C1 S1 117.5(3) . . ?
O4 C2 C3 121.2(3) . . ?
O4 C2 C1 122.6(3) . . ?
C3 C2 C1 116.2(3) . . ?
C4 C3 C2 122.0(3) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 C7 120.6(3) . . ?
C3 C4 C7 119.6(3) . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C1 C6 C5 120.9(4) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
O6 C7 O5 125.8(3) . . ?
O6 C7 C4 118.5(3) . . ?
O5 C7 C4 115.6(3) . . ?
N1 C8 C9 124.0(5) . . ?
N1 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
C10 C9 C8 118.3(5) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
C9 C10 C11 120.8(4) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C19 117.4(5) . . ?
C10 C11 C12 123.6(5) . . ?
C19 C11 C12 119.0(5) . . ?
C13 C12 C11 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 122.1(5) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C15 C14 C18 117.2(5) . . ?
C15 C14 C13 124.8(5) . . ?
C18 C14 C13 118.0(5) . . ?
C16 C15 C14 121.4(5) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 117.9(5) . . ?
C15 C16 H16 121.0 . . ?
C17 C16 H16 121.0 . . ?
N2 C17 C16 123.4(5) . . ?
N2 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
N2 C18 C19 118.4(4) . . ?
N2 C18 C14 121.7(4) . . ?
C19 C18 C14 119.8(4) . . ?
N1 C19 C18 118.6(3) . . ?
N1 C19 C11 121.8(4) . . ?
C18 C19 C11 119.7(4) . . ?

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 Nd1 175.46(17) . . . . ?
O3 S1 O1 Nd1 49.4(2) . . . . ?
C1 S1 O1 Nd1 -67.0(2) . . . . ?
O4 Nd1 O1 S1 33.35(18) . . . . ?
O5 Nd1 O1 S1 -83.88(19) 4_566 . . . ?
O6 Nd1 O1 S1 77.7(2) 3_765 . . . ?
O3 Nd1 O1 S1 -35.8(2) 2_755 . . . ?
O1W Nd1 O1 S1 -146.00(16) . . . . ?
N1 Nd1 O1 S1 120.4(2) . . . . ?
N2 Nd1 O1 S1 -176.6(2) . . . . ?
O2 S1 O3 Nd1 108.6(7) . . . 2_745 ?
O1 S1 O3 Nd1 -124.5(7) . . . 2_745 ?
C1 S1 O3 Nd1 -9.8(7) . . . 2_745 ?
O5 Nd1 O4 C2 95.2(3) 4_566 . . . ?
O6 Nd1 O4 C2 -122.7(3) 3_765 . . . ?
O3 Nd1 O4 C2 167.1(3) 2_755 . . . ?
O1W Nd1 O4 C2 -149.6(3) . . . . ?
O1 Nd1 O4 C2 32.0(3) . . . . ?
N1 Nd1 O4 C2 -49.6(3) . . . . ?
N2 Nd1 O4 C2 -3.8(4) . . . . ?
O4 Nd1 N1 C8 -36.0(3) . . . . ?
O5 Nd1 N1 C8 -149.2(3) 4_566 . . . ?
O6 Nd1 N1 C8 46.5(3) 3_765 . . . ?
O3 Nd1 N1 C8 42.1(4) 2_755 . . . ?
O1W Nd1 N1 C8 125.5(3) . . . . ?
O1 Nd1 N1 C8 -108.1(3) . . . . ?
N2 Nd1 N1 C8 -176.3(4) . . . . ?
O4 Nd1 N1 C19 150.2(3) . . . . ?
O5 Nd1 N1 C19 36.9(4) 4_566 . . . ?
O6 Nd1 N1 C19 -127.4(3) 3_765 . . . ?
O3 Nd1 N1 C19 -131.8(3) 2_755 . . . ?
O1W Nd1 N1 C19 -48.3(3) . . . . ?
O1 Nd1 N1 C19 78.1(3) . . . . ?
N2 Nd1 N1 C19 9.8(3) . . . . ?
O4 Nd1 N2 C17 117.9(3) . . . . ?
O5 Nd1 N2 C17 8.0(3) 4_566 . . . ?
O6 Nd1 N2 C17 -140.6(3) 3_765 . . . ?
O3 Nd1 N2 C17 -46.9(4) 2_755 . . . ?
O1W Nd1 N2 C17 -73.3(3) . . . . ?
O1 Nd1 N2 C17 80.6(3) . . . . ?
N1 Nd1 N2 C17 172.2(4) . . . . ?
O4 Nd1 N2 C18 -63.7(3) . . . . ?
O5 Nd1 N2 C18 -173.6(3) 4_566 . . . ?
O6 Nd1 N2 C18 37.8(3) 3_765 . . . ?
O3 Nd1 N2 C18 131.5(3) 2_755 . . . ?
O1W Nd1 N2 C18 105.1(3) . . . . ?
O1 Nd1 N2 C18 -101.0(3) . . . . ?
N1 Nd1 N2 C18 -9.4(3) . . . . ?
O2 S1 C1 C6 -8.0(4) . . . . ?
O3 S1 C1 C6 112.5(3) . . . . ?
O1 S1 C1 C6 -128.8(3) . . . . ?
O2 S1 C1 C2 169.4(3) . . . . ?
O3 S1 C1 C2 -70.1(3) . . . . ?
O1 S1 C1 C2 48.5(3) . . . . ?
Nd1 O4 C2 C3 128.2(3) . . . . ?
Nd1 O4 C2 C1 -52.7(5) . . . . ?
C6 C1 C2 O4 -178.5(3) . . . . ?
S1 C1 C2 O4 4.1(5) . . . . ?
C6 C1 C2 C3 0.7(5) . . . . ?
S1 C1 C2 C3 -176.7(3) . . . . ?
O4 C2 C3 C4 177.0(3) . . . . ?
C1 C2 C3 C4 -2.2(5) . . . . ?
C2 C3 C4 C5 2.0(5) . . . . ?
C2 C3 C4 C7 -175.5(3) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C7 C4 C5 C6 177.2(3) . . . . ?
C2 C1 C6 C5 1.0(6) . . . . ?
S1 C1 C6 C5 178.3(3) . . . . ?
C4 C5 C6 C1 -1.2(6) . . . . ?
Nd1 O6 C7 O5 48.7(7) 3_765 . . . ?
Nd1 O6 C7 C4 -133.7(4) 3_765 . . . ?
Nd1 O5 C7 O6 9.8(8) 4_565 . . . ?
Nd1 O5 C7 C4 -167.9(4) 4_565 . . . ?
C5 C4 C7 O6 -160.0(3) . . . . ?
C3 C4 C7 O6 17.5(5) . . . . ?
C5 C4 C7 O5 17.9(5) . . . . ?
C3 C4 C7 O5 -164.7(3) . . . . ?
C19 N1 C8 C9 1.4(7) . . . . ?
Nd1 N1 C8 C9 -172.6(4) . . . . ?
N1 C8 C9 C10 0.1(8) . . . . ?
C8 C9 C10 C11 -0.8(8) . . . . ?
C9 C10 C11 C19 0.0(7) . . . . ?
C9 C10 C11 C12 -178.3(5) . . . . ?
C10 C11 C12 C13 174.9(6) . . . . ?
C19 C11 C12 C13 -3.3(9) . . . . ?
C11 C12 C13 C14 0.4(10) . . . . ?
C12 C13 C14 C15 -175.2(6) . . . . ?
C12 C13 C14 C18 3.8(9) . . . . ?
C18 C14 C15 C16 -1.1(8) . . . . ?
C13 C14 C15 C16 177.8(5) . . . . ?
C14 C15 C16 C17 3.4(8) . . . . ?
C18 N2 C17 C16 -1.3(7) . . . . ?
Nd1 N2 C17 C16 177.1(3) . . . . ?
C15 C16 C17 N2 -2.2(7) . . . . ?
C17 N2 C18 C19 -172.9(4) . . . . ?
Nd1 N2 C18 C19 8.7(5) . . . . ?
C17 N2 C18 C14 3.7(6) . . . . ?
Nd1 N2 C18 C14 -174.7(3) . . . . ?
C15 C14 C18 N2 -2.5(7) . . . . ?
C13 C14 C18 N2 178.4(4) . . . . ?
C15 C14 C18 C19 174.0(4) . . . . ?
C13 C14 C18 C19 -5.0(7) . . . . ?
C8 N1 C19 C18 175.8(4) . . . . ?
Nd1 N1 C19 C18 -10.1(5) . . . . ?
C8 N1 C19 C11 -2.2(6) . . . . ?
Nd1 N1 C19 C11 171.9(3) . . . . ?
N2 C18 C19 N1 0.9(6) . . . . ?
C14 C18 C19 N1 -175.8(4) . . . . ?
N2 C18 C19 C11 178.9(4) . . . . ?
C14 C18 C19 C11 2.3(6) . . . . ?
C10 C11 C19 N1 1.5(7) . . . . ?
C12 C11 C19 N1 179.9(5) . . . . ?
C10 C11 C19 C18 -176.4(4) . . . . ?
C12 C11 C19 C18 1.9(7) . . . . ?

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
O1W H1W1 O2 0.85(4) 2.065(15) 2.902(4) 166(5) 1_565
O1W H1W1 O3 0.85(4) 2.61(4) 3.129(4) 120(3) 1_565
O1W H1W2 O4 0.85(4) 1.902(11) 2.757(4) 176(4) 2_755

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.094
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_6-La
_database_code_depnum_ccdc_archive 'CCDC 1549866'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 La N2 O7 S'
_chemical_formula_sum            'C19 H13 La N2 O7 S'
_chemical_formula_weight         552.28

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   12.0291(4)
_cell_length_b                   8.5249(3)
_cell_length_c                   18.2684(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.318(3)
_cell_angle_gamma                90.00
_cell_volume                     1830.24(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3170
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5974
_exptl_absorpt_correction_T_max  0.7058
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6444
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4176
_reflns_number_gt                3500
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0102P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4176
_refine_ls_number_parameters     277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0591
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
La1 La 0.880376(14) 0.45877(2) 0.200492(11) 0.01576(6) Uani 1 1 d . . .
S1 S 1.18189(6) 0.37294(10) 0.32952(5) 0.01817(18) Uani 1 1 d . . .
O1 O 1.07859(18) 0.3988(3) 0.27157(13) 0.0252(6) Uani 1 1 d . . .
O1W O 0.8430(2) 0.2238(3) 0.28204(15) 0.0285(6) Uani 1 1 d D . .
H1W1 H 0.808(2) 0.149(3) 0.2571(19) 0.043 Uiso 1 1 d D . .
H1W2 H 0.901(2) 0.190(3) 0.3125(17) 0.043 Uiso 1 1 d D . .
O2 O 1.23255(17) 0.2205(3) 0.32049(14) 0.0227(5) Uani 1 1 d . . .
O3 O 1.26196(19) 0.5011(3) 0.33252(14) 0.0268(6) Uani 1 1 d . . .
O4 O 1.03927(17) 0.1246(3) 0.37851(13) 0.0208(5) Uani 1 1 d . . .
O5 O 0.96516(18) 0.2432(3) 0.63292(14) 0.0240(5) Uani 1 1 d . . .
O6 O 1.09964(19) 0.4180(3) 0.67966(14) 0.0267(6) Uani 1 1 d . . .
N1 N 0.6571(2) 0.4258(3) 0.20416(18) 0.0262(7) Uani 1 1 d . . .
N2 N 0.7260(2) 0.3927(3) 0.07226(17) 0.0244(7) Uani 1 1 d . . .
C1 C 1.1409(2) 0.3631(4) 0.41593(18) 0.0159(7) Uani 1 1 d . . .
C2 C 1.0751(2) 0.2329(4) 0.42997(19) 0.0165(7) Uani 1 1 d . . .
C3 C 1.0498(3) 0.2260(4) 0.50088(19) 0.0181(7) Uani 1 1 d . . .
H3 H 1.0094 0.1401 0.5128 0.022 Uiso 1 1 calc R . .
C4 C 1.0824(3) 0.3418(4) 0.55417(19) 0.0181(7) Uani 1 1 d . . .
C5 C 1.1468(2) 0.4680(4) 0.53867(19) 0.0170(7) Uani 1 1 d . . .
H5 H 1.1701 0.5455 0.5745 0.020 Uiso 1 1 calc R . .
C6 C 1.1760(2) 0.4774(4) 0.46984(19) 0.0174(7) Uani 1 1 d . . .
H6 H 1.2197 0.5612 0.4595 0.021 Uiso 1 1 calc R . .
C7 C 1.0458(3) 0.3329(4) 0.6275(2) 0.0193(7) Uani 1 1 d . . .
C8 C 0.6204(3) 0.4585(5) 0.2653(3) 0.0378(10) Uani 1 1 d . . .
H8 H 0.6722 0.4970 0.3066 0.045 Uiso 1 1 calc R . .
C9 C 0.5061(4) 0.4380(5) 0.2714(3) 0.0467(12) Uani 1 1 d . . .
H9 H 0.4828 0.4659 0.3150 0.056 Uiso 1 1 calc R . .
C10 C 0.4317(3) 0.3770(5) 0.2124(3) 0.0499(13) Uani 1 1 d . . .
H10 H 0.3567 0.3589 0.2159 0.060 Uiso 1 1 calc R . .
C11 C 0.4662(3) 0.3414(5) 0.1468(3) 0.0417(12) Uani 1 1 d . . .
C12 C 0.3917(4) 0.2828(6) 0.0806(3) 0.0612(16) Uani 1 1 d . . .
H12 H 0.3167 0.2591 0.0821 0.073 Uiso 1 1 calc R . .
C13 C 0.4268(4) 0.2613(6) 0.0169(3) 0.0656(17) Uani 1 1 d . . .
H13 H 0.3763 0.2202 -0.0243 0.079 Uiso 1 1 calc R . .
C14 C 0.5398(3) 0.2996(5) 0.0102(3) 0.0426(12) Uani 1 1 d . . .
C15 C 0.5774(4) 0.2912(5) -0.0564(3) 0.0538(14) Uani 1 1 d . . .
H15 H 0.5284 0.2555 -0.0996 0.065 Uiso 1 1 calc R . .
C16 C 0.6848(4) 0.3345(5) -0.0590(3) 0.0471(12) Uani 1 1 d . . .
H16 H 0.7100 0.3315 -0.1037 0.056 Uiso 1 1 calc R . .
C17 C 0.7567(3) 0.3836(5) 0.0074(2) 0.0346(10) Uani 1 1 d . . .
H17 H 0.8308 0.4117 0.0057 0.041 Uiso 1 1 calc R . .
C18 C 0.6169(3) 0.3529(4) 0.0750(2) 0.0280(9) Uani 1 1 d . . .
C19 C 0.5806(3) 0.3718(4) 0.1437(2) 0.0264(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
La1 O4 2.369(2) 2_755 ?
La1 O6 2.394(2) 3_766 ?
La1 O5 2.463(2) 4_565 ?
La1 O1 2.512(2) . ?
La1 O1W 2.592(3) . ?
La1 O2 2.598(2) 2_755 ?
La1 N1 2.715(3) . ?
La1 N2 2.720(3) . ?
S1 O3 1.450(2) . ?
S1 O2 1.459(2) . ?
S1 O1 1.467(2) . ?
S1 C1 1.753(3) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O2 La1 2.598(2) 2_745 ?
O4 C2 1.323(4) . ?
O4 La1 2.369(2) 2_745 ?
O5 C7 1.256(4) . ?
O5 La1 2.463(2) 4_566 ?
O6 C7 1.261(4) . ?
O6 La1 2.394(2) 3_766 ?
N1 C8 1.316(5) . ?
N1 C19 1.359(5) . ?
N2 C17 1.316(5) . ?
N2 C18 1.367(4) . ?
C1 C6 1.386(4) . ?
C1 C2 1.418(4) . ?
C2 C3 1.394(4) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(4) . ?
C4 C7 1.498(5) . ?
C5 C6 1.378(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.413(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.350(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(6) . ?
C10 H10 0.9300 . ?
C11 C19 1.413(5) . ?
C11 C12 1.434(6) . ?
C12 C13 1.331(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.429(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(7) . ?
C14 C18 1.414(5) . ?
C15 C16 1.354(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(5) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.422(5) . ?

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
O4 La1 O6 108.72(8) 2_755 3_766 ?
O4 La1 O5 81.10(8) 2_755 4_565 ?
O6 La1 O5 142.54(8) 3_766 4_565 ?
O4 La1 O1 88.33(8) 2_755 . ?
O6 La1 O1 73.60(8) 3_766 . ?
O5 La1 O1 70.60(8) 4_565 . ?
O4 La1 O1W 162.66(8) 2_755 . ?
O6 La1 O1W 79.02(8) 3_766 . ?
O5 La1 O1W 83.61(8) 4_565 . ?
O1 La1 O1W 78.89(8) . . ?
O4 La1 O2 70.49(7) 2_755 2_755 ?
O6 La1 O2 72.86(8) 3_766 2_755 ?
O5 La1 O2 141.80(8) 4_565 2_755 ?
O1 La1 O2 131.29(7) . 2_755 ?
O1W La1 O2 126.83(7) . 2_755 ?
O4 La1 N1 127.67(8) 2_755 . ?
O6 La1 N1 85.97(9) 3_766 . ?
O5 La1 N1 117.22(8) 4_565 . ?
O1 La1 N1 143.21(9) . . ?
O1W La1 N1 67.19(8) . . ?
O2 La1 N1 66.66(8) 2_755 . ?
O4 La1 N2 83.74(8) 2_755 . ?
O6 La1 N2 142.71(8) 3_766 . ?
O5 La1 N2 72.73(8) 4_565 . ?
O1 La1 N2 143.25(8) . . ?
O1W La1 N2 99.49(8) . . ?
O2 La1 N2 79.13(8) 2_755 . ?
N1 La1 N2 60.18(9) . . ?
O3 S1 O2 112.66(14) . . ?
O3 S1 O1 111.58(15) . . ?
O2 S1 O1 111.22(14) . . ?
O3 S1 C1 108.31(15) . . ?
O2 S1 C1 105.27(15) . . ?
O1 S1 C1 107.42(14) . . ?
S1 O1 La1 165.45(15) . . ?
La1 O1W H1W1 114(3) . . ?
La1 O1W H1W2 115(3) . . ?
H1W1 O1W H1W2 110.7(17) . . ?
S1 O2 La1 124.31(12) . 2_745 ?
C2 O4 La1 137.39(19) . 2_745 ?
C7 O5 La1 151.0(2) . 4_566 ?
C7 O6 La1 151.5(2) . 3_766 ?
C8 N1 C19 118.1(3) . . ?
C8 N1 La1 120.8(3) . . ?
C19 N1 La1 121.1(2) . . ?
C17 N2 C18 118.3(3) . . ?
C17 N2 La1 121.1(2) . . ?
C18 N2 La1 120.2(2) . . ?
C6 C1 C2 121.3(3) . . ?
C6 C1 S1 120.3(2) . . ?
C2 C1 S1 118.4(2) . . ?
O4 C2 C3 121.9(3) . . ?
O4 C2 C1 121.9(3) . . ?
C3 C2 C1 116.2(3) . . ?
C4 C3 C2 122.6(3) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 C7 120.0(3) . . ?
C5 C4 C7 120.3(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O5 C7 O6 124.8(3) . . ?
O5 C7 C4 118.7(3) . . ?
O6 C7 C4 116.4(3) . . ?
N1 C8 C9 123.3(4) . . ?
N1 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
C10 C9 C8 118.4(4) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C9 C10 C11 120.4(4) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C19 118.1(4) . . ?
C10 C11 C12 124.0(4) . . ?
C19 C11 C12 117.9(5) . . ?
C13 C12 C11 121.8(4) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 121.9(4) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C18 118.2(4) . . ?
C15 C14 C13 123.9(4) . . ?
C18 C14 C13 117.9(5) . . ?
C16 C15 C14 120.6(4) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 118.0(4) . . ?
C15 C16 H16 121.0 . . ?
C17 C16 H16 121.0 . . ?
N2 C17 C16 124.1(4) . . ?
N2 C17 H17 118.0 . . ?
C16 C17 H17 118.0 . . ?
N2 C18 C14 120.8(4) . . ?
N2 C18 C19 118.9(3) . . ?
C14 C18 C19 120.3(4) . . ?
N1 C19 C11 121.7(4) . . ?
N1 C19 C18 118.2(3) . . ?
C11 C19 C18 120.0(4) . . ?

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
O3 S1 O1 La1 -104.8(6) . . . . ?
O2 S1 O1 La1 128.5(6) . . . . ?
C1 S1 O1 La1 13.8(6) . . . . ?
O4 La1 O1 S1 131.0(6) 2_755 . . . ?
O6 La1 O1 S1 20.9(6) 3_766 . . . ?
O5 La1 O1 S1 -147.9(6) 4_565 . . . ?
O1W La1 O1 S1 -60.8(6) . . . . ?
O2 La1 O1 S1 69.0(6) 2_755 . . . ?
N1 La1 O1 S1 -38.1(7) . . . . ?
N2 La1 O1 S1 -151.8(5) . . . . ?
O3 S1 O2 La1 -173.92(15) . . . 2_745 ?
O1 S1 O2 La1 -47.8(2) . . . 2_745 ?
C1 S1 O2 La1 68.25(18) . . . 2_745 ?
O4 La1 N1 C8 -119.3(3) 2_755 . . . ?
O6 La1 N1 C8 -8.7(3) 3_766 . . . ?
O5 La1 N1 C8 140.5(3) 4_565 . . . ?
O1 La1 N1 C8 46.8(3) . . . . ?
O1W La1 N1 C8 71.1(3) . . . . ?
O2 La1 N1 C8 -81.7(3) 2_755 . . . ?
N2 La1 N1 C8 -172.3(3) . . . . ?
O4 La1 N1 C19 62.2(3) 2_755 . . . ?
O6 La1 N1 C19 172.8(3) 3_766 . . . ?
O5 La1 N1 C19 -38.0(3) 4_565 . . . ?
O1 La1 N1 C19 -131.7(2) . . . . ?
O1W La1 N1 C19 -107.4(3) . . . . ?
O2 La1 N1 C19 99.8(3) 2_755 . . . ?
N2 La1 N1 C19 9.2(2) . . . . ?
O4 La1 N2 C17 36.3(3) 2_755 . . . ?
O6 La1 N2 C17 149.2(3) 3_766 . . . ?
O5 La1 N2 C17 -46.3(3) 4_565 . . . ?
O1 La1 N2 C17 -42.4(3) . . . . ?
O1W La1 N2 C17 -126.5(3) . . . . ?
O2 La1 N2 C17 107.5(3) 2_755 . . . ?
N1 La1 N2 C17 176.7(3) . . . . ?
O4 La1 N2 C18 -150.2(3) 2_755 . . . ?
O6 La1 N2 C18 -37.3(3) 3_766 . . . ?
O5 La1 N2 C18 127.2(3) 4_565 . . . ?
O1 La1 N2 C18 131.1(2) . . . . ?
O1W La1 N2 C18 47.0(3) . . . . ?
O2 La1 N2 C18 -79.0(2) 2_755 . . . ?
N1 La1 N2 C18 -9.7(2) . . . . ?
O3 S1 C1 C6 6.4(3) . . . . ?
O2 S1 C1 C6 127.1(3) . . . . ?
O1 S1 C1 C6 -114.3(3) . . . . ?
O3 S1 C1 C2 -171.3(2) . . . . ?
O2 S1 C1 C2 -50.6(3) . . . . ?
O1 S1 C1 C2 68.1(3) . . . . ?
La1 O4 C2 C3 -127.6(3) 2_745 . . . ?
La1 O4 C2 C1 52.8(4) 2_745 . . . ?
C6 C1 C2 O4 178.7(3) . . . . ?
S1 C1 C2 O4 -3.7(4) . . . . ?
C6 C1 C2 C3 -0.9(4) . . . . ?
S1 C1 C2 C3 176.7(2) . . . . ?
O4 C2 C3 C4 -177.1(3) . . . . ?
C1 C2 C3 C4 2.5(4) . . . . ?
C2 C3 C4 C5 -2.6(5) . . . . ?
C2 C3 C4 C7 175.9(3) . . . . ?
C3 C4 C5 C6 1.0(5) . . . . ?
C7 C4 C5 C6 -177.5(3) . . . . ?
C4 C5 C6 C1 0.6(5) . . . . ?
C2 C1 C6 C5 -0.6(5) . . . . ?
S1 C1 C6 C5 -178.1(2) . . . . ?
La1 O5 C7 O6 -46.2(6) 4_566 . . . ?
La1 O5 C7 C4 134.0(4) 4_566 . . . ?
La1 O6 C7 O5 -14.8(7) 3_766 . . . ?
La1 O6 C7 C4 165.1(3) 3_766 . . . ?
C3 C4 C7 O5 -16.9(4) . . . . ?
C5 C4 C7 O5 161.6(3) . . . . ?
C3 C4 C7 O6 163.3(3) . . . . ?
C5 C4 C7 O6 -18.2(4) . . . . ?
C19 N1 C8 C9 1.0(6) . . . . ?
La1 N1 C8 C9 -177.6(3) . . . . ?
N1 C8 C9 C10 2.3(6) . . . . ?
C8 C9 C10 C11 -2.4(7) . . . . ?
C9 C10 C11 C19 -0.5(6) . . . . ?
C9 C10 C11 C12 -177.2(4) . . . . ?
C10 C11 C12 C13 174.8(5) . . . . ?
C19 C11 C12 C13 -1.9(7) . . . . ?
C11 C12 C13 C14 -1.8(8) . . . . ?
C12 C13 C14 C15 -174.6(5) . . . . ?
C12 C13 C14 C18 3.8(7) . . . . ?
C18 C14 C15 C16 -0.6(7) . . . . ?
C13 C14 C15 C16 177.8(4) . . . . ?
C14 C15 C16 C17 1.6(7) . . . . ?
C18 N2 C17 C16 -0.6(6) . . . . ?
La1 N2 C17 C16 173.1(3) . . . . ?
C15 C16 C17 N2 -1.0(7) . . . . ?
C17 N2 C18 C14 1.6(5) . . . . ?
La1 N2 C18 C14 -172.1(3) . . . . ?
C17 N2 C18 C19 -176.0(3) . . . . ?
La1 N2 C18 C19 10.3(4) . . . . ?
C15 C14 C18 N2 -1.0(6) . . . . ?
C13 C14 C18 N2 -179.5(4) . . . . ?
C15 C14 C18 C19 176.5(4) . . . . ?
C13 C14 C18 C19 -2.0(6) . . . . ?
C8 N1 C19 C11 -4.0(5) . . . . ?
La1 N1 C19 C11 174.5(3) . . . . ?
C8 N1 C19 C18 173.1(3) . . . . ?
La1 N1 C19 C18 -8.3(4) . . . . ?
C10 C11 C19 N1 3.8(6) . . . . ?
C12 C11 C19 N1 -179.2(4) . . . . ?
C10 C11 C19 C18 -173.3(4) . . . . ?
C12 C11 C19 C18 3.7(6) . . . . ?
N2 C18 C19 N1 -1.4(5) . . . . ?
C14 C18 C19 N1 -178.9(3) . . . . ?
N2 C18 C19 C11 175.9(3) . . . . ?
C14 C18 C19 C11 -1.7(5) . . . . ?

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
O1W H1W1 O3 0.85(4) 2.094(16) 2.907(4) 162(4) 2_745
O1W H1W1 O1 0.85(4) 2.65(3) 3.149(3) 119(3) 2_745
O1W H1W2 O4 0.85(4) 1.915(10) 2.760(3) 176(4) .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_6-Pr
_database_code_depnum_ccdc_archive 'CCDC 1549867'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 N2 O7 Pr S'
_chemical_formula_sum            'C19 H13 N2 O7 Pr S'
_chemical_formula_weight         554.28

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.9937(4)
_cell_length_b                   8.5177(2)
_cell_length_c                   18.1162(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.778(3)
_cell_angle_gamma                90.00
_cell_volume                     1804.89(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2600
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    2.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5845
_exptl_absorpt_correction_T_max  0.6416
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6322
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4122
_reflns_number_gt                3502
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0240P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4122
_refine_ls_number_parameters     277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_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
Pr1 Pr 0.380547(16) 1.03985(2) 0.199969(9) 0.01504(7) Uani 1 1 d . . .
S1 S 0.68146(8) 1.12708(11) 0.32895(4) 0.01741(19) Uani 1 1 d . . .
O1W O 0.3450(2) 1.2725(3) 0.27967(14) 0.0266(6) Uani 1 1 d D . .
H1W1 H 0.305(3) 1.346(3) 0.256(2) 0.040 Uiso 1 1 d D . .
H1W2 H 0.405(2) 1.309(4) 0.308(2) 0.040 Uiso 1 1 d D . .
O1 O 0.5778(2) 1.0994(3) 0.27026(13) 0.0247(6) Uani 1 1 d . . .
O2 O 0.7309(2) 1.2808(3) 0.31960(13) 0.0234(6) Uani 1 1 d . . .
O3 O 0.7632(2) 1.0001(3) 0.33263(14) 0.0260(6) Uani 1 1 d . . .
O4 O 0.5396(2) 1.3777(3) 0.37779(12) 0.0212(5) Uani 1 1 d . . .
O5 O 0.5971(2) 1.0832(3) 0.68134(13) 0.0269(6) Uani 1 1 d . . .
O6 O 0.4630(2) 1.2588(3) 0.63355(13) 0.0241(6) Uani 1 1 d . . .
N1 N 0.1607(3) 1.0702(4) 0.20520(17) 0.0239(7) Uani 1 1 d . . .
N2 N 0.2283(3) 1.1066(4) 0.07300(16) 0.0248(7) Uani 1 1 d . . .
C1 C 0.6402(3) 1.1375(4) 0.41644(17) 0.0156(7) Uani 1 1 d . . .
C2 C 0.5756(3) 1.2674(4) 0.42962(18) 0.0180(7) Uani 1 1 d . . .
C3 C 0.5493(3) 1.2771(4) 0.50149(18) 0.0188(7) Uani 1 1 d . . .
H3 H 0.5093 1.3636 0.5133 0.023 Uiso 1 1 calc R . .
C4 C 0.5821(3) 1.1596(4) 0.55510(17) 0.0161(7) Uani 1 1 d . . .
C5 C 0.6453(3) 1.0317(4) 0.53975(19) 0.0181(8) Uani 1 1 d . . .
H5 H 0.6671 0.9532 0.5757 0.022 Uiso 1 1 calc R . .
C6 C 0.6754(3) 1.0222(4) 0.47043(19) 0.0175(7) Uani 1 1 d . . .
H6 H 0.7192 0.9384 0.4601 0.021 Uiso 1 1 calc R . .
C7 C 0.5439(3) 1.1702(4) 0.62885(18) 0.0181(8) Uani 1 1 d . . .
C8 C 0.1226(4) 1.0365(5) 0.2666(2) 0.0340(10) Uani 1 1 d . . .
H8 H 0.1747 0.9971 0.3083 0.041 Uiso 1 1 calc R . .
C9 C 0.0102(4) 1.0560(6) 0.2728(3) 0.0416(12) Uani 1 1 d . . .
H9 H -0.0125 1.0265 0.3167 0.050 Uiso 1 1 calc R . .
C10 C -0.0657(4) 1.1192(6) 0.2136(3) 0.0461(12) Uani 1 1 d . . .
H10 H -0.1406 1.1381 0.2173 0.055 Uiso 1 1 calc R . .
C11 C -0.0310(4) 1.1557(5) 0.1469(3) 0.0387(11) Uani 1 1 d . . .
C12 C -0.1072(4) 1.2169(7) 0.0806(3) 0.0579(15) Uani 1 1 d . . .
H12 H -0.1818 1.2426 0.0827 0.069 Uiso 1 1 calc R . .
C13 C -0.0725(5) 1.2376(7) 0.0159(3) 0.0604(16) Uani 1 1 d . . .
H13 H -0.1234 1.2775 -0.0262 0.072 Uiso 1 1 calc R . .
C14 C 0.0406(4) 1.1995(5) 0.0105(2) 0.0399(12) Uani 1 1 d . . .
C15 C 0.0784(5) 1.2082(6) -0.0574(3) 0.0488(14) Uani 1 1 d . . .
H15 H 0.0286 1.2429 -0.1012 0.059 Uiso 1 1 calc R . .
C16 C 0.1859(4) 1.1667(6) -0.0599(2) 0.0426(12) Uani 1 1 d . . .
H16 H 0.2110 1.1716 -0.1048 0.051 Uiso 1 1 calc R . .
C17 C 0.2582(4) 1.1164(5) 0.0069(2) 0.0346(10) Uani 1 1 d . . .
H17 H 0.3324 1.0878 0.0051 0.041 Uiso 1 1 calc R . .
C18 C 0.1194(3) 1.1448(4) 0.0746(2) 0.0259(9) Uani 1 1 d . . .
C19 C 0.0824(3) 1.1253(5) 0.1441(2) 0.0263(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
Pr1 O4 2.325(2) 2_645 ?
Pr1 O5 2.353(2) 3_676 ?
Pr1 O6 2.428(3) 4_585 ?
Pr1 O1 2.479(2) . ?
Pr1 O1W 2.543(3) . ?
Pr1 O2 2.563(3) 2_645 ?
Pr1 N2 2.663(3) . ?
Pr1 N1 2.672(3) . ?
S1 O3 1.452(3) . ?
S1 O2 1.463(3) . ?
S1 O1 1.465(2) . ?
S1 C1 1.764(3) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O2 Pr1 2.563(3) 2_655 ?
O4 C2 1.331(4) . ?
O4 Pr1 2.325(2) 2_655 ?
O5 C7 1.262(4) . ?
O5 Pr1 2.353(2) 3_676 ?
O6 C7 1.247(4) . ?
O6 Pr1 2.428(3) 4_586 ?
N1 C8 1.323(5) . ?
N1 C19 1.367(5) . ?
N2 C17 1.326(5) . ?
N2 C18 1.353(5) . ?
C1 C6 1.385(5) . ?
C1 C2 1.401(5) . ?
C2 C3 1.408(5) . ?
C3 C4 1.389(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(5) . ?
C4 C7 1.508(5) . ?
C5 C6 1.384(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.387(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.356(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(6) . ?
C10 H10 0.9300 . ?
C11 C19 1.396(6) . ?
C11 C12 1.437(7) . ?
C12 C13 1.341(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.418(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.404(7) . ?
C14 C18 1.405(5) . ?
C15 C16 1.347(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.392(5) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.435(6) . ?

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
O4 Pr1 O5 108.08(9) 2_645 3_676 ?
O4 Pr1 O6 81.47(9) 2_645 4_585 ?
O5 Pr1 O6 142.27(9) 3_676 4_585 ?
O4 Pr1 O1 87.61(9) 2_645 . ?
O5 Pr1 O1 73.68(9) 3_676 . ?
O6 Pr1 O1 70.30(8) 4_585 . ?
O4 Pr1 O1W 161.85(9) 2_645 . ?
O5 Pr1 O1W 80.07(9) 3_676 . ?
O6 Pr1 O1W 82.46(9) 4_585 . ?
O1 Pr1 O1W 79.04(9) . . ?
O4 Pr1 O2 71.17(8) 2_645 2_645 ?
O5 Pr1 O2 72.16(9) 3_676 2_645 ?
O6 Pr1 O2 142.81(8) 4_585 2_645 ?
O1 Pr1 O2 131.04(9) . 2_645 ?
O1W Pr1 O2 126.96(9) . 2_645 ?
O4 Pr1 N2 84.21(9) 2_645 . ?
O5 Pr1 N2 143.33(10) 3_676 . ?
O6 Pr1 N2 72.40(9) 4_585 . ?
O1 Pr1 N2 142.59(9) . . ?
O1W Pr1 N2 98.92(9) . . ?
O2 Pr1 N2 80.06(9) 2_645 . ?
O4 Pr1 N1 128.39(9) 2_645 . ?
O5 Pr1 N1 85.66(10) 3_676 . ?
O6 Pr1 N1 117.56(9) 4_585 . ?
O1 Pr1 N1 143.07(9) . . ?
O1W Pr1 N1 67.27(9) . . ?
O2 Pr1 N1 66.39(9) 2_645 . ?
N2 Pr1 N1 61.09(10) . . ?
O3 S1 O2 112.66(17) . . ?
O3 S1 O1 111.69(16) . . ?
O2 S1 O1 111.13(15) . . ?
O3 S1 C1 108.51(16) . . ?
O2 S1 C1 105.09(16) . . ?
O1 S1 C1 107.36(16) . . ?
Pr1 O1W H1W1 115(3) . . ?
Pr1 O1W H1W2 113(3) . . ?
H1W1 O1W H1W2 110.3(17) . . ?
S1 O1 Pr1 165.01(16) . . ?
S1 O2 Pr1 125.04(15) . 2_655 ?
C2 O4 Pr1 137.2(2) . 2_655 ?
C7 O5 Pr1 152.4(3) . 3_676 ?
C7 O6 Pr1 150.4(2) . 4_586 ?
C8 N1 C19 116.9(4) . . ?
C8 N1 Pr1 122.4(3) . . ?
C19 N1 Pr1 120.7(3) . . ?
C17 N2 C18 117.3(3) . . ?
C17 N2 Pr1 121.5(3) . . ?
C18 N2 Pr1 120.9(2) . . ?
C6 C1 C2 122.2(3) . . ?
C6 C1 S1 119.8(3) . . ?
C2 C1 S1 118.0(3) . . ?
O4 C2 C1 122.9(3) . . ?
O4 C2 C3 120.5(3) . . ?
C1 C2 C3 116.7(3) . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C7 118.8(3) . . ?
C5 C4 C7 120.6(3) . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
O6 C7 O5 125.1(3) . . ?
O6 C7 C4 119.3(3) . . ?
O5 C7 C4 115.5(3) . . ?
N1 C8 C9 124.3(4) . . ?
N1 C8 H8 117.8 . . ?
C9 C8 H8 117.8 . . ?
C10 C9 C8 118.5(5) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C19 118.0(4) . . ?
C10 C11 C12 123.2(5) . . ?
C19 C11 C12 118.7(5) . . ?
C13 C12 C11 121.1(5) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 121.1(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C18 116.9(4) . . ?
C15 C14 C13 123.2(4) . . ?
C18 C14 C13 119.8(5) . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 118.0(4) . . ?
C15 C16 H16 121.0 . . ?
C17 C16 H16 121.0 . . ?
N2 C17 C16 124.3(4) . . ?
N2 C17 H17 117.9 . . ?
C16 C17 H17 117.9 . . ?
N2 C18 C14 122.6(4) . . ?
N2 C18 C19 118.6(3) . . ?
C14 C18 C19 118.8(4) . . ?
N1 C19 C11 122.3(4) . . ?
N1 C19 C18 117.4(4) . . ?
C11 C19 C18 120.3(4) . . ?

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
O3 S1 O1 Pr1 107.6(7) . . . . ?
O2 S1 O1 Pr1 -125.7(7) . . . . ?
C1 S1 O1 Pr1 -11.3(7) . . . . ?
O4 Pr1 O1 S1 -133.6(7) 2_645 . . . ?
O5 Pr1 O1 S1 -24.0(7) 3_676 . . . ?
O6 Pr1 O1 S1 144.6(7) 4_585 . . . ?
O1W Pr1 O1 S1 58.7(7) . . . . ?
O2 Pr1 O1 S1 -71.3(7) 2_645 . . . ?
N2 Pr1 O1 S1 149.1(6) . . . . ?
N1 Pr1 O1 S1 34.6(8) . . . . ?
O3 S1 O2 Pr1 175.14(14) . . . 2_655 ?
O1 S1 O2 Pr1 48.9(2) . . . 2_655 ?
C1 S1 O2 Pr1 -66.89(19) . . . 2_655 ?
O4 Pr1 N1 C8 118.2(3) 2_645 . . . ?
O5 Pr1 N1 C8 8.5(3) 3_676 . . . ?
O6 Pr1 N1 C8 -140.3(3) 4_585 . . . ?
O1 Pr1 N1 C8 -46.8(4) . . . . ?
O1W Pr1 N1 C8 -72.6(3) . . . . ?
O2 Pr1 N1 C8 80.9(3) 2_645 . . . ?
N2 Pr1 N1 C8 172.4(3) . . . . ?
O4 Pr1 N1 C19 -63.3(3) 2_645 . . . ?
O5 Pr1 N1 C19 -173.0(3) 3_676 . . . ?
O6 Pr1 N1 C19 38.3(3) 4_585 . . . ?
O1 Pr1 N1 C19 131.8(3) . . . . ?
O1W Pr1 N1 C19 106.0(3) . . . . ?
O2 Pr1 N1 C19 -100.6(3) 2_645 . . . ?
N2 Pr1 N1 C19 -9.1(3) . . . . ?
O4 Pr1 N2 C17 -35.9(3) 2_645 . . . ?
O5 Pr1 N2 C17 -148.7(3) 3_676 . . . ?
O6 Pr1 N2 C17 46.9(3) 4_585 . . . ?
O1 Pr1 N2 C17 42.4(4) . . . . ?
O1W Pr1 N2 C17 126.0(3) . . . . ?
O2 Pr1 N2 C17 -107.8(3) 2_645 . . . ?
N1 Pr1 N2 C17 -176.2(4) . . . . ?
O4 Pr1 N2 C18 149.7(3) 2_645 . . . ?
O5 Pr1 N2 C18 37.0(4) 3_676 . . . ?
O6 Pr1 N2 C18 -127.5(3) 4_585 . . . ?
O1 Pr1 N2 C18 -131.9(3) . . . . ?
O1W Pr1 N2 C18 -48.4(3) . . . . ?
O2 Pr1 N2 C18 77.8(3) 2_645 . . . ?
N1 Pr1 N2 C18 9.4(3) . . . . ?
O3 S1 C1 C6 -7.6(3) . . . . ?
O2 S1 C1 C6 -128.3(3) . . . . ?
O1 S1 C1 C6 113.3(3) . . . . ?
O3 S1 C1 C2 170.1(3) . . . . ?
O2 S1 C1 C2 49.4(3) . . . . ?
O1 S1 C1 C2 -69.0(3) . . . . ?
Pr1 O4 C2 C1 -52.2(5) 2_655 . . . ?
Pr1 O4 C2 C3 127.9(3) 2_655 . . . ?
C6 C1 C2 O4 -178.8(3) . . . . ?
S1 C1 C2 O4 3.5(5) . . . . ?
C6 C1 C2 C3 1.1(5) . . . . ?
S1 C1 C2 C3 -176.5(3) . . . . ?
O4 C2 C3 C4 177.3(3) . . . . ?
C1 C2 C3 C4 -2.7(5) . . . . ?
C2 C3 C4 C5 2.2(5) . . . . ?
C2 C3 C4 C7 -175.4(3) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C7 C4 C5 C6 177.5(3) . . . . ?
C4 C5 C6 C1 -1.6(5) . . . . ?
C2 C1 C6 C5 1.0(5) . . . . ?
S1 C1 C6 C5 178.6(3) . . . . ?
Pr1 O6 C7 O5 48.8(7) 4_586 . . . ?
Pr1 O6 C7 C4 -132.7(4) 4_586 . . . ?
Pr1 O5 C7 O6 12.2(8) 3_676 . . . ?
Pr1 O5 C7 C4 -166.3(4) 3_676 . . . ?
C3 C4 C7 O6 17.5(5) . . . . ?
C5 C4 C7 O6 -160.1(3) . . . . ?
C3 C4 C7 O5 -164.0(3) . . . . ?
C5 C4 C7 O5 18.5(5) . . . . ?
C19 N1 C8 C9 -1.1(6) . . . . ?
Pr1 N1 C8 C9 177.4(3) . . . . ?
N1 C8 C9 C10 -2.6(7) . . . . ?
C8 C9 C10 C11 3.1(7) . . . . ?
C9 C10 C11 C19 -0.1(7) . . . . ?
C9 C10 C11 C12 177.4(5) . . . . ?
C10 C11 C12 C13 -174.2(5) . . . . ?
C19 C11 C12 C13 3.2(8) . . . . ?
C11 C12 C13 C14 0.1(9) . . . . ?
C12 C13 C14 C15 175.1(6) . . . . ?
C12 C13 C14 C18 -2.4(8) . . . . ?
C18 C14 C15 C16 -0.6(7) . . . . ?
C13 C14 C15 C16 -178.2(5) . . . . ?
C14 C15 C16 C17 -0.5(7) . . . . ?
C18 N2 C17 C16 1.6(7) . . . . ?
Pr1 N2 C17 C16 -173.0(3) . . . . ?
C15 C16 C17 N2 0.0(7) . . . . ?
C17 N2 C18 C14 -2.8(6) . . . . ?
Pr1 N2 C18 C14 171.9(3) . . . . ?
C17 N2 C18 C19 175.9(4) . . . . ?
Pr1 N2 C18 C19 -9.5(5) . . . . ?
C15 C14 C18 N2 2.3(6) . . . . ?
C13 C14 C18 N2 180.0(4) . . . . ?
C15 C14 C18 C19 -176.4(4) . . . . ?
C13 C14 C18 C19 1.3(6) . . . . ?
C8 N1 C19 C11 4.4(6) . . . . ?
Pr1 N1 C19 C11 -174.2(3) . . . . ?
C8 N1 C19 C18 -172.9(4) . . . . ?
Pr1 N1 C19 C18 8.5(5) . . . . ?
C10 C11 C19 N1 -3.8(6) . . . . ?
C12 C11 C19 N1 178.6(4) . . . . ?
C10 C11 C19 C18 173.3(4) . . . . ?
C12 C11 C19 C18 -4.2(6) . . . . ?
N2 C18 C19 N1 0.6(5) . . . . ?
C14 C18 C19 N1 179.3(4) . . . . ?
N2 C18 C19 C11 -176.7(4) . . . . ?
C14 C18 C19 C11 2.0(6) . . . . ?

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
O1W H1W1 O3 0.85(4) 2.091(19) 2.901(4) 160(4) 2_655
O1W H1W2 O4 0.85(4) 1.908(11) 2.753(4) 175(4) .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.765
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_4-Yb
_database_code_depnum_ccdc_archive 'CCDC 1549854'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H9 O9 S Yb, H2 O'
_chemical_formula_sum            'C7 H11 O10 S Yb'
_chemical_formula_weight         460.26

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.8598(17)
_cell_length_b                   9.2912(16)
_cell_length_c                   12.0480(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.702(13)
_cell_angle_gamma                90.00
_cell_volume                     1215.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1089
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_absorpt_coefficient_mu    7.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2633
_exptl_absorpt_correction_T_max  0.3147
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4407
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2774
_reflns_number_gt                2288
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.1230P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2774
_refine_ls_number_parameters     184
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1717
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_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
Yb1 Yb 1.02759(4) 0.68307(4) 0.06181(3) 0.0204(2) Uani 1 1 d . . .
S4 S 0.7437(2) 0.7590(3) -0.0707(2) 0.0238(5) Uani 1 1 d . . .
O1W O 1.0895(9) 0.8301(9) -0.0795(9) 0.035(2) Uani 1 1 d D . .
H1W1 H 1.1677(14) 0.836(12) -0.078(14) 0.052 Uiso 1 1 d D . .
H1W2 H 1.058(9) 0.905(8) -0.109(11) 0.052 Uiso 1 1 d D . .
O1 O 0.8629(9) 0.8062(8) -0.0238(9) 0.037(2) Uani 1 1 d . . .
O2 O 0.6551(8) 0.8768(8) -0.0778(6) 0.0302(17) Uani 1 1 d . . .
O2W O 1.2401(8) 0.7350(10) 0.1003(7) 0.0355(19) Uani 1 1 d D . .
H2W1 H 1.296(9) 0.787(13) 0.073(9) 0.053 Uiso 1 1 d D . .
H2W2 H 1.248(13) 0.738(15) 0.1709(12) 0.053 Uiso 1 1 d D . .
O3 O 0.7554(10) 0.6852(8) -0.1777(7) 0.037(2) Uani 1 1 d . . .
O3W O 1.0861(8) 0.5363(8) 0.2084(6) 0.0343(18) Uani 1 1 d . . .
H3W1 H 1.1035 0.5671 0.2734 0.051 Uiso 1 1 d R . .
H3W2 H 1.1337 0.4663 0.1948 0.051 Uiso 1 1 d R . .
O4 O 0.8827(6) 0.5073(7) 0.0264(5) 0.0210(14) Uani 1 1 d . . .
O4W O 1.3320(9) 0.8969(10) -0.0796(8) 0.048(2) Uani 1 1 d . . .
H4W1 H 1.3535 0.9773 -0.0508 0.071 Uiso 1 1 d R . .
H4W2 H 1.3677 0.8885 -0.1418 0.071 Uiso 1 1 d R . .
O5 O 0.5986(8) 0.2291(8) 0.2831(6) 0.0294(17) Uani 1 1 d . . .
O6 O 0.4817(7) 0.4059(8) 0.3425(6) 0.0280(16) Uani 1 1 d . . .
C1 C 0.6889(10) 0.6351(11) 0.0248(8) 0.024(2) Uani 1 1 d . . .
C2 C 0.7669(9) 0.5242(10) 0.0652(7) 0.0187(19) Uani 1 1 d . . .
C3 C 0.7227(9) 0.4341(10) 0.1474(8) 0.0211(19) Uani 1 1 d . . .
H3 H 0.7718 0.3600 0.1757 0.025 Uiso 1 1 calc R . .
C4 C 0.6055(9) 0.4550(10) 0.1872(8) 0.022(2) Uani 1 1 d . . .
C5 C 0.5293(10) 0.5648(11) 0.1478(9) 0.029(2) Uani 1 1 d . . .
H5 H 0.4511 0.5776 0.1755 0.035 Uiso 1 1 calc R . .
C6 C 0.5728(11) 0.6548(12) 0.0662(9) 0.028(2) Uani 1 1 d . . .
H6 H 0.5234 0.7293 0.0390 0.034 Uiso 1 1 calc R . .
C7 C 0.5596(10) 0.3578(12) 0.2760(9) 0.025(2) 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
Yb1 O4 2.295(7) 3_765 ?
Yb1 O4 2.299(7) . ?
Yb1 O1W 2.299(9) . ?
Yb1 O3W 2.305(8) . ?
Yb1 O1 2.337(9) . ?
Yb1 O6 2.373(7) 2_655 ?
Yb1 O5 2.389(7) 2_655 ?
Yb1 O2W 2.390(8) . ?
Yb1 C7 2.731(11) 2_655 ?
Yb1 C2 3.194(9) . ?
Yb1 Yb1 3.7547(9) 3_765 ?
Yb1 H1W1 2.71(11) . ?
Yb1 H2W2 2.74(11) . ?
S4 O2 1.458(8) . ?
S4 O1 1.465(9) . ?
S4 O3 1.469(8) . ?
S4 C1 1.744(11) . ?
O1W H1W1 0.85(3) . ?
O1W H1W2 0.85(3) . ?
O2W H2W1 0.85(3) . ?
O2W H2W2 0.85(3) . ?
O3W H3W1 0.8500 . ?
O3W H3W2 0.8501 . ?
O4 C2 1.364(11) . ?
O4 Yb1 2.295(7) 3_765 ?
O4W H4W1 0.8530 . ?
O4W H4W2 0.8575 . ?
O5 C7 1.271(13) . ?
O5 Yb1 2.389(7) 2_645 ?
O6 C7 1.263(13) . ?
O6 Yb1 2.373(7) 2_645 ?
C1 C6 1.381(15) . ?
C1 C2 1.412(14) . ?
C2 C3 1.392(13) . ?
C3 C4 1.387(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(14) . ?
C4 C7 1.497(14) . ?
C5 C6 1.384(15) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 Yb1 2.731(11) 2_645 ?

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
O4 Yb1 O4 70.4(3) 3_765 . ?
O4 Yb1 O1W 88.7(3) 3_765 . ?
O4 Yb1 O1W 119.9(3) . . ?
O4 Yb1 O3W 77.7(3) 3_765 . ?
O4 Yb1 O3W 83.9(3) . . ?
O1W Yb1 O3W 147.0(3) . . ?
O4 Yb1 O1 120.2(3) 3_765 . ?
O4 Yb1 O1 75.8(3) . . ?
O1W Yb1 O1 67.6(4) . . ?
O3W Yb1 O1 144.8(3) . . ?
O4 Yb1 O6 157.2(2) 3_765 2_655 ?
O4 Yb1 O6 132.1(2) . 2_655 ?
O1W Yb1 O6 81.9(3) . 2_655 ?
O3W Yb1 O6 99.1(3) . 2_655 ?
O1 Yb1 O6 75.2(3) . 2_655 ?
O4 Yb1 O5 139.6(2) 3_765 2_655 ?
O4 Yb1 O5 82.3(3) . 2_655 ?
O1W Yb1 O5 131.3(3) . 2_655 ?
O3W Yb1 O5 70.0(3) . 2_655 ?
O1 Yb1 O5 78.9(3) . 2_655 ?
O6 Yb1 O5 55.3(3) 2_655 2_655 ?
O4 Yb1 O2W 79.9(3) 3_765 . ?
O4 Yb1 O2W 146.2(3) . . ?
O1W Yb1 O2W 73.8(3) . . ?
O3W Yb1 O2W 74.2(3) . . ?
O1 Yb1 O2W 135.1(3) . . ?
O6 Yb1 O2W 77.6(3) 2_655 . ?
O5 Yb1 O2W 112.7(3) 2_655 . ?
O4 Yb1 C7 161.8(3) 3_765 2_655 ?
O4 Yb1 C7 107.8(3) . 2_655 ?
O1W Yb1 C7 107.0(3) . 2_655 ?
O3W Yb1 C7 84.1(3) . 2_655 ?
O1 Yb1 C7 75.4(4) . 2_655 ?
O6 Yb1 C7 27.5(3) 2_655 2_655 ?
O5 Yb1 C7 27.7(3) 2_655 2_655 ?
O2W Yb1 C7 95.4(3) . 2_655 ?
O4 Yb1 C2 92.2(2) 3_765 . ?
O4 Yb1 C2 21.9(2) . . ?
O1W Yb1 C2 124.3(3) . . ?
O3W Yb1 C2 86.6(3) . . ?
O1 Yb1 C2 64.2(3) . . ?
O6 Yb1 C2 110.3(2) 2_655 . ?
O5 Yb1 C2 62.8(3) 2_655 . ?
O2W Yb1 C2 160.4(3) . . ?
C7 Yb1 C2 86.5(3) 2_655 . ?
O4 Yb1 Yb1 35.22(17) 3_765 3_765 ?
O4 Yb1 Yb1 35.16(17) . 3_765 ?
O1W Yb1 Yb1 106.9(2) . 3_765 ?
O3W Yb1 Yb1 78.75(19) . 3_765 ?
O1 Yb1 Yb1 99.1(2) . 3_765 ?
O6 Yb1 Yb1 167.02(17) 2_655 3_765 ?
O5 Yb1 Yb1 112.57(19) 2_655 3_765 ?
O2W Yb1 Yb1 113.7(2) . 3_765 ?
C7 Yb1 Yb1 140.2(2) 2_655 3_765 ?
C2 Yb1 Yb1 57.00(16) . 3_765 ?
O4 Yb1 H1W1 82(3) 3_765 . ?
O4 Yb1 H1W1 131(3) . . ?
O1W Yb1 H1W1 17.1(17) . . ?
O3W Yb1 H1W1 129.9(17) . . ?
O1 Yb1 H1W1 84.5(15) . . ?
O6 Yb1 H1W1 83(3) 2_655 . ?
O5 Yb1 H1W1 138(3) 2_655 . ?
O2W Yb1 H1W1 57(2) . . ?
C7 Yb1 H1W1 110(3) 2_655 . ?
C2 Yb1 H1W1 140(2) . . ?
Yb1 Yb1 H1W1 108(3) 3_765 . ?
O4 Yb1 H2W2 89(3) 3_765 . ?
O4 Yb1 H2W2 143(3) . . ?
O1W Yb1 H2W2 88.6(17) . . ?
O3W Yb1 H2W2 62(2) . . ?
O1 Yb1 H2W2 140(3) . . ?
O6 Yb1 H2W2 70(3) 2_655 . ?
O5 Yb1 H2W2 96.0(19) 2_655 . ?
O2W Yb1 H2W2 17.5(15) . . ?
C7 Yb1 H2W2 82(3) 2_655 . ?
C2 Yb1 H2W2 147.1(17) . . ?
Yb1 Yb1 H2W2 119(3) 3_765 . ?
H1W1 Yb1 H2W2 73(3) . . ?
O2 S4 O1 111.8(5) . . ?
O2 S4 O3 111.9(5) . . ?
O1 S4 O3 112.3(6) . . ?
O2 S4 C1 107.3(5) . . ?
O1 S4 C1 105.0(5) . . ?
O3 S4 C1 108.1(5) . . ?
Yb1 O1W H1W1 110(9) . . ?
Yb1 O1W H1W2 133(9) . . ?
H1W1 O1W H1W2 109.5(18) . . ?
S4 O1 Yb1 132.8(4) . . ?
Yb1 O2W H2W1 137(9) . . ?
Yb1 O2W H2W2 105(9) . . ?
H2W1 O2W H2W2 109.0(18) . . ?
Yb1 O3W H3W1 123.8 . . ?
Yb1 O3W H3W2 117.5 . . ?
H3W1 O3W H3W2 108.3 . . ?
C2 O4 Yb1 131.0(6) . 3_765 ?
C2 O4 Yb1 119.2(6) . . ?
Yb1 O4 Yb1 109.6(3) 3_765 . ?
H4W1 O4W H4W2 108.0 . . ?
C7 O5 Yb1 91.3(6) . 2_645 ?
C7 O6 Yb1 92.2(6) . 2_645 ?
C6 C1 C2 121.1(9) . . ?
C6 C1 S4 119.0(8) . . ?
C2 C1 S4 119.7(8) . . ?
O4 C2 C3 121.0(9) . . ?
O4 C2 C1 121.0(8) . . ?
C3 C2 C1 117.9(9) . . ?
C3 C2 Yb1 127.7(7) . . ?
C1 C2 Yb1 100.4(6) . . ?
C4 C3 C2 120.0(9) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 121.9(9) . . ?
C3 C4 C7 119.4(9) . . ?
C5 C4 C7 118.7(9) . . ?
C6 C5 C4 118.3(10) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C1 C6 C5 120.8(11) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
O6 C7 O5 121.2(10) . . ?
O6 C7 C4 118.9(10) . . ?
O5 C7 C4 119.9(9) . . ?
O6 C7 Yb1 60.3(6) . 2_645 ?
O5 C7 Yb1 61.0(5) . 2_645 ?
C4 C7 Yb1 179.1(8) . 2_645 ?

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 S4 O1 Yb1 159.0(7) . . . . ?
O3 S4 O1 Yb1 -74.2(9) . . . . ?
C1 S4 O1 Yb1 43.0(10) . . . . ?
O4 Yb1 O1 S4 54.4(10) 3_765 . . . ?
O4 Yb1 O1 S4 -2.4(8) . . . . ?
O1W Yb1 O1 S4 128.9(10) . . . . ?
O3W Yb1 O1 S4 -59.1(12) . . . . ?
O6 Yb1 O1 S4 -143.9(9) 2_655 . . . ?
O5 Yb1 O1 S4 -87.2(9) 2_655 . . . ?
O2W Yb1 O1 S4 161.7(7) . . . . ?
C7 Yb1 O1 S4 -115.4(9) 2_655 . . . ?
C2 Yb1 O1 S4 -22.2(8) . . . . ?
Yb1 Yb1 O1 S4 24.2(9) 3_765 . . . ?
O4 Yb1 O4 C2 175.3(8) 3_765 . . . ?
O1W Yb1 O4 C2 -108.1(7) . . . . ?
O3W Yb1 O4 C2 96.2(6) . . . . ?
O1 Yb1 O4 C2 -54.9(7) . . . . ?
O6 Yb1 O4 C2 -0.6(8) 2_655 . . . ?
O5 Yb1 O4 C2 25.6(6) 2_655 . . . ?
O2W Yb1 O4 C2 145.5(6) . . . . ?
C7 Yb1 O4 C2 14.4(7) 2_655 . . . ?
Yb1 Yb1 O4 C2 175.3(8) 3_765 . . . ?
O4 Yb1 O4 Yb1 0.0 3_765 . . 3_765 ?
O1W Yb1 O4 Yb1 76.6(4) . . . 3_765 ?
O3W Yb1 O4 Yb1 -79.1(3) . . . 3_765 ?
O1 Yb1 O4 Yb1 129.8(4) . . . 3_765 ?
O6 Yb1 O4 Yb1 -175.9(3) 2_655 . . 3_765 ?
O5 Yb1 O4 Yb1 -149.7(3) 2_655 . . 3_765 ?
O2W Yb1 O4 Yb1 -29.8(6) . . . 3_765 ?
C7 Yb1 O4 Yb1 -160.9(3) 2_655 . . 3_765 ?
C2 Yb1 O4 Yb1 -175.3(8) . . . 3_765 ?
O2 S4 C1 C6 7.3(10) . . . . ?
O1 S4 C1 C6 126.4(9) . . . . ?
O3 S4 C1 C6 -113.5(9) . . . . ?
O2 S4 C1 C2 -167.4(8) . . . . ?
O1 S4 C1 C2 -48.3(9) . . . . ?
O3 S4 C1 C2 71.7(9) . . . . ?
Yb1 O4 C2 C3 61.2(11) 3_765 . . . ?
Yb1 O4 C2 C3 -113.0(9) . . . . ?
Yb1 O4 C2 C1 -120.0(9) 3_765 . . . ?
Yb1 O4 C2 C1 65.9(10) . . . . ?
Yb1 O4 C2 Yb1 174.1(10) 3_765 . . . ?
C6 C1 C2 O4 -178.2(9) . . . . ?
S4 C1 C2 O4 -3.6(13) . . . . ?
C6 C1 C2 C3 0.7(15) . . . . ?
S4 C1 C2 C3 175.3(7) . . . . ?
C6 C1 C2 Yb1 -142.5(9) . . . . ?
S4 C1 C2 Yb1 32.1(8) . . . . ?
O4 Yb1 C2 O4 -4.4(7) 3_765 . . . ?
O1W Yb1 C2 O4 85.5(7) . . . . ?
O3W Yb1 C2 O4 -82.0(6) . . . . ?
O1 Yb1 C2 O4 118.3(7) . . . . ?
O6 Yb1 C2 O4 179.5(6) 2_655 . . . ?
O5 Yb1 C2 O4 -151.2(7) 2_655 . . . ?
O2W Yb1 C2 O4 -69.9(10) . . . . ?
C7 Yb1 C2 O4 -166.3(7) 2_655 . . . ?
Yb1 Yb1 C2 O4 -3.2(5) 3_765 . . . ?
O4 Yb1 C2 C3 90.2(8) 3_765 . . . ?
O4 Yb1 C2 C3 94.6(10) . . . . ?
O1W Yb1 C2 C3 -179.9(7) . . . . ?
O3W Yb1 C2 C3 12.6(8) . . . . ?
O1 Yb1 C2 C3 -147.1(9) . . . . ?
O6 Yb1 C2 C3 -85.9(8) 2_655 . . . ?
O5 Yb1 C2 C3 -56.6(8) 2_655 . . . ?
O2W Yb1 C2 C3 24.7(13) . . . . ?
C7 Yb1 C2 C3 -71.7(8) 2_655 . . . ?
Yb1 Yb1 C2 C3 91.4(8) 3_765 . . . ?
O4 Yb1 C2 C1 -131.7(6) 3_765 . . . ?
O4 Yb1 C2 C1 -127.3(10) . . . . ?
O1W Yb1 C2 C1 -41.8(7) . . . . ?
O3W Yb1 C2 C1 150.7(6) . . . . ?
O1 Yb1 C2 C1 -9.0(6) . . . . ?
O6 Yb1 C2 C1 52.2(6) 2_655 . . . ?
O5 Yb1 C2 C1 81.4(6) 2_655 . . . ?
O2W Yb1 C2 C1 162.8(8) . . . . ?
C7 Yb1 C2 C1 66.4(6) 2_655 . . . ?
Yb1 Yb1 C2 C1 -130.5(6) 3_765 . . . ?
O4 C2 C3 C4 178.8(8) . . . . ?
C1 C2 C3 C4 -0.1(14) . . . . ?
Yb1 C2 C3 C4 131.8(8) . . . . ?
C2 C3 C4 C5 -0.3(15) . . . . ?
C2 C3 C4 C7 -179.7(9) . . . . ?
C3 C4 C5 C6 0.2(16) . . . . ?
C7 C4 C5 C6 179.6(10) . . . . ?
C2 C1 C6 C5 -0.8(17) . . . . ?
S4 C1 C6 C5 -175.5(9) . . . . ?
C4 C5 C6 C1 0.4(17) . . . . ?
Yb1 O6 C7 O5 -0.1(11) 2_645 . . . ?
Yb1 O6 C7 C4 179.6(9) 2_645 . . . ?
Yb1 O5 C7 O6 0.1(11) 2_645 . . . ?
Yb1 O5 C7 C4 -179.6(9) 2_645 . . . ?
C3 C4 C7 O6 151.4(10) . . . . ?
C5 C4 C7 O6 -28.0(15) . . . . ?
C3 C4 C7 O5 -29.0(15) . . . . ?
C5 C4 C7 O5 151.7(10) . . . . ?

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
O1W H1W1 O4W 0.85(3) 1.87(3) 2.706(13) 166(11) .
O1W H1W2 O6 0.85(3) 2.02(3) 2.864(11) 172(14) 4_675
O2W H2W1 O4W 0.85(3) 2.14(8) 2.843(12) 139(11) .
O2W H2W2 O3 0.85(3) 1.96(5) 2.775(11) 160(14) 4_676
O3W H3W1 O2 0.85 1.93 2.782(11) 174.6 4_676
O3W H3W2 O3 0.85 1.87 2.716(11) 174.9 3_765
O4W H4W1 O2 0.85 2.06 2.832(12) 149.6 3_775
O4W H4W2 O5 0.85 2.06 2.839(11) 149.8 3_765

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         4.998
_refine_diff_density_min         -4.738
_refine_diff_density_rms         0.496
####################################################################### 
# 
# 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_5-Y
_database_code_depnum_ccdc_archive 'CCDC 1549865'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 N2 O7 S Y'
_chemical_formula_sum            'C17 H13 N2 O7 S Y'
_chemical_formula_weight         478.26

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.1787(7)
_cell_length_b                   8.5094(3)
_cell_length_c                   17.7717(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.669(7)
_cell_angle_gamma                90.00
_cell_volume                     1610.77(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1532
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    3.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5170
_exptl_absorpt_correction_T_max  0.5815
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5641
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3677
_reflns_number_gt                2751
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0403P)²+0.3531P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3677
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1161
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_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
Y1 Y 0.17744(4) -0.03624(5) 0.30706(3) 0.01440(13) Uani 1 1 d . . .
S1 S 0.14617(11) 0.36990(14) 0.33918(7) 0.0162(3) Uani 1 1 d . . .
O1W O 0.0727(3) -0.2630(4) 0.2363(2) 0.0251(8) Uani 1 1 d D . .
H1W1 H 0.103(5) -0.301(5) 0.202(2) 0.038 Uiso 1 1 d D . .
H1W2 H 0.065(5) -0.334(4) 0.268(2) 0.038 Uiso 1 1 d D . .
O1 O 0.0867(3) 0.2149(4) 0.33111(18) 0.0201(7) Uani 1 1 d . . .
O2 O 0.0645(3) 0.4944(4) 0.35017(19) 0.0217(8) Uani 1 1 d . . .
O3 O 0.1940(3) 0.4043(4) 0.27347(18) 0.0203(7) Uani 1 1 d . . .
O4 O 0.3362(3) 0.1140(4) 0.37890(18) 0.0191(7) Uani 1 1 d . . .
O5 O 0.5907(3) 0.4157(4) 0.68992(18) 0.0213(7) Uani 1 1 d . . .
O6 O 0.6756(3) 0.2320(4) 0.63202(18) 0.0205(7) Uani 1 1 d . . .
N1 N 0.1427(4) -0.1106(5) 0.4372(2) 0.0222(9) Uani 1 1 d . . .
N2 N -0.0498(4) -0.0629(5) 0.3105(2) 0.0209(9) Uani 1 1 d . . .
C1 C 0.2744(4) 0.3570(6) 0.4258(3) 0.0180(10) Uani 1 1 d . . .
C2 C 0.3529(4) 0.2235(5) 0.4349(3) 0.0178(10) Uani 1 1 d . . .
C3 C 0.4526(4) 0.2152(6) 0.5051(3) 0.0187(10) Uani 1 1 d . . .
H3A H 0.5056 0.1283 0.5138 0.022 Uiso 1 1 calc R . .
C4 C 0.4751(4) 0.3320(5) 0.5618(3) 0.0170(10) Uani 1 1 d . . .
C5 C 0.3939(4) 0.4607(6) 0.5515(3) 0.0193(10) Uani 1 1 d . . .
H5 H 0.4069 0.5383 0.5900 0.023 Uiso 1 1 calc R . .
C6 C 0.2940(4) 0.4704(5) 0.4831(3) 0.0177(10) Uani 1 1 d . . .
H6 H 0.2392 0.5552 0.4757 0.021 Uiso 1 1 calc R . .
C7 C 0.5889(4) 0.3245(5) 0.6340(3) 0.0169(10) Uani 1 1 d . . .
C8 C 0.2419(5) -0.1200(6) 0.5033(3) 0.0280(12) Uani 1 1 d . . .
H8 H 0.3187 -0.0803 0.5018 0.034 Uiso 1 1 calc R . .
C9 C 0.2352(5) -0.1855(6) 0.5727(3) 0.0307(13) Uani 1 1 d . . .
H9 H 0.3058 -0.1903 0.6169 0.037 Uiso 1 1 calc R . .
C10 C 0.1220(6) -0.2434(7) 0.5752(3) 0.0391(15) Uani 1 1 d . . .
H10 H 0.1144 -0.2881 0.6213 0.047 Uiso 1 1 calc R . .
C11 C 0.0205(5) -0.2346(7) 0.5090(3) 0.0362(15) Uani 1 1 d . . .
H11 H -0.0562 -0.2757 0.5099 0.043 Uiso 1 1 calc R . .
C12 C 0.0305(5) -0.1658(6) 0.4413(3) 0.0247(12) Uani 1 1 d . . .
C13 C -0.0768(5) -0.1367(6) 0.3699(3) 0.0215(11) Uani 1 1 d . . .
C14 C -0.2003(5) -0.1715(7) 0.3673(3) 0.0329(13) Uani 1 1 d . . .
H14 H -0.2166 -0.2287 0.4077 0.039 Uiso 1 1 calc R . .
C15 C -0.2965(5) -0.1204(7) 0.3046(4) 0.0374(14) Uani 1 1 d . . .
H15 H -0.3793 -0.1423 0.3015 0.045 Uiso 1 1 calc R . .
C16 C -0.2693(5) -0.0360(7) 0.2460(3) 0.0335(13) Uani 1 1 d . . .
H16 H -0.3331 0.0049 0.2039 0.040 Uiso 1 1 calc R . .
C17 C -0.1446(5) -0.0134(6) 0.2512(3) 0.0273(12) Uani 1 1 d . . .
H17 H -0.1265 0.0400 0.2103 0.033 Uiso 1 1 calc R . .


_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 O4 2.245(3) . ?
Y1 O5 2.259(3) 4_565 ?
Y1 O6 2.359(3) 3_656 ?
Y1 O3 2.370(3) 2_545 ?
Y1 O1W 2.404(3) . ?
Y1 O1 2.458(3) . ?
Y1 N1 2.539(4) . ?
Y1 N2 2.570(4) . ?
S1 O2 1.450(3) . ?
S1 O3 1.454(3) . ?
S1 O1 1.465(3) . ?
S1 C1 1.760(5) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O3 Y1 2.370(3) 2 ?
O4 C2 1.334(5) . ?
O5 C7 1.257(5) . ?
O5 Y1 2.259(3) 4_666 ?
O6 C7 1.257(5) . ?
O6 Y1 2.359(3) 3_656 ?
N1 C8 1.350(6) . ?
N1 C12 1.362(6) . ?
N2 C17 1.317(6) . ?
N2 C13 1.339(6) . ?
C1 C6 1.371(6) . ?
C1 C2 1.415(6) . ?
C2 C3 1.400(7) . ?
C3 C4 1.384(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.399(6) . ?
C4 C7 1.509(7) . ?
C5 C6 1.381(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.376(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.371(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.365(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.478(7) . ?
C13 C14 1.398(7) . ?
C14 C15 1.364(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.373(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Y1 O5 108.04(12) . 4_565 ?
O4 Y1 O6 79.70(12) . 3_656 ?
O5 Y1 O6 142.00(11) 4_565 3_656 ?
O4 Y1 O3 86.88(11) . 2_545 ?
O5 Y1 O3 73.13(11) 4_565 2_545 ?
O6 Y1 O3 70.19(11) 3_656 2_545 ?
O4 Y1 O1W 158.43(11) . . ?
O5 Y1 O1W 82.99(12) 4_565 . ?
O6 Y1 O1W 80.43(12) 3_656 . ?
O3 Y1 O1W 78.53(11) 2_545 . ?
O4 Y1 O1 72.70(11) . . ?
O5 Y1 O1 71.39(11) 4_565 . ?
O6 Y1 O1 143.21(11) 3_656 . ?
O3 Y1 O1 130.42(11) 2_545 . ?
O1W Y1 O1 128.86(11) . . ?
O4 Y1 N1 86.38(12) . . ?
O5 Y1 N1 144.22(12) 4_565 . ?
O6 Y1 N1 71.56(11) 3_656 . ?
O3 Y1 N1 141.74(12) 2_545 . ?
O1W Y1 N1 95.25(13) . . ?
O1 Y1 N1 82.70(11) . . ?
O4 Y1 N2 130.79(11) . . ?
O5 Y1 N2 84.90(12) 4_565 . ?
O6 Y1 N2 118.83(12) 3_656 . ?
O3 Y1 N2 141.31(12) 2_545 . ?
O1W Y1 N2 67.27(11) . . ?
O1 Y1 N2 67.01(11) . . ?
N1 Y1 N2 62.01(13) . . ?
O2 S1 O3 111.17(19) . . ?
O2 S1 O1 112.67(18) . . ?
O3 S1 O1 111.68(19) . . ?
O2 S1 C1 107.9(2) . . ?
O3 S1 C1 108.35(19) . . ?
O1 S1 C1 104.8(2) . . ?
Y1 O1W H1W1 116(3) . . ?
Y1 O1W H1W2 111(4) . . ?
H1W1 O1W H1W2 110.7(18) . . ?
S1 O1 Y1 126.93(17) . . ?
S1 O3 Y1 165.0(2) . 2 ?
C2 O4 Y1 136.9(3) . . ?
C7 O5 Y1 155.4(3) . 4_666 ?
C7 O6 Y1 149.9(3) . 3_656 ?
C8 N1 C12 117.4(4) . . ?
C8 N1 Y1 119.6(3) . . ?
C12 N1 Y1 122.1(3) . . ?
C17 N2 C13 117.5(4) . . ?
C17 N2 Y1 120.9(3) . . ?
C13 N2 Y1 121.4(3) . . ?
C6 C1 C2 121.8(4) . . ?
C6 C1 S1 120.6(4) . . ?
C2 C1 S1 117.5(4) . . ?
O4 C2 C3 121.5(4) . . ?
O4 C2 C1 122.3(4) . . ?
C3 C2 C1 116.1(4) . . ?
C4 C3 C2 122.2(4) . . ?
C4 C3 H3A 118.9 . . ?
C2 C3 H3A 118.9 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 C7 120.6(4) . . ?
C5 C4 C7 119.4(4) . . ?
C6 C5 C4 118.8(4) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C1 C6 C5 121.0(4) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
O5 C7 O6 125.5(4) . . ?
O5 C7 C4 116.9(4) . . ?
O6 C7 C4 117.5(4) . . ?
N1 C8 C9 123.3(5) . . ?
N1 C8 H8 118.3 . . ?
C9 C8 H8 118.3 . . ?
C10 C9 C8 118.4(5) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C11 C10 C9 119.1(5) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 120.7(5) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
N1 C12 C11 120.9(5) . . ?
N1 C12 C13 114.7(4) . . ?
C11 C12 C13 124.3(5) . . ?
N2 C13 C14 122.0(5) . . ?
N2 C13 C12 115.9(4) . . ?
C14 C13 C12 121.9(5) . . ?
C15 C14 C13 119.0(5) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 119.1(5) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C15 C16 C17 118.2(5) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
N2 C17 C16 124.0(5) . . ?
N2 C17 H17 118.0 . . ?
C16 C17 H17 118.0 . . ?

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 Y1 177.85(19) . . . . ?
O3 S1 O1 Y1 51.9(3) . . . . ?
C1 S1 O1 Y1 -65.2(3) . . . . ?
O4 Y1 O1 S1 32.0(2) . . . . ?
O5 Y1 O1 S1 -84.6(2) 4_565 . . . ?
O6 Y1 O1 S1 75.2(3) 3_656 . . . ?
O3 Y1 O1 S1 -38.1(3) 2_545 . . . ?
O1W Y1 O1 S1 -148.7(2) . . . . ?
N1 Y1 O1 S1 120.5(2) . . . . ?
N2 Y1 O1 S1 -176.9(3) . . . . ?
O2 S1 O3 Y1 114.1(8) . . . 2 ?
O1 S1 O3 Y1 -119.1(8) . . . 2 ?
C1 S1 O3 Y1 -4.2(9) . . . 2 ?
O5 Y1 O4 C2 96.0(4) 4_565 . . . ?
O6 Y1 O4 C2 -122.4(4) 3_656 . . . ?
O3 Y1 O4 C2 167.2(4) 2_545 . . . ?
O1W Y1 O4 C2 -145.6(4) . . . . ?
O1 Y1 O4 C2 33.0(4) . . . . ?
N1 Y1 O4 C2 -50.5(4) . . . . ?
N2 Y1 O4 C2 -3.0(5) . . . . ?
O4 Y1 N1 C8 -32.9(4) . . . . ?
O5 Y1 N1 C8 -149.2(3) 4_565 . . . ?
O6 Y1 N1 C8 47.4(4) 3_656 . . . ?
O3 Y1 N1 C8 47.4(5) 2_545 . . . ?
O1W Y1 N1 C8 125.5(4) . . . . ?
O1 Y1 N1 C8 -105.9(4) . . . . ?
N2 Y1 N1 C8 -173.7(4) . . . . ?
O4 Y1 N1 C12 157.7(4) . . . . ?
O5 Y1 N1 C12 41.4(5) 4_565 . . . ?
O6 Y1 N1 C12 -121.9(4) 3_656 . . . ?
O3 Y1 N1 C12 -122.0(3) 2_545 . . . ?
O1W Y1 N1 C12 -43.9(4) . . . . ?
O1 Y1 N1 C12 84.7(4) . . . . ?
N2 Y1 N1 C12 16.9(3) . . . . ?
O4 Y1 N2 C17 111.9(4) . . . . ?
O5 Y1 N2 C17 2.4(4) 4_565 . . . ?
O6 Y1 N2 C17 -146.2(4) 3_656 . . . ?
O3 Y1 N2 C17 -52.3(4) 2_545 . . . ?
O1W Y1 N2 C17 -82.1(4) . . . . ?
O1 Y1 N2 C17 74.4(4) . . . . ?
N1 Y1 N2 C17 168.4(4) . . . . ?
O4 Y1 N2 C13 -72.6(4) . . . . ?
O5 Y1 N2 C13 177.9(4) 4_565 . . . ?
O6 Y1 N2 C13 29.3(4) 3_656 . . . ?
O3 Y1 N2 C13 123.2(3) 2_545 . . . ?
O1W Y1 N2 C13 93.4(3) . . . . ?
O1 Y1 N2 C13 -110.1(4) . . . . ?
N1 Y1 N2 C13 -16.2(3) . . . . ?
O2 S1 C1 C6 -10.5(4) . . . . ?
O3 S1 C1 C6 110.0(4) . . . . ?
O1 S1 C1 C6 -130.7(4) . . . . ?
O2 S1 C1 C2 167.5(3) . . . . ?
O3 S1 C1 C2 -72.1(4) . . . . ?
O1 S1 C1 C2 47.2(4) . . . . ?
Y1 O4 C2 C3 130.0(4) . . . . ?
Y1 O4 C2 C1 -52.4(6) . . . . ?
C6 C1 C2 O4 -178.6(4) . . . . ?
S1 C1 C2 O4 3.4(6) . . . . ?
C6 C1 C2 C3 -0.9(7) . . . . ?
S1 C1 C2 C3 -178.8(3) . . . . ?
O4 C2 C3 C4 176.5(4) . . . . ?
C1 C2 C3 C4 -1.2(7) . . . . ?
C2 C3 C4 C5 2.6(7) . . . . ?
C2 C3 C4 C7 -175.6(4) . . . . ?
C3 C4 C5 C6 -1.7(7) . . . . ?
C7 C4 C5 C6 176.4(4) . . . . ?
C2 C1 C6 C5 1.7(7) . . . . ?
S1 C1 C6 C5 179.6(4) . . . . ?
C4 C5 C6 C1 -0.4(7) . . . . ?
Y1 O5 C7 O6 5.7(10) 4_666 . . . ?
Y1 O5 C7 C4 -171.7(5) 4_666 . . . ?
Y1 O6 C7 O5 48.4(8) 3_656 . . . ?
Y1 O6 C7 C4 -134.2(5) 3_656 . . . ?
C3 C4 C7 O5 -166.3(4) . . . . ?
C5 C4 C7 O5 15.6(6) . . . . ?
C3 C4 C7 O6 16.1(6) . . . . ?
C5 C4 C7 O6 -162.0(4) . . . . ?
C12 N1 C8 C9 1.7(8) . . . . ?
Y1 N1 C8 C9 -168.2(4) . . . . ?
N1 C8 C9 C10 -0.3(8) . . . . ?
C8 C9 C10 C11 0.2(9) . . . . ?
C9 C10 C11 C12 -1.4(9) . . . . ?
C8 N1 C12 C11 -2.9(7) . . . . ?
Y1 N1 C12 C11 166.7(4) . . . . ?
C8 N1 C12 C13 173.8(4) . . . . ?
Y1 N1 C12 C13 -16.7(6) . . . . ?
C10 C11 C12 N1 2.8(9) . . . . ?
C10 C11 C12 C13 -173.5(5) . . . . ?
C17 N2 C13 C14 4.8(7) . . . . ?
Y1 N2 C13 C14 -170.8(4) . . . . ?
C17 N2 C13 C12 -169.7(4) . . . . ?
Y1 N2 C13 C12 14.6(6) . . . . ?
N1 C12 C13 N2 1.1(6) . . . . ?
C11 C12 C13 N2 177.6(5) . . . . ?
N1 C12 C13 C14 -173.5(5) . . . . ?
C11 C12 C13 C14 3.0(8) . . . . ?
N2 C13 C14 C15 -4.1(8) . . . . ?
C12 C13 C14 C15 170.1(5) . . . . ?
C13 C14 C15 C16 -0.1(8) . . . . ?
C14 C15 C16 C17 3.3(8) . . . . ?
C13 N2 C17 C16 -1.4(8) . . . . ?
Y1 N2 C17 C16 174.2(4) . . . . ?
C15 C16 C17 N2 -2.6(8) . . . . ?

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
O1W H1W1 O4 0.85(4) 1.910(11) 2.755(4) 178(5) 2_545
O1W H1W2 O2 0.85(4) 2.065(12) 2.911(5) 175(6) 1_545

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.128
####################################################################### 
# 
# 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_4-Lu
_database_code_depnum_ccdc_archive 'CCDC 1549855'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H9 Lu O9 S, H2 O'
_chemical_formula_sum            'C7 H11 Lu O10 S'
_chemical_formula_weight         462.19

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.8405(4)
_cell_length_b                   9.2489(3)
_cell_length_c                   12.0420(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.702(3)
_cell_angle_gamma                90.00
_cell_volume                     1206.82(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1825
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    8.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2594
_exptl_absorpt_correction_T_max  0.3467
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4275
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2752
_reflns_number_gt                2394
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0228P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2752
_refine_ls_number_parameters     190
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0630
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.002
_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
Lu1 Lu -0.02729(2) 0.31712(2) 0.938368(16) 0.01521(8) Uani 1 1 d . . .
S1 S 0.25616(14) 0.24132(14) 1.07095(10) 0.0189(3) Uani 1 1 d . . .
O1 O 0.1373(4) 0.1946(4) 1.0243(3) 0.0288(10) Uani 1 1 d . . .
O1W O -0.0864(4) 0.4633(4) 0.7913(3) 0.0290(10) Uani 1 1 d D . .
H1W1 H -0.134(5) 0.533(5) 0.806(4) 0.044 Uiso 1 1 d D . .
H1W2 H -0.102(6) 0.430(6) 0.727(2) 0.044 Uiso 1 1 d D . .
O2W O -0.2380(4) 0.2659(4) 0.9004(3) 0.0278(9) Uani 1 1 d D . .
H2W1 H -0.282(6) 0.213(6) 0.940(4) 0.042 Uiso 1 1 d D . .
H2W2 H -0.239(6) 0.235(6) 0.8340(17) 0.042 Uiso 1 1 d D . .
O2 O 0.2430(5) 0.3139(4) 1.1775(3) 0.0311(11) Uani 1 1 d . . .
O3W O -0.0884(4) 0.1724(4) 1.0806(3) 0.0275(9) Uani 1 1 d . . .
H3W1 H -0.1656 0.1564 1.0787 0.041 Uiso 1 1 d R . .
H3W2 H -0.0518 0.0961 1.1032 0.041 Uiso 1 1 d R . .
O3 O 0.3445(4) 0.1242(4) 1.0784(3) 0.0234(9) Uani 1 1 d . . .
O4 O 0.1170(3) 0.4930(4) 0.9730(3) 0.0163(7) Uani 1 1 d . . .
O4W O 0.3323(5) -0.1028(5) 0.9207(4) 0.0441(13) Uani 1 1 d D . .
H4W1 H 0.359(7) -0.125(6) 0.858(3) 0.066 Uiso 1 1 d D . .
H4W2 H 0.352(8) -0.017(3) 0.937(5) 0.066 Uiso 1 1 d D . .
O5 O 0.5205(4) 0.5971(4) 0.6588(3) 0.0248(9) Uani 1 1 d . . .
O6 O 0.4000(4) 0.7710(4) 0.7152(3) 0.0253(9) Uani 1 1 d . . .
C1 C 0.3104(5) 0.3666(5) 0.9737(4) 0.0175(11) Uani 1 1 d . . .
C2 C 0.2321(5) 0.4758(5) 0.9344(4) 0.0154(10) Uani 1 1 d . . .
C3 C 0.2780(5) 0.5658(5) 0.8527(4) 0.0189(11) Uani 1 1 d . . .
H3A H 0.2293 0.6409 0.8245 0.023 Uiso 1 1 calc R . .
C4 C 0.3950(5) 0.5451(5) 0.8128(4) 0.0188(11) Uani 1 1 d . . .
C5 C 0.4702(5) 0.4361(6) 0.8517(4) 0.0219(12) Uani 1 1 d . . .
H5A H 0.5483 0.4232 0.8234 0.026 Uiso 1 1 calc R . .
C6 C 0.4277(6) 0.3450(6) 0.9339(4) 0.0224(12) Uani 1 1 d . . .
H6A H 0.4772 0.2706 0.9620 0.027 Uiso 1 1 calc R . .
C7 C 0.4400(5) 0.6435(6) 0.7236(4) 0.0175(11) 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
Lu1 O4 2.287(4) . ?
Lu1 O4 2.287(3) 3_567 ?
Lu1 O3W 2.287(4) . ?
Lu1 O1W 2.303(4) . ?
Lu1 O1 2.330(4) . ?
Lu1 O5 2.349(4) 2_546 ?
Lu1 O2W 2.364(4) . ?
Lu1 O6 2.379(4) 2_546 ?
Lu1 C7 2.718(5) 2_546 ?
Lu1 Lu1 3.7343(4) 3_567 ?
S1 O3 1.447(4) . ?
S1 O1 1.456(5) . ?
S1 O2 1.459(4) . ?
S1 C1 1.761(5) . ?
O1W H1W1 0.85(6) . ?
O1W H1W2 0.85(6) . ?
O2W H2W1 0.85(6) . ?
O2W H2W2 0.85(6) . ?
O3W H3W1 0.8501 . ?
O3W H3W2 0.8500 . ?
O4 C2 1.353(6) . ?
O4 Lu1 2.287(3) 3_567 ?
O4W H4W1 0.85(6) . ?
O4W H4W2 0.85(6) . ?
O5 C7 1.263(6) . ?
O5 Lu1 2.349(4) 2_556 ?
O6 C7 1.259(6) . ?
O6 Lu1 2.379(4) 2_556 ?
C1 C6 1.386(8) . ?
C1 C2 1.393(7) . ?
C2 C3 1.393(7) . ?
C3 C4 1.383(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(7) . ?
C4 C7 1.500(7) . ?
C5 C6 1.390(7) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 Lu1 2.718(5) 2_556 ?

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
O4 Lu1 O4 70.52(15) . 3_567 ?
O4 Lu1 O3W 119.41(14) . . ?
O4 Lu1 O3W 87.90(12) 3_567 . ?
O4 Lu1 O1W 84.03(14) . . ?
O4 Lu1 O1W 78.20(12) 3_567 . ?
O3W Lu1 O1W 147.04(17) . . ?
O4 Lu1 O1 75.77(13) . . ?
O4 Lu1 O1 119.79(14) 3_567 . ?
O3W Lu1 O1 67.52(15) . . ?
O1W Lu1 O1 144.96(15) . . ?
O4 Lu1 O5 132.52(13) . 2_546 ?
O4 Lu1 O5 156.55(14) 3_567 2_546 ?
O3W Lu1 O5 83.12(13) . 2_546 ?
O1W Lu1 O5 97.91(13) . 2_546 ?
O1 Lu1 O5 76.42(14) . 2_546 ?
O4 Lu1 O2W 146.07(13) . . ?
O4 Lu1 O2W 79.77(13) 3_567 . ?
O3W Lu1 O2W 74.24(15) . . ?
O1W Lu1 O2W 73.96(15) . . ?
O1 Lu1 O2W 135.34(14) . . ?
O5 Lu1 O2W 76.96(14) 2_546 . ?
O4 Lu1 O6 81.96(13) . 2_546 ?
O4 Lu1 O6 139.90(12) 3_567 2_546 ?
O3W Lu1 O6 131.68(13) . 2_546 ?
O1W Lu1 O6 70.25(14) . 2_546 ?
O1 Lu1 O6 78.70(15) . 2_546 ?
O5 Lu1 O6 55.26(13) 2_546 2_546 ?
O2W Lu1 O6 113.14(14) . 2_546 ?
O4 Lu1 C7 107.49(14) . 2_546 ?
O4 Lu1 C7 161.87(14) 3_567 2_546 ?
O3W Lu1 C7 107.85(15) . 2_546 ?
O1W Lu1 C7 83.67(15) . 2_546 ?
O1 Lu1 C7 75.72(15) . 2_546 ?
O5 Lu1 C7 27.67(14) 2_546 2_546 ?
O2W Lu1 C7 95.59(15) . 2_546 ?
O6 Lu1 C7 27.60(14) 2_546 2_546 ?
O4 Lu1 Lu1 35.26(9) . 3_567 ?
O4 Lu1 Lu1 35.26(9) 3_567 3_567 ?
O3W Lu1 Lu1 106.16(10) . 3_567 ?
O1W Lu1 Lu1 79.11(10) . 3_567 ?
O1 Lu1 Lu1 98.84(10) . 3_567 ?
O5 Lu1 Lu1 167.32(10) 2_546 3_567 ?
O2W Lu1 Lu1 113.53(10) . 3_567 ?
O6 Lu1 Lu1 112.50(9) 2_546 3_567 ?
C7 Lu1 Lu1 139.99(12) 2_546 3_567 ?
O3 S1 O1 112.2(2) . . ?
O3 S1 O2 111.8(2) . . ?
O1 S1 O2 111.5(3) . . ?
O3 S1 C1 107.5(2) . . ?
O1 S1 C1 104.4(2) . . ?
O2 S1 C1 109.0(2) . . ?
S1 O1 Lu1 133.2(2) . . ?
Lu1 O1W H1W1 117(4) . . ?
Lu1 O1W H1W2 122(4) . . ?
H1W1 O1W H1W2 111.1(18) . . ?
Lu1 O2W H2W1 125(5) . . ?
Lu1 O2W H2W2 104(4) . . ?
H2W1 O2W H2W2 110.6(18) . . ?
Lu1 O3W H3W1 112.8 . . ?
Lu1 O3W H3W2 125.6 . . ?
H3W1 O3W H3W2 108.2 . . ?
C2 O4 Lu1 119.1(3) . . ?
C2 O4 Lu1 131.3(3) . 3_567 ?
Lu1 O4 Lu1 109.48(15) . 3_567 ?
H4W1 O4W H4W2 110.3(18) . . ?
C7 O5 Lu1 92.6(3) . 2_556 ?
C7 O6 Lu1 91.4(3) . 2_556 ?
C6 C1 C2 122.9(5) . . ?
C6 C1 S1 117.6(4) . . ?
C2 C1 S1 119.4(4) . . ?
O4 C2 C3 121.7(5) . . ?
O4 C2 C1 121.8(4) . . ?
C3 C2 C1 116.5(5) . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C5 C4 C3 121.7(5) . . ?
C5 C4 C7 119.2(5) . . ?
C3 C4 C7 119.1(5) . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
C1 C6 C5 119.1(5) . . ?
C1 C6 H6A 120.5 . . ?
C5 C6 H6A 120.5 . . ?
O6 C7 O5 120.7(5) . . ?
O6 C7 C4 120.4(5) . . ?
O5 C7 C4 118.8(5) . . ?
O6 C7 Lu1 61.0(3) . 2_556 ?
O5 C7 Lu1 59.7(3) . 2_556 ?
C4 C7 Lu1 178.4(4) . 2_556 ?

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
O3 S1 O1 Lu1 -158.8(3) . . . . ?
O2 S1 O1 Lu1 74.8(3) . . . . ?
C1 S1 O1 Lu1 -42.7(4) . . . . ?
O4 Lu1 O1 S1 2.3(3) . . . . ?
O4 Lu1 O1 S1 -54.9(4) 3_567 . . . ?
O3W Lu1 O1 S1 -128.5(4) . . . . ?
O1W Lu1 O1 S1 59.1(4) . . . . ?
O5 Lu1 O1 S1 143.5(4) 2_546 . . . ?
O2W Lu1 O1 S1 -161.6(3) . . . . ?
O6 Lu1 O1 S1 86.8(3) 2_546 . . . ?
C7 Lu1 O1 S1 114.9(4) 2_546 . . . ?
Lu1 Lu1 O1 S1 -24.5(3) 3_567 . . . ?
O4 Lu1 O4 C2 -175.7(4) 3_567 . . . ?
O3W Lu1 O4 C2 108.4(3) . . . . ?
O1W Lu1 O4 C2 -96.2(3) . . . . ?
O1 Lu1 O4 C2 55.0(3) . . . . ?
O5 Lu1 O4 C2 -0.9(4) 2_546 . . . ?
O2W Lu1 O4 C2 -145.4(3) . . . . ?
O6 Lu1 O4 C2 -25.3(3) 2_546 . . . ?
C7 Lu1 O4 C2 -14.8(4) 2_546 . . . ?
Lu1 Lu1 O4 C2 -175.7(4) 3_567 . . . ?
O4 Lu1 O4 Lu1 0.0 3_567 . . 3_567 ?
O3W Lu1 O4 Lu1 -75.88(18) . . . 3_567 ?
O1W Lu1 O4 Lu1 79.56(15) . . . 3_567 ?
O1 Lu1 O4 Lu1 -129.30(17) . . . 3_567 ?
O5 Lu1 O4 Lu1 174.84(13) 2_546 . . 3_567 ?
O2W Lu1 O4 Lu1 30.3(3) . . . 3_567 ?
O6 Lu1 O4 Lu1 150.40(16) 2_546 . . 3_567 ?
C7 Lu1 O4 Lu1 160.99(15) 2_546 . . 3_567 ?
O3 S1 C1 C6 -7.9(5) . . . . ?
O1 S1 C1 C6 -127.2(4) . . . . ?
O2 S1 C1 C6 113.5(4) . . . . ?
O3 S1 C1 C2 167.7(4) . . . . ?
O1 S1 C1 C2 48.4(5) . . . . ?
O2 S1 C1 C2 -70.9(5) . . . . ?
Lu1 O4 C2 C3 113.6(4) . . . . ?
Lu1 O4 C2 C3 -61.1(6) 3_567 . . . ?
Lu1 O4 C2 C1 -65.9(5) . . . . ?
Lu1 O4 C2 C1 119.5(4) 3_567 . . . ?
C6 C1 C2 O4 178.7(5) . . . . ?
S1 C1 C2 O4 3.3(7) . . . . ?
C6 C1 C2 C3 -0.8(8) . . . . ?
S1 C1 C2 C3 -176.2(4) . . . . ?
O4 C2 C3 C4 -178.9(4) . . . . ?
C1 C2 C3 C4 0.7(7) . . . . ?
C2 C3 C4 C5 0.0(8) . . . . ?
C2 C3 C4 C7 179.2(5) . . . . ?
C3 C4 C5 C6 -0.6(8) . . . . ?
C7 C4 C5 C6 -179.8(5) . . . . ?
C2 C1 C6 C5 0.3(8) . . . . ?
S1 C1 C6 C5 175.7(4) . . . . ?
C4 C5 C6 C1 0.4(8) . . . . ?
Lu1 O6 C7 O5 0.8(5) 2_556 . . . ?
Lu1 O6 C7 C4 179.3(4) 2_556 . . . ?
Lu1 O5 C7 O6 -0.8(5) 2_556 . . . ?
Lu1 O5 C7 C4 -179.4(4) 2_556 . . . ?
C5 C4 C7 O6 -152.8(5) . . . . ?
C3 C4 C7 O6 28.0(8) . . . . ?
C5 C4 C7 O5 25.8(8) . . . . ?
C3 C4 C7 O5 -153.4(5) . . . . ?

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
O1W H1W1 O2 0.85(6) 1.861(13) 2.703(6) 174(5) 3_567
O1W H1W2 O3 0.85(6) 1.934(15) 2.770(5) 171(5) 4_565
O2W H2W1 O4W 0.85(6) 2.04(3) 2.845(6) 157(6) 3_557
O2W H2W2 O2 0.85(6) 1.943(15) 2.785(5) 172(7) 4_565
O3W H3W1 O4W 0.85 1.87 2.721(7) 174.4 3_557
O3W H3W2 O5 0.85 2.06 2.903(5) 174.7 4_566
O4W H4W1 O6 0.85(6) 2.026(18) 2.851(5) 165(6) 1_545
O4W H4W2 O3 0.85(6) 2.15(4) 2.831(6) 138(5) .

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.556
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.184
####################################################################### 
# 
# 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_5-Pr
_database_code_depnum_ccdc_archive 'CCDC 1549857'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 N2 O7 Pr S'
_chemical_formula_sum            'C17 H13 N2 O7 Pr S'
_chemical_formula_weight         530.26

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.2702(3)
_cell_length_b                   8.58496(16)
_cell_length_c                   18.2760(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.839(2)
_cell_angle_gamma                90.00
_cell_volume                     1683.26(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2632
_cell_measurement_theta_min      3.80
_cell_measurement_theta_max      29.32

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    3.066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_T_max  0.6563
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6183
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3876
_reflns_number_gt                3289
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0164P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3876
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.034
_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
Pr1 Pr 0.369476(16) 1.03976(2) 0.193056(11) 0.01351(7) Uani 1 1 d . . .
S1 S 0.69505(7) 1.13019(10) 0.34058(5) 0.01523(19) Uani 1 1 d . . .
O1W O 0.3329(2) 1.2739(3) 0.26916(17) 0.0263(7) Uani 1 1 d D . .
H1W1 H 0.296(3) 1.350(3) 0.2424(19) 0.039 Uiso 1 1 d D . .
H1W2 H 0.391(3) 1.307(4) 0.3075(16) 0.039 Uiso 1 1 d D . .
O1 O 0.5817(2) 1.1008(3) 0.27679(15) 0.0235(6) Uani 1 1 d . . .
O2 O 0.7485(2) 1.2824(3) 0.33250(15) 0.0201(6) Uani 1 1 d . . .
O3 O 0.7839(2) 1.0039(3) 0.34914(16) 0.0231(6) Uani 1 1 d . . .
O4 O 0.5430(2) 1.3809(3) 0.38126(15) 0.0200(6) Uani 1 1 d . . .
O5 O 0.4612(2) 1.2615(3) 0.63166(16) 0.0234(6) Uani 1 1 d . . .
O6 O 0.6068(2) 1.0839(3) 0.68700(15) 0.0230(6) Uani 1 1 d . . .
N1 N 0.1315(3) 1.0735(4) 0.1858(2) 0.0221(7) Uani 1 1 d . . .
N2 N 0.2000(3) 1.1151(4) 0.06013(19) 0.0219(7) Uani 1 1 d . . .
C1 C 0.6534(3) 1.1436(4) 0.4259(2) 0.0158(7) Uani 1 1 d . . .
C2 C 0.5826(3) 1.2728(4) 0.4356(2) 0.0171(8) Uani 1 1 d . . .
C3 C 0.5540(3) 1.2793(4) 0.5050(2) 0.0180(8) Uani 1 1 d . . .
H3 H 0.5091 1.3641 0.5141 0.022 Uiso 1 1 calc R . .
C4 C 0.5902(3) 1.1639(4) 0.5603(2) 0.0150(7) Uani 1 1 d . . .
C5 C 0.6611(3) 1.0387(4) 0.5489(2) 0.0179(8) Uani 1 1 d . . .
H5 H 0.6868 0.9617 0.5862 0.021 Uiso 1 1 calc R . .
C6 C 0.6928(3) 1.0296(4) 0.4821(2) 0.0179(8) Uani 1 1 d . . .
H6 H 0.7408 0.9467 0.4745 0.021 Uiso 1 1 calc R . .
C7 C 0.5494(3) 1.1719(4) 0.6318(2) 0.0173(8) Uani 1 1 d . . .
C8 C 0.0947(4) 1.0290(5) 0.2453(3) 0.0307(10) Uani 1 1 d . . .
H8 H 0.1525 0.9796 0.2861 0.037 Uiso 1 1 calc R . .
C9 C -0.0234(4) 1.0518(5) 0.2498(3) 0.0357(11) Uani 1 1 d . . .
H9 H -0.0463 1.0136 0.2911 0.043 Uiso 1 1 calc R . .
C10 C -0.1069(4) 1.1328(6) 0.1916(3) 0.0419(13) Uani 1 1 d . . .
H10 H -0.1861 1.1555 0.1942 0.050 Uiso 1 1 calc R . .
C11 C -0.0721(3) 1.1796(5) 0.1296(3) 0.0359(11) Uani 1 1 d . . .
H11 H -0.1276 1.2349 0.0899 0.043 Uiso 1 1 calc R . .
C12 C 0.0468(3) 1.1443(4) 0.1260(3) 0.0235(9) Uani 1 1 d . . .
C13 C 0.0854(3) 1.1696(4) 0.0571(3) 0.0257(9) Uani 1 1 d . . .
C14 C 0.0082(4) 1.2337(6) -0.0100(3) 0.0417(13) Uani 1 1 d . . .
H14 H -0.0697 1.2720 -0.0114 0.050 Uiso 1 1 calc R . .
C15 C 0.0457(4) 1.2413(6) -0.0745(3) 0.0466(14) Uani 1 1 d . . .
H15 H -0.0064 1.2846 -0.1196 0.056 Uiso 1 1 calc R . .
C16 C 0.1608(4) 1.1843(5) -0.0721(3) 0.0339(11) Uani 1 1 d . . .
H16 H 0.1883 1.1870 -0.1152 0.041 Uiso 1 1 calc R . .
C17 C 0.2340(4) 1.1228(5) -0.0030(2) 0.0278(9) Uani 1 1 d . . .
H17 H 0.3122 1.0845 -0.0008 0.033 Uiso 1 1 calc R . .


_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
Pr1 O4 2.345(3) 2_645 ?
Pr1 O6 2.376(3) 3_676 ?
Pr1 O5 2.439(3) 4_585 ?
Pr1 O1 2.468(2) . ?
Pr1 O2 2.547(2) 2_645 ?
Pr1 O1W 2.548(3) . ?
Pr1 N1 2.661(3) . ?
Pr1 N2 2.669(3) . ?
S1 O3 1.452(2) . ?
S1 O1 1.464(2) . ?
S1 O2 1.466(2) . ?
S1 C1 1.764(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O2 Pr1 2.547(2) 2_655 ?
O4 C2 1.332(4) . ?
O4 Pr1 2.345(3) 2_655 ?
O5 C7 1.257(4) . ?
O5 Pr1 2.439(3) 4_586 ?
O6 C7 1.268(4) . ?
O6 Pr1 2.376(3) 3_676 ?
N1 C8 1.331(5) . ?
N1 C12 1.355(5) . ?
N2 C17 1.325(5) . ?
N2 C13 1.359(5) . ?
C1 C6 1.389(5) . ?
C1 C2 1.409(5) . ?
C2 C3 1.403(5) . ?
C3 C4 1.386(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.392(5) . ?
C4 C7 1.513(5) . ?
C5 C6 1.376(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.374(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.374(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.394(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.468(6) . ?
C13 C14 1.383(6) . ?
C14 C15 1.370(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.374(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Pr1 O6 109.02(9) 2_645 3_676 ?
O4 Pr1 O5 80.08(9) 2_645 4_585 ?
O6 Pr1 O5 142.49(9) 3_676 4_585 ?
O4 Pr1 O1 89.03(8) 2_645 . ?
O6 Pr1 O1 73.08(9) 3_676 . ?
O5 Pr1 O1 70.75(9) 4_585 . ?
O4 Pr1 O2 71.21(8) 2_645 2_645 ?
O6 Pr1 O2 71.73(9) 3_676 2_645 ?
O5 Pr1 O2 142.51(9) 4_585 2_645 ?
O1 Pr1 O2 130.55(8) . 2_645 ?
O4 Pr1 O1W 160.37(9) 2_645 . ?
O6 Pr1 O1W 80.80(9) 3_676 . ?
O5 Pr1 O1W 82.05(9) 4_585 . ?
O1 Pr1 O1W 77.42(8) . . ?
O2 Pr1 O1W 128.42(9) 2_645 . ?
O4 Pr1 N1 129.13(9) 2_645 . ?
O6 Pr1 N1 85.48(10) 3_676 . ?
O5 Pr1 N1 117.64(9) 4_585 . ?
O1 Pr1 N1 141.09(10) . . ?
O2 Pr1 N1 67.87(8) 2_645 . ?
O1W Pr1 N1 67.18(9) . . ?
O4 Pr1 N2 85.67(9) 2_645 . ?
O6 Pr1 N2 142.64(9) 3_676 . ?
O5 Pr1 N2 72.41(9) 4_585 . ?
O1 Pr1 N2 143.14(9) . . ?
O2 Pr1 N2 81.68(9) 2_645 . ?
O1W Pr1 N2 96.63(9) . . ?
N1 Pr1 N2 59.94(10) . . ?
O3 S1 O1 111.23(16) . . ?
O3 S1 O2 112.67(15) . . ?
O1 S1 O2 111.06(15) . . ?
O3 S1 C1 108.35(17) . . ?
O1 S1 C1 108.15(16) . . ?
O2 S1 C1 105.06(17) . . ?
Pr1 O1W H1W1 115(3) . . ?
Pr1 O1W H1W2 120(3) . . ?
H1W1 O1W H1W2 109.7(17) . . ?
S1 O1 Pr1 166.88(18) . . ?
S1 O2 Pr1 125.74(13) . 2_655 ?
C2 O4 Pr1 137.1(2) . 2_655 ?
C7 O5 Pr1 150.9(2) . 4_586 ?
C7 O6 Pr1 152.4(2) . 3_676 ?
C8 N1 C12 118.0(3) . . ?
C8 N1 Pr1 119.3(3) . . ?
C12 N1 Pr1 122.6(3) . . ?
C17 N2 C13 118.2(3) . . ?
C17 N2 Pr1 119.2(2) . . ?
C13 N2 Pr1 121.8(3) . . ?
C6 C1 C2 121.8(4) . . ?
C6 C1 S1 119.8(3) . . ?
C2 C1 S1 118.4(3) . . ?
O4 C2 C3 121.9(3) . . ?
O4 C2 C1 121.9(3) . . ?
C3 C2 C1 116.2(3) . . ?
C4 C3 C2 122.2(3) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 C7 119.9(3) . . ?
C5 C4 C7 120.3(3) . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O5 C7 O6 125.2(4) . . ?
O5 C7 C4 118.4(3) . . ?
O6 C7 C4 116.4(3) . . ?
N1 C8 C9 123.9(4) . . ?
N1 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
C8 C9 C10 118.1(5) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C11 C10 C9 119.2(4) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
N1 C12 C11 120.6(4) . . ?
N1 C12 C13 116.0(3) . . ?
C11 C12 C13 123.3(4) . . ?
N2 C13 C14 120.3(4) . . ?
N2 C13 C12 116.2(3) . . ?
C14 C13 C12 123.3(4) . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C17 117.2(4) . . ?
C15 C16 H16 121.4 . . ?
C17 C16 H16 121.4 . . ?
N2 C17 C16 124.3(4) . . ?
N2 C17 H17 117.8 . . ?
C16 C17 H17 117.8 . . ?

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
O3 S1 O1 Pr1 106.8(7) . . . . ?
O2 S1 O1 Pr1 -126.9(7) . . . . ?
C1 S1 O1 Pr1 -12.1(8) . . . . ?
O4 Pr1 O1 S1 -134.3(7) 2_645 . . . ?
O6 Pr1 O1 S1 -24.1(7) 3_676 . . . ?
O5 Pr1 O1 S1 145.8(8) 4_585 . . . ?
O2 Pr1 O1 S1 -70.3(8) 2_645 . . . ?
O1W Pr1 O1 S1 60.0(7) . . . . ?
N1 Pr1 O1 S1 35.4(8) . . . . ?
N2 Pr1 O1 S1 144.2(7) . . . . ?
O3 S1 O2 Pr1 175.66(16) . . . 2_655 ?
O1 S1 O2 Pr1 50.1(2) . . . 2_655 ?
C1 S1 O2 Pr1 -66.6(2) . . . 2_655 ?
O4 Pr1 N1 C8 115.2(3) 2_645 . . . ?
O6 Pr1 N1 C8 4.3(3) 3_676 . . . ?
O5 Pr1 N1 C8 -144.7(3) 4_585 . . . ?
O1 Pr1 N1 C8 -51.5(4) . . . . ?
O2 Pr1 N1 C8 76.4(3) 2_645 . . . ?
O1W Pr1 N1 C8 -77.6(3) . . . . ?
N2 Pr1 N1 C8 169.5(3) . . . . ?
O4 Pr1 N1 C12 -69.5(3) 2_645 . . . ?
O6 Pr1 N1 C12 179.6(3) 3_676 . . . ?
O5 Pr1 N1 C12 30.6(3) 4_585 . . . ?
O1 Pr1 N1 C12 123.8(3) . . . . ?
O2 Pr1 N1 C12 -108.3(3) 2_645 . . . ?
O1W Pr1 N1 C12 97.7(3) . . . . ?
N2 Pr1 N1 C12 -15.2(3) . . . . ?
O4 Pr1 N2 C17 -33.7(3) 2_645 . . . ?
O6 Pr1 N2 C17 -149.8(3) 3_676 . . . ?
O5 Pr1 N2 C17 47.2(3) 4_585 . . . ?
O1 Pr1 N2 C17 48.8(4) . . . . ?
O2 Pr1 N2 C17 -105.4(3) 2_645 . . . ?
O1W Pr1 N2 C17 126.7(3) . . . . ?
N1 Pr1 N2 C17 -174.6(3) . . . . ?
O4 Pr1 N2 C13 156.9(3) 2_645 . . . ?
O6 Pr1 N2 C13 40.8(3) 3_676 . . . ?
O5 Pr1 N2 C13 -122.1(3) 4_585 . . . ?
O1 Pr1 N2 C13 -120.5(3) . . . . ?
O2 Pr1 N2 C13 85.3(3) 2_645 . . . ?
O1W Pr1 N2 C13 -42.7(3) . . . . ?
N1 Pr1 N2 C13 16.1(3) . . . . ?
O3 S1 C1 C6 -8.2(3) . . . . ?
O1 S1 C1 C6 112.5(3) . . . . ?
O2 S1 C1 C6 -128.8(3) . . . . ?
O3 S1 C1 C2 170.6(3) . . . . ?
O1 S1 C1 C2 -68.8(3) . . . . ?
O2 S1 C1 C2 49.9(3) . . . . ?
Pr1 O4 C2 C3 129.5(3) 2_655 . . . ?
Pr1 O4 C2 C1 -51.9(5) 2_655 . . . ?
C6 C1 C2 O4 -178.8(3) . . . . ?
S1 C1 C2 O4 2.4(4) . . . . ?
C6 C1 C2 C3 -0.2(5) . . . . ?
S1 C1 C2 C3 -178.9(3) . . . . ?
O4 C2 C3 C4 177.1(3) . . . . ?
C1 C2 C3 C4 -1.6(5) . . . . ?
C2 C3 C4 C5 2.2(5) . . . . ?
C2 C3 C4 C7 -176.0(3) . . . . ?
C3 C4 C5 C6 -1.0(5) . . . . ?
C7 C4 C5 C6 177.2(3) . . . . ?
C4 C5 C6 C1 -0.6(5) . . . . ?
C2 C1 C6 C5 1.3(5) . . . . ?
S1 C1 C6 C5 180.0(3) . . . . ?
Pr1 O5 C7 O6 47.5(7) 4_586 . . . ?
Pr1 O5 C7 C4 -134.0(4) 4_586 . . . ?
Pr1 O6 C7 O5 11.5(7) 3_676 . . . ?
Pr1 O6 C7 C4 -167.1(3) 3_676 . . . ?
C3 C4 C7 O5 16.3(5) . . . . ?
C5 C4 C7 O5 -162.0(3) . . . . ?
C3 C4 C7 O6 -165.1(3) . . . . ?
C5 C4 C7 O6 16.7(5) . . . . ?
C12 N1 C8 C9 -0.6(6) . . . . ?
Pr1 N1 C8 C9 175.0(3) . . . . ?
N1 C8 C9 C10 -3.7(7) . . . . ?
C8 C9 C10 C11 3.7(7) . . . . ?
C9 C10 C11 C12 0.3(7) . . . . ?
C8 N1 C12 C11 4.7(6) . . . . ?
Pr1 N1 C12 C11 -170.7(3) . . . . ?
C8 N1 C12 C13 -171.0(4) . . . . ?
Pr1 N1 C12 C13 13.7(4) . . . . ?
C10 C11 C12 N1 -4.6(6) . . . . ?
C10 C11 C12 C13 170.7(4) . . . . ?
C17 N2 C13 C14 -1.2(6) . . . . ?
Pr1 N2 C13 C14 168.3(3) . . . . ?
C17 N2 C13 C12 174.1(4) . . . . ?
Pr1 N2 C13 C12 -16.5(4) . . . . ?
N1 C12 C13 N2 1.9(5) . . . . ?
C11 C12 C13 N2 -173.7(4) . . . . ?
N1 C12 C13 C14 177.0(4) . . . . ?
C11 C12 C13 C14 1.4(6) . . . . ?
N2 C13 C14 C15 0.8(7) . . . . ?
C12 C13 C14 C15 -174.0(4) . . . . ?
C13 C14 C15 C16 0.1(8) . . . . ?
C14 C15 C16 C17 -0.6(7) . . . . ?
C13 N2 C17 C16 0.6(6) . . . . ?
Pr1 N2 C17 C16 -169.1(3) . . . . ?
C15 C16 C17 N2 0.3(7) . . . . ?

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
O1W H1W1 O3 0.85(4) 2.104(15) 2.926(4) 163(4) 2_655
O1W H1W1 O1 0.85(4) 2.64(3) 3.163(4) 121(3) 2_655
O1W H1W2 O4 0.85(4) 1.934(14) 2.771(3) 169(5) .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.990
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.132
####################################################################### 
# 
# 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_5-Nd
_database_code_depnum_ccdc_archive 'CCDC 1549858'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 N2 Nd O7 S'
_chemical_formula_sum            'C17 H13 N2 Nd O7 S'
_chemical_formula_weight         533.59

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.2649(8)
_cell_length_b                   8.5729(3)
_cell_length_c                   18.2321(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.005(8)
_cell_angle_gamma                90.00
_cell_volume                     1674.51(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2888
_cell_measurement_theta_min      3.80
_cell_measurement_theta_max      29.28

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    3.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5752
_exptl_absorpt_correction_T_max  0.6756
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5847
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3802
_reflns_number_gt                2564
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3802
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_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 0.67638(2) -0.03972(3) 0.306956(13) 0.01312(9) Uani 1 1 d . . .
S1 S 0.64580(11) 0.36937(12) 0.34039(6) 0.0153(3) Uani 1 1 d . . .
C5 C 0.8884(5) 0.4609(5) 0.5494(3) 0.0185(11) Uani 1 1 d . . .
H5 H 0.8995 0.5377 0.5869 0.022 Uiso 1 1 calc R . .
C17 C 0.3515(5) -0.0275(6) 0.2546(3) 0.0285(13) Uani 1 1 d . . .
H17 H 0.3693 0.0219 0.2138 0.034 Uiso 1 1 calc R . .
N2 N 0.4461(4) -0.0726(4) 0.3139(2) 0.0227(10) Uani 1 1 d . . .
O4 O 0.8379(3) 0.1180(3) 0.38097(18) 0.0192(7) Uani 1 1 d . . .
O2 O 0.6948(3) 0.3994(4) 0.27611(17) 0.0219(8) Uani 1 1 d . . .
O1W O 0.5639(3) -0.2729(3) 0.23169(19) 0.0258(8) Uani 1 1 d D . .
H1W1 H 0.555(5) -0.349(3) 0.259(2) 0.039 Uiso 1 1 d D . .
H1W2 H 0.596(4) -0.306(4) 0.198(2) 0.039 Uiso 1 1 d D . .
O1 O 0.5845(3) 0.2161(3) 0.33239(18) 0.0203(8) Uani 1 1 d . . .
O5 O 1.1713(3) 0.2385(4) 0.63169(18) 0.0220(8) Uani 1 1 d . . .
O3 O 0.5658(3) 0.4957(3) 0.3494(2) 0.0233(8) Uani 1 1 d . . .
O6 O 1.0823(3) 0.4163(4) 0.68702(18) 0.0239(8) Uani 1 1 d . . .
N1 N 0.6407(4) -0.1151(4) 0.4401(2) 0.0216(10) Uani 1 1 d . . .
C6 C 0.7904(5) 0.4710(5) 0.4820(3) 0.0190(11) Uani 1 1 d . . .
H6 H 0.7357 0.5551 0.4744 0.023 Uiso 1 1 calc R . .
C1 C 0.7720(4) 0.3571(5) 0.4250(2) 0.0137(10) Uani 1 1 d . . .
C3 C 0.9507(4) 0.2193(5) 0.5050(3) 0.0186(11) Uani 1 1 d . . .
H3 H 1.0038 0.1336 0.5140 0.022 Uiso 1 1 calc R . .
C4 C 0.9712(4) 0.3346(5) 0.5612(2) 0.0140(10) Uani 1 1 d . . .
C13 C 0.4210(5) -0.1440(5) 0.3737(3) 0.0214(12) Uani 1 1 d . . .
C2 C 0.8539(4) 0.2270(5) 0.4356(3) 0.0168(11) Uani 1 1 d . . .
C7 C 1.0822(4) 0.3278(5) 0.6315(3) 0.0168(11) Uani 1 1 d . . .
C15 C 0.2028(5) -0.1309(7) 0.3081(4) 0.0412(17) Uani 1 1 d . . .
H15 H 0.1208 -0.1536 0.3053 0.049 Uiso 1 1 calc R . .
C16 C 0.2273(5) -0.0490(6) 0.2494(3) 0.0361(15) Uani 1 1 d . . .
H16 H 0.1633 -0.0099 0.2080 0.043 Uiso 1 1 calc R . .
C12 C 0.5277(5) -0.1699(5) 0.4423(3) 0.0231(12) Uani 1 1 d . . .
C14 C 0.2982(5) -0.1786(6) 0.3703(4) 0.0347(15) Uani 1 1 d . . .
H14 H 0.2819 -0.2337 0.4100 0.042 Uiso 1 1 calc R . .
C8 C 0.7376(5) -0.1227(6) 0.5028(3) 0.0273(13) Uani 1 1 d . . .
H8 H 0.8135 -0.0842 0.5004 0.033 Uiso 1 1 calc R . .
C9 C 0.7336(5) -0.1847(6) 0.5727(3) 0.0330(14) Uani 1 1 d . . .
H9 H 0.8039 -0.1875 0.6160 0.040 Uiso 1 1 calc R . .
C11 C 0.5190(5) -0.2340(6) 0.5101(3) 0.0378(15) Uani 1 1 d . . .
H11 H 0.4426 -0.2723 0.5118 0.045 Uiso 1 1 calc R . .
C10 C 0.6196(6) -0.2417(7) 0.5741(3) 0.0417(16) Uani 1 1 d . . .
H10 H 0.6120 -0.2855 0.6191 0.050 Uiso 1 1 calc R . .


_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 O4 2.333(3) . ?
Nd1 O6 2.365(3) 4_565 ?
Nd1 O5 2.432(3) 3_756 ?
Nd1 O2 2.455(2) 2_645 ?
Nd1 O1 2.528(3) . ?
Nd1 O1W 2.531(3) . ?
Nd1 N2 2.650(4) . ?
Nd1 N1 2.659(3) . ?
S1 O3 1.451(3) . ?
S1 O2 1.465(3) . ?
S1 O1 1.471(3) . ?
S1 C1 1.748(5) . ?
C5 C6 1.377(7) . ?
C5 C4 1.402(6) . ?
C5 H5 0.9300 . ?
C17 N2 1.319(7) . ?
C17 C16 1.384(7) . ?
C17 H17 0.9300 . ?
N2 C13 1.354(5) . ?
O4 C2 1.336(5) . ?
O2 Nd1 2.455(2) 2_655 ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O5 C7 1.261(5) . ?
O5 Nd1 2.432(3) 3_756 ?
O6 C7 1.266(5) . ?
O6 Nd1 2.365(3) 4_666 ?
N1 C8 1.316(6) . ?
N1 C12 1.369(5) . ?
C6 C1 1.394(6) . ?
C6 H6 0.9300 . ?
C1 C2 1.422(6) . ?
C3 C4 1.392(6) . ?
C3 C2 1.393(6) . ?
C3 H3 0.9300 . ?
C4 C7 1.489(7) . ?
C13 C14 1.397(6) . ?
C13 C12 1.460(7) . ?
C15 C14 1.361(8) . ?
C15 C16 1.379(7) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C12 C11 1.385(6) . ?
C14 H14 0.9300 . ?
C8 C9 1.394(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(7) . ?
C9 H9 0.9300 . ?
C11 C10 1.353(7) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?

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
O4 Nd1 O6 108.79(11) . 4_565 ?
O4 Nd1 O5 80.03(11) . 3_756 ?
O6 Nd1 O5 142.17(9) 4_565 3_756 ?
O4 Nd1 O2 88.64(10) . 2_645 ?
O6 Nd1 O2 72.92(10) 4_565 2_645 ?
O5 Nd1 O2 70.57(10) 3_756 2_645 ?
O4 Nd1 O1 71.43(10) . . ?
O6 Nd1 O1 71.92(10) 4_565 . ?
O5 Nd1 O1 142.57(11) 3_756 . ?
O2 Nd1 O1 130.62(9) 2_645 . ?
O4 Nd1 O1W 160.29(10) . . ?
O6 Nd1 O1W 81.13(11) 4_565 . ?
O5 Nd1 O1W 81.94(11) 3_756 . ?
O2 Nd1 O1W 77.87(10) 2_645 . ?
O1 Nd1 O1W 128.29(10) . . ?
O4 Nd1 N2 129.33(10) . . ?
O6 Nd1 N2 85.75(11) 4_565 . ?
O5 Nd1 N2 117.73(11) 3_756 . ?
O2 Nd1 N2 141.28(12) 2_645 . ?
O1 Nd1 N2 67.74(10) . . ?
O1W Nd1 N2 66.97(10) . . ?
O4 Nd1 N1 85.64(11) . . ?
O6 Nd1 N1 143.28(11) 4_565 . ?
O5 Nd1 N1 72.18(10) 3_756 . ?
O2 Nd1 N1 142.75(11) 2_645 . ?
O1 Nd1 N1 81.80(10) . . ?
O1W Nd1 N1 96.39(11) . . ?
N2 Nd1 N1 60.30(13) . . ?
O3 S1 O2 111.17(18) . . ?
O3 S1 O1 112.89(17) . . ?
O2 S1 O1 111.05(18) . . ?
O3 S1 C1 108.0(2) . . ?
O2 S1 C1 108.18(18) . . ?
O1 S1 C1 105.2(2) . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
N2 C17 C16 124.1(5) . . ?
N2 C17 H17 117.9 . . ?
C16 C17 H17 117.9 . . ?
C17 N2 C13 118.3(4) . . ?
C17 N2 Nd1 119.0(3) . . ?
C13 N2 Nd1 122.5(3) . . ?
C2 O4 Nd1 137.5(2) . . ?
S1 O2 Nd1 166.4(2) . 2_655 ?
Nd1 O1W H1W1 115(3) . . ?
Nd1 O1W H1W2 114(3) . . ?
H1W1 O1W H1W2 109.0(17) . . ?
S1 O1 Nd1 125.94(15) . . ?
C7 O5 Nd1 151.0(3) . 3_756 ?
C7 O6 Nd1 153.8(3) . 4_666 ?
C8 N1 C12 119.1(4) . . ?
C8 N1 Nd1 119.1(3) . . ?
C12 N1 Nd1 121.0(3) . . ?
C5 C6 C1 120.9(4) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C6 C1 C2 120.5(5) . . ?
C6 C1 S1 120.6(3) . . ?
C2 C1 S1 118.9(3) . . ?
C4 C3 C2 122.8(4) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 C7 120.7(4) . . ?
C5 C4 C7 120.3(4) . . ?
N2 C13 C14 120.7(5) . . ?
N2 C13 C12 115.9(4) . . ?
C14 C13 C12 123.2(4) . . ?
O4 C2 C3 122.1(4) . . ?
O4 C2 C1 121.0(5) . . ?
C3 C2 C1 116.9(4) . . ?
O5 C7 O6 123.9(5) . . ?
O5 C7 C4 118.8(4) . . ?
O6 C7 C4 117.2(4) . . ?
C14 C15 C16 120.2(5) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C17 117.1(6) . . ?
C15 C16 H16 121.5 . . ?
C17 C16 H16 121.5 . . ?
N1 C12 C11 119.1(5) . . ?
N1 C12 C13 116.7(4) . . ?
C11 C12 C13 124.0(4) . . ?
C15 C14 C13 119.3(5) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
N1 C8 C9 124.1(5) . . ?
N1 C8 H8 117.9 . . ?
C9 C8 H8 117.9 . . ?
C10 C9 C8 116.4(6) . . ?
C10 C9 H9 121.8 . . ?
C8 C9 H9 121.8 . . ?
C10 C11 C12 121.2(5) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?

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
C16 C17 N2 C13 -0.3(7) . . . . ?
C16 C17 N2 Nd1 175.2(4) . . . . ?
O4 Nd1 N2 C17 114.9(3) . . . . ?
O6 Nd1 N2 C17 4.0(3) 4_565 . . . ?
O5 Nd1 N2 C17 -144.9(3) 3_756 . . . ?
O2 Nd1 N2 C17 -51.7(4) 2_645 . . . ?
O1 Nd1 N2 C17 76.2(3) . . . . ?
O1W Nd1 N2 C17 -78.2(3) . . . . ?
N1 Nd1 N2 C17 169.4(4) . . . . ?
O4 Nd1 N2 C13 -69.9(3) . . . . ?
O6 Nd1 N2 C13 179.2(3) 4_565 . . . ?
O5 Nd1 N2 C13 30.4(4) 3_756 . . . ?
O2 Nd1 N2 C13 123.5(3) 2_645 . . . ?
O1 Nd1 N2 C13 -108.6(3) . . . . ?
O1W Nd1 N2 C13 97.1(3) . . . . ?
N1 Nd1 N2 C13 -15.4(3) . . . . ?
O6 Nd1 O4 C2 95.2(4) 4_565 . . . ?
O5 Nd1 O4 C2 -122.9(4) 3_756 . . . ?
O2 Nd1 O4 C2 166.6(4) 2_645 . . . ?
O1 Nd1 O4 C2 32.6(4) . . . . ?
O1W Nd1 O4 C2 -147.0(4) . . . . ?
N2 Nd1 O4 C2 -5.1(5) . . . . ?
N1 Nd1 O4 C2 -50.2(4) . . . . ?
O3 S1 O2 Nd1 107.6(8) . . . 2_655 ?
O1 S1 O2 Nd1 -125.8(8) . . . 2_655 ?
C1 S1 O2 Nd1 -10.8(9) . . . 2_655 ?
O3 S1 O1 Nd1 176.0(2) . . . . ?
O2 S1 O1 Nd1 50.3(3) . . . . ?
C1 S1 O1 Nd1 -66.5(2) . . . . ?
O4 Nd1 O1 S1 32.6(2) . . . . ?
O6 Nd1 O1 S1 -85.3(2) 4_565 . . . ?
O5 Nd1 O1 S1 74.9(3) 3_756 . . . ?
O2 Nd1 O1 S1 -38.7(3) 2_645 . . . ?
O1W Nd1 O1 S1 -147.6(2) . . . . ?
N2 Nd1 O1 S1 -178.1(3) . . . . ?
N1 Nd1 O1 S1 120.7(2) . . . . ?
O4 Nd1 N1 C8 -33.5(3) . . . . ?
O6 Nd1 N1 C8 -149.5(3) 4_565 . . . ?
O5 Nd1 N1 C8 47.4(3) 3_756 . . . ?
O2 Nd1 N1 C8 48.4(4) 2_645 . . . ?
O1 Nd1 N1 C8 -105.4(3) . . . . ?
O1W Nd1 N1 C8 126.8(3) . . . . ?
N2 Nd1 N1 C8 -174.4(4) . . . . ?
O4 Nd1 N1 C12 157.0(3) . . . . ?
O6 Nd1 N1 C12 41.0(4) 4_565 . . . ?
O5 Nd1 N1 C12 -122.1(3) 3_756 . . . ?
O2 Nd1 N1 C12 -121.0(3) 2_645 . . . ?
O1 Nd1 N1 C12 85.2(3) . . . . ?
O1W Nd1 N1 C12 -42.7(3) . . . . ?
N2 Nd1 N1 C12 16.2(3) . . . . ?
C4 C5 C6 C1 0.0(6) . . . . ?
C5 C6 C1 C2 0.5(6) . . . . ?
C5 C6 C1 S1 178.9(3) . . . . ?
O3 S1 C1 C6 -8.2(4) . . . . ?
O2 S1 C1 C6 112.2(3) . . . . ?
O1 S1 C1 C6 -129.1(3) . . . . ?
O3 S1 C1 C2 170.2(3) . . . . ?
O2 S1 C1 C2 -69.3(3) . . . . ?
O1 S1 C1 C2 49.4(3) . . . . ?
C2 C3 C4 C5 2.7(6) . . . . ?
C2 C3 C4 C7 -174.8(3) . . . . ?
C6 C5 C4 C3 -1.5(6) . . . . ?
C6 C5 C4 C7 175.9(3) . . . . ?
C17 N2 C13 C14 4.4(6) . . . . ?
Nd1 N2 C13 C14 -170.9(3) . . . . ?
C17 N2 C13 C12 -171.0(4) . . . . ?
Nd1 N2 C13 C12 13.7(5) . . . . ?
Nd1 O4 C2 C3 128.7(4) . . . . ?
Nd1 O4 C2 C1 -51.5(5) . . . . ?
C4 C3 C2 O4 177.6(3) . . . . ?
C4 C3 C2 C1 -2.1(6) . . . . ?
C6 C1 C2 O4 -179.2(3) . . . . ?
S1 C1 C2 O4 2.3(5) . . . . ?
C6 C1 C2 C3 0.6(5) . . . . ?
S1 C1 C2 C3 -177.9(3) . . . . ?
Nd1 O5 C7 O6 49.5(8) 3_756 . . . ?
Nd1 O5 C7 C4 -132.5(5) 3_756 . . . ?
Nd1 O6 C7 O5 9.3(8) 4_666 . . . ?
Nd1 O6 C7 C4 -168.8(4) 4_666 . . . ?
C3 C4 C7 O5 16.0(5) . . . . ?
C5 C4 C7 O5 -161.5(3) . . . . ?
C3 C4 C7 O6 -165.8(3) . . . . ?
C5 C4 C7 O6 16.7(5) . . . . ?
C14 C15 C16 C17 4.0(8) . . . . ?
N2 C17 C16 C15 -3.9(8) . . . . ?
C8 N1 C12 C11 -1.0(6) . . . . ?
Nd1 N1 C12 C11 168.5(3) . . . . ?
C8 N1 C12 C13 173.8(4) . . . . ?
Nd1 N1 C12 C13 -16.7(5) . . . . ?
N2 C13 C12 N1 2.1(6) . . . . ?
C14 C13 C12 N1 -173.2(4) . . . . ?
N2 C13 C12 C11 176.6(4) . . . . ?
C14 C13 C12 C11 1.3(7) . . . . ?
C16 C15 C14 C13 -0.1(8) . . . . ?
N2 C13 C14 C15 -4.2(7) . . . . ?
C12 C13 C14 C15 170.9(5) . . . . ?
C12 N1 C8 C9 0.4(7) . . . . ?
Nd1 N1 C8 C9 -169.2(4) . . . . ?
N1 C8 C9 C10 0.4(7) . . . . ?
N1 C12 C11 C10 0.6(8) . . . . ?
C13 C12 C11 C10 -173.8(5) . . . . ?
C12 C11 C10 C9 0.3(8) . . . . ?
C8 C9 C10 C11 -0.8(8) . . . . ?

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
O1W H1W1 O3 0.85(4) 2.086(16) 2.918(4) 166(5) 1_545
O1W H1W1 O2 0.85(4) 2.63(3) 3.161(4) 122(3) 1_545
O1W H1W2 O4 0.85(4) 1.928(11) 2.779(4) 178(5) 2_645

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_5-Ho
_database_code_depnum_ccdc_archive 'CCDC 1549864'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 Ho N2 O7 S'
_chemical_formula_sum            'C17 H13 Ho N2 O7 S'
_chemical_formula_weight         554.28

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.1687(4)
_cell_length_b                   8.4946(3)
_cell_length_c                   17.7855(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.588(4)
_cell_angle_gamma                90.00
_cell_volume                     1608.50(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1893
_cell_measurement_theta_min      3.53
_cell_measurement_theta_max      28.75

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    5.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4140
_exptl_absorpt_correction_T_max  0.4959
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5614
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3676
_reflns_number_gt                2915
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0083P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3676
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0579
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.000
_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 0.82293(2) 0.96368(3) 0.192767(15) 0.01235(7) Uani 1 1 d . . .
S1 S 0.85384(11) 1.36979(18) 0.16073(8) 0.0144(3) Uani 1 1 d . . .
O1 O 0.9137(3) 1.2150(5) 0.1689(2) 0.0207(10) Uani 1 1 d . . .
O1W O 0.9273(4) 0.7368(5) 0.2640(2) 0.0224(10) Uani 1 1 d D . .
H1W1 H 0.941(5) 0.655(4) 0.240(3) 0.034 Uiso 1 1 d D . .
H1W2 H 0.901(5) 0.710(6) 0.302(2) 0.034 Uiso 1 1 d D . .
O2 O 0.8059(3) 1.4037(5) 0.2270(2) 0.0204(10) Uani 1 1 d . . .
O3 O 0.9355(3) 1.4945(5) 0.1498(2) 0.0192(10) Uani 1 1 d . . .
O4 O 0.6642(3) 1.1137(5) 0.1210(2) 0.0154(8) Uani 1 1 d . . .
O5 O 0.3236(3) 1.2322(5) -0.1319(2) 0.0184(9) Uani 1 1 d . . .
O6 O 0.4098(3) 1.4163(5) -0.1902(2) 0.0187(9) Uani 1 1 d . . .
N1 N 1.0502(4) 0.9378(6) 0.1890(3) 0.0182(11) Uani 1 1 d . . .
N2 N 0.8563(4) 0.8887(6) 0.0624(3) 0.0202(11) Uani 1 1 d . . .
C1 C 0.7260(4) 1.3563(7) 0.0740(3) 0.0122(12) Uani 1 1 d . . .
C2 C 0.6455(4) 1.2228(7) 0.0656(3) 0.0150(12) Uani 1 1 d . . .
C3 C 0.5479(5) 1.2162(7) -0.0056(3) 0.0158(12) Uani 1 1 d . . .
H3A H 0.4954 1.1288 -0.0152 0.019 Uiso 1 1 calc R . .
C4 C 0.5257(4) 1.3317(7) -0.0619(3) 0.0139(12) Uani 1 1 d . . .
C5 C 0.6067(4) 1.4608(7) -0.0508(3) 0.0154(12) Uani 1 1 d . . .
H5A H 0.5934 1.5393 -0.0888 0.018 Uiso 1 1 calc R . .
C6 C 0.7064(5) 1.4704(8) 0.0171(3) 0.0189(13) Uani 1 1 d . . .
H6A H 0.7612 1.5555 0.0245 0.023 Uiso 1 1 calc R . .
C7 C 0.4103(5) 1.3254(7) -0.1339(3) 0.0147(12) Uani 1 1 d . . .
C8 C 1.1454(5) 0.9864(8) 0.2499(3) 0.0250(15) Uani 1 1 d . . .
H8A H 1.1271 1.0382 0.2911 0.030 Uiso 1 1 calc R . .
C9 C 1.2695(5) 0.9637(10) 0.2546(4) 0.0350(17) Uani 1 1 d . . .
H9A H 1.3335 1.0048 0.2965 0.042 Uiso 1 1 calc R . .
C10 C 1.2962(5) 0.8793(9) 0.1963(4) 0.0320(17) Uani 1 1 d . . .
H10A H 1.3792 0.8573 0.1995 0.038 Uiso 1 1 calc R . .
C11 C 1.2002(5) 0.8268(9) 0.1328(4) 0.0337(17) Uani 1 1 d . . .
H11A H 1.2171 0.7685 0.0929 0.040 Uiso 1 1 calc R . .
C12 C 1.0763(5) 0.8633(7) 0.1295(3) 0.0207(14) Uani 1 1 d . . .
C13 C 0.9680(5) 0.8341(8) 0.0582(4) 0.0218(14) Uani 1 1 d . . .
C14 C 0.9794(5) 0.7650(9) -0.0091(4) 0.0316(17) Uani 1 1 d . . .
H14A H 1.0564 0.7243 -0.0098 0.038 Uiso 1 1 calc R . .
C15 C 0.8777(6) 0.7561(9) -0.0749(4) 0.0343(18) Uani 1 1 d . . .
H15A H 0.8847 0.7101 -0.1208 0.041 Uiso 1 1 calc R . .
C16 C 0.7646(5) 0.8161(9) -0.0723(4) 0.0285(16) Uani 1 1 d . . .
H16A H 0.6940 0.8131 -0.1164 0.034 Uiso 1 1 calc R . .
C17 C 0.7589(5) 0.8801(8) -0.0033(4) 0.0237(14) Uani 1 1 d . . .
H17A H 0.6823 0.9204 -0.0017 0.028 Uiso 1 1 calc R . .


_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 O4 2.243(4) . ?
Ho1 O6 2.256(4) 4_686 ?
Ho1 O5 2.355(4) 3_675 ?
Ho1 O2 2.367(3) 2_645 ?
Ho1 O1W 2.405(4) . ?
Ho1 O1 2.455(4) . ?
Ho1 N2 2.539(5) . ?
Ho1 N1 2.568(4) . ?
S1 O3 1.449(4) . ?
S1 O1 1.462(4) . ?
S1 O2 1.464(4) . ?
S1 C1 1.761(5) . ?
O1W H1W1 0.85(6) . ?
O1W H1W2 0.85(6) . ?
O2 Ho1 2.367(3) 2_655 ?
O4 C2 1.322(6) . ?
O5 C7 1.260(6) . ?
O5 Ho1 2.355(4) 3_675 ?
O6 C7 1.263(6) . ?
O6 Ho1 2.256(4) 4_585 ?
N1 C8 1.333(7) . ?
N1 C12 1.339(7) . ?
N2 C17 1.336(7) . ?
N2 C13 1.353(6) . ?
C1 C6 1.370(8) . ?
C1 C2 1.427(7) . ?
C2 C3 1.401(7) . ?
C3 C4 1.370(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.397(7) . ?
C4 C7 1.519(7) . ?
C5 C6 1.375(7) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C8 C9 1.376(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.367(9) . ?
C9 H9A 0.9300 . ?
C10 C11 1.375(9) . ?
C10 H10A 0.9300 . ?
C11 C12 1.403(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.485(8) . ?
C13 C14 1.373(8) . ?
C14 C15 1.365(8) . ?
C14 H14A 0.9300 . ?
C15 C16 1.376(8) . ?
C15 H15A 0.9300 . ?
C16 C17 1.361(8) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?

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
O4 Ho1 O6 108.32(14) . 4_686 ?
O4 Ho1 O5 79.61(14) . 3_675 ?
O6 Ho1 O5 142.03(13) 4_686 3_675 ?
O4 Ho1 O2 86.88(13) . 2_645 ?
O6 Ho1 O2 73.26(13) 4_686 2_645 ?
O5 Ho1 O2 70.13(13) 3_675 2_645 ?
O4 Ho1 O1W 158.30(13) . . ?
O6 Ho1 O1W 82.61(14) 4_686 . ?
O5 Ho1 O1W 80.50(14) 3_675 . ?
O2 Ho1 O1W 78.26(13) 2_645 . ?
O4 Ho1 O1 72.79(12) . . ?
O6 Ho1 O1 71.44(13) 4_686 . ?
O5 Ho1 O1 143.21(13) 3_675 . ?
O2 Ho1 O1 130.49(14) 2_645 . ?
O1W Ho1 O1 128.91(13) . . ?
O4 Ho1 N2 86.07(14) . . ?
O6 Ho1 N2 144.58(13) 4_686 . ?
O5 Ho1 N2 71.13(14) 3_675 . ?
O2 Ho1 N2 141.27(14) 2_645 . ?
O1W Ho1 N2 95.64(15) . . ?
O1 Ho1 N2 82.98(15) . . ?
O4 Ho1 N1 130.64(14) . . ?
O6 Ho1 N1 84.81(14) 4_686 . ?
O5 Ho1 N1 118.85(14) 3_675 . ?
O2 Ho1 N1 141.49(13) 2_645 . ?
O1W Ho1 N1 67.63(14) . . ?
O1 Ho1 N1 66.86(14) . . ?
N2 Ho1 N1 62.34(14) . . ?
O3 S1 O1 112.5(2) . . ?
O3 S1 O2 111.3(2) . . ?
O1 S1 O2 111.4(2) . . ?
O3 S1 C1 107.9(2) . . ?
O1 S1 C1 104.7(3) . . ?
O2 S1 C1 108.8(2) . . ?
S1 O1 Ho1 126.78(19) . . ?
Ho1 O1W H1W1 122(4) . . ?
Ho1 O1W H1W2 114(4) . . ?
H1W1 O1W H1W2 109.7(18) . . ?
S1 O2 Ho1 164.7(2) . 2_655 ?
C2 O4 Ho1 137.9(3) . . ?
C7 O5 Ho1 149.8(3) . 3_675 ?
C7 O6 Ho1 154.8(3) . 4_585 ?
C8 N1 C12 118.5(5) . . ?
C8 N1 Ho1 120.3(4) . . ?
C12 N1 Ho1 120.9(3) . . ?
C17 N2 C13 117.0(5) . . ?
C17 N2 Ho1 120.4(4) . . ?
C13 N2 Ho1 121.9(4) . . ?
C6 C1 C2 122.0(5) . . ?
C6 C1 S1 120.5(4) . . ?
C2 C1 S1 117.5(4) . . ?
O4 C2 C3 123.4(5) . . ?
O4 C2 C1 121.8(5) . . ?
C3 C2 C1 114.8(5) . . ?
C4 C3 C2 123.5(5) . . ?
C4 C3 H3A 118.2 . . ?
C2 C3 H3A 118.2 . . ?
C3 C4 C5 119.5(5) . . ?
C3 C4 C7 120.7(5) . . ?
C5 C4 C7 119.7(5) . . ?
C6 C5 C4 119.3(6) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
C1 C6 C5 120.8(5) . . ?
C1 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
O5 C7 O6 126.0(5) . . ?
O5 C7 C4 117.5(5) . . ?
O6 C7 C4 116.5(5) . . ?
N1 C8 C9 123.2(6) . . ?
N1 C8 H8A 118.4 . . ?
C9 C8 H8A 118.4 . . ?
C10 C9 C8 118.3(6) . . ?
C10 C9 H9A 120.9 . . ?
C8 C9 H9A 120.9 . . ?
C9 C10 C11 119.9(5) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C10 C11 C12 118.5(6) . . ?
C10 C11 H11A 120.7 . . ?
C12 C11 H11A 120.7 . . ?
N1 C12 C11 121.3(5) . . ?
N1 C12 C13 116.0(5) . . ?
C11 C12 C13 122.5(6) . . ?
N2 C13 C14 121.6(5) . . ?
N2 C13 C12 115.0(5) . . ?
C14 C13 C12 123.3(5) . . ?
C15 C14 C13 119.9(5) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C14 C15 C16 119.0(6) . . ?
C14 C15 H15A 120.5 . . ?
C16 C15 H15A 120.5 . . ?
C17 C16 C15 118.1(6) . . ?
C17 C16 H16A 120.9 . . ?
C15 C16 H16A 120.9 . . ?
N2 C17 C16 124.3(5) . . ?
N2 C17 H17A 117.9 . . ?
C16 C17 H17A 117.9 . . ?

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
O3 S1 O1 Ho1 177.9(2) . . . . ?
O2 S1 O1 Ho1 52.2(3) . . . . ?
C1 S1 O1 Ho1 -65.2(3) . . . . ?
O4 Ho1 O1 S1 31.9(3) . . . . ?
O6 Ho1 O1 S1 -84.9(3) 4_686 . . . ?
O5 Ho1 O1 S1 75.1(4) 3_675 . . . ?
O2 Ho1 O1 S1 -38.2(3) 2_645 . . . ?
O1W Ho1 O1 S1 -148.4(2) . . . . ?
N2 Ho1 O1 S1 120.0(3) . . . . ?
N1 Ho1 O1 S1 -177.1(3) . . . . ?
O3 S1 O2 Ho1 112.9(10) . . . 2_655 ?
O1 S1 O2 Ho1 -120.6(10) . . . 2_655 ?
C1 S1 O2 Ho1 -5.7(12) . . . 2_655 ?
O6 Ho1 O4 C2 95.7(5) 4_686 . . . ?
O5 Ho1 O4 C2 -122.7(5) 3_675 . . . ?
O2 Ho1 O4 C2 167.0(5) 2_645 . . . ?
O1W Ho1 O4 C2 -146.5(5) . . . . ?
O1 Ho1 O4 C2 32.7(5) . . . . ?
N2 Ho1 O4 C2 -51.2(5) . . . . ?
N1 Ho1 O4 C2 -3.4(6) . . . . ?
O4 Ho1 N1 C8 113.1(4) . . . . ?
O6 Ho1 N1 C8 3.4(5) 4_686 . . . ?
O5 Ho1 N1 C8 -145.3(4) 3_675 . . . ?
O2 Ho1 N1 C8 -51.3(6) 2_645 . . . ?
O1W Ho1 N1 C8 -80.8(5) . . . . ?
O1 Ho1 N1 C8 75.4(5) . . . . ?
N2 Ho1 N1 C8 169.6(5) . . . . ?
O4 Ho1 N1 C12 -72.7(5) . . . . ?
O6 Ho1 N1 C12 177.5(5) 4_686 . . . ?
O5 Ho1 N1 C12 28.9(5) 3_675 . . . ?
O2 Ho1 N1 C12 122.9(4) 2_645 . . . ?
O1W Ho1 N1 C12 93.4(5) . . . . ?
O1 Ho1 N1 C12 -110.5(5) . . . . ?
N2 Ho1 N1 C12 -16.2(4) . . . . ?
O4 Ho1 N2 C17 -32.3(5) . . . . ?
O6 Ho1 N2 C17 -148.9(4) 4_686 . . . ?
O5 Ho1 N2 C17 48.0(5) 3_675 . . . ?
O2 Ho1 N2 C17 47.7(6) 2_645 . . . ?
O1W Ho1 N2 C17 126.0(5) . . . . ?
O1 Ho1 N2 C17 -105.4(5) . . . . ?
N1 Ho1 N2 C17 -172.9(5) . . . . ?
O4 Ho1 N2 C13 157.5(5) . . . . ?
O6 Ho1 N2 C13 40.9(6) 4_686 . . . ?
O5 Ho1 N2 C13 -122.1(5) 3_675 . . . ?
O2 Ho1 N2 C13 -122.5(4) 2_645 . . . ?
O1W Ho1 N2 C13 -44.2(5) . . . . ?
O1 Ho1 N2 C13 84.4(5) . . . . ?
N1 Ho1 N2 C13 16.9(4) . . . . ?
O3 S1 C1 C6 -11.0(5) . . . . ?
O1 S1 C1 C6 -131.0(4) . . . . ?
O2 S1 C1 C6 109.8(5) . . . . ?
O3 S1 C1 C2 168.7(4) . . . . ?
O1 S1 C1 C2 48.7(5) . . . . ?
O2 S1 C1 C2 -70.5(5) . . . . ?
Ho1 O4 C2 C3 128.7(5) . . . . ?
Ho1 O4 C2 C1 -50.3(8) . . . . ?
C6 C1 C2 O4 -179.4(5) . . . . ?
S1 C1 C2 O4 0.9(7) . . . . ?
C6 C1 C2 C3 1.5(8) . . . . ?
S1 C1 C2 C3 -178.1(4) . . . . ?
O4 C2 C3 C4 177.7(5) . . . . ?
C1 C2 C3 C4 -3.3(8) . . . . ?
C2 C3 C4 C5 3.1(8) . . . . ?
C2 C3 C4 C7 -173.6(5) . . . . ?
C3 C4 C5 C6 -0.9(8) . . . . ?
C7 C4 C5 C6 175.8(5) . . . . ?
C2 C1 C6 C5 0.4(8) . . . . ?
S1 C1 C6 C5 -179.9(4) . . . . ?
C4 C5 C6 C1 -0.8(8) . . . . ?
Ho1 O5 C7 O6 47.3(11) 3_675 . . . ?
Ho1 O5 C7 C4 -133.7(6) 3_675 . . . ?
Ho1 O6 C7 O5 7.3(13) 4_585 . . . ?
Ho1 O6 C7 C4 -171.7(6) 4_585 . . . ?
C3 C4 C7 O5 15.1(8) . . . . ?
C5 C4 C7 O5 -161.6(5) . . . . ?
C3 C4 C7 O6 -165.8(5) . . . . ?
C5 C4 C7 O6 17.5(7) . . . . ?
C12 N1 C8 C9 -0.1(9) . . . . ?
Ho1 N1 C8 C9 174.2(5) . . . . ?
N1 C8 C9 C10 -3.9(11) . . . . ?
C8 C9 C10 C11 3.5(11) . . . . ?
C9 C10 C11 C12 0.6(11) . . . . ?
C8 N1 C12 C11 4.4(9) . . . . ?
Ho1 N1 C12 C11 -169.9(5) . . . . ?
C8 N1 C12 C13 -170.9(5) . . . . ?
Ho1 N1 C12 C13 14.9(7) . . . . ?
C10 C11 C12 N1 -4.6(10) . . . . ?
C10 C11 C12 C13 170.3(6) . . . . ?
C17 N2 C13 C14 -3.5(9) . . . . ?
Ho1 N2 C13 C14 167.0(5) . . . . ?
C17 N2 C13 C12 173.0(5) . . . . ?
Ho1 N2 C13 C12 -16.4(7) . . . . ?
N1 C12 C13 N2 0.8(8) . . . . ?
C11 C12 C13 N2 -174.4(6) . . . . ?
N1 C12 C13 C14 177.3(6) . . . . ?
C11 C12 C13 C14 2.1(10) . . . . ?
N2 C13 C14 C15 2.8(10) . . . . ?
C12 C13 C14 C15 -173.5(6) . . . . ?
C13 C14 C15 C16 -0.4(11) . . . . ?
C14 C15 C16 C17 -0.9(10) . . . . ?
C13 N2 C17 C16 2.1(9) . . . . ?
Ho1 N2 C17 C16 -168.5(5) . . . . ?
C15 C16 C17 N2 0.1(10) . . . . ?

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
O1W H1W1 O3 0.85(6) 2.10(2) 2.913(6) 161(5) 1_545
O1W H1W1 O2 0.85(6) 2.59(4) 3.121(6) 122(4) 1_545
O1W H1W2 O4 0.85(6) 1.919(16) 2.755(5) 170(5) 2_645

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.189
####################################################################### 
# 
# 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_5-Dy
_database_code_depnum_ccdc_archive 'CCDC 1549863'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 Dy N2 O7 S'
_chemical_formula_sum            'C17 H13 Dy N2 O7 S'
_chemical_formula_weight         551.85

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.1794(2)
_cell_length_b                   8.50490(16)
_cell_length_c                   17.8416(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.657(2)
_cell_angle_gamma                90.00
_cell_volume                     1616.45(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2748
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1068
_exptl_absorpt_coefficient_mu    4.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4181
_exptl_absorpt_correction_T_max  0.5138
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5613
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3691
_reflns_number_gt                3064
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0139P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3691
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0532
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Dy1 Dy 0.176984(18) 1.03670(2) 0.307253(11) 0.01140(6) Uani 1 1 d . . .
S1 S 0.14628(9) 0.63030(13) 0.33963(6) 0.0130(2) Uani 1 1 d . . .
O1W O 0.0720(3) 1.2644(3) 0.23581(19) 0.0210(7) Uani 1 1 d D . .
H1W1 H 0.098(4) 1.299(4) 0.1987(19) 0.032 Uiso 1 1 d D . .
H1W2 H 0.054(4) 1.342(3) 0.261(2) 0.032 Uiso 1 1 d D . .
O1 O 0.0866(2) 0.7856(3) 0.33124(17) 0.0159(7) Uani 1 1 d . . .
O2 O 0.0642(3) 0.5052(3) 0.35028(17) 0.0186(7) Uani 1 1 d . . .
O3 O 0.1940(3) 0.5958(4) 0.27383(17) 0.0194(7) Uani 1 1 d . . .
O4 O 0.3365(2) 0.8857(3) 0.37935(17) 0.0165(6) Uani 1 1 d . . .
O5 O 0.6756(3) 0.7672(3) 0.63216(17) 0.0172(7) Uani 1 1 d . . .
O6 O 0.5891(3) 0.5846(3) 0.68969(16) 0.0188(7) Uani 1 1 d . . .
N1 N 0.1431(3) 1.1105(4) 0.4383(2) 0.0195(8) Uani 1 1 d . . .
N2 N -0.0508(3) 1.0652(4) 0.3112(2) 0.0182(8) Uani 1 1 d . . .
C1 C 0.2735(4) 0.6435(5) 0.4253(2) 0.0119(9) Uani 1 1 d . . .
C2 C 0.3537(4) 0.7765(5) 0.4351(2) 0.0139(9) Uani 1 1 d . . .
C3 C 0.4525(4) 0.7831(5) 0.5058(3) 0.0154(9) Uani 1 1 d . . .
H3 H 0.5056 0.8698 0.5151 0.018 Uiso 1 1 calc R . .
C4 C 0.4740(4) 0.6672(5) 0.5619(2) 0.0130(9) Uani 1 1 d . . .
C5 C 0.3923(4) 0.5389(5) 0.5510(2) 0.0167(9) Uani 1 1 d . . .
H5 H 0.4049 0.4610 0.5892 0.020 Uiso 1 1 calc R . .
C6 C 0.2928(4) 0.5296(5) 0.4828(2) 0.0163(9) Uani 1 1 d . . .
H6 H 0.2377 0.4451 0.4755 0.020 Uiso 1 1 calc R . .
C7 C 0.5879(4) 0.6744(5) 0.6333(2) 0.0130(9) Uani 1 1 d . . .
C8 C 0.2395(4) 1.1204(6) 0.5024(3) 0.0248(11) Uani 1 1 d . . .
H8 H 0.3161 1.0809 0.5004 0.030 Uiso 1 1 calc R . .
C9 C 0.2348(5) 1.1853(6) 0.5721(3) 0.0286(12) Uani 1 1 d . . .
H9 H 0.3059 1.1891 0.6158 0.034 Uiso 1 1 calc R . .
C10 C 0.1223(5) 1.2441(7) 0.5752(3) 0.0391(14) Uani 1 1 d . . .
H10 H 0.1154 1.2894 0.6212 0.047 Uiso 1 1 calc R . .
C11 C 0.0209(5) 1.2350(6) 0.5097(3) 0.0356(14) Uani 1 1 d . . .
H11 H -0.0559 1.2746 0.5112 0.043 Uiso 1 1 calc R . .
C12 C 0.0299(4) 1.1677(5) 0.4408(3) 0.0198(10) Uani 1 1 d . . .
C13 C -0.0766(4) 1.1386(5) 0.3710(3) 0.0203(10) Uani 1 1 d . . .
C14 C -0.1998(4) 1.1732(6) 0.3679(3) 0.0311(13) Uani 1 1 d . . .
H14 H -0.2163 1.2300 0.4082 0.037 Uiso 1 1 calc R . .
C15 C -0.2968(5) 1.1225(7) 0.3047(3) 0.0366(14) Uani 1 1 d . . .
H15 H -0.3796 1.1450 0.3017 0.044 Uiso 1 1 calc R . .
C16 C -0.2702(4) 1.0383(6) 0.2461(3) 0.0299(11) Uani 1 1 d . . .
H16 H -0.3343 0.9979 0.2042 0.036 Uiso 1 1 calc R . .
C17 C -0.1456(4) 1.0149(6) 0.2509(3) 0.0231(11) Uani 1 1 d . . .
H17 H -0.1273 0.9617 0.2102 0.028 Uiso 1 1 calc R . .


_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
Dy1 O4 2.257(3) . ?
Dy1 O6 2.276(3) 4_575 ?
Dy1 O5 2.364(3) 3_676 ?
Dy1 O3 2.386(3) 2 ?
Dy1 O1W 2.417(3) . ?
Dy1 O1 2.455(3) . ?
Dy1 N1 2.558(3) . ?
Dy1 N2 2.580(3) . ?
S1 O2 1.454(3) . ?
S1 O3 1.459(3) . ?
S1 O1 1.467(3) . ?
S1 C1 1.747(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O3 Dy1 2.386(3) 2_545 ?
O4 C2 1.332(5) . ?
O5 C7 1.263(5) . ?
O5 Dy1 2.364(3) 3_676 ?
O6 C7 1.260(5) . ?
O6 Dy1 2.276(3) 4_676 ?
N1 C8 1.314(6) . ?
N1 C12 1.369(5) . ?
N2 C17 1.331(6) . ?
N2 C13 1.342(5) . ?
C1 C6 1.380(5) . ?
C1 C2 1.420(6) . ?
C2 C3 1.403(6) . ?
C3 C4 1.372(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(6) . ?
C4 C7 1.506(6) . ?
C5 C6 1.380(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.377(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.370(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.362(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.459(6) . ?
C13 C14 1.393(6) . ?
C14 C15 1.376(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Dy1 O6 108.25(11) . 4_575 ?
O4 Dy1 O5 79.63(10) . 3_676 ?
O6 Dy1 O5 141.96(10) 4_575 3_676 ?
O4 Dy1 O3 86.95(10) . 2 ?
O6 Dy1 O3 73.02(10) 4_575 2 ?
O5 Dy1 O3 70.28(10) 3_676 2 ?
O4 Dy1 O1W 158.38(10) . . ?
O6 Dy1 O1W 82.66(11) 4_575 . ?
O5 Dy1 O1W 80.53(11) 3_676 . ?
O3 Dy1 O1W 78.32(10) 2 . ?
O4 Dy1 O1 72.64(9) . . ?
O6 Dy1 O1 71.39(10) 4_575 . ?
O5 Dy1 O1 143.22(10) 3_676 . ?
O3 Dy1 O1 130.20(9) 2 . ?
O1W Dy1 O1 128.98(10) . . ?
O4 Dy1 N1 85.94(11) . . ?
O6 Dy1 N1 144.24(11) 4_575 . ?
O5 Dy1 N1 71.64(10) 3_676 . ?
O3 Dy1 N1 141.92(11) 2 . ?
O1W Dy1 N1 95.89(11) . . ?
O1 Dy1 N1 82.59(10) . . ?
O4 Dy1 N2 130.84(10) . . ?
O6 Dy1 N2 85.06(11) 4_575 . ?
O5 Dy1 N2 118.58(10) 3_676 . ?
O3 Dy1 N2 141.25(11) 2 . ?
O1W Dy1 N2 67.28(10) . . ?
O1 Dy1 N2 67.37(10) . . ?
N1 Dy1 N2 62.03(12) . . ?
O2 S1 O3 110.92(18) . . ?
O2 S1 O1 112.75(16) . . ?
O3 S1 O1 111.41(17) . . ?
O2 S1 C1 108.13(18) . . ?
O3 S1 C1 108.50(17) . . ?
O1 S1 C1 104.82(19) . . ?
Dy1 O1W H1W1 117(3) . . ?
Dy1 O1W H1W2 120(3) . . ?
H1W1 O1W H1W2 109.3(17) . . ?
S1 O1 Dy1 127.06(15) . . ?
S1 O3 Dy1 165.05(19) . 2_545 ?
C2 O4 Dy1 137.1(2) . . ?
C7 O5 Dy1 150.5(3) . 3_676 ?
C7 O6 Dy1 155.2(3) . 4_676 ?
C8 N1 C12 118.2(4) . . ?
C8 N1 Dy1 120.0(3) . . ?
C12 N1 Dy1 120.7(3) . . ?
C17 N2 C13 118.8(4) . . ?
C17 N2 Dy1 119.9(3) . . ?
C13 N2 Dy1 121.2(3) . . ?
C6 C1 C2 121.1(4) . . ?
C6 C1 S1 120.5(3) . . ?
C2 C1 S1 118.4(3) . . ?
O4 C2 C3 122.6(4) . . ?
O4 C2 C1 121.4(4) . . ?
C3 C2 C1 116.0(4) . . ?
C4 C3 C2 122.8(4) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 C7 120.3(4) . . ?
C5 C4 C7 119.9(4) . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 121.2(4) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
O6 C7 O5 124.8(4) . . ?
O6 C7 C4 116.9(4) . . ?
O5 C7 C4 118.3(4) . . ?
N1 C8 C9 124.4(4) . . ?
N1 C8 H8 117.8 . . ?
C9 C8 H8 117.8 . . ?
C10 C9 C8 118.0(5) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
C11 C10 C9 118.7(5) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 121.3(5) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
N1 C12 C11 119.4(4) . . ?
N1 C12 C13 115.8(4) . . ?
C11 C12 C13 124.5(4) . . ?
N2 C13 C14 121.0(5) . . ?
N2 C13 C12 116.2(4) . . ?
C14 C13 C12 122.6(4) . . ?
C15 C14 C13 119.4(4) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 119.3(4) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 118.3(5) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N2 C17 C16 123.0(4) . . ?
N2 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?

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 Dy1 -177.65(18) . . . . ?
O3 S1 O1 Dy1 -52.2(3) . . . . ?
C1 S1 O1 Dy1 65.0(2) . . . . ?
O4 Dy1 O1 S1 -31.8(2) . . . . ?
O6 Dy1 O1 S1 85.0(2) 4_575 . . . ?
O5 Dy1 O1 S1 -74.7(3) 3_676 . . . ?
O3 Dy1 O1 S1 38.5(3) 2 . . . ?
O1W Dy1 O1 S1 148.52(18) . . . . ?
N1 Dy1 O1 S1 -119.9(2) . . . . ?
N2 Dy1 O1 S1 177.4(2) . . . . ?
O2 S1 O3 Dy1 -114.9(7) . . . 2_545 ?
O1 S1 O3 Dy1 118.6(7) . . . 2_545 ?
C1 S1 O3 Dy1 3.7(8) . . . 2_545 ?
O6 Dy1 O4 C2 -95.9(4) 4_575 . . . ?
O5 Dy1 O4 C2 122.6(4) 3_676 . . . ?
O3 Dy1 O4 C2 -166.9(4) 2 . . . ?
O1W Dy1 O4 C2 146.2(4) . . . . ?
O1 Dy1 O4 C2 -33.0(4) . . . . ?
N1 Dy1 O4 C2 50.5(4) . . . . ?
N2 Dy1 O4 C2 3.6(4) . . . . ?
O4 Dy1 N1 C8 33.3(4) . . . . ?
O6 Dy1 N1 C8 149.3(3) 4_575 . . . ?
O5 Dy1 N1 C8 -47.1(4) 3_676 . . . ?
O3 Dy1 N1 C8 -46.5(4) 2 . . . ?
O1W Dy1 N1 C8 -125.1(4) . . . . ?
O1 Dy1 N1 C8 106.3(4) . . . . ?
N2 Dy1 N1 C8 174.6(4) . . . . ?
O4 Dy1 N1 C12 -158.7(3) . . . . ?
O6 Dy1 N1 C12 -42.7(4) 4_575 . . . ?
O5 Dy1 N1 C12 120.9(3) 3_676 . . . ?
O3 Dy1 N1 C12 121.5(3) 2 . . . ?
O1W Dy1 N1 C12 42.9(3) . . . . ?
O1 Dy1 N1 C12 -85.7(3) . . . . ?
N2 Dy1 N1 C12 -17.5(3) . . . . ?
O4 Dy1 N2 C17 -112.4(3) . . . . ?
O6 Dy1 N2 C17 -2.5(3) 4_575 . . . ?
O5 Dy1 N2 C17 146.1(3) 3_676 . . . ?
O3 Dy1 N2 C17 52.4(4) 2 . . . ?
O1W Dy1 N2 C17 81.6(3) . . . . ?
O1 Dy1 N2 C17 -74.4(3) . . . . ?
N1 Dy1 N2 C17 -168.0(4) . . . . ?
O4 Dy1 N2 C13 71.6(3) . . . . ?
O6 Dy1 N2 C13 -178.4(3) 4_575 . . . ?
O5 Dy1 N2 C13 -29.9(3) 3_676 . . . ?
O3 Dy1 N2 C13 -123.6(3) 2 . . . ?
O1W Dy1 N2 C13 -94.3(3) . . . . ?
O1 Dy1 N2 C13 109.7(3) . . . . ?
N1 Dy1 N2 C13 16.0(3) . . . . ?
O2 S1 C1 C6 10.1(4) . . . . ?
O3 S1 C1 C6 -110.3(3) . . . . ?
O1 S1 C1 C6 130.6(3) . . . . ?
O2 S1 C1 C2 -167.9(3) . . . . ?
O3 S1 C1 C2 71.7(3) . . . . ?
O1 S1 C1 C2 -47.4(3) . . . . ?
Dy1 O4 C2 C3 -129.6(4) . . . . ?
Dy1 O4 C2 C1 51.9(6) . . . . ?
C6 C1 C2 O4 179.1(3) . . . . ?
S1 C1 C2 O4 -2.9(5) . . . . ?
C6 C1 C2 C3 0.4(6) . . . . ?
S1 C1 C2 C3 178.4(3) . . . . ?
O4 C2 C3 C4 -176.9(4) . . . . ?
C1 C2 C3 C4 1.7(6) . . . . ?
C2 C3 C4 C5 -2.8(6) . . . . ?
C2 C3 C4 C7 174.7(3) . . . . ?
C3 C4 C5 C6 1.5(6) . . . . ?
C7 C4 C5 C6 -176.0(4) . . . . ?
C2 C1 C6 C5 -1.6(6) . . . . ?
S1 C1 C6 C5 -179.6(3) . . . . ?
C4 C5 C6 C1 0.6(6) . . . . ?
Dy1 O6 C7 O5 -8.4(9) 4_676 . . . ?
Dy1 O6 C7 C4 170.5(4) 4_676 . . . ?
Dy1 O5 C7 O6 -47.8(8) 3_676 . . . ?
Dy1 O5 C7 C4 133.3(4) 3_676 . . . ?
C3 C4 C7 O6 165.6(4) . . . . ?
C5 C4 C7 O6 -16.9(5) . . . . ?
C3 C4 C7 O5 -15.4(6) . . . . ?
C5 C4 C7 O5 162.1(4) . . . . ?
C12 N1 C8 C9 -0.3(7) . . . . ?
Dy1 N1 C8 C9 168.0(4) . . . . ?
N1 C8 C9 C10 -0.2(7) . . . . ?
C8 C9 C10 C11 0.3(8) . . . . ?
C9 C10 C11 C12 0.0(8) . . . . ?
C8 N1 C12 C11 0.6(6) . . . . ?
Dy1 N1 C12 C11 -167.6(3) . . . . ?
C8 N1 C12 C13 -173.6(4) . . . . ?
Dy1 N1 C12 C13 18.2(5) . . . . ?
C10 C11 C12 N1 -0.5(8) . . . . ?
C10 C11 C12 C13 173.2(5) . . . . ?
C17 N2 C13 C14 -5.0(7) . . . . ?
Dy1 N2 C13 C14 171.0(3) . . . . ?
C17 N2 C13 C12 170.3(4) . . . . ?
Dy1 N2 C13 C12 -13.7(5) . . . . ?
N1 C12 C13 N2 -2.8(6) . . . . ?
C11 C12 C13 N2 -176.7(4) . . . . ?
N1 C12 C13 C14 172.4(4) . . . . ?
C11 C12 C13 C14 -1.5(7) . . . . ?
N2 C13 C14 C15 4.1(7) . . . . ?
C12 C13 C14 C15 -170.9(5) . . . . ?
C13 C14 C15 C16 0.3(8) . . . . ?
C14 C15 C16 C17 -3.5(8) . . . . ?
C13 N2 C17 C16 1.6(7) . . . . ?
Dy1 N2 C17 C16 -174.4(3) . . . . ?
C15 C16 C17 N2 2.7(7) . . . . ?

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
O1W H1W1 O4 0.85(4) 1.910(11) 2.758(4) 176(4) 2
O1W H1W2 O2 0.85(4) 2.095(18) 2.913(4) 161(5) 1_565
O1W H1W2 O3 0.85(4) 2.63(4) 3.115(4) 117(3) 1_565

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.148
####################################################################### 
# 
# 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_2-Eu
_database_code_depnum_ccdc_archive 'CCDC 1549842'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 Eu2 O28 S2, 2(C7 H5 O6 S), 8(H2 O)'
_chemical_formula_sum            'C30 H60 Eu2 O48 S4'
_chemical_formula_weight         1620.94

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9008(4)
_cell_length_b                   12.3804(6)
_cell_length_c                   15.0796(7)
_cell_angle_alpha                107.260(4)
_cell_angle_beta                 96.890(4)
_cell_angle_gamma                96.645(4)
_cell_volume                     1380.48(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4418
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             814
_exptl_absorpt_coefficient_mu    2.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6065
_exptl_absorpt_correction_T_max  0.7187
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8219
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6310
_reflns_number_gt                5538
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0246P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6310
_refine_ls_number_parameters     451
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.005
_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 0.79601(2) 0.705690(15) 0.518907(12) 0.01695(6) Uani 1 1 d . . .
S1 S 0.74140(12) 0.64583(8) 0.74797(6) 0.0208(2) Uani 1 1 d . . .
S2 S 0.56406(14) 1.13671(8) 0.76833(7) 0.0291(2) Uani 1 1 d . . .
O1 O 0.7900(3) 0.6981(2) 0.67808(17) 0.0257(6) Uani 1 1 d . . .
O1W O 0.6343(4) 0.8656(2) 0.5928(2) 0.0311(7) Uani 1 1 d D . .
H1W1 H 0.696(5) 0.929(2) 0.624(2) 0.047 Uiso 1 1 d D . .
H1W2 H 0.584(5) 0.837(3) 0.630(2) 0.047 Uiso 1 1 d D . .
O2W O 0.9939(4) 0.8760(3) 0.62877(19) 0.0343(7) Uani 1 1 d D . .
H2W1 H 1.029(5) 0.889(4) 0.6872(10) 0.051 Uiso 1 1 d D . .
H2W2 H 1.080(3) 0.891(4) 0.603(2) 0.051 Uiso 1 1 d D . .
O2 O 0.5634(3) 0.5904(2) 0.72614(19) 0.0312(7) Uani 1 1 d . . .
O3 O 0.8616(4) 0.5716(2) 0.76711(19) 0.0297(6) Uani 1 1 d . . .
O3W O 0.8654(4) 0.8501(2) 0.4444(2) 0.0341(7) Uani 1 1 d D . .
H3W1 H 0.890(6) 0.830(3) 0.3892(15) 0.051 Uiso 1 1 d D . .
H3W2 H 0.820(6) 0.910(2) 0.454(3) 0.051 Uiso 1 1 d D . .
O4 O 0.5625(4) 0.8496(2) 0.77992(18) 0.0274(6) Uani 1 1 d D . .
H4O H 0.534(5) 0.9152(18) 0.790(3) 0.041 Uiso 1 1 d D . .
O4W O 0.6022(4) 0.6474(2) 0.36326(19) 0.0289(6) Uani 1 1 d D . .
H4W1 H 0.548(5) 0.5805(14) 0.334(2) 0.043 Uiso 1 1 d D . .
H4W2 H 0.578(5) 0.692(2) 0.332(2) 0.043 Uiso 1 1 d D . .
O5 O 0.7421(4) 1.1222(2) 1.1046(2) 0.0351(7) Uani 1 1 d D . .
H5O H 0.765(6) 1.180(2) 1.153(2) 0.053 Uiso 1 1 d D . .
O5W O 0.9488(4) 0.6260(3) 0.38834(19) 0.0336(7) Uani 1 1 d D . .
H5W1 H 1.052(2) 0.659(4) 0.394(3) 0.050 Uiso 1 1 d D . .
H5W2 H 0.900(4) 0.605(4) 0.3316(12) 0.050 Uiso 1 1 d D . .
O6 O 0.9247(4) 1.0410(3) 1.1801(2) 0.0395(8) Uani 1 1 d . . .
O6W O 1.0585(4) 0.6472(3) 0.5678(2) 0.0357(7) Uani 1 1 d D . .
H6W1 H 1.113(5) 0.599(3) 0.536(2) 0.054 Uiso 1 1 d D . .
H6W2 H 1.097(5) 0.665(4) 0.6257(8) 0.054 Uiso 1 1 d D . .
O7W O 0.7271(4) 0.2499(3) 0.5763(2) 0.0415(8) Uani 1 1 d D . .
H7W1 H 0.684(5) 0.244(4) 0.624(2) 0.062 Uiso 1 1 d D . .
H7W2 H 0.656(5) 0.272(4) 0.541(3) 0.062 Uiso 1 1 d D . .
O7 O 0.7233(4) 1.0966(3) 0.7429(2) 0.0507(9) Uani 1 1 d . . .
O8 O 0.4747(5) 1.1712(3) 0.6946(2) 0.0613(11) Uani 1 1 d . . .
O8W O 0.7328(4) 1.0421(3) 0.4503(3) 0.0547(10) Uani 1 1 d D . .
H8W1 H 0.631(3) 1.013(4) 0.423(3) 0.082 Uiso 1 1 d D . .
H8W2 H 0.733(6) 1.107(2) 0.491(3) 0.082 Uiso 1 1 d D . .
O9W O 0.7723(4) 1.3162(2) 1.2500(2) 0.0340(7) Uani 1 1 d D . .
H9W1 H 0.675(3) 1.329(3) 1.265(3) 0.051 Uiso 1 1 d D . .
H9W2 H 0.821(5) 1.372(2) 1.236(3) 0.051 Uiso 1 1 d D . .
O9 O 0.4550(4) 1.0533(2) 0.7955(2) 0.0352(7) Uani 1 1 d . . .
O10 O 0.7615(5) 1.3612(2) 0.7812(2) 0.0409(8) Uani 1 1 d D . .
H10O H 0.802(6) 1.4277(19) 0.781(4) 0.061 Uiso 1 1 d D . .
O10W O 0.9317(4) 1.8292(3) 1.2562(2) 0.0422(8) Uani 1 1 d D . .
HAW H 1.0381(19) 1.842(4) 1.252(4) 0.063 Uiso 1 1 d D . .
HBW H 0.879(5) 1.876(3) 1.238(4) 0.063 Uiso 1 1 d D . .
O11 O 0.8294(5) 1.6425(3) 1.1052(2) 0.0489(9) Uani 1 1 d D . .
H11O H 0.861(7) 1.696(3) 1.157(2) 0.073 Uiso 1 1 d D . .
O12 O 0.7821(4) 1.5340(3) 1.1964(2) 0.0455(8) Uani 1 1 d . . .
O13 O 0.7162(3) 0.5026(2) 0.48639(19) 0.0247(6) Uani 1 1 d . . .
O14 O 0.5110(3) 0.3543(2) 0.47053(18) 0.0228(6) Uani 1 1 d . . .
C1 C 0.7647(5) 0.7617(3) 0.8540(2) 0.0201(8) Uani 1 1 d . . .
C2 C 0.6710(5) 0.8533(3) 0.8581(2) 0.0210(8) Uani 1 1 d . . .
C3 C 0.6935(5) 0.9433(3) 0.9414(3) 0.0231(8) Uani 1 1 d . . .
H3A H 0.6332 1.0043 0.9449 0.028 Uiso 1 1 calc R . .
C4 C 0.8055(5) 0.9431(3) 1.0197(3) 0.0226(8) Uani 1 1 d . . .
C5 C 0.8984(5) 0.8536(3) 1.0153(3) 0.0266(9) Uani 1 1 d . . .
H5A H 0.9738 0.8540 1.0678 0.032 Uiso 1 1 calc R . .
C6 C 0.8780(5) 0.7640(3) 0.9324(3) 0.0255(8) Uani 1 1 d . . .
H6A H 0.9411 0.7044 0.9291 0.031 Uiso 1 1 calc R . .
C7 C 0.8313(5) 1.0402(3) 1.1093(3) 0.0266(9) Uani 1 1 d . . .
C8 C 0.6223(5) 1.2594(3) 0.8695(3) 0.0239(8) Uani 1 1 d . . .
C9 C 0.7171(5) 1.3599(3) 0.8650(3) 0.0278(9) Uani 1 1 d . . .
C10 C 0.7630(5) 1.4538(3) 0.9456(3) 0.0295(9) Uani 1 1 d . . .
H10A H 0.8243 1.5213 0.9430 0.035 Uiso 1 1 calc R . .
C11 C 0.7178(5) 1.4476(3) 1.0300(3) 0.0274(9) Uani 1 1 d . . .
C12 C 0.6204(6) 1.3496(3) 1.0347(3) 0.0325(10) Uani 1 1 d . . .
H12A H 0.5869 1.3465 1.0911 0.039 Uiso 1 1 calc R . .
C13 C 0.5741(5) 1.2566(4) 0.9541(3) 0.0323(10) Uani 1 1 d . . .
H13A H 0.5088 1.1904 0.9566 0.039 Uiso 1 1 calc R . .
C14 C 0.7786(5) 1.5458(4) 1.1193(3) 0.0299(9) Uani 1 1 d . . .
C15 C 0.5647(5) 0.4580(3) 0.4869(2) 0.0182(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
Eu1 O6W 2.380(3) . ?
Eu1 O13 2.406(2) . ?
Eu1 O3W 2.423(3) . ?
Eu1 O1 2.436(2) . ?
Eu1 O5W 2.450(3) . ?
Eu1 O2W 2.486(3) . ?
Eu1 O14 2.492(2) 2_666 ?
Eu1 O4W 2.500(3) . ?
Eu1 O1W 2.532(3) . ?
Eu1 C15 3.254(4) . ?
S1 O2 1.445(3) . ?
S1 O1 1.457(3) . ?
S1 O3 1.457(3) . ?
S1 C1 1.776(4) . ?
S2 O8 1.442(3) . ?
S2 O9 1.452(3) . ?
S2 O7 1.457(3) . ?
S2 C8 1.773(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O2W H2W1 0.85(4) . ?
O2W H2W2 0.85(4) . ?
O3W H3W1 0.85(4) . ?
O3W H3W2 0.85(4) . ?
O4 C2 1.358(4) . ?
O4 H4O 0.85(4) . ?
O4W H4W1 0.85(4) . ?
O4W H4W2 0.85(4) . ?
O5 C7 1.314(5) . ?
O5 H5O 0.85(4) . ?
O5W H5W1 0.85(4) . ?
O5W H5W2 0.85(4) . ?
O6 C7 1.220(5) . ?
O6W H6W1 0.85(4) . ?
O6W H6W2 0.85(4) . ?
O7W H7W1 0.85(4) . ?
O7W H7W2 0.85(4) . ?
O8W H8W1 0.85(4) . ?
O8W H8W2 0.85(4) . ?
O9W H9W1 0.85(4) . ?
O9W H9W2 0.85(4) . ?
O10 C9 1.356(5) . ?
O10 H10O 0.85(4) . ?
O10W HAW 0.85(4) . ?
O10W HBW 0.85(4) . ?
O11 C14 1.304(5) . ?
O11 H11O 0.85(4) . ?
O12 C14 1.211(5) . ?
O13 C15 1.261(4) . ?
O14 C15 1.245(4) . ?
O14 Eu1 2.492(2) 2_666 ?
C1 C6 1.385(5) . ?
C1 C2 1.414(5) . ?
C2 C3 1.386(5) . ?
C3 C4 1.389(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(5) . ?
C4 C7 1.492(5) . ?
C5 C6 1.381(5) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C8 C13 1.383(5) . ?
C8 C9 1.399(5) . ?
C9 C10 1.385(5) . ?
C10 C11 1.383(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.385(5) . ?
C11 C14 1.504(5) . ?
C12 C13 1.380(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C15 1.543(7) 2_666 ?

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
O6W Eu1 O13 76.62(10) . . ?
O6W Eu1 O3W 107.87(11) . . ?
O13 Eu1 O3W 142.60(9) . . ?
O6W Eu1 O1 72.96(9) . . ?
O13 Eu1 O1 79.95(9) . . ?
O3W Eu1 O1 137.37(9) . . ?
O6W Eu1 O5W 66.97(10) . . ?
O13 Eu1 O5W 77.52(10) . . ?
O3W Eu1 O5W 71.02(10) . . ?
O1 Eu1 O5W 137.44(9) . . ?
O6W Eu1 O2W 71.21(11) . . ?
O13 Eu1 O2W 142.30(10) . . ?
O3W Eu1 O2W 68.22(10) . . ?
O1 Eu1 O2W 72.33(9) . . ?
O5W Eu1 O2W 106.45(10) . . ?
O6W Eu1 O14 132.78(10) . 2_666 ?
O13 Eu1 O14 65.98(8) . 2_666 ?
O3W Eu1 O14 119.34(10) . 2_666 ?
O1 Eu1 O14 73.05(9) . 2_666 ?
O5W Eu1 O14 126.92(9) . 2_666 ?
O2W Eu1 O14 126.14(9) . 2_666 ?
O6W Eu1 O4W 131.78(10) . . ?
O13 Eu1 O4W 77.44(9) . . ?
O3W Eu1 O4W 72.49(10) . . ?
O1 Eu1 O4W 139.61(9) . . ?
O5W Eu1 O4W 68.15(10) . . ?
O2W Eu1 O4W 139.59(10) . . ?
O14 Eu1 O4W 67.28(9) 2_666 . ?
O6W Eu1 O1W 134.22(10) . . ?
O13 Eu1 O1W 128.80(9) . . ?
O3W Eu1 O1W 75.38(10) . . ?
O1 Eu1 O1W 75.51(9) . . ?
O5W Eu1 O1W 145.19(10) . . ?
O2W Eu1 O1W 68.08(10) . . ?
O14 Eu1 O1W 64.13(9) 2_666 . ?
O4W Eu1 O1W 93.43(9) . . ?
O6W Eu1 C15 93.65(10) . . ?
O13 Eu1 C15 19.19(8) . . ?
O3W Eu1 C15 143.64(9) . . ?
O1 Eu1 C15 76.34(9) . . ?
O5W Eu1 C15 92.20(10) . . ?
O2W Eu1 C15 148.00(9) . . ?
O14 Eu1 C15 46.80(8) 2_666 . ?
O4W Eu1 C15 71.32(9) . . ?
O1W Eu1 C15 110.16(9) . . ?
O6W Eu1 H1W2 129.0(8) . . ?
O13 Eu1 H1W2 113.7(5) . . ?
O3W Eu1 H1W2 92.6(4) . . ?
O1 Eu1 H1W2 61.2(7) . . ?
O5W Eu1 H1W2 161.2(6) . . ?
O2W Eu1 H1W2 74.5(7) . . ?
O14 Eu1 H1W2 52.9(7) 2_666 . ?
O4W Eu1 H1W2 98.6(9) . . ?
O1W Eu1 H1W2 17.3(4) . . ?
C15 Eu1 H1W2 96.1(5) . . ?
O2 S1 O1 112.80(17) . . ?
O2 S1 O3 112.88(17) . . ?
O1 S1 O3 112.17(16) . . ?
O2 S1 C1 107.68(17) . . ?
O1 S1 C1 105.03(16) . . ?
O3 S1 C1 105.59(17) . . ?
O8 S2 O9 112.6(2) . . ?
O8 S2 O7 111.1(2) . . ?
O9 S2 O7 111.81(19) . . ?
O8 S2 C8 107.58(18) . . ?
O9 S2 C8 106.14(18) . . ?
O7 S2 C8 107.25(19) . . ?
S1 O1 Eu1 154.70(16) . . ?
Eu1 O1W H1W1 116(3) . . ?
Eu1 O1W H1W2 101(3) . . ?
H1W1 O1W H1W2 109.7(17) . . ?
Eu1 O2W H2W1 127(3) . . ?
Eu1 O2W H2W2 109(3) . . ?
H2W1 O2W H2W2 108.7(17) . . ?
Eu1 O3W H3W1 119(3) . . ?
Eu1 O3W H3W2 123(3) . . ?
H3W1 O3W H3W2 110.2(17) . . ?
C2 O4 H4O 106(3) . . ?
Eu1 O4W H4W1 125(2) . . ?
Eu1 O4W H4W2 125(2) . . ?
H4W1 O4W H4W2 109.8(17) . . ?
C7 O5 H5O 114(3) . . ?
Eu1 O5W H5W1 116(3) . . ?
Eu1 O5W H5W2 122(3) . . ?
H5W1 O5W H5W2 110.4(17) . . ?
Eu1 O6W H6W1 129(3) . . ?
Eu1 O6W H6W2 119(3) . . ?
H6W1 O6W H6W2 110.4(17) . . ?
H7W1 O7W H7W2 110.0(17) . . ?
H8W1 O8W H8W2 109.8(18) . . ?
H9W1 O9W H9W2 110.8(17) . . ?
C9 O10 H10O 113(4) . . ?
HAW O10W HBW 109.1(17) . . ?
C14 O11 H11O 111(4) . . ?
C15 O13 Eu1 122.0(2) . . ?
C15 O14 Eu1 118.7(2) . 2_666 ?
C6 C1 C2 119.7(3) . . ?
C6 C1 S1 120.0(3) . . ?
C2 C1 S1 120.2(3) . . ?
O4 C2 C3 122.5(3) . . ?
O4 C2 C1 118.5(3) . . ?
C3 C2 C1 119.0(3) . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 C7 118.8(4) . . ?
C3 C4 C7 120.7(3) . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C1 120.9(4) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
O6 C7 O5 124.0(4) . . ?
O6 C7 C4 122.3(4) . . ?
O5 C7 C4 113.7(3) . . ?
C13 C8 C9 119.3(4) . . ?
C13 C8 S2 120.0(3) . . ?
C9 C8 S2 120.7(3) . . ?
O10 C9 C10 122.3(4) . . ?
O10 C9 C8 118.3(3) . . ?
C10 C9 C8 119.4(4) . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 C14 120.6(4) . . ?
C12 C11 C14 118.5(4) . . ?
C13 C12 C11 118.6(4) . . ?
C13 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
C12 C13 C8 121.6(4) . . ?
C12 C13 H13A 119.2 . . ?
C8 C13 H13A 119.2 . . ?
O12 C14 O11 124.1(4) . . ?
O12 C14 C11 122.3(4) . . ?
O11 C14 C11 113.6(4) . . ?
O14 C15 O13 126.6(3) . . ?
O14 C15 C15 117.4(4) . 2_666 ?
O13 C15 C15 116.0(4) . 2_666 ?
O14 C15 Eu1 165.5(2) . . ?
C15 C15 Eu1 77.1(3) 2_666 . ?

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 Eu1 -42.1(4) . . . . ?
O3 S1 O1 Eu1 86.7(4) . . . . ?
C1 S1 O1 Eu1 -159.1(4) . . . . ?
O6W Eu1 O1 S1 -98.4(4) . . . . ?
O13 Eu1 O1 S1 -19.4(4) . . . . ?
O3W Eu1 O1 S1 163.5(3) . . . . ?
O5W Eu1 O1 S1 -78.3(4) . . . . ?
O2W Eu1 O1 S1 -173.6(4) . . . . ?
O14 Eu1 O1 S1 48.4(4) 2_666 . . . ?
O4W Eu1 O1 S1 37.3(4) . . . . ?
O1W Eu1 O1 S1 115.3(4) . . . . ?
C15 Eu1 O1 S1 -0.2(4) . . . . ?
O6W Eu1 O13 C15 152.0(3) . . . . ?
O3W Eu1 O13 C15 -106.0(3) . . . . ?
O1 Eu1 O13 C15 77.3(3) . . . . ?
O5W Eu1 O13 C15 -139.1(3) . . . . ?
O2W Eu1 O13 C15 120.1(3) . . . . ?
O14 Eu1 O13 C15 1.5(3) 2_666 . . . ?
O4W Eu1 O13 C15 -69.0(3) . . . . ?
O1W Eu1 O13 C15 15.2(3) . . . . ?
O2 S1 C1 C6 119.3(3) . . . . ?
O1 S1 C1 C6 -120.2(3) . . . . ?
O3 S1 C1 C6 -1.5(4) . . . . ?
O2 S1 C1 C2 -62.2(3) . . . . ?
O1 S1 C1 C2 58.3(3) . . . . ?
O3 S1 C1 C2 177.0(3) . . . . ?
C6 C1 C2 O4 179.2(3) . . . . ?
S1 C1 C2 O4 0.7(5) . . . . ?
C6 C1 C2 C3 -0.6(5) . . . . ?
S1 C1 C2 C3 -179.2(3) . . . . ?
O4 C2 C3 C4 179.7(3) . . . . ?
C1 C2 C3 C4 -0.4(5) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C2 C3 C4 C7 179.5(3) . . . . ?
C3 C4 C5 C6 -0.4(6) . . . . ?
C7 C4 C5 C6 -178.9(3) . . . . ?
C4 C5 C6 C1 -0.7(6) . . . . ?
C2 C1 C6 C5 1.2(6) . . . . ?
S1 C1 C6 C5 179.7(3) . . . . ?
C5 C4 C7 O6 -3.7(6) . . . . ?
C3 C4 C7 O6 177.7(4) . . . . ?
C5 C4 C7 O5 177.5(3) . . . . ?
C3 C4 C7 O5 -1.0(5) . . . . ?
O8 S2 C8 C13 125.8(4) . . . . ?
O9 S2 C8 C13 5.1(4) . . . . ?
O7 S2 C8 C13 -114.6(4) . . . . ?
O8 S2 C8 C9 -54.2(4) . . . . ?
O9 S2 C8 C9 -175.0(3) . . . . ?
O7 S2 C8 C9 65.4(4) . . . . ?
C13 C8 C9 O10 -179.3(4) . . . . ?
S2 C8 C9 O10 0.7(5) . . . . ?
C13 C8 C9 C10 1.0(6) . . . . ?
S2 C8 C9 C10 -179.0(3) . . . . ?
O10 C9 C10 C11 -178.7(4) . . . . ?
C8 C9 C10 C11 1.1(6) . . . . ?
C9 C10 C11 C12 -2.7(7) . . . . ?
C9 C10 C11 C14 175.3(4) . . . . ?
C10 C11 C12 C13 2.2(6) . . . . ?
C14 C11 C12 C13 -175.8(4) . . . . ?
C11 C12 C13 C8 -0.1(7) . . . . ?
C9 C8 C13 C12 -1.5(6) . . . . ?
S2 C8 C13 C12 178.5(3) . . . . ?
C10 C11 C14 O12 -160.1(4) . . . . ?
C12 C11 C14 O12 17.9(6) . . . . ?
C10 C11 C14 O11 18.6(6) . . . . ?
C12 C11 C14 O11 -163.4(4) . . . . ?
Eu1 O14 C15 O13 178.5(3) 2_666 . . . ?
Eu1 O14 C15 C15 0.3(5) 2_666 . . 2_666 ?
Eu1 O14 C15 Eu1 179.5(9) 2_666 . . . ?
Eu1 O13 C15 O14 179.6(3) . . . . ?
Eu1 O13 C15 C15 -2.1(5) . . . 2_666 ?
O6W Eu1 C15 O14 -28.5(10) . . . . ?
O13 Eu1 C15 O14 -1.3(9) . . . . ?
O3W Eu1 C15 O14 98.7(10) . . . . ?
O1 Eu1 C15 O14 -100.0(10) . . . . ?
O5W Eu1 C15 O14 38.5(10) . . . . ?
O2W Eu1 C15 O14 -88.1(10) . . . . ?
O14 Eu1 C15 O14 -179.4(10) 2_666 . . . ?
O4W Eu1 C15 O14 104.6(10) . . . . ?
O1W Eu1 C15 O14 -168.7(10) . . . . ?
O6W Eu1 C15 O13 -27.2(3) . . . . ?
O3W Eu1 C15 O13 100.0(3) . . . . ?
O1 Eu1 C15 O13 -98.7(3) . . . . ?
O5W Eu1 C15 O13 39.8(3) . . . . ?
O2W Eu1 C15 O13 -86.8(3) . . . . ?
O14 Eu1 C15 O13 -178.1(3) 2_666 . . . ?
O4W Eu1 C15 O13 105.8(3) . . . . ?
O1W Eu1 C15 O13 -167.4(3) . . . . ?
O6W Eu1 C15 C15 150.8(3) . . . 2_666 ?
O13 Eu1 C15 C15 178.0(5) . . . 2_666 ?
O3W Eu1 C15 C15 -82.0(3) . . . 2_666 ?
O1 Eu1 C15 C15 79.3(3) . . . 2_666 ?
O5W Eu1 C15 C15 -142.2(3) . . . 2_666 ?
O2W Eu1 C15 C15 91.2(3) . . . 2_666 ?
O14 Eu1 C15 C15 -0.1(2) 2_666 . . 2_666 ?
O4W Eu1 C15 C15 -76.1(3) . . . 2_666 ?
O1W Eu1 C15 C15 10.6(3) . . . 2_666 ?

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
O1W H1W1 O7 0.85(4) 2.27(2) 3.019(4) 148(4) .
O1W H1W2 O4 0.85(4) 2.26(2) 3.002(4) 147(3) .
O2W H2W1 O6 0.85(4) 1.900(18) 2.724(4) 162(5) 2_777
O2W H2W2 O8W 0.85(4) 1.979(15) 2.818(5) 168(5) 2_776
O3W H3W1 O10W 0.85(4) 2.069(17) 2.889(4) 162(4) 1_544
O3W H3W2 O8W 0.85(4) 1.856(15) 2.690(4) 168(4) .
O4 H4O O9 0.85(4)) 1.870(12) 2.707(4) 172(5) .
O4W H4W1 O2 0.85(4) 2.078(11) 2.920(4) 173(3) 2_666
O4W H4W2 O8 0.85(4) 1.930(16) 2.743(4) 160(4) 2_676
O5 H5O O9W 0.85(4) 1.861(15) 2.693(4) 168(5) .
O5W H5W1 O7W 0.85(4) 1.894(12) 2.734(4) 171(4) 2_766
O5W H5W2 O12 0.85(4) 2.022(12) 2.862(4) 173(5) 1_544
O6W H6W1 O13 0.85(4) 1.937(19) 2.736(4) 157(4) 2_766
O6W H6W2 O9W 0.85(4) 1.961(15) 2.789(4) 167(4) 2_777
O7W H7W1 O8 0.85(4) 2.31(3) 3.089(5) 153(5) 1_545
O7W H7W1 O10 0.85(4) 2.34(4) 2.950(4) 129(4) 1_545
O7W H7W2 O14 0.85(4) 2.030(15) 2.866(4) 169(5) .
O8W H8W1 O8 0.85(4) 2.42(3) 3.025(5) 129(4) 2_676
O8W H8W2 O7W 0.85(4) 1.864(12) 2.715(5) 178(5) 1_565
O9W H9W1 O2 0.85(4) 2.234(19) 3.032(4) 157(4) 2_677
O9W H9W1 O4 0.85(4) 2.59(4) 3.053(4) 116(3) 2_677
O9W H9W2 O12 0.85(4) 2.30(3) 3.032(4) 145(3) .
O9W H9W2 O3 0.85(4) 2.53(3) 3.134(4) 129(3) 2_777
O10 H10O O3 0.85(4) 1.870(13) 2.711(4) 171(5) 1_565
O10W HAW O7 0.85(4) 1.931(16) 2.771(5) 168(5) 2_787
O10W HBW O6 0.85(4) 2.45(3) 3.162(4) 142(3) 1_565
O11 H11O O10W 0.85(4) 1.845(15) 2.680(4) 170(5) .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.121
####################################################################### 
# 
# 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_5-La
_database_code_depnum_ccdc_archive 'CCDC 1549856'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 La N2 O7 S'
_chemical_formula_sum            'C17 H13 La N2 O7 S'
_chemical_formula_weight         528.26

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.3057(3)
_cell_length_b                   8.60327(20)
_cell_length_c                   18.4261(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.497(3)
_cell_angle_gamma                90.00
_cell_volume                     1709.31(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3015
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    2.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5914
_exptl_absorpt_correction_T_max  0.6748
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6145
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3898
_reflns_number_gt                3306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0169P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3898
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
La1 La 0.630702(18) 0.45885(2) 0.806469(11) 0.01436(7) Uani 1 1 d . . .
S1 S 0.30443(8) 0.37007(11) 0.65897(5) 0.01666(19) Uani 1 1 d . . .
O1 O 0.4178(2) 0.3980(3) 0.72203(14) 0.0247(6) Uani 1 1 d . . .
O1W O 0.6681(3) 0.2223(3) 0.72825(17) 0.0292(7) Uani 1 1 d D . .
H1W1 H 0.705(3) 0.149(3) 0.757(2) 0.044 Uiso 1 1 d D . .
H1W2 H 0.602(2) 0.187(4) 0.6964(18) 0.044 Uiso 1 1 d D . .
O2 O 0.2171(2) 0.4968(3) 0.65105(15) 0.0253(6) Uani 1 1 d . . .
O3 O 0.2500(2) 0.2187(3) 0.66685(14) 0.0218(6) Uani 1 1 d . . .
O4 O 0.4566(2) 0.1207(3) 0.61796(14) 0.0211(6) Uani 1 1 d . . .
O5 O 0.5366(2) 0.2413(3) 0.36841(15) 0.0247(6) Uani 1 1 d . . .
O6 O 0.3910(2) 0.4162(3) 0.31481(15) 0.0254(6) Uani 1 1 d . . .
N1 N 0.8021(3) 0.3826(4) 0.93998(18) 0.0235(7) Uani 1 1 d . . .
N2 N 0.8722(3) 0.4223(4) 0.81528(19) 0.0242(7) Uani 1 1 d . . .
C1 C 0.3461(3) 0.3581(4) 0.5746(2) 0.0162(8) Uani 1 1 d . . .
C2 C 0.4179(3) 0.2286(4) 0.5644(2) 0.0172(8) Uani 1 1 d . . .
C3 C 0.4464(3) 0.2213(4) 0.4953(2) 0.0192(8) Uani 1 1 d . . .
H3 H 0.4915 0.1373 0.4861 0.023 Uiso 1 1 calc R . .
C4 C 0.4088(3) 0.3368(4) 0.4406(2) 0.0157(8) Uani 1 1 d . . .
C5 C 0.3372(3) 0.4616(4) 0.4518(2) 0.0187(8) Uani 1 1 d . . .
H5 H 0.3107 0.5377 0.4146 0.022 Uiso 1 1 calc R . .
C6 C 0.3061(3) 0.4709(4) 0.5188(2) 0.0206(8) Uani 1 1 d . . .
H6 H 0.2581 0.5534 0.5264 0.025 Uiso 1 1 calc R . .
C7 C 0.4484(3) 0.3303(4) 0.3689(2) 0.0191(8) Uani 1 1 d . . .
C8 C 0.7667(4) 0.3764(5) 1.0031(2) 0.0293(9) Uani 1 1 d . . .
H8 H 0.6886 0.4142 1.0007 0.035 Uiso 1 1 calc R . .
C9 C 0.8400(4) 0.3169(5) 1.0714(2) 0.0365(11) Uani 1 1 d . . .
H9 H 0.8125 0.3149 1.1141 0.044 Uiso 1 1 calc R . .
C10 C 0.9551(4) 0.2605(6) 1.0741(3) 0.0458(13) Uani 1 1 d . . .
H10 H 1.0069 0.2189 1.1190 0.055 Uiso 1 1 calc R . .
C11 C 0.9930(4) 0.2660(5) 1.0102(3) 0.0429(12) Uani 1 1 d . . .
H11 H 1.0704 0.2271 1.0116 0.052 Uiso 1 1 calc R . .
C12 C 0.9161(4) 0.3297(4) 0.9434(2) 0.0245(9) Uani 1 1 d . . .
C13 C 0.9559(3) 0.3526(4) 0.8751(2) 0.0236(9) Uani 1 1 d . . .
C14 C 1.0743(4) 0.3183(5) 0.8718(3) 0.0384(12) Uani 1 1 d . . .
H14 H 1.1300 0.2657 0.9118 0.046 Uiso 1 1 calc R . .
C15 C 1.1090(4) 0.3621(6) 0.8096(3) 0.0460(13) Uani 1 1 d . . .
H15 H 1.1879 0.3383 0.8071 0.055 Uiso 1 1 calc R . .
C16 C 1.0270(4) 0.4410(5) 0.7513(3) 0.0376(11) Uani 1 1 d . . .
H16 H 1.0500 0.4773 0.7100 0.045 Uiso 1 1 calc R . .
C17 C 0.9088(4) 0.4644(5) 0.7562(3) 0.0312(10) Uani 1 1 d . . .
H17 H 0.8513 0.5126 0.7155 0.037 Uiso 1 1 calc R . .


_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
La1 O4 2.383(2) 2_656 ?
La1 O6 2.425(3) 3_666 ?
La1 O5 2.476(3) 4_566 ?
La1 O1 2.497(2) . ?
La1 O3 2.581(3) 2_656 ?
La1 O1W 2.601(3) . ?
La1 N2 2.705(3) . ?
La1 N1 2.715(3) . ?
S1 O2 1.449(3) . ?
S1 O3 1.466(3) . ?
S1 O1 1.468(3) . ?
S1 C1 1.758(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O3 La1 2.581(2) 2_646 ?
O4 C2 1.330(4) . ?
O4 La1 2.383(2) 2_646 ?
O5 C7 1.259(4) . ?
O5 La1 2.476(3) 4_565 ?
O6 C7 1.254(4) . ?
O6 La1 2.425(3) 3_666 ?
N1 C8 1.339(5) . ?
N1 C12 1.351(5) . ?
N2 C17 1.326(5) . ?
N2 C13 1.357(5) . ?
C1 C6 1.387(5) . ?
C1 C2 1.424(5) . ?
C2 C3 1.405(5) . ?
C3 C4 1.387(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(5) . ?
C4 C7 1.518(5) . ?
C5 C6 1.383(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.381(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.376(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.369(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.472(6) . ?
C13 C14 1.390(5) . ?
C14 C15 1.370(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.370(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 La1 O6 109.55(9) 2_656 3_666 ?
O4 La1 O5 80.00(9) 2_656 4_566 ?
O6 La1 O5 142.62(9) 3_666 4_566 ?
O4 La1 O1 89.75(8) 2_656 . ?
O6 La1 O1 72.99(9) 3_666 . ?
O5 La1 O1 70.97(9) 4_566 . ?
O4 La1 O3 70.55(8) 2_656 2_656 ?
O6 La1 O3 72.17(9) 3_666 2_656 ?
O5 La1 O3 141.92(8) 4_566 2_656 ?
O1 La1 O3 130.63(8) . 2_656 ?
O4 La1 O1W 161.09(9) 2_656 . ?
O6 La1 O1W 79.88(9) 3_666 . ?
O5 La1 O1W 82.84(9) 4_566 . ?
O1 La1 O1W 77.15(9) . . ?
O3 La1 O1W 128.35(8) 2_656 . ?
O4 La1 N2 128.38(9) 2_656 . ?
O6 La1 N2 85.83(10) 3_666 . ?
O5 La1 N2 117.24(9) 4_566 . ?
O1 La1 N2 141.23(9) . . ?
O3 La1 N2 68.20(8) 2_656 . ?
O1W La1 N2 67.22(9) . . ?
O4 La1 N1 85.41(9) 2_656 . ?
O6 La1 N1 142.09(9) 3_666 . ?
O5 La1 N1 72.72(9) 4_566 . ?
O1 La1 N1 143.67(9) . . ?
O3 La1 N1 81.18(9) 2_656 . ?
O1W La1 N1 97.04(9) . . ?
N2 La1 N1 58.99(10) . . ?
O2 S1 O3 112.63(15) . . ?
O2 S1 O1 111.29(16) . . ?
O3 S1 O1 111.07(16) . . ?
O2 S1 C1 108.10(17) . . ?
O3 S1 C1 105.52(16) . . ?
O1 S1 C1 107.91(16) . . ?
S1 O1 La1 167.43(16) . . ?
La1 O1W H1W1 112(3) . . ?
La1 O1W H1W2 114(3) . . ?
H1W1 O1W H1W2 109.2(17) . . ?
S1 O3 La1 125.25(14) . 2_646 ?
C2 O4 La1 137.7(2) . 2_646 ?
C7 O5 La1 151.3(2) . 4_565 ?
C7 O6 La1 151.5(3) . 3_666 ?
C8 N1 C12 118.4(3) . . ?
C8 N1 La1 118.6(3) . . ?
C12 N1 La1 122.4(3) . . ?
C17 N2 C13 118.3(3) . . ?
C17 N2 La1 118.5(3) . . ?
C13 N2 La1 123.0(3) . . ?
C6 C1 C2 121.4(3) . . ?
C6 C1 S1 120.0(3) . . ?
C2 C1 S1 118.5(3) . . ?
O4 C2 C3 121.9(3) . . ?
O4 C2 C1 121.4(3) . . ?
C3 C2 C1 116.7(3) . . ?
C4 C3 C2 121.5(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C7 120.0(3) . . ?
C5 C4 C7 119.5(3) . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O6 C7 O5 125.0(4) . . ?
O6 C7 C4 116.9(3) . . ?
O5 C7 C4 118.1(3) . . ?
N1 C8 C9 123.5(4) . . ?
N1 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 117.8(4) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C11 C10 C9 119.6(4) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.1(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
N1 C12 C11 120.6(4) . . ?
N1 C12 C13 116.5(3) . . ?
C11 C12 C13 122.7(4) . . ?
N2 C13 C14 120.3(4) . . ?
N2 C13 C12 115.9(3) . . ?
C14 C13 C12 123.7(4) . . ?
C15 C14 C13 119.9(4) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 117.5(4) . . ?
C15 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
N2 C17 C16 124.1(4) . . ?
N2 C17 H17 118.0 . . ?
C16 C17 H17 118.0 . . ?

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 La1 -104.4(8) . . . . ?
O3 S1 O1 La1 129.2(8) . . . . ?
C1 S1 O1 La1 14.0(8) . . . . ?
O4 La1 O1 S1 132.0(8) 2_656 . . . ?
O6 La1 O1 S1 21.5(8) 3_666 . . . ?
O5 La1 O1 S1 -148.5(8) 4_566 . . . ?
O3 La1 O1 S1 68.3(8) 2_656 . . . ?
O1W La1 O1 S1 -61.7(8) . . . . ?
N2 La1 O1 S1 -38.4(9) . . . . ?
N1 La1 O1 S1 -146.1(7) . . . . ?
O2 S1 O3 La1 -174.72(15) . . . 2_646 ?
O1 S1 O3 La1 -49.1(2) . . . 2_646 ?
C1 S1 O3 La1 67.6(2) . . . 2_646 ?
O4 La1 N1 C8 33.6(3) 2_656 . . . ?
O6 La1 N1 C8 149.9(3) 3_666 . . . ?
O5 La1 N1 C8 -47.4(3) 4_566 . . . ?
O1 La1 N1 C8 -49.8(4) . . . . ?
O3 La1 N1 C8 104.6(3) 2_656 . . . ?
O1W La1 N1 C8 -127.6(3) . . . . ?
N2 La1 N1 C8 174.4(3) . . . . ?
O4 La1 N1 C12 -156.1(3) 2_656 . . . ?
O6 La1 N1 C12 -39.8(4) 3_666 . . . ?
O5 La1 N1 C12 123.0(3) 4_566 . . . ?
O1 La1 N1 C12 120.6(3) . . . . ?
O3 La1 N1 C12 -85.1(3) 2_656 . . . ?
O1W La1 N1 C12 42.8(3) . . . . ?
N2 La1 N1 C12 -15.3(3) . . . . ?
O4 La1 N2 C17 -116.8(3) 2_656 . . . ?
O6 La1 N2 C17 -5.0(3) 3_666 . . . ?
O5 La1 N2 C17 144.1(3) 4_566 . . . ?
O1 La1 N2 C17 51.0(4) . . . . ?
O3 La1 N2 C17 -77.5(3) 2_656 . . . ?
O1W La1 N2 C17 75.7(3) . . . . ?
N1 La1 N2 C17 -170.2(3) . . . . ?
O4 La1 N2 C13 68.2(3) 2_656 . . . ?
O6 La1 N2 C13 179.9(3) 3_666 . . . ?
O5 La1 N2 C13 -30.9(3) 4_566 . . . ?
O1 La1 N2 C13 -124.1(3) . . . . ?
O3 La1 N2 C13 107.5(3) 2_656 . . . ?
O1W La1 N2 C13 -99.3(3) . . . . ?
N1 La1 N2 C13 14.7(3) . . . . ?
O2 S1 C1 C6 6.8(3) . . . . ?
O3 S1 C1 C6 127.5(3) . . . . ?
O1 S1 C1 C6 -113.7(3) . . . . ?
O2 S1 C1 C2 -171.4(3) . . . . ?
O3 S1 C1 C2 -50.7(3) . . . . ?
O1 S1 C1 C2 68.1(3) . . . . ?
La1 O4 C2 C3 -129.2(3) 2_646 . . . ?
La1 O4 C2 C1 51.4(5) 2_646 . . . ?
C6 C1 C2 O4 179.7(3) . . . . ?
S1 C1 C2 O4 -2.1(5) . . . . ?
C6 C1 C2 C3 0.2(5) . . . . ?
S1 C1 C2 C3 178.4(3) . . . . ?
O4 C2 C3 C4 -178.0(3) . . . . ?
C1 C2 C3 C4 1.5(5) . . . . ?
C2 C3 C4 C5 -2.3(5) . . . . ?
C2 C3 C4 C7 176.0(3) . . . . ?
C3 C4 C5 C6 1.3(5) . . . . ?
C7 C4 C5 C6 -177.0(3) . . . . ?
C4 C5 C6 C1 0.4(5) . . . . ?
C2 C1 C6 C5 -1.1(5) . . . . ?
S1 C1 C6 C5 -179.3(3) . . . . ?
La1 O6 C7 O5 -13.0(7) 3_666 . . . ?
La1 O6 C7 C4 166.3(3) 3_666 . . . ?
La1 O5 C7 O6 -46.8(7) 4_565 . . . ?
La1 O5 C7 C4 134.0(4) 4_565 . . . ?
C3 C4 C7 O6 164.8(3) . . . . ?
C5 C4 C7 O6 -16.8(5) . . . . ?
C3 C4 C7 O5 -15.9(5) . . . . ?
C5 C4 C7 O5 162.4(3) . . . . ?
C12 N1 C8 C9 -0.8(6) . . . . ?
La1 N1 C8 C9 169.9(3) . . . . ?
N1 C8 C9 C10 -0.3(7) . . . . ?
C8 C9 C10 C11 0.4(7) . . . . ?
C9 C10 C11 C12 0.7(8) . . . . ?
C8 N1 C12 C11 1.9(6) . . . . ?
La1 N1 C12 C11 -168.4(3) . . . . ?
C8 N1 C12 C13 -174.2(4) . . . . ?
La1 N1 C12 C13 15.4(4) . . . . ?
C10 C11 C12 N1 -1.9(7) . . . . ?
C10 C11 C12 C13 174.0(4) . . . . ?
C17 N2 C13 C14 -3.8(6) . . . . ?
La1 N2 C13 C14 171.2(3) . . . . ?
C17 N2 C13 C12 171.2(4) . . . . ?
La1 N2 C13 C12 -13.7(4) . . . . ?
N1 C12 C13 N2 -1.2(5) . . . . ?
C11 C12 C13 N2 -177.3(4) . . . . ?
N1 C12 C13 C14 173.7(4) . . . . ?
C11 C12 C13 C14 -2.4(6) . . . . ?
N2 C13 C14 C15 3.3(7) . . . . ?
C12 C13 C14 C15 -171.3(4) . . . . ?
C13 C14 C15 C16 0.7(7) . . . . ?
C14 C15 C16 C17 -3.9(7) . . . . ?
C13 N2 C17 C16 0.4(6) . . . . ?
La1 N2 C17 C16 -174.9(3) . . . . ?
C15 C16 C17 N2 3.5(7) . . . . ?

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
O1W H1W1 O2 0.85(4) 2.112(15) 2.942(4) 165(4) 2_646
O1W H1W1 O1 0.85(4) 2.66(3) 3.179(4) 121(3) 2_646
O1W H1W2 O4 0.85(4) 1.923(11) 2.773(4) 175(4) .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.748
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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_5-Eu
_database_code_depnum_ccdc_archive 'CCDC 1549860'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 Eu N2 O7 S'
_chemical_formula_sum            'C17 H13 Eu N2 O7 S'
_chemical_formula_weight         541.31

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'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.2266(4)
_cell_length_b                   8.5445(3)
_cell_length_c                   18.0467(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.810(4)
_cell_angle_gamma                90.00
_cell_volume                     1648.18(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2930
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_exptl_absorpt_coefficient_mu    3.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4484
_exptl_absorpt_correction_T_max  0.5343
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5763
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3780
_reflns_number_gt                3127
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0170P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3780
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0609
_refine_ls_wR_factor_gt          0.0564
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.010
_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 0.323308(19) 0.53820(2) 0.192908(12) 0.01373(7) Uani 1 1 d . . .
S1 S 0.14598(10) 0.63056(12) 0.33999(6) 0.0154(2) Uani 1 1 d . . .
O1W O 0.4322(3) 0.7688(3) 0.2664(2) 0.0253(7) Uani 1 1 d D . .
H1W1 H 0.441(5) 0.842(3) 0.237(2) 0.038 Uiso 1 1 d D . .
H1W2 H 0.408(5) 0.807(4) 0.3030(19) 0.038 Uiso 1 1 d D . .
O1 O 0.1948(3) 0.5986(4) 0.27511(17) 0.0225(7) Uani 1 1 d . . .
O2 O 0.0855(3) 0.7847(3) 0.33171(18) 0.0201(7) Uani 1 1 d . . .
O3 O 0.0652(3) 0.5059(3) 0.34979(18) 0.0230(7) Uani 1 1 d . . .
O4 O 0.3375(3) 0.8847(3) 0.38022(17) 0.0186(6) Uani 1 1 d . . .
O5 O 0.6735(3) 0.7646(3) 0.63191(17) 0.0203(7) Uani 1 1 d . . .
O6 O 0.5852(3) 0.5837(3) 0.68817(17) 0.0225(7) Uani 1 1 d . . .
N1 N 0.5515(3) 0.5688(4) 0.1874(2) 0.0213(8) Uani 1 1 d . . .
N2 N 0.3586(3) 0.6123(4) 0.0617(2) 0.0217(8) Uani 1 1 d . . .
C1 C 0.2735(4) 0.6442(4) 0.4259(2) 0.0144(9) Uani 1 1 d . . .
C2 C 0.3537(4) 0.7755(5) 0.4354(2) 0.0158(9) Uani 1 1 d . . .
C3 C 0.4514(4) 0.7823(5) 0.5048(2) 0.0167(9) Uani 1 1 d . . .
H3 H 0.5050 0.8680 0.5139 0.020 Uiso 1 1 calc R . .
C4 C 0.4720(4) 0.6663(4) 0.5611(2) 0.0148(9) Uani 1 1 d . . .
C5 C 0.3905(4) 0.5391(5) 0.5502(2) 0.0186(9) Uani 1 1 d . . .
H5 H 0.4030 0.4615 0.5879 0.022 Uiso 1 1 calc R . .
C6 C 0.2917(4) 0.5298(5) 0.4830(2) 0.0184(9) Uani 1 1 d . . .
H6 H 0.2364 0.4460 0.4756 0.022 Uiso 1 1 calc R . .
C7 C 0.5859(4) 0.6737(5) 0.6327(2) 0.0151(9) Uani 1 1 d . . .
C8 C 0.6475(4) 0.5215(5) 0.2477(3) 0.0291(11) Uani 1 1 d . . .
H8 H 0.6298 0.4709 0.2887 0.035 Uiso 1 1 calc R . .
C9 C 0.7711(5) 0.5434(6) 0.2524(3) 0.0340(12) Uani 1 1 d . . .
H9 H 0.8349 0.5037 0.2941 0.041 Uiso 1 1 calc R . .
C10 C 0.7976(5) 0.6253(6) 0.1942(3) 0.0388(14) Uani 1 1 d . . .
H10 H 0.8801 0.6468 0.1970 0.047 Uiso 1 1 calc R . .
C11 C 0.7007(5) 0.6756(6) 0.1312(3) 0.0349(13) Uani 1 1 d . . .
H11 H 0.7170 0.7322 0.0914 0.042 Uiso 1 1 calc R . .
C12 C 0.5781(4) 0.6405(5) 0.1281(3) 0.0233(10) Uani 1 1 d . . .
C13 C 0.4700(4) 0.6671(5) 0.0584(3) 0.0241(11) Uani 1 1 d . . .
C14 C 0.4808(5) 0.7343(6) -0.0096(3) 0.0391(14) Uani 1 1 d . . .
H14 H 0.5575 0.7736 -0.0107 0.047 Uiso 1 1 calc R . .
C15 C 0.3794(6) 0.7428(6) -0.0746(3) 0.0420(15) Uani 1 1 d . . .
H15 H 0.3865 0.7873 -0.1201 0.050 Uiso 1 1 calc R . .
C16 C 0.2661(5) 0.6847(5) -0.0721(3) 0.0312(12) Uani 1 1 d . . .
H16 H 0.1956 0.6876 -0.1156 0.037 Uiso 1 1 calc R . .
C17 C 0.2613(4) 0.6226(5) -0.0029(3) 0.0259(11) Uani 1 1 d . . .
H17 H 0.1846 0.5848 -0.0009 0.031 Uiso 1 1 calc R . .


_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 O4 2.294(3) 2_545 ?
Eu1 O6 2.323(3) 3_666 ?
Eu1 O5 2.398(3) 4_575 ?
Eu1 O1 2.420(3) . ?
Eu1 O1W 2.479(3) . ?
Eu1 O2 2.493(3) 2_545 ?
Eu1 N2 2.597(4) . ?
Eu1 N1 2.607(4) . ?
S1 O3 1.445(3) . ?
S1 O1 1.462(3) . ?
S1 O2 1.468(3) . ?
S1 C1 1.763(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O2 Eu1 2.493(3) 2 ?
O4 C2 1.336(5) . ?
O4 Eu1 2.294(3) 2 ?
O5 C7 1.257(5) . ?
O5 Eu1 2.398(3) 4_676 ?
O6 C7 1.264(5) . ?
O6 Eu1 2.323(3) 3_666 ?
N1 C8 1.338(6) . ?
N1 C12 1.344(6) . ?
N2 C17 1.335(6) . ?
N2 C13 1.354(5) . ?
C1 C6 1.389(5) . ?
C1 C2 1.416(5) . ?
C2 C3 1.392(6) . ?
C3 C4 1.387(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(5) . ?
C4 C7 1.515(6) . ?
C5 C6 1.373(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.377(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.369(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.380(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.393(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.475(7) . ?
C13 C14 1.392(7) . ?
C14 C15 1.364(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.379(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.372(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Eu1 O6 108.83(10) 2_545 3_666 ?
O4 Eu1 O5 79.61(10) 2_545 4_575 ?
O6 Eu1 O5 142.11(10) 3_666 4_575 ?
O4 Eu1 O1 87.88(10) 2_545 . ?
O6 Eu1 O1 72.99(10) 3_666 . ?
O5 Eu1 O1 70.46(10) 4_575 . ?
O4 Eu1 O1W 159.19(10) 2_545 . ?
O6 Eu1 O1W 81.73(10) 3_666 . ?
O5 Eu1 O1W 81.30(11) 4_575 . ?
O1 Eu1 O1W 77.97(10) . . ?
O4 Eu1 O2 72.22(10) 2_545 2_545 ?
O6 Eu1 O2 71.66(10) 3_666 2_545 ?
O5 Eu1 O2 142.90(10) 4_575 2_545 ?
O1 Eu1 O2 130.45(10) . 2_545 ?
O1W Eu1 O2 128.59(10) . 2_545 ?
O4 Eu1 N2 85.84(11) 2_545 . ?
O6 Eu1 N2 143.54(11) 3_666 . ?
O5 Eu1 N2 72.01(11) 4_575 . ?
O1 Eu1 N2 142.46(11) . . ?
O1W Eu1 N2 96.08(11) . . ?
O2 Eu1 N2 82.17(10) 2_545 . ?
O4 Eu1 N1 130.17(11) 2_545 . ?
O6 Eu1 N1 85.29(11) 3_666 . ?
O5 Eu1 N1 118.14(10) 4_575 . ?
O1 Eu1 N1 141.14(11) . . ?
O1W Eu1 N1 67.10(11) . . ?
O2 Eu1 N1 67.57(10) 2_545 . ?
N2 Eu1 N1 60.99(12) . . ?
O3 S1 O1 111.32(18) . . ?
O3 S1 O2 112.68(18) . . ?
O1 S1 O2 111.16(18) . . ?
O3 S1 C1 108.19(19) . . ?
O1 S1 C1 108.32(19) . . ?
O2 S1 C1 104.84(18) . . ?
Eu1 O1W H1W1 113(3) . . ?
Eu1 O1W H1W2 120(3) . . ?
H1W1 O1W H1W2 109.2(17) . . ?
S1 O1 Eu1 165.99(19) . . ?
S1 O2 Eu1 126.51(17) . 2 ?
C2 O4 Eu1 137.1(3) . 2 ?
C7 O5 Eu1 150.5(3) . 4_676 ?
C7 O6 Eu1 153.7(3) . 3_666 ?
C8 N1 C12 117.7(4) . . ?
C8 N1 Eu1 119.7(3) . . ?
C12 N1 Eu1 122.5(3) . . ?
C17 N2 C13 117.4(4) . . ?
C17 N2 Eu1 120.0(3) . . ?
C13 N2 Eu1 121.7(3) . . ?
C6 C1 C2 121.6(4) . . ?
C6 C1 S1 120.1(3) . . ?
C2 C1 S1 118.3(3) . . ?
O4 C2 C3 122.1(4) . . ?
O4 C2 C1 121.8(4) . . ?
C3 C2 C1 116.0(4) . . ?
C4 C3 C2 122.6(4) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 C7 120.2(4) . . ?
C5 C4 C7 119.9(4) . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O5 C7 O6 125.4(4) . . ?
O5 C7 C4 118.4(4) . . ?
O6 C7 C4 116.3(4) . . ?
N1 C8 C9 123.7(5) . . ?
N1 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 118.3(5) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C9 C10 C11 119.3(5) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C12 119.1(5) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N1 C12 C11 121.6(5) . . ?
N1 C12 C13 115.1(4) . . ?
C11 C12 C13 123.1(4) . . ?
N2 C13 C14 120.8(5) . . ?
N2 C13 C12 116.1(4) . . ?
C14 C13 C12 123.0(5) . . ?
C15 C14 C13 120.3(5) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.2(5) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 117.6(5) . . ?
C17 C16 H16 121.2 . . ?
C15 C16 H16 121.2 . . ?
N2 C17 C16 124.7(5) . . ?
N2 C17 H17 117.6 . . ?
C16 C17 H17 117.6 . . ?

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
O3 S1 O1 Eu1 -110.6(8) . . . . ?
O2 S1 O1 Eu1 122.9(8) . . . . ?
C1 S1 O1 Eu1 8.2(9) . . . . ?
O4 Eu1 O1 S1 138.7(8) 2_545 . . . ?
O6 Eu1 O1 S1 28.2(8) 3_666 . . . ?
O5 Eu1 O1 S1 -141.6(8) 4_575 . . . ?
O1W Eu1 O1 S1 -56.7(8) . . . . ?
O2 Eu1 O1 S1 74.3(8) 2_545 . . . ?
N2 Eu1 O1 S1 -141.0(7) . . . . ?
N1 Eu1 O1 S1 -30.7(9) . . . . ?
O3 S1 O2 Eu1 -176.90(18) . . . 2 ?
O1 S1 O2 Eu1 -51.2(3) . . . 2 ?
C1 S1 O2 Eu1 65.7(2) . . . 2 ?
O4 Eu1 N1 C8 -114.2(3) 2_545 . . . ?
O6 Eu1 N1 C8 -3.4(3) 3_666 . . . ?
O5 Eu1 N1 C8 145.3(3) 4_575 . . . ?
O1 Eu1 N1 C8 51.9(4) . . . . ?
O1W Eu1 N1 C8 79.6(3) . . . . ?
O2 Eu1 N1 C8 -75.5(3) 2_545 . . . ?
N2 Eu1 N1 C8 -168.9(4) . . . . ?
O4 Eu1 N1 C12 70.4(3) 2_545 . . . ?
O6 Eu1 N1 C12 -178.8(3) 3_666 . . . ?
O5 Eu1 N1 C12 -30.2(3) 4_575 . . . ?
O1 Eu1 N1 C12 -123.6(3) . . . . ?
O1W Eu1 N1 C12 -95.8(3) . . . . ?
O2 Eu1 N1 C12 109.1(3) 2_545 . . . ?
N2 Eu1 N1 C12 15.6(3) . . . . ?
O4 Eu1 N2 C17 33.7(3) 2_545 . . . ?
O6 Eu1 N2 C17 150.2(3) 3_666 . . . ?
O5 Eu1 N2 C17 -46.7(3) 4_575 . . . ?
O1 Eu1 N2 C17 -47.4(4) . . . . ?
O1W Eu1 N2 C17 -125.5(3) . . . . ?
O2 Eu1 N2 C17 106.3(3) 2_545 . . . ?
N1 Eu1 N2 C17 174.9(4) . . . . ?
O4 Eu1 N2 C13 -157.7(3) 2_545 . . . ?
O6 Eu1 N2 C13 -41.2(4) 3_666 . . . ?
O5 Eu1 N2 C13 121.8(3) 4_575 . . . ?
O1 Eu1 N2 C13 121.2(3) . . . . ?
O1W Eu1 N2 C13 43.1(3) . . . . ?
O2 Eu1 N2 C13 -85.1(3) 2_545 . . . ?
N1 Eu1 N2 C13 -16.5(3) . . . . ?
O3 S1 C1 C6 9.5(4) . . . . ?
O1 S1 C1 C6 -111.3(3) . . . . ?
O2 S1 C1 C6 130.0(3) . . . . ?
O3 S1 C1 C2 -169.1(3) . . . . ?
O1 S1 C1 C2 70.1(4) . . . . ?
O2 S1 C1 C2 -48.7(4) . . . . ?
Eu1 O4 C2 C3 -129.8(4) 2 . . . ?
Eu1 O4 C2 C1 51.3(6) 2 . . . ?
C6 C1 C2 O4 179.1(4) . . . . ?
S1 C1 C2 O4 -2.3(5) . . . . ?
C6 C1 C2 C3 0.2(6) . . . . ?
S1 C1 C2 C3 178.8(3) . . . . ?
O4 C2 C3 C4 -177.3(4) . . . . ?
C1 C2 C3 C4 1.6(6) . . . . ?
C2 C3 C4 C5 -2.2(6) . . . . ?
C2 C3 C4 C7 175.1(4) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
C7 C4 C5 C6 -176.4(4) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C2 C1 C6 C5 -1.4(6) . . . . ?
S1 C1 C6 C5 -179.9(3) . . . . ?
Eu1 O5 C7 O6 -48.2(8) 4_676 . . . ?
Eu1 O5 C7 C4 133.4(4) 4_676 . . . ?
Eu1 O6 C7 O5 -8.4(9) 3_666 . . . ?
Eu1 O6 C7 C4 170.0(4) 3_666 . . . ?
C3 C4 C7 O5 -15.5(6) . . . . ?
C5 C4 C7 O5 161.8(4) . . . . ?
C3 C4 C7 O6 165.9(4) . . . . ?
C5 C4 C7 O6 -16.8(6) . . . . ?
C12 N1 C8 C9 0.6(7) . . . . ?
Eu1 N1 C8 C9 -175.1(4) . . . . ?
N1 C8 C9 C10 3.5(8) . . . . ?
C8 C9 C10 C11 -3.3(8) . . . . ?
C9 C10 C11 C12 -0.6(8) . . . . ?
C8 N1 C12 C11 -4.8(6) . . . . ?
Eu1 N1 C12 C11 170.7(3) . . . . ?
C8 N1 C12 C13 170.6(4) . . . . ?
Eu1 N1 C12 C13 -13.9(5) . . . . ?
C10 C11 C12 N1 4.9(7) . . . . ?
C10 C11 C12 C13 -170.2(5) . . . . ?
C17 N2 C13 C14 1.4(6) . . . . ?
Eu1 N2 C13 C14 -167.5(3) . . . . ?
C17 N2 C13 C12 -174.3(4) . . . . ?
Eu1 N2 C13 C12 16.8(5) . . . . ?
N1 C12 C13 N2 -1.9(6) . . . . ?
C11 C12 C13 N2 173.5(4) . . . . ?
N1 C12 C13 C14 -177.5(4) . . . . ?
C11 C12 C13 C14 -2.1(7) . . . . ?
N2 C13 C14 C15 -1.5(7) . . . . ?
C12 C13 C14 C15 173.9(5) . . . . ?
C13 C14 C15 C16 0.3(8) . . . . ?
C14 C15 C16 C17 0.9(7) . . . . ?
C13 N2 C17 C16 -0.2(7) . . . . ?
Eu1 N2 C17 C16 168.9(3) . . . . ?
C15 C16 C17 N2 -1.0(7) . . . . ?

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
O1W H1W1 O3 0.85(4) 2.083(14) 2.921(4) 170(5) 2
O1W H1W1 O1 0.85(4) 2.64(4) 3.143(4) 119(3) 2
O1W H1W2 O4 0.85(4) 1.921(12) 2.770(4) 174(5) .

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.138
####################################################################### 
# 
# 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_5-Tb
_database_code_depnum_ccdc_archive 'CCDC 1549862'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 N2 O7 S Tb'
_chemical_formula_sum            'C17 H13 N2 O7 S Tb'
_chemical_formula_weight         548.27

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.1852(3)
_cell_length_b                   8.5087(2)
_cell_length_c                   17.9015(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.712(3)
_cell_angle_gamma                90.00
_cell_volume                     1622.96(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2353
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    4.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4795
_exptl_absorpt_correction_T_max  0.5494
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5837
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3700
_reflns_number_gt                3014
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0326P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3700
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_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 0.32310(2) 1.03746(3) 0.192842(14) 0.01346(8) Uani 1 1 d . . .
S1 S 0.14623(12) 1.13063(15) 0.33968(8) 0.0147(3) Uani 1 1 d . . .
O1W O 0.4304(4) 1.2665(5) 0.2651(2) 0.0237(9) Uani 1 1 d D . .
H1W1 H 0.412(6) 1.324(5) 0.2247(19) 0.036 Uiso 1 1 d D . .
H1W2 H 0.409(6) 1.311(6) 0.301(2) 0.036 Uiso 1 1 d D . .
O1 O 0.1941(4) 1.0978(5) 0.2743(2) 0.0216(9) Uani 1 1 d . . .
O2 O 0.0865(3) 1.2843(4) 0.3316(2) 0.0185(8) Uani 1 1 d . . .
O3 O 0.0640(3) 1.0060(4) 0.3504(2) 0.0213(9) Uani 1 1 d . . .
O4 O 0.3373(3) 1.3854(4) 0.3800(2) 0.0201(8) Uani 1 1 d . . .
O5 O 0.6749(3) 1.2659(5) 0.6319(2) 0.0219(9) Uani 1 1 d . . .
O6 O 0.5875(3) 1.0847(4) 0.6892(2) 0.0199(8) Uani 1 1 d . . .
N1 N 0.5512(4) 1.0659(5) 0.1889(3) 0.0209(10) Uani 1 1 d . . .
N2 N 0.3576(4) 1.1108(6) 0.0617(3) 0.0201(10) Uani 1 1 d . . .
C1 C 0.2737(5) 1.1448(6) 0.4255(3) 0.0160(11) Uani 1 1 d . . .
C2 C 0.3527(5) 1.2766(6) 0.4345(3) 0.0167(11) Uani 1 1 d . . .
C3 C 0.4518(5) 1.2836(6) 0.5051(3) 0.0170(11) Uani 1 1 d . . .
H3 H 0.5051 1.3701 0.5143 0.020 Uiso 1 1 calc R . .
C4 C 0.4731(5) 1.1671(6) 0.5617(3) 0.0143(11) Uani 1 1 d . . .
C5 C 0.3926(5) 1.0391(6) 0.5508(3) 0.0166(11) Uani 1 1 d . . .
H5 H 0.4059 0.9607 0.5887 0.020 Uiso 1 1 calc R . .
C6 C 0.2922(5) 1.0298(6) 0.4827(3) 0.0188(11) Uani 1 1 d . . .
H6 H 0.2367 0.9457 0.4753 0.023 Uiso 1 1 calc R . .
C7 C 0.5877(5) 1.1733(6) 0.6331(3) 0.0159(11) Uani 1 1 d . . .
C8 C 0.6469(6) 1.0166(8) 0.2489(4) 0.0297(14) Uani 1 1 d . . .
H8 H 0.6292 0.9640 0.2898 0.036 Uiso 1 1 calc R . .
C9 C 0.7703(6) 1.0396(8) 0.2534(4) 0.0326(15) Uani 1 1 d . . .
H9 H 0.8344 0.9987 0.2949 0.039 Uiso 1 1 calc R . .
C10 C 0.7966(6) 1.1236(9) 0.1954(4) 0.0385(17) Uani 1 1 d . . .
H10 H 0.8794 1.1463 0.1987 0.046 Uiso 1 1 calc R . .
C11 C 0.7002(6) 1.1749(7) 0.1321(4) 0.0336(16) Uani 1 1 d . . .
H11 H 0.7172 1.2319 0.0922 0.040 Uiso 1 1 calc R . .
C12 C 0.5768(5) 1.1401(6) 0.1286(4) 0.0234(13) Uani 1 1 d . . .
C13 C 0.4693(5) 1.1671(7) 0.0589(4) 0.0237(13) Uani 1 1 d . . .
C14 C 0.4803(6) 1.2345(8) -0.0090(4) 0.0378(17) Uani 1 1 d . . .
H14 H 0.5570 1.2752 -0.0100 0.045 Uiso 1 1 calc R . .
C15 C 0.3785(7) 1.2414(8) -0.0747(4) 0.0399(18) Uani 1 1 d . . .
H15 H 0.3861 1.2847 -0.1207 0.048 Uiso 1 1 calc R . .
C16 C 0.2656(6) 1.1845(7) -0.0724(4) 0.0317(15) Uani 1 1 d . . .
H16 H 0.1948 1.1893 -0.1161 0.038 Uiso 1 1 calc R . .
C17 C 0.2602(6) 1.1194(7) -0.0027(4) 0.0279(14) Uani 1 1 d . . .
H17 H 0.1838 1.0794 -0.0010 0.034 Uiso 1 1 calc R . .


_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 O4 2.274(4) 2_545 ?
Tb1 O6 2.292(4) 3_676 ?
Tb1 O5 2.374(4) 4_585 ?
Tb1 O1 2.398(3) . ?
Tb1 O1W 2.443(4) . ?
Tb1 O2 2.475(4) 2_545 ?
Tb1 N2 2.569(4) . ?
Tb1 N1 2.586(4) . ?
S1 O3 1.454(4) . ?
S1 O2 1.455(4) . ?
S1 O1 1.455(3) . ?
S1 C1 1.753(5) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2 Tb1 2.475(4) 2 ?
O4 C2 1.318(6) . ?
O4 Tb1 2.274(4) 2 ?
O5 C7 1.259(6) . ?
O5 Tb1 2.374(4) 4_686 ?
O6 C7 1.257(6) . ?
O6 Tb1 2.292(4) 3_676 ?
N1 C8 1.332(8) . ?
N1 C12 1.354(7) . ?
N2 C17 1.326(8) . ?
N2 C13 1.354(6) . ?
C1 C6 1.385(7) . ?
C1 C2 1.407(7) . ?
C2 C3 1.406(7) . ?
C3 C4 1.385(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(7) . ?
C4 C7 1.511(7) . ?
C5 C6 1.387(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.371(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.364(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.463(8) . ?
C13 C14 1.384(8) . ?
C14 C15 1.366(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.365(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Tb1 O6 108.48(14) 2_545 3_676 ?
O4 Tb1 O5 79.57(14) 2_545 4_585 ?
O6 Tb1 O5 142.24(12) 3_676 4_585 ?
O4 Tb1 O1 87.40(13) 2_545 . ?
O6 Tb1 O1 73.23(13) 3_676 . ?
O5 Tb1 O1 70.32(13) 4_585 . ?
O4 Tb1 O1W 158.83(13) 2_545 . ?
O6 Tb1 O1W 82.38(14) 3_676 . ?
O5 Tb1 O1W 80.96(14) 4_585 . ?
O1 Tb1 O1W 78.27(13) . . ?
O4 Tb1 O2 72.35(12) 2_545 2_545 ?
O6 Tb1 O2 71.39(13) 3_676 2_545 ?
O5 Tb1 O2 142.96(13) 4_585 2_545 ?
O1 Tb1 O2 130.35(12) . 2_545 ?
O1W Tb1 O2 128.81(13) . 2_545 ?
O4 Tb1 N2 85.75(14) 2_545 . ?
O6 Tb1 N2 143.83(13) 3_676 . ?
O5 Tb1 N2 71.76(13) 4_585 . ?
O1 Tb1 N2 142.08(14) . . ?
O1W Tb1 N2 95.99(14) . . ?
O2 Tb1 N2 82.36(13) 2_545 . ?
O4 Tb1 N1 130.61(13) 2_545 . ?
O6 Tb1 N1 84.85(14) 3_676 . ?
O5 Tb1 N1 118.57(14) 4_585 . ?
O1 Tb1 N1 141.07(14) . . ?
O1W Tb1 N1 67.03(13) . . ?
O2 Tb1 N1 67.49(13) 2_545 . ?
N2 Tb1 N1 61.87(15) . . ?
O3 S1 O2 112.3(2) . . ?
O3 S1 O1 111.6(2) . . ?
O2 S1 O1 111.3(2) . . ?
O3 S1 C1 108.2(2) . . ?
O2 S1 C1 104.6(2) . . ?
O1 S1 C1 108.5(2) . . ?
Tb1 O1W H1W1 93(4) . . ?
Tb1 O1W H1W2 123(4) . . ?
H1W1 O1W H1W2 110.1(18) . . ?
S1 O1 Tb1 165.3(3) . . ?
S1 O2 Tb1 126.86(19) . 2 ?
C2 O4 Tb1 136.6(3) . 2 ?
C7 O5 Tb1 150.4(3) . 4_686 ?
C7 O6 Tb1 154.5(4) . 3_676 ?
C8 N1 C12 118.5(5) . . ?
C8 N1 Tb1 120.4(4) . . ?
C12 N1 Tb1 121.0(4) . . ?
C17 N2 C13 118.1(5) . . ?
C17 N2 Tb1 119.8(3) . . ?
C13 N2 Tb1 121.1(4) . . ?
C6 C1 C2 122.1(5) . . ?
C6 C1 S1 119.9(4) . . ?
C2 C1 S1 118.1(4) . . ?
O4 C2 C3 121.7(5) . . ?
O4 C2 C1 122.6(5) . . ?
C3 C2 C1 115.6(5) . . ?
C4 C3 C2 122.7(5) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 119.9(5) . . ?
C3 C4 C7 120.4(5) . . ?
C5 C4 C7 119.5(5) . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 120.6(5) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
O6 C7 O5 125.3(5) . . ?
O6 C7 C4 116.6(4) . . ?
O5 C7 C4 118.1(5) . . ?
N1 C8 C9 123.4(6) . . ?
N1 C8 H8 118.3 . . ?
C9 C8 H8 118.3 . . ?
C10 C9 C8 118.5(6) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C9 C10 C11 119.7(6) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 119.1(6) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
N1 C12 C11 120.6(6) . . ?
N1 C12 C13 115.8(5) . . ?
C11 C12 C13 123.4(5) . . ?
N2 C13 C14 120.6(6) . . ?
N2 C13 C12 116.2(5) . . ?
C14 C13 C12 123.0(5) . . ?
C15 C14 C13 120.0(6) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 119.7(6) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 117.6(6) . . ?
C15 C16 H16 121.2 . . ?
C17 C16 H16 121.2 . . ?
N2 C17 C16 123.9(6) . . ?
N2 C17 H17 118.0 . . ?
C16 C17 H17 118.0 . . ?

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
O3 S1 O1 Tb1 -112.2(10) . . . . ?
O2 S1 O1 Tb1 121.6(10) . . . . ?
C1 S1 O1 Tb1 7.0(11) . . . . ?
O4 Tb1 O1 S1 140.1(10) 2_545 . . . ?
O6 Tb1 O1 S1 29.9(10) 3_676 . . . ?
O5 Tb1 O1 S1 -140.0(10) 4_585 . . . ?
O1W Tb1 O1 S1 -55.5(10) . . . . ?
O2 Tb1 O1 S1 76.0(10) 2_545 . . . ?
N2 Tb1 O1 S1 -140.2(9) . . . . ?
N1 Tb1 O1 S1 -28.6(11) . . . . ?
O3 S1 O2 Tb1 -177.6(2) . . . 2 ?
O1 S1 O2 Tb1 -51.6(3) . . . 2 ?
C1 S1 O2 Tb1 65.3(3) . . . 2 ?
O4 Tb1 N1 C8 -112.8(4) 2_545 . . . ?
O6 Tb1 N1 C8 -2.8(4) 3_676 . . . ?
O5 Tb1 N1 C8 145.9(4) 4_585 . . . ?
O1 Tb1 N1 C8 52.3(5) . . . . ?
O1W Tb1 N1 C8 81.1(4) . . . . ?
O2 Tb1 N1 C8 -74.8(4) 2_545 . . . ?
N2 Tb1 N1 C8 -168.1(5) . . . . ?
O4 Tb1 N1 C12 71.5(4) 2_545 . . . ?
O6 Tb1 N1 C12 -178.5(4) 3_676 . . . ?
O5 Tb1 N1 C12 -29.7(4) 4_585 . . . ?
O1 Tb1 N1 C12 -123.4(4) . . . . ?
O1W Tb1 N1 C12 -94.6(4) . . . . ?
O2 Tb1 N1 C12 109.6(4) 2_545 . . . ?
N2 Tb1 N1 C12 16.2(4) . . . . ?
O4 Tb1 N2 C17 32.9(4) 2_545 . . . ?
O6 Tb1 N2 C17 148.9(4) 3_676 . . . ?
O5 Tb1 N2 C17 -47.5(4) 4_585 . . . ?
O1 Tb1 N2 C17 -47.3(5) . . . . ?
O1W Tb1 N2 C17 -125.9(4) . . . . ?
O2 Tb1 N2 C17 105.7(4) 2_545 . . . ?
N1 Tb1 N2 C17 174.2(5) . . . . ?
O4 Tb1 N2 C13 -158.6(4) 2_545 . . . ?
O6 Tb1 N2 C13 -42.7(5) 3_676 . . . ?
O5 Tb1 N2 C13 121.0(4) 4_585 . . . ?
O1 Tb1 N2 C13 121.1(4) . . . . ?
O1W Tb1 N2 C13 42.6(4) . . . . ?
O2 Tb1 N2 C13 -85.9(4) 2_545 . . . ?
N1 Tb1 N2 C13 -17.4(4) . . . . ?
O3 S1 C1 C6 10.5(5) . . . . ?
O2 S1 C1 C6 130.4(4) . . . . ?
O1 S1 C1 C6 -110.8(4) . . . . ?
O3 S1 C1 C2 -168.0(4) . . . . ?
O2 S1 C1 C2 -48.1(4) . . . . ?
O1 S1 C1 C2 70.7(4) . . . . ?
Tb1 O4 C2 C3 -130.3(5) 2 . . . ?
Tb1 O4 C2 C1 51.2(7) 2 . . . ?
C6 C1 C2 O4 178.8(4) . . . . ?
S1 C1 C2 O4 -2.7(7) . . . . ?
C6 C1 C2 C3 0.2(7) . . . . ?
S1 C1 C2 C3 178.7(3) . . . . ?
O4 C2 C3 C4 -177.0(4) . . . . ?
C1 C2 C3 C4 1.6(7) . . . . ?
C2 C3 C4 C5 -2.1(7) . . . . ?
C2 C3 C4 C7 174.4(4) . . . . ?
C3 C4 C5 C6 0.5(7) . . . . ?
C7 C4 C5 C6 -176.0(4) . . . . ?
C2 C1 C6 C5 -1.7(8) . . . . ?
S1 C1 C6 C5 179.9(4) . . . . ?
C4 C5 C6 C1 1.3(8) . . . . ?
Tb1 O6 C7 O5 -10.4(11) 3_676 . . . ?
Tb1 O6 C7 C4 169.6(5) 3_676 . . . ?
Tb1 O5 C7 O6 -46.7(10) 4_686 . . . ?
Tb1 O5 C7 C4 133.2(6) 4_686 . . . ?
C3 C4 C7 O6 165.2(4) . . . . ?
C5 C4 C7 O6 -18.3(7) . . . . ?
C3 C4 C7 O5 -14.7(7) . . . . ?
C5 C4 C7 O5 161.8(4) . . . . ?
C12 N1 C8 C9 1.2(9) . . . . ?
Tb1 N1 C8 C9 -174.6(5) . . . . ?
N1 C8 C9 C10 3.3(10) . . . . ?
C8 C9 C10 C11 -3.9(10) . . . . ?
C9 C10 C11 C12 0.3(10) . . . . ?
C8 N1 C12 C11 -5.0(8) . . . . ?
Tb1 N1 C12 C11 170.8(4) . . . . ?
C8 N1 C12 C13 169.9(5) . . . . ?
Tb1 N1 C12 C13 -14.4(6) . . . . ?
C10 C11 C12 N1 4.3(9) . . . . ?
C10 C11 C12 C13 -170.1(6) . . . . ?
C17 N2 C13 C14 1.3(8) . . . . ?
Tb1 N2 C13 C14 -167.3(4) . . . . ?
C17 N2 C13 C12 -173.7(5) . . . . ?
Tb1 N2 C13 C12 17.6(6) . . . . ?
N1 C12 C13 N2 -2.0(7) . . . . ?
C11 C12 C13 N2 172.7(5) . . . . ?
N1 C12 C13 C14 -176.9(6) . . . . ?
C11 C12 C13 C14 -2.2(9) . . . . ?
N2 C13 C14 C15 -1.6(10) . . . . ?
C12 C13 C14 C15 173.1(6) . . . . ?
C13 C14 C15 C16 1.4(10) . . . . ?
C14 C15 C16 C17 -0.9(10) . . . . ?
C13 N2 C17 C16 -0.9(9) . . . . ?
Tb1 N2 C17 C16 167.9(4) . . . . ?
C15 C16 C17 N2 0.7(9) . . . . ?

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
O1W H1W1 O3 0.85(5) 2.12(3) 2.918(5) 157(6) 2
O1W H1W1 O1 0.85(5) 2.61(4) 3.128(6) 120(4) 2
O1W H1W2 O4 0.85(5) 1.925(15) 2.763(5) 170(6) .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.375
_refine_diff_density_min         -2.502
_refine_diff_density_rms         0.175
####################################################################### 
# 
# 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_2-Sm
_database_code_depnum_ccdc_archive 'CCDC 1549841'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 O28 S2 Sm2, 2(C7 H5 O6 S), 8(H2 O)'
_chemical_formula_sum            'C30 H60 O48 S4 Sm2'
_chemical_formula_weight         1617.72

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9111(5)
_cell_length_b                   12.3804(6)
_cell_length_c                   15.0892(9)
_cell_angle_alpha                107.252(5)
_cell_angle_beta                 96.881(5)
_cell_angle_gamma                96.565(5)
_cell_volume                     1383.61(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3445
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8258
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6315
_reflns_number_gt                5462
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0494P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6315
_refine_ls_number_parameters     439
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.0984
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.035
_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
Sm1 Sm 0.79629(3) 0.706307(19) 0.518998(15) 0.01867(9) Uani 1 1 d . . .
S1 S 0.74189(16) 0.64613(10) 0.74842(8) 0.0224(2) Uani 1 1 d . . .
S2 S 0.56336(18) 1.13718(11) 0.76880(9) 0.0309(3) Uani 1 1 d . . .
O1 O 0.7909(4) 0.6980(3) 0.6783(2) 0.0276(8) Uani 1 1 d . . .
O1W O 1.0594(5) 0.6465(4) 0.5679(3) 0.0387(10) Uani 1 1 d D . .
H1W1 H 1.096(7) 0.667(5) 0.6265(9) 0.058 Uiso 1 1 d D . .
H1W2 H 1.118(7) 0.598(4) 0.539(3) 0.058 Uiso 1 1 d D . .
O2 O 0.5626(4) 0.5912(3) 0.7265(2) 0.0315(8) Uani 1 1 d . . .
O2W O 0.9503(5) 0.6267(4) 0.3881(2) 0.0387(10) Uani 1 1 d D . .
H2W1 H 0.898(6) 0.609(6) 0.3324(16) 0.058 Uiso 1 1 d D . .
H2W2 H 1.053(3) 0.658(5) 0.393(4) 0.058 Uiso 1 1 d D . .
O3W O 0.6017(5) 0.6469(3) 0.3630(2) 0.0334(8) Uani 1 1 d D . .
H3W1 H 0.553(7) 0.5794(17) 0.332(3) 0.050 Uiso 1 1 d D . .
H3W2 H 0.578(7) 0.693(3) 0.333(3) 0.050 Uiso 1 1 d D . .
O3 O 0.8607(5) 0.5714(3) 0.7670(2) 0.0309(8) Uani 1 1 d . . .
O4 O 0.5634(5) 0.8505(3) 0.7805(2) 0.0282(8) Uani 1 1 d D . .
H4O H 0.544(7) 0.9190(19) 0.793(4) 0.042 Uiso 1 1 d D . .
O4W O 0.8656(6) 0.8505(3) 0.4437(3) 0.0394(10) Uani 1 1 d D . .
H4W1 H 0.884(8) 0.836(5) 0.3873(17) 0.059 Uiso 1 1 d D . .
H4W2 H 0.842(8) 0.918(2) 0.463(4) 0.059 Uiso 1 1 d D . .
O5 O 0.7431(5) 1.1220(3) 1.1047(2) 0.0352(9) Uani 1 1 d D . .
H5O H 0.751(8) 1.182(3) 1.151(3) 0.053 Uiso 1 1 d D . .
O5W O 0.6342(5) 0.8667(3) 0.5941(3) 0.0335(8) Uani 1 1 d D . .
H5W1 H 0.690(7) 0.933(2) 0.624(3) 0.050 Uiso 1 1 d D . .
H5W2 H 0.591(7) 0.838(4) 0.632(3) 0.050 Uiso 1 1 d D . .
O6W O 0.9940(5) 0.8768(3) 0.6284(3) 0.0381(9) Uani 1 1 d D . .
H6W1 H 1.020(6) 0.896(6) 0.6878(8) 0.057 Uiso 1 1 d D . .
H6W2 H 1.081(5) 0.897(5) 0.605(3) 0.057 Uiso 1 1 d D . .
O6 O 0.9242(5) 1.0410(3) 1.1803(3) 0.0408(10) Uani 1 1 d . . .
O7 O 0.4733(7) 1.1717(4) 0.6960(3) 0.0644(15) Uani 1 1 d . . .
O7W O 1.2735(5) 0.7503(4) 0.4230(3) 0.0437(10) Uani 1 1 d D . .
H7W1 H 1.330(7) 0.713(5) 0.452(4) 0.066 Uiso 1 1 d D . .
H7W2 H 1.324(7) 0.760(6) 0.379(3) 0.066 Uiso 1 1 d D . .
O8 O 0.4549(5) 1.0537(3) 0.7966(3) 0.0379(9) Uani 1 1 d . . .
O8W O 1.2687(6) 0.9565(4) 0.5501(4) 0.0567(13) Uani 1 1 d D . .
H8W1 H 1.366(5) 0.976(6) 0.586(4) 0.085 Uiso 1 1 d D . .
H8W2 H 1.271(8) 0.896(4) 0.505(4) 0.085 Uiso 1 1 d D . .
O9 O 0.7228(6) 1.0980(4) 0.7431(3) 0.0550(12) Uani 1 1 d . . .
O9W O 0.9317(5) 1.8283(3) 1.2556(3) 0.0452(10) Uani 1 1 d . . .
H9W1 H 1.0410 1.8360 1.2618 0.068 Uiso 1 1 d R . .
H9W2 H 0.8997 1.8807 1.2348 0.068 Uiso 1 1 d R . .
O10 O 0.7612(6) 1.3612(3) 0.7814(3) 0.0422(10) Uani 1 1 d D . .
H10O H 0.791(9) 1.429(2) 0.782(5) 0.063 Uiso 1 1 d D . .
O10W O 0.7725(5) 1.3168(3) 1.2499(2) 0.0352(9) Uani 1 1 d . . .
HAW H 0.6714 1.3232 1.2623 0.053 Uiso 1 1 d R . .
HBW H 0.8074 1.3730 1.2317 0.053 Uiso 1 1 d R . .
O11 O 0.8278(6) 1.6420(3) 1.1052(3) 0.0496(12) Uani 1 1 d D . .
H11O H 0.869(9) 1.696(4) 1.155(3) 0.074 Uiso 1 1 d D . .
O12 O 0.7824(6) 1.5337(4) 1.1965(3) 0.0479(11) Uani 1 1 d . . .
O13 O 0.7159(4) 0.5022(3) 0.4866(2) 0.0268(8) Uani 1 1 d . . .
O14 O 0.5108(4) 0.3543(3) 0.4705(2) 0.0251(7) Uani 1 1 d . . .
C1 C 0.7642(6) 0.7622(4) 0.8545(3) 0.0210(9) Uani 1 1 d . . .
C2 C 0.6714(6) 0.8533(4) 0.8586(3) 0.0217(10) Uani 1 1 d . . .
C3 C 0.6931(6) 0.9427(4) 0.9417(3) 0.0253(10) Uani 1 1 d . . .
H3 H 0.6316 1.0031 0.9454 0.030 Uiso 1 1 calc R . .
C4 C 0.8061(6) 0.9432(4) 1.0200(3) 0.0245(10) Uani 1 1 d . . .
C5 C 0.8990(6) 0.8534(4) 1.0151(3) 0.0265(11) Uani 1 1 d . . .
H5A H 0.9749 0.8536 1.0672 0.032 Uiso 1 1 calc R . .
C6 C 0.8779(6) 0.7644(4) 0.9325(3) 0.0253(10) Uani 1 1 d . . .
H6 H 0.9409 0.7047 0.9290 0.030 Uiso 1 1 calc R . .
C7 C 0.8309(6) 1.0393(4) 1.1095(3) 0.0276(11) Uani 1 1 d . . .
C8 C 0.6225(6) 1.2599(4) 0.8700(3) 0.0259(10) Uani 1 1 d . . .
C9 C 0.7162(7) 1.3601(4) 0.8648(3) 0.0280(11) Uani 1 1 d . . .
C10 C 0.7641(7) 1.4539(5) 0.9460(3) 0.0320(12) Uani 1 1 d . . .
H10A H 0.8274 1.5208 0.9437 0.038 Uiso 1 1 calc R . .
C11 C 0.7173(6) 1.4478(4) 1.0307(3) 0.0271(11) Uani 1 1 d . . .
C12 C 0.6205(7) 1.3492(5) 1.0348(4) 0.0356(13) Uani 1 1 d . . .
H12 H 0.5875 1.3460 1.0912 0.043 Uiso 1 1 calc R . .
C13 C 0.5735(7) 1.2559(5) 0.9544(4) 0.0324(12) Uani 1 1 d . . .
H13 H 0.5082 1.1898 0.9569 0.039 Uiso 1 1 calc R . .
C14 C 0.7777(7) 1.5455(5) 1.1193(4) 0.0309(11) Uani 1 1 d . . .
C15 C 0.5644(6) 0.4581(4) 0.4869(3) 0.0203(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
Sm1 O1W 2.394(4) . ?
Sm1 O13 2.420(3) . ?
Sm1 O4W 2.430(4) . ?
Sm1 O1 2.441(3) . ?
Sm1 O2W 2.460(4) . ?
Sm1 O6W 2.487(3) . ?
Sm1 O14 2.497(3) 2_666 ?
Sm1 O3W 2.509(3) . ?
Sm1 O5W 2.543(4) . ?
S1 O3 1.452(4) . ?
S1 O2 1.455(4) . ?
S1 O1 1.458(3) . ?
S1 C1 1.780(5) . ?
S2 O7 1.435(4) . ?
S2 O8 1.456(4) . ?
S2 O9 1.457(4) . ?
S2 C8 1.774(5) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2W H2W1 0.85(5) . ?
O2W H2W2 0.85(5) . ?
O3W H3W1 0.85(5) . ?
O3W H3W2 0.85(5) . ?
O4 C2 1.359(5) . ?
O4 H4O 0.85(5) . ?
O4W H4W1 0.85(5) . ?
O4W H4W2 0.85(5) . ?
O5 C7 1.315(6) . ?
O5 H5O 0.85(5) . ?
O5W H5W1 0.85(5) . ?
O5W H5W2 0.85(5) . ?
O6W H6W1 0.85(5) . ?
O6W H6W2 0.85(5) . ?
O6 C7 1.217(6) . ?
O7W H7W1 0.85(5) . ?
O7W H7W2 0.85(5) . ?
O8W H8W1 0.85(5) . ?
O8W H8W2 0.85(5) . ?
O9W H9W1 0.8500 . ?
O9W H9W2 0.8501 . ?
O10 C9 1.352(6) . ?
O10 H10O 0.85(5) . ?
O10W HAW 0.8500 . ?
O10W HBW 0.8500 . ?
O11 C14 1.302(7) . ?
O11 H11O 0.85(5) . ?
O12 C14 1.212(6) . ?
O13 C15 1.259(5) . ?
O14 C15 1.247(5) . ?
O14 Sm1 2.497(3) 2_666 ?
C1 C6 1.385(7) . ?
C1 C2 1.405(7) . ?
C2 C3 1.381(6) . ?
C3 C4 1.392(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(7) . ?
C4 C7 1.485(6) . ?
C5 C6 1.375(7) . ?
C5 H5A 0.9300 . ?
C6 H6 0.9300 . ?
C8 C13 1.389(7) . ?
C8 C9 1.398(7) . ?
C9 C10 1.392(7) . ?
C10 C11 1.393(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.386(7) . ?
C11 C14 1.495(7) . ?
C12 C13 1.380(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C15 C15 1.539(9) 2_666 ?

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
O1W Sm1 O13 76.45(13) . . ?
O1W Sm1 O4W 108.04(15) . . ?
O13 Sm1 O4W 142.48(12) . . ?
O1W Sm1 O1 72.72(12) . . ?
O13 Sm1 O1 79.67(12) . . ?
O4W Sm1 O1 137.76(12) . . ?
O1W Sm1 O2W 66.89(13) . . ?
O13 Sm1 O2W 77.80(13) . . ?
O4W Sm1 O2W 70.71(14) . . ?
O1 Sm1 O2W 137.20(13) . . ?
O1W Sm1 O6W 71.47(14) . . ?
O13 Sm1 O6W 142.42(13) . . ?
O4W Sm1 O6W 68.24(13) . . ?
O1 Sm1 O6W 72.59(12) . . ?
O2W Sm1 O6W 106.17(14) . . ?
O1W Sm1 O14 132.46(14) . 2_666 ?
O13 Sm1 O14 65.69(10) . 2_666 ?
O4W Sm1 O14 119.49(13) . 2_666 ?
O1 Sm1 O14 73.11(11) . 2_666 ?
O2W Sm1 O14 126.98(12) . 2_666 ?
O6W Sm1 O14 126.35(12) . 2_666 ?
O1W Sm1 O3W 131.55(13) . . ?
O13 Sm1 O3W 77.15(12) . . ?
O4W Sm1 O3W 72.65(13) . . ?
O1 Sm1 O3W 139.43(12) . . ?
O2W Sm1 O3W 68.26(13) . . ?
O6W Sm1 O3W 139.76(13) . . ?
O14 Sm1 O3W 67.12(12) 2_666 . ?
O1W Sm1 O5W 134.11(13) . . ?
O13 Sm1 O5W 128.55(11) . . ?
O4W Sm1 O5W 75.83(13) . . ?
O1 Sm1 O5W 75.43(12) . . ?
O2W Sm1 O5W 145.43(14) . . ?
O6W Sm1 O5W 67.99(13) . . ?
O14 Sm1 O5W 64.25(11) 2_666 . ?
O3W Sm1 O5W 93.87(13) . . ?
O3 S1 O2 113.0(2) . . ?
O3 S1 O1 112.0(2) . . ?
O2 S1 O1 112.6(2) . . ?
O3 S1 C1 106.1(2) . . ?
O2 S1 C1 107.2(2) . . ?
O1 S1 C1 105.3(2) . . ?
O7 S2 O8 112.5(3) . . ?
O7 S2 O9 111.2(3) . . ?
O8 S2 O9 112.3(3) . . ?
O7 S2 C8 107.5(2) . . ?
O8 S2 C8 106.0(2) . . ?
O9 S2 C8 106.8(2) . . ?
S1 O1 Sm1 154.9(2) . . ?
Sm1 O1W H1W1 117(3) . . ?
Sm1 O1W H1W2 132(3) . . ?
H1W1 O1W H1W2 109.3(18) . . ?
Sm1 O2W H2W1 119(4) . . ?
Sm1 O2W H2W2 117(4) . . ?
H2W1 O2W H2W2 110.9(18) . . ?
Sm1 O3W H3W1 126(3) . . ?
Sm1 O3W H3W2 124(3) . . ?
H3W1 O3W H3W2 110.3(18) . . ?
C2 O4 H4O 103(4) . . ?
Sm1 O4W H4W1 124(4) . . ?
Sm1 O4W H4W2 123(4) . . ?
H4W1 O4W H4W2 109.4(18) . . ?
C7 O5 H5O 121(5) . . ?
Sm1 O5W H5W1 119(4) . . ?
Sm1 O5W H5W2 98(4) . . ?
H5W1 O5W H5W2 109.5(18) . . ?
Sm1 O6W H6W1 129(4) . . ?
Sm1 O6W H6W2 113(4) . . ?
H6W1 O6W H6W2 109.4(18) . . ?
H7W1 O7W H7W2 109.8(18) . . ?
H8W1 O8W H8W2 109.5(18) . . ?
H9W1 O9W H9W2 107.8 . . ?
C9 O10 H10O 111(5) . . ?
HAW O10W HBW 107.7 . . ?
C14 O11 H11O 113(5) . . ?
C15 O13 Sm1 121.8(3) . . ?
C15 O14 Sm1 118.9(3) . 2_666 ?
C6 C1 C2 119.8(4) . . ?
C6 C1 S1 119.7(4) . . ?
C2 C1 S1 120.4(4) . . ?
O4 C2 C3 122.3(4) . . ?
O4 C2 C1 118.8(4) . . ?
C3 C2 C1 118.9(4) . . ?
C2 C3 C4 120.7(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 C7 119.0(4) . . ?
C3 C4 C7 121.0(5) . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C1 121.0(5) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O6 C7 O5 123.5(5) . . ?
O6 C7 C4 122.8(5) . . ?
O5 C7 C4 113.7(4) . . ?
C13 C8 C9 120.1(5) . . ?
C13 C8 S2 119.4(4) . . ?
C9 C8 S2 120.5(4) . . ?
O10 C9 C10 122.3(5) . . ?
O10 C9 C8 118.6(5) . . ?
C10 C9 C8 119.1(5) . . ?
C9 C10 C11 120.1(5) . . ?
C9 C10 H10A 119.9 . . ?
C11 C10 H10A 119.9 . . ?
C12 C11 C10 120.5(5) . . ?
C12 C11 C14 119.1(5) . . ?
C10 C11 C14 120.4(5) . . ?
C13 C12 C11 119.5(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C8 120.7(5) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
O12 C14 O11 124.0(5) . . ?
O12 C14 C11 122.3(5) . . ?
O11 C14 C11 113.6(5) . . ?
O14 C15 O13 126.4(4) . . ?
O14 C15 C15 117.3(5) . 2_666 ?
O13 C15 C15 116.2(5) . 2_666 ?

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
O3 S1 O1 Sm1 87.2(5) . . . . ?
O2 S1 O1 Sm1 -41.4(6) . . . . ?
C1 S1 O1 Sm1 -157.9(5) . . . . ?
O1W Sm1 O1 S1 -99.2(5) . . . . ?
O13 Sm1 O1 S1 -20.3(5) . . . . ?
O4W Sm1 O1 S1 162.8(5) . . . . ?
O2W Sm1 O1 S1 -79.4(6) . . . . ?
O6W Sm1 O1 S1 -174.7(5) . . . . ?
O14 Sm1 O1 S1 47.2(5) 2_666 . . . ?
O3W Sm1 O1 S1 35.6(6) . . . . ?
O5W Sm1 O1 S1 114.3(5) . . . . ?
O1W Sm1 O13 C15 152.3(4) . . . . ?
O4W Sm1 O13 C15 -105.6(4) . . . . ?
O1 Sm1 O13 C15 77.8(4) . . . . ?
O2W Sm1 O13 C15 -138.8(4) . . . . ?
O6W Sm1 O13 C15 120.4(4) . . . . ?
O14 Sm1 O13 C15 1.8(3) 2_666 . . . ?
O3W Sm1 O13 C15 -68.7(4) . . . . ?
O5W Sm1 O13 C15 16.0(4) . . . . ?
O3 S1 C1 C6 -0.9(4) . . . . ?
O2 S1 C1 C6 120.1(4) . . . . ?
O1 S1 C1 C6 -119.8(4) . . . . ?
O3 S1 C1 C2 177.1(4) . . . . ?
O2 S1 C1 C2 -62.0(4) . . . . ?
O1 S1 C1 C2 58.2(4) . . . . ?
C6 C1 C2 O4 178.6(4) . . . . ?
S1 C1 C2 O4 0.7(6) . . . . ?
C6 C1 C2 C3 -1.4(7) . . . . ?
S1 C1 C2 C3 -179.3(4) . . . . ?
O4 C2 C3 C4 -179.4(4) . . . . ?
C1 C2 C3 C4 0.6(7) . . . . ?
C2 C3 C4 C5 0.2(7) . . . . ?
C2 C3 C4 C7 179.6(4) . . . . ?
C3 C4 C5 C6 -0.2(7) . . . . ?
C7 C4 C5 C6 -179.6(4) . . . . ?
C4 C5 C6 C1 -0.7(7) . . . . ?
C2 C1 C6 C5 1.4(7) . . . . ?
S1 C1 C6 C5 179.4(4) . . . . ?
C5 C4 C7 O6 -3.0(7) . . . . ?
C3 C4 C7 O6 177.5(5) . . . . ?
C5 C4 C7 O5 176.8(4) . . . . ?
C3 C4 C7 O5 -2.6(7) . . . . ?
O7 S2 C8 C13 125.2(5) . . . . ?
O8 S2 C8 C13 4.6(5) . . . . ?
O9 S2 C8 C13 -115.3(5) . . . . ?
O7 S2 C8 C9 -54.1(5) . . . . ?
O8 S2 C8 C9 -174.8(4) . . . . ?
O9 S2 C8 C9 65.3(5) . . . . ?
C13 C8 C9 O10 -179.7(5) . . . . ?
S2 C8 C9 O10 -0.3(7) . . . . ?
C13 C8 C9 C10 2.1(8) . . . . ?
S2 C8 C9 C10 -178.5(4) . . . . ?
O10 C9 C10 C11 -178.8(5) . . . . ?
C8 C9 C10 C11 -0.7(8) . . . . ?
C9 C10 C11 C12 -1.1(8) . . . . ?
C9 C10 C11 C14 176.1(5) . . . . ?
C10 C11 C12 C13 1.3(9) . . . . ?
C14 C11 C12 C13 -175.9(5) . . . . ?
C11 C12 C13 C8 0.2(9) . . . . ?
C9 C8 C13 C12 -1.9(8) . . . . ?
S2 C8 C13 C12 178.7(4) . . . . ?
C12 C11 C14 O12 18.2(8) . . . . ?
C10 C11 C14 O12 -159.1(6) . . . . ?
C12 C11 C14 O11 -163.5(5) . . . . ?
C10 C11 C14 O11 19.3(7) . . . . ?
Sm1 O14 C15 O13 178.2(4) 2_666 . . . ?
Sm1 O14 C15 C15 0.2(6) 2_666 . . 2_666 ?
Sm1 O13 C15 O14 179.4(3) . . . . ?
Sm1 O13 C15 C15 -2.5(7) . . . 2_666 ?

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
O1W H1W1 O10W 0.85(5) 1.964(19) 2.789(5) 164(5) 2_777
O1W H1W2 O13 0.85(5) 1.91(2) 2.726(5) 162(5) 2_766
O2W H2W1 O12 0.85(5) 2.034(18) 2.865(5) 168(7) 1_544
O2W H2W2 O7W 0.85(5) 1.896(16) 2.732(6) 169(6) .
O3W H3W1 O2 0.85(5) 2.083(12) 2.923(5) 172(5) 2_666
O3W H3W2 O7 0.85(5) 1.930(19) 2.749(6) 163(5) 2_676
O4 H4O O8 0.85(5) 1.874(19) 2.703(5) 166(6) .
O4W H4W1 O9W 0.85(5) 2.043(15) 2.886(5) 171(5) 1_544
O4W H4W2 O8W 0.85(5) 1.92(3) 2.705(6) 154(6) 2_776
O5 H5O O10W 0.85(5) 1.855(12) 2.699(5) 177(6) .
O5W H5W1 O9 0.85(5) 2.25(3) 3.014(5) 150(5) .
O5W H5W2 O4 0.85(5) 2.23(3) 2.993(5) 149(4) .
O5W H5W2 O1 0.85(5) 2.65(6) 3.050(5) 110(5) .
O6W H6W1 O6 0.85(5) 1.885(15) 2.730(5) 172(7) 2_777
O6W H6W2 O8W 0.85(5) 1.966(14) 2.812(6) 174(7) .
O7W H7W1 O14 0.85(5) 2.027(16) 2.873(5) 172(7) 2_766
O7W H7W2 O7 0.85(5) 2.29(3) 3.101(7) 160(7) 2_776
O7W H7W2 O10 0.85(5) 2.41(6) 2.946(6) 122(6) 2_776
O8W H8W1 O7 0.85(5) 2.48(5) 3.041(6) 124(5) 1_655
O8W H8W2 O7W 0.85(5) 1.87(2) 2.708(6) 169(8) .
O9W H9W1 O9 0.85 1.97 2.777(6) 157.9 2_787
O9W H9W2 O6 0.85 2.36 3.166(6) 158.4 1_565
O10 H10O O3 0.85(5) 1.866(14) 2.711(5) 173(7) 1_565
O10W HAW O2 0.85 2.23 3.021(5) 153.9 2_677
O10W HAW O4 0.85 2.54 3.073(5) 121.4 2_677
O10W HBW O12 0.85 2.23 3.020(6) 154.5 .
O10W HBW O3 0.85 2.63 3.142(5) 119.6 2_777
O11 H11O O9W 0.85(5) 1.839(18) 2.676(5) 170(8) .

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.157
####################################################################### 
# 
# 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_2-Gd
_database_code_depnum_ccdc_archive 'CCDC 1549843'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 Gd2 O28 S2, 2(C7 H5 O6 S), 8(H2 O)'
_chemical_formula_sum            'C30 H60 Gd2 O48 S4'
_chemical_formula_weight         1631.52

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9036(7)
_cell_length_b                   12.3541(8)
_cell_length_c                   15.0517(10)
_cell_angle_alpha                107.339(6)
_cell_angle_beta                 96.737(6)
_cell_angle_gamma                96.821(6)
_cell_volume                     1374.76(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4018
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5914
_exptl_absorpt_correction_T_max  0.7652
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9118
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.55
_reflns_number_total             6281
_reflns_number_gt                5664
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0250P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6281
_refine_ls_number_parameters     439
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0655
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.024
_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 0.204383(19) 0.294846(12) 0.481122(10) 0.01591(5) Uani 1 1 d . . .
S1 S 0.25841(11) 0.35449(7) 0.25251(5) 0.02020(17) Uani 1 1 d . . .
S2 S 0.43532(12) -0.13645(7) 0.23213(6) 0.0285(2) Uani 1 1 d . . .
O1W O 0.3981(3) 0.3525(2) 0.63606(16) 0.0294(6) Uani 1 1 d D . .
H1W1 H 0.449(5) 0.4196(13) 0.668(2) 0.044 Uiso 1 1 d D . .
H1W2 H 0.413(5) 0.307(2) 0.667(2) 0.044 Uiso 1 1 d D . .
O1 O 0.2102(3) 0.30202(19) 0.32260(15) 0.0259(5) Uani 1 1 d . . .
O2 O 0.1382(3) 0.4287(2) 0.23351(16) 0.0285(6) Uani 1 1 d . . .
O2W O 0.0524(3) 0.3745(2) 0.61137(17) 0.0336(6) Uani 1 1 d D . .
H2W1 H -0.050(2) 0.343(3) 0.607(2) 0.050 Uiso 1 1 d D . .
H2W2 H 0.101(4) 0.399(3) 0.6684(11) 0.050 Uiso 1 1 d D . .
O3W O -0.0571(3) 0.3534(2) 0.43213(17) 0.0338(6) Uani 1 1 d D . .
H3W1 H -0.111(4) 0.402(3) 0.4665(19) 0.051 Uiso 1 1 d D . .
H3W2 H -0.099(5) 0.341(3) 0.3746(9) 0.051 Uiso 1 1 d D . .
O3 O 0.4374(3) 0.4102(2) 0.27418(17) 0.0298(6) Uani 1 1 d . . .
O4 O 0.4374(3) 0.1500(2) 0.22038(15) 0.0255(5) Uani 1 1 d D . .
H4O H 0.475(5) 0.0868(18) 0.210(3) 0.038 Uiso 1 1 d D . .
O4W O 0.0067(3) 0.1253(2) 0.37213(17) 0.0333(6) Uani 1 1 d D . .
H4W1 H -0.080(3) 0.100(3) 0.393(2) 0.050 Uiso 1 1 d D . .
H4W2 H -0.024(4) 0.118(4) 0.3140(10) 0.050 Uiso 1 1 d D . .
O5 O 0.2580(3) -0.1220(2) -0.10426(17) 0.0341(6) Uani 1 1 d D . .
H5O H 0.243(6) -0.185(2) -0.148(2) 0.051 Uiso 1 1 d D . .
O5W O 0.3655(3) 0.1358(2) 0.40812(17) 0.0299(6) Uani 1 1 d D . .
H5W1 H 0.310(5) 0.0684(16) 0.385(2) 0.045 Uiso 1 1 d D . .
H5W2 H 0.410(5) 0.158(3) 0.3672(19) 0.045 Uiso 1 1 d D . .
O6 O 0.0755(4) -0.0411(2) -0.17991(17) 0.0395(7) Uani 1 1 d . . .
O6W O 0.1345(4) 0.1511(2) 0.55502(17) 0.0346(6) Uani 1 1 d D . .
H6W1 H 0.110(5) 0.172(3) 0.6105(14) 0.052 Uiso 1 1 d D . .
H6W2 H 0.190(5) 0.095(3) 0.548(2) 0.052 Uiso 1 1 d D . .
O7 O 0.2759(4) -0.0959(2) 0.2567(2) 0.0515(8) Uani 1 1 d . . .
O7W O -0.2721(3) 0.2509(2) 0.57665(18) 0.0391(7) Uani 1 1 d . . .
H7W1 H -0.3367 0.2271 0.6105 0.059 Uiso 1 1 d RD . .
H7W2 H -0.3314 0.2823 0.5435 0.059 Uiso 1 1 d RD . .
O8 O 0.5455(3) -0.0535(2) 0.20459(18) 0.0356(6) Uani 1 1 d . . .
O8W O -0.2656(4) 0.0426(3) 0.4502(2) 0.0551(9) Uani 1 1 d D . .
H8W1 H -0.275(5) 0.107(2) 0.490(3) 0.083 Uiso 1 1 d D . .
H8W2 H -0.366(3) 0.008(3) 0.423(3) 0.083 Uiso 1 1 d D . .
O9 O 0.5242(5) -0.1713(2) 0.3057(2) 0.0599(10) Uani 1 1 d . . .
O9W O 0.2275(3) -0.3168(2) -0.25046(16) 0.0332(6) Uani 1 1 d . . .
H9W1 H 0.3287 -0.3235 -0.2629 0.050 Uiso 1 1 d RD . .
H9W2 H 0.1920 -0.3730 -0.2321 0.050 Uiso 1 1 d RD . .
O10 O 0.2371(4) -0.3610(2) 0.21921(18) 0.0408(7) Uani 1 1 d D . .
H10O H 0.201(6) -0.4284(17) 0.219(3) 0.061 Uiso 1 1 d D . .
O10W O 0.0694(4) -0.8293(2) -0.2563(2) 0.0427(7) Uani 1 1 d D . .
HAW H -0.034(2) -0.853(4) -0.253(3) 0.064 Uiso 1 1 d D . .
HBW H 0.135(4) -0.873(3) -0.242(3) 0.064 Uiso 1 1 d D . .
O11 O 0.1712(5) -0.6430(2) -0.10527(19) 0.0484(8) Uani 1 1 d D . .
H11O H 0.132(6) -0.699(3) -0.155(2) 0.073 Uiso 1 1 d D . .
O12 O 0.2178(4) -0.5340(2) -0.19685(18) 0.0452(8) Uani 1 1 d . . .
O13 O 0.4892(3) 0.64558(18) 0.52984(15) 0.0219(5) Uani 1 1 d . . .
O14 O 0.2840(3) 0.49751(19) 0.51395(17) 0.0247(5) Uani 1 1 d . . .
C1 C 0.2363(4) 0.2383(3) 0.1465(2) 0.0203(7) Uani 1 1 d . . .
C2 C 0.3282(4) 0.1481(3) 0.1426(2) 0.0196(7) Uani 1 1 d . . .
C3 C 0.3066(4) 0.0570(3) 0.0589(2) 0.0217(7) Uani 1 1 d . . .
H3 H 0.3670 -0.0039 0.0555 0.026 Uiso 1 1 calc R . .
C4 C 0.1948(4) 0.0572(3) -0.0194(2) 0.0228(7) Uani 1 1 d . . .
C5 C 0.1013(4) 0.1464(3) -0.0149(2) 0.0257(7) Uani 1 1 d . . .
H5A H 0.0252 0.1453 -0.0673 0.031 Uiso 1 1 calc R . .
C6 C 0.1221(4) 0.2367(3) 0.0677(2) 0.0253(7) Uani 1 1 d . . .
H6 H 0.0600 0.2967 0.0710 0.030 Uiso 1 1 calc R . .
C7 C 0.1688(4) -0.0403(3) -0.1097(2) 0.0248(7) Uani 1 1 d . . .
C8 C 0.3775(4) -0.2595(3) 0.1308(2) 0.0249(7) Uani 1 1 d . . .
C9 C 0.2831(5) -0.3593(3) 0.1360(2) 0.0268(8) Uani 1 1 d . . .
C10 C 0.2362(5) -0.4539(3) 0.0543(2) 0.0293(8) Uani 1 1 d . . .
H10 H 0.1736 -0.5214 0.0567 0.035 Uiso 1 1 calc R . .
C11 C 0.2825(5) -0.4478(3) -0.0305(2) 0.0263(8) Uani 1 1 d . . .
C12 C 0.3795(5) -0.3495(3) -0.0345(2) 0.0329(9) Uani 1 1 d . . .
H12 H 0.4122 -0.3461 -0.0911 0.040 Uiso 1 1 calc R . .
C13 C 0.4278(5) -0.2560(3) 0.0464(3) 0.0321(8) Uani 1 1 d . . .
H13 H 0.4948 -0.1900 0.0442 0.039 Uiso 1 1 calc R . .
C14 C 0.2235(5) -0.5453(3) -0.1192(2) 0.0290(8) Uani 1 1 d . . .
C15 C 0.4340(4) 0.5413(3) 0.5128(2) 0.0177(6) 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 O3W 2.378(2) . ?
Gd1 O14 2.392(2) . ?
Gd1 O6W 2.406(3) . ?
Gd1 O1 2.420(2) . ?
Gd1 O2W 2.437(2) . ?
Gd1 O4W 2.468(2) . ?
Gd1 O13 2.485(2) 2_666 ?
Gd1 O1W 2.491(2) . ?
Gd1 O5W 2.516(2) . ?
S1 O3 1.452(2) . ?
S1 O1 1.456(2) . ?
S1 O2 1.457(3) . ?
S1 C1 1.774(3) . ?
S2 O9 1.442(3) . ?
S2 O8 1.451(3) . ?
S2 O7 1.458(3) . ?
S2 C8 1.770(3) . ?
O1W H1W1 0.85(3) . ?
O1W H1W2 0.85(3) . ?
O2W H2W1 0.85(3) . ?
O2W H2W2 0.85(3) . ?
O3W H3W1 0.85(3) . ?
O3W H3W2 0.85(3) . ?
O4 C2 1.363(4) . ?
O4 H4O 0.85(3) . ?
O4W H4W1 0.85(3) . ?
O4W H4W2 0.85(3) . ?
O5 C7 1.314(4) . ?
O5 H5O 0.85(3) . ?
O5W H5W1 0.85(3) . ?
O5W H5W2 0.85(3) . ?
O6 C7 1.212(4) . ?
O6W H6W1 0.85(3) . ?
O6W H6W2 0.85(3) . ?
O7W H7W1 0.8500 . ?
O7W H7W2 0.8500 . ?
O8W H8W1 0.85(3) . ?
O8W H8W2 0.85(3) . ?
O9W H9W1 0.8500 . ?
O9W H9W2 0.8501 . ?
O10 C9 1.350(4) . ?
O10 H10O 0.85(3) . ?
O10W HAW 0.85(3) . ?
O10W HBW 0.85(3) . ?
O11 C14 1.313(5) . ?
O11 H11O 0.85(3) . ?
O12 C14 1.214(4) . ?
O13 C15 1.248(4) . ?
O13 Gd1 2.485(2) 2_666 ?
O14 C15 1.248(4) . ?
C1 C2 1.392(5) . ?
C1 C6 1.397(5) . ?
C2 C3 1.393(4) . ?
C3 C4 1.388(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(5) . ?
C4 C7 1.497(4) . ?
C5 C6 1.378(5) . ?
C5 H5A 0.9300 . ?
C6 H6 0.9300 . ?
C8 C13 1.386(5) . ?
C8 C9 1.392(5) . ?
C9 C10 1.396(4) . ?
C10 C11 1.388(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(5) . ?
C11 C14 1.489(5) . ?
C12 C13 1.382(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C15 C15 1.547(6) 2_666 ?

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
O3W Gd1 O14 76.54(9) . . ?
O3W Gd1 O6W 107.91(10) . . ?
O14 Gd1 O6W 142.52(8) . . ?
O3W Gd1 O1 72.76(9) . . ?
O14 Gd1 O1 80.13(8) . . ?
O6W Gd1 O1 137.26(8) . . ?
O3W Gd1 O2W 67.05(9) . . ?
O14 Gd1 O2W 77.34(9) . . ?
O6W Gd1 O2W 71.06(9) . . ?
O1 Gd1 O2W 137.36(9) . . ?
O3W Gd1 O4W 71.06(9) . . ?
O14 Gd1 O4W 142.29(9) . . ?
O6W Gd1 O4W 68.10(9) . . ?
O1 Gd1 O4W 72.35(8) . . ?
O2W Gd1 O4W 106.25(9) . . ?
O3W Gd1 O13 132.76(9) . 2_666 ?
O14 Gd1 O13 66.24(7) . 2_666 ?
O6W Gd1 O13 119.32(9) . 2_666 ?
O1 Gd1 O13 73.10(8) . 2_666 ?
O2W Gd1 O13 127.05(8) . 2_666 ?
O4W Gd1 O13 126.20(8) . 2_666 ?
O3W Gd1 O1W 132.15(8) . . ?
O14 Gd1 O1W 77.57(8) . . ?
O6W Gd1 O1W 72.48(9) . . ?
O1 Gd1 O1W 139.62(9) . . ?
O2W Gd1 O1W 68.42(9) . . ?
O4W Gd1 O1W 139.43(9) . . ?
O13 Gd1 O1W 67.21(8) 2_666 . ?
O3W Gd1 O5W 134.42(8) . . ?
O14 Gd1 O5W 128.89(8) . . ?
O6W Gd1 O5W 75.28(9) . . ?
O1 Gd1 O5W 75.75(8) . . ?
O2W Gd1 O5W 145.05(9) . . ?
O4W Gd1 O5W 68.47(9) . . ?
O13 Gd1 O5W 63.86(8) 2_666 . ?
O1W Gd1 O5W 92.87(9) . . ?
O3 S1 O1 112.64(15) . . ?
O3 S1 O2 113.10(14) . . ?
O1 S1 O2 112.27(14) . . ?
O3 S1 C1 107.20(15) . . ?
O1 S1 C1 105.06(14) . . ?
O2 S1 C1 105.85(15) . . ?
O9 S2 O8 112.46(19) . . ?
O9 S2 O7 111.8(2) . . ?
O8 S2 O7 111.84(18) . . ?
O9 S2 C8 107.32(17) . . ?
O8 S2 C8 105.78(16) . . ?
O7 S2 C8 107.15(17) . . ?
Gd1 O1W H1W1 127(2) . . ?
Gd1 O1W H1W2 123(2) . . ?
H1W1 O1W H1W2 110.0(17) . . ?
S1 O1 Gd1 154.69(14) . . ?
Gd1 O2W H2W1 117(3) . . ?
Gd1 O2W H2W2 123(3) . . ?
H2W1 O2W H2W2 110.3(17) . . ?
Gd1 O3W H3W1 127(2) . . ?
Gd1 O3W H3W2 124(2) . . ?
H3W1 O3W H3W2 108.4(17) . . ?
C2 O4 H4O 109(3) . . ?
Gd1 O4W H4W1 117(3) . . ?
Gd1 O4W H4W2 123(3) . . ?
H4W1 O4W H4W2 108.7(17) . . ?
C7 O5 H5O 121(3) . . ?
Gd1 O5W H5W1 118(3) . . ?
Gd1 O5W H5W2 103(3) . . ?
H5W1 O5W H5W2 111.7(17) . . ?
Gd1 O6W H6W1 119(3) . . ?
Gd1 O6W H6W2 120(3) . . ?
H6W1 O6W H6W2 109.9(17) . . ?
H7W1 O7W H7W2 108.3 . . ?
H8W1 O8W H8W2 108.5(17) . . ?
H9W1 O9W H9W2 107.7 . . ?
C9 O10 H10O 113(3) . . ?
HAW O10W HBW 109.2(17) . . ?
C14 O11 H11O 115(4) . . ?
C15 O13 Gd1 118.9(2) . 2_666 ?
C15 O14 Gd1 121.63(19) . . ?
C2 C1 C6 120.3(3) . . ?
C2 C1 S1 120.3(2) . . ?
C6 C1 S1 119.4(3) . . ?
O4 C2 C1 119.7(3) . . ?
O4 C2 C3 121.1(3) . . ?
C1 C2 C3 119.2(3) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 C7 118.5(3) . . ?
C3 C4 C7 120.8(3) . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
O6 C7 O5 124.7(3) . . ?
O6 C7 C4 122.2(3) . . ?
O5 C7 C4 113.1(3) . . ?
C13 C8 C9 120.1(3) . . ?
C13 C8 S2 119.6(3) . . ?
C9 C8 S2 120.3(3) . . ?
O10 C9 C8 119.1(3) . . ?
O10 C9 C10 122.1(3) . . ?
C8 C9 C10 118.8(3) . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 C14 118.7(3) . . ?
C10 C11 C14 120.8(3) . . ?
C11 C12 C13 119.4(3) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C8 120.8(3) . . ?
C12 C13 H13 119.6 . . ?
C8 C13 H13 119.6 . . ?
O12 C14 O11 123.5(3) . . ?
O12 C14 C11 122.8(3) . . ?
O11 C14 C11 113.6(3) . . ?
O14 C15 O13 126.7(3) . . ?
O14 C15 C15 117.1(3) . 2_666 ?
O13 C15 C15 116.1(3) . 2_666 ?

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
O3 S1 O1 Gd1 42.7(4) . . . . ?
O2 S1 O1 Gd1 -86.4(4) . . . . ?
C1 S1 O1 Gd1 159.1(3) . . . . ?
O3W Gd1 O1 S1 97.9(4) . . . . ?
O14 Gd1 O1 S1 19.1(3) . . . . ?
O6W Gd1 O1 S1 -164.1(3) . . . . ?
O2W Gd1 O1 S1 77.9(4) . . . . ?
O4W Gd1 O1 S1 173.0(4) . . . . ?
O13 Gd1 O1 S1 -48.9(3) 2_666 . . . ?
O1W Gd1 O1 S1 -38.1(4) . . . . ?
O5W Gd1 O1 S1 -115.5(4) . . . . ?
O3W Gd1 O14 C15 -151.3(2) . . . . ?
O6W Gd1 O14 C15 106.7(3) . . . . ?
O1 Gd1 O14 C15 -76.9(2) . . . . ?
O2W Gd1 O14 C15 139.6(2) . . . . ?
O4W Gd1 O14 C15 -120.1(2) . . . . ?
O13 Gd1 O14 C15 -1.1(2) 2_666 . . . ?
O1W Gd1 O14 C15 69.3(2) . . . . ?
O5W Gd1 O14 C15 -14.3(3) . . . . ?
O3 S1 C1 C2 62.3(3) . . . . ?
O1 S1 C1 C2 -57.7(3) . . . . ?
O2 S1 C1 C2 -176.7(3) . . . . ?
O3 S1 C1 C6 -119.4(3) . . . . ?
O1 S1 C1 C6 120.5(3) . . . . ?
O2 S1 C1 C6 1.6(3) . . . . ?
C6 C1 C2 O4 -179.1(3) . . . . ?
S1 C1 C2 O4 -0.9(4) . . . . ?
C6 C1 C2 C3 0.8(5) . . . . ?
S1 C1 C2 C3 179.1(2) . . . . ?
O4 C2 C3 C4 -179.9(3) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C2 C3 C4 C5 -1.2(5) . . . . ?
C2 C3 C4 C7 -179.5(3) . . . . ?
C3 C4 C5 C6 1.1(5) . . . . ?
C7 C4 C5 C6 179.5(3) . . . . ?
C4 C5 C6 C1 -0.1(5) . . . . ?
C2 C1 C6 C5 -0.8(5) . . . . ?
S1 C1 C6 C5 -179.1(3) . . . . ?
C5 C4 C7 O6 3.5(5) . . . . ?
C3 C4 C7 O6 -178.1(3) . . . . ?
C5 C4 C7 O5 -177.1(3) . . . . ?
C3 C4 C7 O5 1.3(5) . . . . ?
O9 S2 C8 C13 -125.3(3) . . . . ?
O8 S2 C8 C13 -5.1(3) . . . . ?
O7 S2 C8 C13 114.4(3) . . . . ?
O9 S2 C8 C9 54.3(4) . . . . ?
O8 S2 C8 C9 174.5(3) . . . . ?
O7 S2 C8 C9 -66.0(3) . . . . ?
C13 C8 C9 O10 179.3(3) . . . . ?
S2 C8 C9 O10 -0.3(5) . . . . ?
C13 C8 C9 C10 -1.9(6) . . . . ?
S2 C8 C9 C10 178.5(3) . . . . ?
O10 C9 C10 C11 178.4(4) . . . . ?
C8 C9 C10 C11 -0.3(6) . . . . ?
C9 C10 C11 C12 1.9(6) . . . . ?
C9 C10 C11 C14 -176.0(4) . . . . ?
C10 C11 C12 C13 -1.2(6) . . . . ?
C14 C11 C12 C13 176.7(4) . . . . ?
C11 C12 C13 C8 -1.0(6) . . . . ?
C9 C8 C13 C12 2.6(6) . . . . ?
S2 C8 C13 C12 -177.8(3) . . . . ?
C12 C11 C14 O12 -19.1(6) . . . . ?
C10 C11 C14 O12 158.8(4) . . . . ?
C12 C11 C14 O11 163.8(4) . . . . ?
C10 C11 C14 O11 -18.3(5) . . . . ?
Gd1 O14 C15 O13 -179.1(2) . . . . ?
Gd1 O14 C15 C15 1.1(4) . . . 2_666 ?
Gd1 O13 C15 O14 -179.0(2) 2_666 . . . ?
Gd1 O13 C15 C15 0.8(4) 2_666 . . 2_666 ?

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
O1W H1W1 O3 0.85(3) 2.065(10) 2.905(3) 171(3) 2_666
O1W H1W2 O9 0.85(3) 1.939(17) 2.743(4) 158(4) 2_656
O2W H2W1 O7W 0.85(3) 1.897(12) 2.731(4) 169(4) .
O2W H2W2 O12 0.85(3) 2.006(11) 2.853(3) 177(4) 1_566
O3W H3W1 O14 0.85(3) 1.949(19) 2.739(3) 153(3) 2_566
O3W H3W2 O9W 0.85(3) 1.940(13) 2.784(3) 171(4) 2
O4 H4O O8 0.85(3) 1.867(12) 2.704(4) 171(4) .
O4W H4W1 O8W 0.85(3) 1.948(11) 2.801(4) 176(3) .
O4W H4W2 O6 0.85(3) 1.926(19) 2.735(3) 158(4) 2
O5 H5O O9W 0.85(3) 1.856(12) 2.697(3) 174(4) .
O5W H5W1 O7 0.85(3) 2.31(2) 3.023(3) 143(3) .
O5W H5W2 O4 0.85(3) 2.219(19) 2.998(3) 154(3) .
O6W H6W1 O10W 0.85(3) 2.072(17) 2.890(4) 161(3) 1_566
O6W H6W2 O8W 0.85(3) 1.877(16) 2.702(4) 164(4) 2_556
O7W H7W1 O9 0.85 2.23 3.078(5) 175.0 2_556
O7W H7W2 O13 0.85 2.02 2.872(4) 175.3 2_566
O8W H8W1 O7W 0.85(3) 1.864(11) 2.717(4) 175(4) .
O8W H8W2 O9 0.85(3) 2.37(3) 3.026(4) 134(4) 1_455
O9W H9W1 O3 0.85 2.24 3.028(4) 153.8 2_655
O9W H9W1 O4 0.85 2.53 3.055(4) 121.2 2_655
O9W H9W2 O12 0.85 2.23 3.018(4) 153.9 .
O9W H9W2 O2 0.85 2.61 3.125(4) 119.7 2
O10 H10O O2 0.85(3) 1.857(12) 2.702(3) 173(5) 1_545
O10W HAW O7 0.85(3) 1.925(11) 2.773(4) 174(4) 2_545
O10W HBW O6 0.85(3) 2.53(3) 3.159(4) 132(3) 1_545
O11 H11O O10W 0.85(3) 1.825(13) 2.669(4) 173(5) .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_2-Dy
_database_code_depnum_ccdc_archive 'CCDC 1549845'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 Dy2 O28 S2, 2(C7 H5 O6 S), 8(H2 O)'
_chemical_formula_sum            'C30 H60 Dy2 O48 S4'
_chemical_formula_weight         1642.02

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8588(3)
_cell_length_b                   12.3336(6)
_cell_length_c                   15.0079(10)
_cell_angle_alpha                107.378(5)
_cell_angle_beta                 97.003(4)
_cell_angle_gamma                96.478(3)
_cell_volume                     1360.71(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4433
_cell_measurement_theta_min      3.76
_cell_measurement_theta_max      29.26

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    3.004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5326
_exptl_absorpt_correction_T_max  0.6450
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9131
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6216
_reflns_number_gt                5471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6216
_refine_ls_number_parameters     451
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0606
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.009
_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
Dy1 Dy 0.79381(2) 0.703750(14) 0.519022(13) 0.01789(6) Uani 1 1 d . . .
S1 S 0.74263(12) 0.64516(8) 0.74708(7) 0.0211(2) Uani 1 1 d . . .
S2 S 0.43426(14) 0.86409(8) 0.23331(8) 0.0291(2) Uani 1 1 d . . .
O1 O 0.7899(3) 0.6972(2) 0.67644(18) 0.0243(6) Uani 1 1 d . . .
O1W O 0.6343(4) 0.8620(2) 0.5900(2) 0.0319(7) Uani 1 1 d D . .
H1W1 H 0.704(4) 0.924(2) 0.619(2) 0.048 Uiso 1 1 d D . .
H1W2 H 0.591(5) 0.836(3) 0.630(2) 0.048 Uiso 1 1 d D . .
O2 O 0.5633(3) 0.5894(2) 0.72536(19) 0.0289(7) Uani 1 1 d . . .
O2W O 0.9899(4) 0.8721(3) 0.6270(2) 0.0359(7) Uani 1 1 d D . .
H2W1 H 1.023(5) 0.881(4) 0.6856(11) 0.054 Uiso 1 1 d D . .
H2W2 H 1.077(3) 0.897(4) 0.605(2) 0.054 Uiso 1 1 d D . .
O3 O 0.8640(3) 0.5713(2) 0.76591(19) 0.0283(6) Uani 1 1 d . . .
O3W O 1.0537(4) 0.6460(3) 0.5672(2) 0.0366(7) Uani 1 1 d D . .
H3W1 H 1.089(5) 0.660(3) 0.6260(8) 0.055 Uiso 1 1 d D . .
H3W2 H 1.106(5) 0.594(3) 0.536(2) 0.055 Uiso 1 1 d D . .
O4 O 0.5627(3) 0.8489(2) 0.7787(2) 0.0268(6) Uani 1 1 d D . .
H4O H 0.521(5) 0.909(2) 0.782(3) 0.040 Uiso 1 1 d D . .
O4W O 0.9451(4) 0.6243(3) 0.3897(2) 0.0350(7) Uani 1 1 d D . .
H4W1 H 1.047(2) 0.660(4) 0.397(3) 0.052 Uiso 1 1 d D . .
H4W2 H 0.893(4) 0.613(4) 0.3343(14) 0.052 Uiso 1 1 d D . .
O5 O 0.7413(4) 1.1228(2) 1.1043(2) 0.0333(7) Uani 1 1 d D . .
H5O H 0.762(6) 1.176(3) 1.1568(16) 0.050 Uiso 1 1 d D . .
O5W O 0.8638(4) 0.8459(3) 0.4457(2) 0.0356(7) Uani 1 1 d D . .
H5W1 H 0.890(6) 0.831(3) 0.3906(15) 0.053 Uiso 1 1 d D . .
H5W2 H 0.811(5) 0.903(3) 0.458(3) 0.053 Uiso 1 1 d D . .
O6W O 0.6014(4) 0.6481(2) 0.3662(2) 0.0300(7) Uani 1 1 d D . .
H6W1 H 0.579(5) 0.694(2) 0.335(2) 0.045 Uiso 1 1 d D . .
H6W2 H 0.551(5) 0.5805(13) 0.335(2) 0.045 Uiso 1 1 d D . .
O6 O 0.9249(4) 1.0419(2) 1.1809(2) 0.0391(8) Uani 1 1 d . . .
O7 O 0.5237(5) 0.8295(3) 0.3076(2) 0.0581(11) Uani 1 1 d . . .
O7W O 0.7381(4) 1.0416(3) 0.4504(3) 0.0592(10) Uani 1 1 d D . .
H7W1 H 0.725(6) 1.097(3) 0.498(3) 0.089 Uiso 1 1 d D . .
H7W2 H 0.639(3) 1.004(4) 0.422(3) 0.089 Uiso 1 1 d D . .
O8 O 0.5458(3) 0.9468(2) 0.2060(2) 0.0351(7) Uani 1 1 d . . .
O8W O 0.9280(4) 0.8297(3) 0.2572(2) 0.0440(8) Uani 1 1 d D . .
H8W1 H 1.033(2) 0.846(4) 0.251(4) 0.066 Uiso 1 1 d D . .
H8W2 H 0.872(4) 0.883(3) 0.251(4) 0.066 Uiso 1 1 d D . .
O9W O 0.2692(4) 0.7500(3) 0.4248(2) 0.0432(8) Uani 1 1 d D . .
H9W1 H 0.311(5) 0.748(4) 0.3748(19) 0.065 Uiso 1 1 d D . .
H9W2 H 0.328(5) 0.715(4) 0.456(3) 0.065 Uiso 1 1 d D . .
O9 O 0.2753(4) 0.9046(3) 0.2574(2) 0.0516(9) Uani 1 1 d . . .
O10 O 0.2361(4) 0.6395(2) 0.2195(2) 0.0413(8) Uani 1 1 d D . .
H10O H 0.202(6) 0.573(2) 0.223(4) 0.062 Uiso 1 1 d D . .
O10W O 0.7726(4) 1.3169(2) 1.2507(2) 0.0339(7) Uani 1 1 d D . .
HAW H 0.674(3) 1.328(3) 1.264(3) 0.051 Uiso 1 1 d D . .
HBW H 0.823(4) 1.373(3) 1.237(3) 0.051 Uiso 1 1 d D . .
O11 O 0.1719(5) 0.3566(3) -0.1058(2) 0.0490(9) Uani 1 1 d D . .
H11O H 0.122(6) 0.307(3) -0.157(2) 0.074 Uiso 1 1 d D . .
O12 O 0.2224(4) 0.4649(3) -0.1968(2) 0.0466(9) Uani 1 1 d . . .
O13 O 0.4889(3) 0.6459(2) 0.53094(19) 0.0238(6) Uani 1 1 d . . .
O14 O 0.2842(3) 0.4967(2) 0.51433(19) 0.0241(6) Uani 1 1 d . . .
C1 C 0.7650(5) 0.7611(3) 0.8526(3) 0.0202(8) Uani 1 1 d . . .
C2 C 0.6718(4) 0.8520(3) 0.8570(3) 0.0191(8) Uani 1 1 d . . .
C3 C 0.6929(5) 0.9426(3) 0.9410(3) 0.0222(8) Uani 1 1 d . . .
H3A H 0.6307 1.0032 0.9443 0.027 Uiso 1 1 calc R . .
C4 C 0.8053(4) 0.9437(3) 1.0195(3) 0.0209(8) Uani 1 1 d . . .
C5 C 0.8994(5) 0.8535(3) 1.0151(3) 0.0255(9) Uani 1 1 d . . .
H5A H 0.9760 0.8545 1.0678 0.031 Uiso 1 1 calc R . .
C6 C 0.8784(5) 0.7632(3) 0.9324(3) 0.0241(9) Uani 1 1 d . . .
H6A H 0.9405 0.7027 0.9296 0.029 Uiso 1 1 calc R . .
C7 C 0.8306(5) 1.0401(3) 1.1102(3) 0.0256(9) Uani 1 1 d . . .
C8 C 0.3770(5) 0.7404(3) 0.1314(3) 0.0240(9) Uani 1 1 d . . .
C9 C 0.2825(5) 0.6407(3) 0.1365(3) 0.0262(9) Uani 1 1 d . . .
C10 C 0.2362(5) 0.5470(3) 0.0548(3) 0.0289(9) Uani 1 1 d . . .
H10A H 0.1727 0.4797 0.0569 0.035 Uiso 1 1 calc R . .
C11 C 0.2839(5) 0.5524(3) -0.0305(3) 0.0259(9) Uani 1 1 d . . .
C12 C 0.3807(5) 0.6511(4) -0.0336(3) 0.0338(10) Uani 1 1 d . . .
H12A H 0.4140 0.6550 -0.0901 0.041 Uiso 1 1 calc R . .
C13 C 0.4276(5) 0.7437(4) 0.0476(3) 0.0312(10) Uani 1 1 d . . .
H13A H 0.4950 0.8098 0.0458 0.037 Uiso 1 1 calc R . .
C14 C 0.2249(5) 0.4546(4) -0.1196(3) 0.0303(10) Uani 1 1 d . . .
C15 C 0.4352(4) 0.5414(3) 0.5131(3) 0.0210(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
Dy1 O3W 2.340(3) . ?
Dy1 O14 2.363(2) 2_666 ?
Dy1 O5W 2.381(3) . ?
Dy1 O1 2.391(2) . ?
Dy1 O4W 2.415(3) . ?
Dy1 O2W 2.444(3) . ?
Dy1 O6W 2.449(3) . ?
Dy1 O13 2.465(2) . ?
Dy1 O1W 2.480(3) . ?
S1 O2 1.450(3) . ?
S1 O3 1.451(3) . ?
S1 O1 1.457(2) . ?
S1 C1 1.762(4) . ?
S2 O7 1.442(3) . ?
S2 O9 1.444(3) . ?
S2 O8 1.453(3) . ?
S2 C8 1.775(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O2W H2W1 0.85(4) . ?
O2W H2W2 0.85(4) . ?
O3W H3W1 0.85(4) . ?
O3W H3W2 0.85(4) . ?
O4 C2 1.356(4) . ?
O4 H4O 0.85(4) . ?
O4W H4W1 0.85(4) . ?
O4W H4W2 0.85(4) . ?
O5 C7 1.320(5) . ?
O5 H5O 0.85(4) . ?
O5W H5W1 0.85(4) . ?
O5W H5W2 0.85(4) . ?
O6W H6W1 0.85(4) . ?
O6W H6W2 0.85(4) . ?
O6 C7 1.210(4) . ?
O7W H7W1 0.85(4) . ?
O7W H7W2 0.85(4) . ?
O8W H8W1 0.85(4) . ?
O8W H8W2 0.85(4) . ?
O9W H9W1 0.85(4) . ?
O9W H9W2 0.85(4) . ?
O10 C9 1.344(5) . ?
O10 H10O 0.85(4) . ?
O10W HAW 0.85(4) . ?
O10W HBW 0.85(4) . ?
O11 C14 1.316(5) . ?
O11 H11O 0.85(4) . ?
O12 C14 1.201(5) . ?
O13 C15 1.247(4) . ?
O14 C15 1.255(4) . ?
O14 Dy1 2.363(2) 2_666 ?
C1 C6 1.395(5) . ?
C1 C2 1.397(5) . ?
C2 C3 1.389(5) . ?
C3 C4 1.380(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.393(5) . ?
C4 C7 1.490(5) . ?
C5 C6 1.376(5) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C8 C13 1.376(6) . ?
C8 C9 1.390(5) . ?
C9 C10 1.386(5) . ?
C10 C11 1.396(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.377(5) . ?
C11 C14 1.488(5) . ?
C12 C13 1.374(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C15 1.524(7) 2_666 ?

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
O3W Dy1 O14 76.70(10) . 2_666 ?
O3W Dy1 O5W 107.41(12) . . ?
O14 Dy1 O5W 142.20(10) 2_666 . ?
O3W Dy1 O1 72.82(10) . . ?
O14 Dy1 O1 80.55(9) 2_666 . ?
O5W Dy1 O1 137.11(10) . . ?
O3W Dy1 O4W 66.86(10) . . ?
O14 Dy1 O4W 77.08(10) 2_666 . ?
O5W Dy1 O4W 70.89(11) . . ?
O1 Dy1 O4W 137.26(9) . . ?
O3W Dy1 O2W 71.21(11) . . ?
O14 Dy1 O2W 142.72(9) 2_666 . ?
O5W Dy1 O2W 67.75(10) . . ?
O1 Dy1 O2W 72.35(9) . . ?
O4W Dy1 O2W 106.23(10) . . ?
O3W Dy1 O6W 132.28(10) . . ?
O14 Dy1 O6W 77.58(9) 2_666 . ?
O5W Dy1 O6W 72.48(10) . . ?
O1 Dy1 O6W 139.85(9) . . ?
O4W Dy1 O6W 68.59(10) . . ?
O2W Dy1 O6W 138.97(9) . . ?
O3W Dy1 O13 132.87(10) . . ?
O14 Dy1 O13 66.53(8) 2_666 . ?
O5W Dy1 O13 119.72(10) . . ?
O1 Dy1 O13 72.95(8) . . ?
O4W Dy1 O13 127.45(9) . . ?
O2W Dy1 O13 125.81(10) . . ?
O6W Dy1 O13 67.55(9) . . ?
O3W Dy1 O1W 134.66(10) . . ?
O14 Dy1 O1W 129.44(9) 2_666 . ?
O5W Dy1 O1W 74.98(11) . . ?
O1 Dy1 O1W 76.27(9) . . ?
O4W Dy1 O1W 144.55(10) . . ?
O2W Dy1 O1W 68.26(10) . . ?
O6W Dy1 O1W 92.37(10) . . ?
O13 Dy1 O1W 63.91(8) . . ?
O2 S1 O3 113.08(15) . . ?
O2 S1 O1 112.60(16) . . ?
O3 S1 O1 112.05(16) . . ?
O2 S1 C1 107.38(17) . . ?
O3 S1 C1 105.98(17) . . ?
O1 S1 C1 105.07(16) . . ?
O7 S2 O9 111.7(2) . . ?
O7 S2 O8 112.14(18) . . ?
O9 S2 O8 112.08(18) . . ?
O7 S2 C8 107.40(18) . . ?
O9 S2 C8 107.30(19) . . ?
O8 S2 C8 105.76(18) . . ?
S1 O1 Dy1 154.73(16) . . ?
Dy1 O1W H1W1 111(3) . . ?
Dy1 O1W H1W2 100(3) . . ?
H1W1 O1W H1W2 109.0(17) . . ?
Dy1 O2W H2W1 123(3) . . ?
Dy1 O2W H2W2 116(3) . . ?
H2W1 O2W H2W2 107.8(16) . . ?
Dy1 O3W H3W1 119(3) . . ?
Dy1 O3W H3W2 129(3) . . ?
H3W1 O3W H3W2 108.9(17) . . ?
C2 O4 H4O 115(3) . . ?
Dy1 O4W H4W1 113(3) . . ?
Dy1 O4W H4W2 117(3) . . ?
H4W1 O4W H4W2 110.8(17) . . ?
C7 O5 H5O 109(3) . . ?
Dy1 O5W H5W1 124(3) . . ?
Dy1 O5W H5W2 117(3) . . ?
H5W1 O5W H5W2 110.5(17) . . ?
Dy1 O6W H6W1 125(2) . . ?
Dy1 O6W H6W2 125(2) . . ?
H6W1 O6W H6W2 110.1(17) . . ?
H7W1 O7W H7W2 108.9(17) . . ?
H8W1 O8W H8W2 110.3(17) . . ?
H9W1 O9W H9W2 109.4(17) . . ?
C9 O10 H10O 115(4) . . ?
HAW O10W HBW 111.1(17) . . ?
C14 O11 H11O 111(4) . . ?
C15 O13 Dy1 118.0(2) . . ?
C15 O14 Dy1 122.0(2) . 2_666 ?
C6 C1 C2 119.4(3) . . ?
C6 C1 S1 119.9(3) . . ?
C2 C1 S1 120.7(3) . . ?
O4 C2 C3 121.9(3) . . ?
O4 C2 C1 118.7(3) . . ?
C3 C2 C1 119.4(3) . . ?
C4 C3 C2 120.6(4) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 C7 121.6(4) . . ?
C5 C4 C7 118.3(3) . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
O6 C7 O5 124.2(4) . . ?
O6 C7 C4 123.1(4) . . ?
O5 C7 C4 112.7(3) . . ?
C13 C8 C9 120.2(4) . . ?
C13 C8 S2 119.6(3) . . ?
C9 C8 S2 120.2(3) . . ?
O10 C9 C10 122.4(3) . . ?
O10 C9 C8 119.0(4) . . ?
C10 C9 C8 118.5(4) . . ?
C9 C10 C11 120.8(4) . . ?
C9 C10 H10A 119.6 . . ?
C11 C10 H10A 119.6 . . ?
C12 C11 C10 119.8(4) . . ?
C12 C11 C14 119.2(4) . . ?
C10 C11 C14 120.9(4) . . ?
C13 C12 C11 119.4(4) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C12 C13 C8 121.3(4) . . ?
C12 C13 H13A 119.4 . . ?
C8 C13 H13A 119.4 . . ?
O12 C14 O11 123.2(4) . . ?
O12 C14 C11 123.0(4) . . ?
O11 C14 C11 113.8(4) . . ?
O13 C15 O14 126.5(3) . . ?
O13 C15 C15 117.3(4) . 2_666 ?
O14 C15 C15 116.2(4) . 2_666 ?

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 Dy1 -42.4(4) . . . . ?
O3 S1 O1 Dy1 86.4(4) . . . . ?
C1 S1 O1 Dy1 -158.9(4) . . . . ?
O3W Dy1 O1 S1 -98.0(4) . . . . ?
O14 Dy1 O1 S1 -19.2(4) 2_666 . . . ?
O5W Dy1 O1 S1 164.6(3) . . . . ?
O4W Dy1 O1 S1 -78.2(4) . . . . ?
O2W Dy1 O1 S1 -173.2(4) . . . . ?
O6W Dy1 O1 S1 38.5(5) . . . . ?
O13 Dy1 O1 S1 49.1(4) . . . . ?
O1W Dy1 O1 S1 115.6(4) . . . . ?
O3W Dy1 O13 C15 -42.9(3) . . . . ?
O14 Dy1 O13 C15 -1.1(2) 2_666 . . . ?
O5W Dy1 O13 C15 137.0(3) . . . . ?
O1 Dy1 O13 C15 -88.0(3) . . . . ?
O4W Dy1 O13 C15 49.1(3) . . . . ?
O2W Dy1 O13 C15 -140.3(3) . . . . ?
O6W Dy1 O13 C15 84.6(3) . . . . ?
O1W Dy1 O13 C15 -170.8(3) . . . . ?
O2 S1 C1 C6 118.6(3) . . . . ?
O3 S1 C1 C6 -2.6(3) . . . . ?
O1 S1 C1 C6 -121.4(3) . . . . ?
O2 S1 C1 C2 -62.2(3) . . . . ?
O3 S1 C1 C2 176.7(3) . . . . ?
O1 S1 C1 C2 57.9(3) . . . . ?
C6 C1 C2 O4 179.7(3) . . . . ?
S1 C1 C2 O4 0.4(5) . . . . ?
C6 C1 C2 C3 -0.3(5) . . . . ?
S1 C1 C2 C3 -179.6(3) . . . . ?
O4 C2 C3 C4 -179.8(3) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C2 C3 C4 C7 179.8(3) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C7 C4 C5 C6 179.8(3) . . . . ?
C4 C5 C6 C1 0.5(6) . . . . ?
C2 C1 C6 C5 -0.1(5) . . . . ?
S1 C1 C6 C5 179.2(3) . . . . ?
C3 C4 C7 O6 178.1(4) . . . . ?
C5 C4 C7 O6 -2.4(6) . . . . ?
C3 C4 C7 O5 -2.7(5) . . . . ?
C5 C4 C7 O5 176.9(3) . . . . ?
O7 S2 C8 C13 -125.3(4) . . . . ?
O9 S2 C8 C13 114.4(4) . . . . ?
O8 S2 C8 C13 -5.3(4) . . . . ?
O7 S2 C8 C9 54.3(4) . . . . ?
O9 S2 C8 C9 -65.9(4) . . . . ?
O8 S2 C8 C9 174.3(3) . . . . ?
C13 C8 C9 O10 179.3(4) . . . . ?
S2 C8 C9 O10 -0.3(5) . . . . ?
C13 C8 C9 C10 -2.1(6) . . . . ?
S2 C8 C9 C10 178.3(3) . . . . ?
O10 C9 C10 C11 178.7(4) . . . . ?
C8 C9 C10 C11 0.2(6) . . . . ?
C9 C10 C11 C12 1.2(6) . . . . ?
C9 C10 C11 C14 -176.1(4) . . . . ?
C10 C11 C12 C13 -0.7(6) . . . . ?
C14 C11 C12 C13 176.6(4) . . . . ?
C11 C12 C13 C8 -1.2(7) . . . . ?
C9 C8 C13 C12 2.7(6) . . . . ?
S2 C8 C13 C12 -177.7(3) . . . . ?
C12 C11 C14 O12 -17.4(6) . . . . ?
C10 C11 C14 O12 159.9(4) . . . . ?
C12 C11 C14 O11 164.2(4) . . . . ?
C10 C11 C14 O11 -18.5(6) . . . . ?
Dy1 O13 C15 O14 -179.0(3) . . . . ?
Dy1 O13 C15 C15 1.0(5) . . . 2_666 ?
Dy1 O14 C15 O13 -178.9(3) 2_666 . . . ?
Dy1 O14 C15 C15 1.1(5) 2_666 . . 2_666 ?

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
O1W H1W1 O9 0.85(4) 2.33(3) 3.040(4) 141(4) 2_676
O1W H1W2 O4 0.85(4) 2.23(2) 3.000(4) 151(3) .
O2W H2W1 O6 0.85(4) 1.91(2) 2.726(4) 157(5) 2_777
O2W H2W2 O7W 0.85(4) 1.957(11) 2.808(5) 175(4) 2_776
O3W H3W1 O10W 0.85(4) 1.954(16) 2.783(4) 165(4) 2_777
O3W H3W2 O14 0.85(4) 1.94(2) 2.745(4) 157(4) 1_655
O4 H4O O8 0.85(4) 1.868(12) 2.705(4) 173(4) 2_676
O4W H4W1 O9W 0.85(4) 1.891(11) 2.731(4) 174(5) 1_655
O4W H4W2 O12 0.85(4) 2.039(17) 2.857(4) 163(4) 2_665
O5 H5O O10W 0.85(4) 1.871(17) 2.685(4) 162(4) .
O5W H5W1 O8W 0.85(4) 2.056(15) 2.887(5) 167(4) .
O5W H5W2 O7W 0.85(4) 1.891(19) 2.695(5) 159(4) .
O6W H6W1 O7 0.85(4) 1.925(16) 2.740(4) 161(4) .
O6W H6W2 O2 0.85(4) 2.065(10) 2.906(4) 173(3) 2_666
O7W H7W1 O9W 0.85(4) 1.89(2) 2.702(5) 158(6) 2_676
O7W H7W2 O7 0.85(4) 2.32(3) 3.009(4) 138(4) .
O8W H8W1 O9 0.85(4) 1.940(14) 2.780(4) 170(5) 1_655
O8W H8W2 O6 0.85(4) 2.51(3) 3.157(4) 134(3) 1_554
O9W H9W1 O10 0.85(4) 2.28(4) 2.939(5) 135(4) .
O9W H9W1 O7 0.85(4) 2.34(3) 3.084(5) 147(4) .
O9W H9W2 O13 0.85(4) 2.018(12) 2.867(4) 174(4) .
O10 H10O O3 0.85(4) 1.860(11) 2.710(3) 177(5) 2_666
O10W HAW O2 0.85(4) 2.218(18) 3.017(4) 158(3) 2_677
O10W HAW O4 0.85(4) 2.57(3) 3.047(4) 117(3) 2_677
O10W HBW O12 0.85(4) 2.31(2) 3.031(4) 143(3) 2_676
O10W HBW O3 0.85(4) 2.49(3) 3.100(4) 130(3) 2_777
O11 H11O O8W 0.85(4) 1.85(2) 2.664(4) 160(5) 2_665

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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_5-Gd
_database_code_depnum_ccdc_archive 'CCDC 1549861'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 Gd N2 O7 S'
_chemical_formula_sum            'C17 H13 Gd N2 O7 S'
_chemical_formula_weight         546.60

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.2180(5)
_cell_length_b                   8.5475(3)
_cell_length_c                   17.9929(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.729(5)
_cell_angle_gamma                90.00
_cell_volume                     1643.33(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2909
_cell_measurement_theta_min      3.47
_cell_measurement_theta_max      27.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1060
_exptl_absorpt_coefficient_mu    4.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4717
_exptl_absorpt_correction_T_max  0.5707
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5652
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3770
_reflns_number_gt                3118
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0167P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3770
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0729
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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 0.17653(2) 1.03791(3) 0.307003(15) 0.01200(8) Uani 1 1 d . . .
S1 S 0.14636(12) 0.63085(15) 0.33990(8) 0.0139(3) Uani 1 1 d . . .
O1W O 0.0687(4) 1.2684(4) 0.2345(2) 0.0223(9) Uani 1 1 d D . .
H1W1 H 0.059(6) 1.340(4) 0.265(3) 0.033 Uiso 1 1 d D . .
H1W2 H 0.104(5) 1.308(5) 0.203(3) 0.033 Uiso 1 1 d D . .
O1 O 0.0858(3) 0.7855(4) 0.3315(2) 0.0186(8) Uani 1 1 d . . .
O2 O 0.0644(3) 0.5065(4) 0.3502(2) 0.0207(9) Uani 1 1 d . . .
O3 O 0.1947(3) 0.5974(4) 0.2747(2) 0.0205(9) Uani 1 1 d . . .
O4 O 0.3375(3) 0.8852(4) 0.3798(2) 0.0171(8) Uani 1 1 d . . .
O5 O 0.6743(3) 0.7645(4) 0.6320(2) 0.0207(9) Uani 1 1 d . . .
O6 O 0.5861(3) 0.5836(4) 0.6886(2) 0.0217(9) Uani 1 1 d . . .
N1 N 0.1415(4) 1.1124(5) 0.4383(3) 0.0198(10) Uani 1 1 d . . .
N2 N -0.0519(4) 1.0673(5) 0.3118(3) 0.0179(10) Uani 1 1 d . . .
C1 C 0.2735(5) 0.6442(6) 0.4248(3) 0.0158(11) Uani 1 1 d . . .
C2 C 0.3539(5) 0.7764(6) 0.4345(3) 0.0147(11) Uani 1 1 d . . .
C3 C 0.4518(5) 0.7829(6) 0.5054(3) 0.0170(12) Uani 1 1 d . . .
H3 H 0.5047 0.8693 0.5149 0.020 Uiso 1 1 calc R . .
C4 C 0.4735(5) 0.6668(6) 0.5618(3) 0.0143(11) Uani 1 1 d . . .
C5 C 0.3917(5) 0.5392(6) 0.5502(3) 0.0159(11) Uani 1 1 d . . .
H5 H 0.4045 0.4610 0.5877 0.019 Uiso 1 1 calc R . .
C6 C 0.2916(5) 0.5301(6) 0.4824(3) 0.0160(11) Uani 1 1 d . . .
H6 H 0.2360 0.4467 0.4752 0.019 Uiso 1 1 calc R . .
C7 C 0.5868(5) 0.6737(6) 0.6328(3) 0.0154(11) Uani 1 1 d . . .
C8 C 0.2393(6) 1.1212(7) 0.5026(3) 0.0254(13) Uani 1 1 d . . .
H8 H 0.3156 1.0821 0.5006 0.030 Uiso 1 1 calc R . .
C9 C 0.2339(6) 1.1855(7) 0.5723(4) 0.0307(15) Uani 1 1 d . . .
H9 H 0.3043 1.1892 0.6160 0.037 Uiso 1 1 calc R . .
C10 C 0.1208(7) 1.2433(8) 0.5743(4) 0.0412(18) Uani 1 1 d . . .
H10 H 0.1137 1.2883 0.6198 0.049 Uiso 1 1 calc R . .
C11 C 0.0186(6) 1.2347(7) 0.5094(4) 0.0336(16) Uani 1 1 d . . .
H11 H -0.0582 1.2733 0.5108 0.040 Uiso 1 1 calc R . .
C12 C 0.0296(5) 1.1678(6) 0.4411(4) 0.0207(13) Uani 1 1 d . . .
C13 C -0.0772(5) 1.1399(6) 0.3716(3) 0.0192(12) Uani 1 1 d . . .
C14 C -0.2020(6) 1.1738(7) 0.3673(4) 0.0326(16) Uani 1 1 d . . .
H14 H -0.2192 1.2300 0.4071 0.039 Uiso 1 1 calc R . .
C15 C -0.2970(6) 1.1246(8) 0.3052(4) 0.0391(18) Uani 1 1 d . . .
H15 H -0.3794 1.1480 0.3020 0.047 Uiso 1 1 calc R . .
C16 C -0.2713(5) 1.0401(7) 0.2471(4) 0.0298(14) Uani 1 1 d . . .
H16 H -0.3350 0.9987 0.2058 0.036 Uiso 1 1 calc R . .
C17 C -0.1466(5) 1.0190(7) 0.2524(4) 0.0273(14) Uani 1 1 d . . .
H17 H -0.1283 0.9675 0.2117 0.033 Uiso 1 1 calc R . .


_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 O4 2.289(4) . ?
Gd1 O6 2.308(4) 4_575 ?
Gd1 O5 2.395(4) 3_676 ?
Gd1 O3 2.409(3) 2 ?
Gd1 O1W 2.467(4) . ?
Gd1 O1 2.482(3) . ?
Gd1 N1 2.589(4) . ?
Gd1 N2 2.603(4) . ?
S1 O2 1.454(3) . ?
S1 O3 1.462(3) . ?
S1 O1 1.473(4) . ?
S1 C1 1.747(6) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O3 Gd1 2.409(3) 2_545 ?
O4 C2 1.325(6) . ?
O5 C7 1.255(6) . ?
O5 Gd1 2.395(4) 3_676 ?
O6 C7 1.268(6) . ?
O6 Gd1 2.308(4) 4_676 ?
N1 C8 1.332(8) . ?
N1 C12 1.357(6) . ?
N2 C17 1.322(8) . ?
N2 C13 1.346(6) . ?
C1 C6 1.392(7) . ?
C1 C2 1.423(7) . ?
C2 C3 1.409(8) . ?
C3 C4 1.387(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(7) . ?
C4 C7 1.503(8) . ?
C5 C6 1.386(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.388(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.373(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.366(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.464(8) . ?
C13 C14 1.409(7) . ?
C14 C15 1.355(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(8) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Gd1 O6 108.65(13) . 4_575 ?
O4 Gd1 O5 79.67(13) . 3_676 ?
O6 Gd1 O5 142.14(12) 4_575 3_676 ?
O4 Gd1 O3 87.39(12) . 2 ?
O6 Gd1 O3 73.04(12) 4_575 2 ?
O5 Gd1 O3 70.49(12) 3_676 2 ?
O4 Gd1 O1W 158.80(13) . . ?
O6 Gd1 O1W 82.20(13) 4_575 . ?
O5 Gd1 O1W 80.84(13) 3_676 . ?
O3 Gd1 O1W 78.28(12) 2 . ?
O4 Gd1 O1 72.38(12) . . ?
O6 Gd1 O1 71.60(13) 4_575 . ?
O5 Gd1 O1 142.97(13) 3_676 . ?
O3 Gd1 O1 130.31(12) 2 . ?
O1W Gd1 O1 128.82(13) . . ?
O4 Gd1 N1 86.03(13) . . ?
O6 Gd1 N1 143.74(13) 4_575 . ?
O5 Gd1 N1 71.78(13) 3_676 . ?
O3 Gd1 N1 142.26(14) 2 . ?
O1W Gd1 N1 95.74(13) . . ?
O1 Gd1 N1 82.36(13) . . ?
O4 Gd1 N2 130.49(12) . . ?
O6 Gd1 N2 85.04(14) 4_575 . ?
O5 Gd1 N2 118.31(13) 3_676 . ?
O3 Gd1 N2 141.22(14) 2 . ?
O1W Gd1 N2 67.14(12) . . ?
O1 Gd1 N2 67.45(12) . . ?
N1 Gd1 N2 61.42(15) . . ?
O2 S1 O3 111.3(2) . . ?
O2 S1 O1 112.3(2) . . ?
O3 S1 O1 111.5(2) . . ?
O2 S1 C1 108.4(2) . . ?
O3 S1 C1 108.1(2) . . ?
O1 S1 C1 105.0(2) . . ?
Gd1 O1W H1W1 112(4) . . ?
Gd1 O1W H1W2 114(4) . . ?
H1W1 O1W H1W2 109.0(17) . . ?
S1 O1 Gd1 126.63(19) . . ?
S1 O3 Gd1 165.6(3) . 2_545 ?
C2 O4 Gd1 137.0(3) . . ?
C7 O5 Gd1 150.5(3) . 3_676 ?
C7 O6 Gd1 153.9(4) . 4_676 ?
C8 N1 C12 118.3(5) . . ?
C8 N1 Gd1 119.5(3) . . ?
C12 N1 Gd1 121.3(4) . . ?
C17 N2 C13 118.5(5) . . ?
C17 N2 Gd1 120.0(3) . . ?
C13 N2 Gd1 121.3(4) . . ?
C6 C1 C2 121.4(5) . . ?
C6 C1 S1 120.0(4) . . ?
C2 C1 S1 118.5(4) . . ?
O4 C2 C3 122.6(5) . . ?
O4 C2 C1 121.8(5) . . ?
C3 C2 C1 115.6(5) . . ?
C4 C3 C2 123.3(5) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C3 C4 C5 119.2(5) . . ?
C3 C4 C7 120.5(5) . . ?
C5 C4 C7 120.3(5) . . ?
C6 C5 C4 119.6(5) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.7(5) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O5 C7 O6 125.3(5) . . ?
O5 C7 C4 118.5(5) . . ?
O6 C7 C4 116.2(5) . . ?
N1 C8 C9 123.8(6) . . ?
N1 C8 H8 118.1 . . ?
C9 C8 H8 118.1 . . ?
C10 C9 C8 117.5(6) . . ?
C10 C9 H9 121.2 . . ?
C8 C9 H9 121.2 . . ?
C11 C10 C9 120.0(6) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 119.9(6) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
N1 C12 C11 120.5(6) . . ?
N1 C12 C13 115.9(5) . . ?
C11 C12 C13 123.4(5) . . ?
N2 C13 C14 119.9(6) . . ?
N2 C13 C12 116.2(5) . . ?
C14 C13 C12 123.7(5) . . ?
C15 C14 C13 120.1(6) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 119.7(6) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 117.3(6) . . ?
C15 C16 H16 121.4 . . ?
C17 C16 H16 121.4 . . ?
N2 C17 C16 124.2(6) . . ?
N2 C17 H17 117.9 . . ?
C16 C17 H17 117.9 . . ?

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 Gd1 -177.3(2) . . . . ?
O3 S1 O1 Gd1 -51.7(3) . . . . ?
C1 S1 O1 Gd1 65.2(3) . . . . ?
O4 Gd1 O1 S1 -32.0(3) . . . . ?
O6 Gd1 O1 S1 85.3(3) 4_575 . . . ?
O5 Gd1 O1 S1 -74.8(3) 3_676 . . . ?
O3 Gd1 O1 S1 38.6(3) 2 . . . ?
O1W Gd1 O1 S1 148.5(2) . . . . ?
N1 Gd1 O1 S1 -120.2(3) . . . . ?
N2 Gd1 O1 S1 177.6(3) . . . . ?
O2 S1 O3 Gd1 -113.5(9) . . . 2_545 ?
O1 S1 O3 Gd1 120.3(9) . . . 2_545 ?
C1 S1 O3 Gd1 5.4(10) . . . 2_545 ?
O6 Gd1 O4 C2 -95.2(5) 4_575 . . . ?
O5 Gd1 O4 C2 123.1(5) 3_676 . . . ?
O3 Gd1 O4 C2 -166.3(5) 2 . . . ?
O1W Gd1 O4 C2 146.5(4) . . . . ?
O1 Gd1 O4 C2 -32.3(5) . . . . ?
N1 Gd1 O4 C2 50.9(5) . . . . ?
N2 Gd1 O4 C2 4.5(5) . . . . ?
O4 Gd1 N1 C8 33.0(4) . . . . ?
O6 Gd1 N1 C8 149.6(4) 4_575 . . . ?
O5 Gd1 N1 C8 -47.4(4) 3_676 . . . ?
O3 Gd1 N1 C8 -47.5(5) 2 . . . ?
O1W Gd1 N1 C8 -125.8(4) . . . . ?
O1 Gd1 N1 C8 105.8(4) . . . . ?
N2 Gd1 N1 C8 174.2(5) . . . . ?
O4 Gd1 N1 C12 -158.1(4) . . . . ?
O6 Gd1 N1 C12 -41.5(5) 4_575 . . . ?
O5 Gd1 N1 C12 121.5(4) 3_676 . . . ?
O3 Gd1 N1 C12 121.4(4) 2 . . . ?
O1W Gd1 N1 C12 43.1(4) . . . . ?
O1 Gd1 N1 C12 -85.3(4) . . . . ?
N2 Gd1 N1 C12 -16.9(4) . . . . ?
O4 Gd1 N2 C17 -113.1(4) . . . . ?
O6 Gd1 N2 C17 -2.8(4) 4_575 . . . ?
O5 Gd1 N2 C17 145.8(4) 3_676 . . . ?
O3 Gd1 N2 C17 52.1(5) 2 . . . ?
O1W Gd1 N2 C17 80.8(4) . . . . ?
O1 Gd1 N2 C17 -74.9(4) . . . . ?
N1 Gd1 N2 C17 -168.5(5) . . . . ?
O4 Gd1 N2 C13 71.0(4) . . . . ?
O6 Gd1 N2 C13 -178.6(4) 4_575 . . . ?
O5 Gd1 N2 C13 -30.0(4) 3_676 . . . ?
O3 Gd1 N2 C13 -123.7(4) 2 . . . ?
O1W Gd1 N2 C13 -95.0(4) . . . . ?
O1 Gd1 N2 C13 109.3(4) . . . . ?
N1 Gd1 N2 C13 15.7(4) . . . . ?
O2 S1 C1 C6 9.5(5) . . . . ?
O3 S1 C1 C6 -111.3(4) . . . . ?
O1 S1 C1 C6 129.6(4) . . . . ?
O2 S1 C1 C2 -168.2(4) . . . . ?
O3 S1 C1 C2 71.1(4) . . . . ?
O1 S1 C1 C2 -48.0(4) . . . . ?
Gd1 O4 C2 C3 -129.3(5) . . . . ?
Gd1 O4 C2 C1 51.2(7) . . . . ?
C6 C1 C2 O4 179.7(4) . . . . ?
S1 C1 C2 O4 -2.7(6) . . . . ?
C6 C1 C2 C3 0.2(7) . . . . ?
S1 C1 C2 C3 177.8(3) . . . . ?
O4 C2 C3 C4 -177.2(4) . . . . ?
C1 C2 C3 C4 2.3(7) . . . . ?
C2 C3 C4 C5 -2.8(7) . . . . ?
C2 C3 C4 C7 174.3(4) . . . . ?
C3 C4 C5 C6 0.7(7) . . . . ?
C7 C4 C5 C6 -176.4(4) . . . . ?
C4 C5 C6 C1 1.7(7) . . . . ?
C2 C1 C6 C5 -2.2(7) . . . . ?
S1 C1 C6 C5 -179.8(4) . . . . ?
Gd1 O5 C7 O6 -48.5(10) 3_676 . . . ?
Gd1 O5 C7 C4 132.8(6) 3_676 . . . ?
Gd1 O6 C7 O5 -8.5(11) 4_676 . . . ?
Gd1 O6 C7 C4 170.2(5) 4_676 . . . ?
C3 C4 C7 O5 -15.7(7) . . . . ?
C5 C4 C7 O5 161.4(4) . . . . ?
C3 C4 C7 O6 165.5(4) . . . . ?
C5 C4 C7 O6 -17.4(7) . . . . ?
C12 N1 C8 C9 -0.7(8) . . . . ?
Gd1 N1 C8 C9 168.5(4) . . . . ?
N1 C8 C9 C10 -0.2(9) . . . . ?
C8 C9 C10 C11 0.7(10) . . . . ?
C9 C10 C11 C12 -0.3(10) . . . . ?
C8 N1 C12 C11 1.1(8) . . . . ?
Gd1 N1 C12 C11 -167.9(4) . . . . ?
C8 N1 C12 C13 -173.7(5) . . . . ?
Gd1 N1 C12 C13 17.3(6) . . . . ?
C10 C11 C12 N1 -0.6(9) . . . . ?
C10 C11 C12 C13 173.8(6) . . . . ?
C17 N2 C13 C14 -5.0(8) . . . . ?
Gd1 N2 C13 C14 170.9(4) . . . . ?
C17 N2 C13 C12 170.2(5) . . . . ?
Gd1 N2 C13 C12 -13.9(6) . . . . ?
N1 C12 C13 N2 -2.1(7) . . . . ?
C11 C12 C13 N2 -176.8(5) . . . . ?
N1 C12 C13 C14 172.9(5) . . . . ?
C11 C12 C13 C14 -1.7(9) . . . . ?
N2 C13 C14 C15 4.2(9) . . . . ?
C12 C13 C14 C15 -170.7(6) . . . . ?
C13 C14 C15 C16 0.8(10) . . . . ?
C14 C15 C16 C17 -4.6(10) . . . . ?
C13 N2 C17 C16 1.0(9) . . . . ?
Gd1 N2 C17 C16 -175.0(4) . . . . ?
C15 C16 C17 N2 3.9(9) . . . . ?

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
O1W H1W1 O2 0.85(5) 2.080(15) 2.923(5) 171(6) 1_565
O1W H1W1 O3 0.85(5) 2.66(4) 3.131(5) 117(3) 1_565
O1W H1W2 O4 0.85(5) 1.922(14) 2.765(5) 171(6) 2

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.177
####################################################################### 
# 
# 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_5-Sm
_database_code_depnum_ccdc_archive 'CCDC 1549859'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 N2 O7 S Sm'
_chemical_formula_sum            'C17 H13 N2 O7 S Sm'
_chemical_formula_weight         539.70

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.2394(3)
_cell_length_b                   8.5661(2)
_cell_length_c                   18.1081(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.825(3)
_cell_angle_gamma                90.00
_cell_volume                     1659.72(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2515
_cell_measurement_theta_min      3.47
_cell_measurement_theta_max      29.14

_exptl_crystal_description       prism
_exptl_crystal_colour            'rose pink'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1052
_exptl_absorpt_coefficient_mu    3.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4956
_exptl_absorpt_correction_T_max  0.6059
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6873
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         27.56
_reflns_number_total             3835
_reflns_number_gt                3135
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0139P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3835
_refine_ls_number_parameters     259
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_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
Sm1 Sm 0.323292(19) 1.03867(3) 0.192917(12) 0.01510(7) Uani 1 1 d . . .
S1 S 0.14605(9) 1.13096(14) 0.34021(6) 0.0166(2) Uani 1 1 d . . .
O1W O 0.4329(3) 1.2696(4) 0.26677(19) 0.0270(8) Uani 1 1 d D . .
H1W1 H 0.444(5) 1.346(3) 0.240(2) 0.040 Uiso 1 1 d D . .
H1W2 H 0.401(4) 1.301(4) 0.301(2) 0.040 Uiso 1 1 d D . .
O1 O 0.1957(3) 1.0993(4) 0.27564(16) 0.0232(7) Uani 1 1 d . . .
O2 O 0.0853(3) 1.2840(4) 0.33198(17) 0.0212(7) Uani 1 1 d . . .
O3 O 0.0649(3) 1.0051(4) 0.34951(17) 0.0231(7) Uani 1 1 d . . .
O4 O 0.3375(3) 1.3835(4) 0.38056(16) 0.0211(7) Uani 1 1 d . . .
O5 O 0.6730(3) 1.2635(4) 0.63206(17) 0.0228(7) Uani 1 1 d . . .
O6 O 0.5839(3) 1.0836(4) 0.68788(16) 0.0239(7) Uani 1 1 d . . .
N1 N 0.5525(3) 1.0701(5) 0.1873(2) 0.0230(9) Uani 1 1 d . . .
N2 N 0.3586(3) 1.1128(5) 0.0611(2) 0.0239(9) Uani 1 1 d . . .
C1 C 0.2734(4) 1.1435(6) 0.4255(2) 0.0181(10) Uani 1 1 d . . .
C2 C 0.3530(4) 1.2746(6) 0.4353(2) 0.0179(10) Uani 1 1 d . . .
C3 C 0.4514(4) 1.2810(6) 0.5052(2) 0.0187(10) Uani 1 1 d . . .
H3 H 0.5049 1.3665 0.5143 0.022 Uiso 1 1 calc R . .
C4 C 0.4723(4) 1.1656(5) 0.5611(2) 0.0182(10) Uani 1 1 d . . .
C5 C 0.3904(4) 1.0383(6) 0.5501(2) 0.0211(10) Uani 1 1 d . . .
H5 H 0.4026 0.9607 0.5876 0.025 Uiso 1 1 calc R . .
C6 C 0.2908(4) 1.0301(6) 0.4824(2) 0.0209(10) Uani 1 1 d . . .
H6 H 0.2349 0.9473 0.4751 0.025 Uiso 1 1 calc R . .
C7 C 0.5855(4) 1.1740(5) 0.6326(2) 0.0180(10) Uani 1 1 d . . .
C8 C 0.6482(4) 1.0233(6) 0.2471(3) 0.0305(12) Uani 1 1 d . . .
H8 H 0.6305 0.9733 0.2882 0.037 Uiso 1 1 calc R . .
C9 C 0.7726(5) 1.0448(7) 0.2518(3) 0.0368(13) Uani 1 1 d . . .
H9 H 0.8366 1.0040 0.2928 0.044 Uiso 1 1 calc R . .
C10 C 0.7981(5) 1.1279(7) 0.1940(3) 0.0430(15) Uani 1 1 d . . .
H10 H 0.8803 1.1515 0.1973 0.052 Uiso 1 1 calc R . .
C11 C 0.7010(5) 1.1770(7) 0.1305(3) 0.0380(14) Uani 1 1 d . . .
H11 H 0.7175 1.2325 0.0906 0.046 Uiso 1 1 calc R . .
C12 C 0.5778(4) 1.1419(6) 0.1273(3) 0.0235(11) Uani 1 1 d . . .
C13 C 0.4711(4) 1.1690(6) 0.0582(3) 0.0267(11) Uani 1 1 d . . .
C14 C 0.4807(5) 1.2348(7) -0.0097(3) 0.0393(14) Uani 1 1 d . . .
H14 H 0.5571 1.2739 -0.0111 0.047 Uiso 1 1 calc R . .
C15 C 0.3785(5) 1.2428(7) -0.0747(3) 0.0427(15) Uani 1 1 d . . .
H15 H 0.3853 1.2872 -0.1201 0.051 Uiso 1 1 calc R . .
C16 C 0.2673(5) 1.1853(6) -0.0721(3) 0.0323(13) Uani 1 1 d . . .
H16 H 0.1970 1.1889 -0.1156 0.039 Uiso 1 1 calc R . .
C17 C 0.2608(4) 1.1213(7) -0.0034(3) 0.0319(12) Uani 1 1 d . . .
H17 H 0.1844 1.0821 -0.0020 0.038 Uiso 1 1 calc R . .


_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
Sm1 O4 2.309(3) 2_545 ?
Sm1 O6 2.338(3) 3_676 ?
Sm1 O5 2.408(3) 4_585 ?
Sm1 O1 2.426(3) . ?
Sm1 O1W 2.492(3) . ?
Sm1 O2 2.510(3) 2_545 ?
Sm1 N2 2.615(3) . ?
Sm1 N1 2.623(3) . ?
S1 O3 1.455(3) . ?
S1 O2 1.465(3) . ?
S1 O1 1.467(3) . ?
S1 C1 1.758(4) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2 Sm1 2.510(3) 2 ?
O4 C2 1.333(5) . ?
O4 Sm1 2.309(3) 2 ?
O5 C7 1.250(5) . ?
O5 Sm1 2.408(3) 4_686 ?
O6 C7 1.270(5) . ?
O6 Sm1 2.338(3) 3_676 ?
N1 C8 1.334(6) . ?
N1 C12 1.352(5) . ?
N2 C17 1.339(6) . ?
N2 C13 1.368(6) . ?
C1 C6 1.386(6) . ?
C1 C2 1.413(6) . ?
C2 C3 1.404(6) . ?
C3 C4 1.383(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(6) . ?
C4 C7 1.514(6) . ?
C5 C6 1.386(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.388(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.366(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.386(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.401(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.463(7) . ?
C13 C14 1.387(6) . ?
C14 C15 1.372(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.358(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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
O4 Sm1 O6 108.88(11) 2_545 3_676 ?
O4 Sm1 O5 79.96(11) 2_545 4_585 ?
O6 Sm1 O5 142.19(10) 3_676 4_585 ?
O4 Sm1 O1 88.44(10) 2_545 . ?
O6 Sm1 O1 72.95(10) 3_676 . ?
O5 Sm1 O1 70.58(10) 4_585 . ?
O4 Sm1 O1W 159.61(11) 2_545 . ?
O6 Sm1 O1W 81.52(11) 3_676 . ?
O5 Sm1 O1W 81.33(11) 4_585 . ?
O1 Sm1 O1W 77.72(10) . . ?
O4 Sm1 O2 71.78(10) 2_545 2_545 ?
O6 Sm1 O2 71.64(10) 3_676 2_545 ?
O5 Sm1 O2 142.90(10) 4_585 2_545 ?
O1 Sm1 O2 130.45(10) . 2_545 ?
O1W Sm1 O2 128.61(10) . 2_545 ?
O4 Sm1 N2 85.67(11) 2_545 . ?
O6 Sm1 N2 143.32(11) 3_676 . ?
O5 Sm1 N2 72.10(11) 4_585 . ?
O1 Sm1 N2 142.68(11) . . ?
O1W Sm1 N2 96.25(12) . . ?
O2 Sm1 N2 82.08(11) 2_545 . ?
O4 Sm1 N1 129.90(11) 2_545 . ?
O6 Sm1 N1 85.18(11) 3_676 . ?
O5 Sm1 N1 118.00(11) 4_585 . ?
O1 Sm1 N1 140.83(11) . . ?
O1W Sm1 N1 67.01(11) . . ?
O2 Sm1 N1 67.75(11) 2_545 . ?
N2 Sm1 N1 60.94(12) . . ?
O3 S1 O2 112.70(18) . . ?
O3 S1 O1 111.11(19) . . ?
O2 S1 O1 111.32(19) . . ?
O3 S1 C1 108.3(2) . . ?
O2 S1 C1 105.3(2) . . ?
O1 S1 C1 107.77(18) . . ?
Sm1 O1W H1W1 116(3) . . ?
Sm1 O1W H1W2 113(3) . . ?
H1W1 O1W H1W2 110.4(18) . . ?
S1 O1 Sm1 166.61(19) . . ?
S1 O2 Sm1 126.35(16) . 2 ?
C2 O4 Sm1 137.1(2) . 2 ?
C7 O5 Sm1 150.7(3) . 4_686 ?
C7 O6 Sm1 153.0(3) . 3_676 ?
C8 N1 C12 118.3(4) . . ?
C8 N1 Sm1 119.6(3) . . ?
C12 N1 Sm1 121.9(3) . . ?
C17 N2 C13 117.9(4) . . ?
C17 N2 Sm1 119.8(3) . . ?
C13 N2 Sm1 121.4(3) . . ?
C6 C1 C2 121.6(4) . . ?
C6 C1 S1 120.2(3) . . ?
C2 C1 S1 118.2(3) . . ?
O4 C2 C3 122.1(4) . . ?
O4 C2 C1 121.9(4) . . ?
C3 C2 C1 116.0(4) . . ?
C4 C3 C2 122.9(4) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 C7 120.2(4) . . ?
C5 C4 C7 120.1(4) . . ?
C6 C5 C4 118.8(4) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 121.0(4) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O5 C7 O6 125.5(4) . . ?
O5 C7 C4 118.7(4) . . ?
O6 C7 C4 115.7(4) . . ?
N1 C8 C9 123.8(5) . . ?
N1 C8 H8 118.1 . . ?
C9 C8 H8 118.1 . . ?
C10 C9 C8 117.8(5) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C9 C10 C11 119.8(5) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 119.1(5) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N1 C12 C11 120.9(5) . . ?
N1 C12 C13 116.1(4) . . ?
C11 C12 C13 122.9(4) . . ?
N2 C13 C14 120.0(5) . . ?
N2 C13 C12 115.9(4) . . ?
C14 C13 C12 123.8(4) . . ?
C15 C14 C13 120.6(5) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C14 119.3(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 118.6(5) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
N2 C17 C16 123.5(5) . . ?
N2 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?

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
O3 S1 O1 Sm1 -109.6(9) . . . . ?
O2 S1 O1 Sm1 123.9(9) . . . . ?
C1 S1 O1 Sm1 8.9(10) . . . . ?
O4 Sm1 O1 S1 137.5(9) 2_545 . . . ?
O6 Sm1 O1 S1 27.2(9) 3_676 . . . ?
O5 Sm1 O1 S1 -142.6(10) 4_585 . . . ?
O1W Sm1 O1 S1 -57.5(9) . . . . ?
O2 Sm1 O1 S1 73.3(10) 2_545 . . . ?
N2 Sm1 O1 S1 -141.7(9) . . . . ?
N1 Sm1 O1 S1 -31.7(10) . . . . ?
O3 S1 O2 Sm1 -176.40(18) . . . 2 ?
O1 S1 O2 Sm1 -50.8(3) . . . 2 ?
C1 S1 O2 Sm1 65.7(2) . . . 2 ?
O4 Sm1 N1 C8 -114.1(4) 2_545 . . . ?
O6 Sm1 N1 C8 -3.4(4) 3_676 . . . ?
O5 Sm1 N1 C8 145.1(4) 4_585 . . . ?
O1 Sm1 N1 C8 51.9(4) . . . . ?
O1W Sm1 N1 C8 79.4(4) . . . . ?
O2 Sm1 N1 C8 -75.5(4) 2_545 . . . ?
N2 Sm1 N1 C8 -168.8(4) . . . . ?
O4 Sm1 N1 C12 70.3(4) 2_545 . . . ?
O6 Sm1 N1 C12 -179.1(4) 3_676 . . . ?
O5 Sm1 N1 C12 -30.5(4) 4_585 . . . ?
O1 Sm1 N1 C12 -123.8(3) . . . . ?
O1W Sm1 N1 C12 -96.3(4) . . . . ?
O2 Sm1 N1 C12 108.8(4) 2_545 . . . ?
N2 Sm1 N1 C12 15.5(3) . . . . ?
O4 Sm1 N2 C17 33.4(4) 2_545 . . . ?
O6 Sm1 N2 C17 149.6(4) 3_676 . . . ?
O5 Sm1 N2 C17 -47.4(4) 4_585 . . . ?
O1 Sm1 N2 C17 -48.3(5) . . . . ?
O1W Sm1 N2 C17 -126.2(4) . . . . ?
O2 Sm1 N2 C17 105.6(4) 2_545 . . . ?
N1 Sm1 N2 C17 174.5(4) . . . . ?
O4 Sm1 N2 C13 -157.9(4) 2_545 . . . ?
O6 Sm1 N2 C13 -41.7(4) 3_676 . . . ?
O5 Sm1 N2 C13 121.3(4) 4_585 . . . ?
O1 Sm1 N2 C13 120.4(3) . . . . ?
O1W Sm1 N2 C13 42.5(4) . . . . ?
O2 Sm1 N2 C13 -85.7(4) 2_545 . . . ?
N1 Sm1 N2 C13 -16.8(3) . . . . ?
O3 S1 C1 C6 8.3(4) . . . . ?
O2 S1 C1 C6 129.1(3) . . . . ?
O1 S1 C1 C6 -112.0(4) . . . . ?
O3 S1 C1 C2 -169.0(3) . . . . ?
O2 S1 C1 C2 -48.2(4) . . . . ?
O1 S1 C1 C2 70.7(4) . . . . ?
Sm1 O4 C2 C3 -129.9(4) 2 . . . ?
Sm1 O4 C2 C1 52.0(6) 2 . . . ?
C6 C1 C2 O4 179.5(4) . . . . ?
S1 C1 C2 O4 -3.3(6) . . . . ?
C6 C1 C2 C3 1.2(6) . . . . ?
S1 C1 C2 C3 178.5(3) . . . . ?
O4 C2 C3 C4 -177.0(4) . . . . ?
C1 C2 C3 C4 1.2(6) . . . . ?
C2 C3 C4 C5 -2.3(7) . . . . ?
C2 C3 C4 C7 175.6(4) . . . . ?
C3 C4 C5 C6 1.0(6) . . . . ?
C7 C4 C5 C6 -177.0(4) . . . . ?
C4 C5 C6 C1 1.4(7) . . . . ?
C2 C1 C6 C5 -2.6(7) . . . . ?
S1 C1 C6 C5 -179.8(3) . . . . ?
Sm1 O5 C7 O6 -49.0(8) 4_686 . . . ?
Sm1 O5 C7 C4 133.2(5) 4_686 . . . ?
Sm1 O6 C7 O5 -8.5(9) 3_676 . . . ?
Sm1 O6 C7 C4 169.4(4) 3_676 . . . ?
C3 C4 C7 O5 -16.3(6) . . . . ?
C5 C4 C7 O5 161.6(4) . . . . ?
C3 C4 C7 O6 165.7(4) . . . . ?
C5 C4 C7 O6 -16.4(6) . . . . ?
C12 N1 C8 C9 0.4(8) . . . . ?
Sm1 N1 C8 C9 -175.4(4) . . . . ?
N1 C8 C9 C10 4.5(8) . . . . ?
C8 C9 C10 C11 -5.0(8) . . . . ?
C9 C10 C11 C12 0.8(9) . . . . ?
C8 N1 C12 C11 -4.8(7) . . . . ?
Sm1 N1 C12 C11 170.9(4) . . . . ?
C8 N1 C12 C13 170.8(4) . . . . ?
Sm1 N1 C12 C13 -13.5(6) . . . . ?
C10 C11 C12 N1 4.2(8) . . . . ?
C10 C11 C12 C13 -171.0(5) . . . . ?
C17 N2 C13 C14 1.2(7) . . . . ?
Sm1 N2 C13 C14 -167.7(4) . . . . ?
C17 N2 C13 C12 -173.6(5) . . . . ?
Sm1 N2 C13 C12 17.5(6) . . . . ?
N1 C12 C13 N2 -2.5(6) . . . . ?
C11 C12 C13 N2 172.9(5) . . . . ?
N1 C12 C13 C14 -177.1(5) . . . . ?
C11 C12 C13 C14 -1.6(8) . . . . ?
N2 C13 C14 C15 -0.8(8) . . . . ?
C12 C13 C14 C15 173.6(5) . . . . ?
C13 C14 C15 C16 -0.1(9) . . . . ?
C14 C15 C16 C17 0.4(9) . . . . ?
C13 N2 C17 C16 -0.8(8) . . . . ?
Sm1 N2 C17 C16 168.3(4) . . . . ?
C15 C16 C17 N2 0.0(9) . . . . ?

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
O1W H1W1 O1 0.85(5) 2.65(4) 3.158(5) 120(3) 2
O1W H1W1 O3 0.85(5) 2.096(17) 2.922(5) 165(5) 2
O1W H1W2 O4 0.85(5) 1.930(12) 2.775(4) 176(5) .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.867
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.154
####################################################################### 
# 
# 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_2-Tb
_database_code_depnum_ccdc_archive 'CCDC 1549844'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 O28 S2 Tb2, 2(C7 H5 O6 S), 8(H2 O)'
_chemical_formula_sum            'C30 H60 O48 S4 Tb2'
_chemical_formula_weight         1634.86

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8714(5)
_cell_length_b                   12.3614(7)
_cell_length_c                   15.0485(8)
_cell_angle_alpha                107.370(5)
_cell_angle_beta                 97.074(5)
_cell_angle_gamma                96.371(5)
_cell_volume                     1369.86(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3180
_cell_measurement_theta_min      3.75
_cell_measurement_theta_max      28.75

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             818
_exptl_absorpt_coefficient_mu    2.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5741
_exptl_absorpt_correction_T_max  0.6921
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8764
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6253
_reflns_number_gt                5486
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_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)+(0.0337P)²+0.0698P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6253
_refine_ls_number_parameters     451
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.028
_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 0.79392(2) 0.704388(15) 0.019118(13) 0.01917(7) Uani 1 1 d . . .
S1 S 0.74294(13) 0.64531(8) 0.24747(7) 0.0210(2) Uani 1 1 d . . .
S2 S 0.56558(15) 0.13609(9) 0.26707(8) 0.0285(2) Uani 1 1 d . . .
O1 O 0.7900(4) 0.6971(2) 0.17705(19) 0.0262(7) Uani 1 1 d . . .
O1W O 0.6333(4) 0.8633(3) 0.0917(2) 0.0358(8) Uani 1 1 d D . .
H1W1 H 0.707(5) 0.922(3) 0.124(3) 0.054 Uiso 1 1 d D . .
H1W2 H 0.592(6) 0.830(4) 0.128(3) 0.054 Uiso 1 1 d D . .
O2 O 0.8645(4) 0.5709(2) 0.2668(2) 0.0289(7) Uani 1 1 d . . .
O2W O 0.9910(4) 0.8733(3) 0.1274(2) 0.0389(8) Uani 1 1 d D . .
H2W1 H 1.029(5) 0.883(5) 0.1853(13) 0.058 Uiso 1 1 d D . .
H2W2 H 1.076(4) 0.890(5) 0.101(3) 0.058 Uiso 1 1 d D . .
O3 O 0.5633(4) 0.5893(2) 0.2257(2) 0.0304(7) Uani 1 1 d . . .
O3W O 0.8628(5) 0.8478(3) -0.0543(2) 0.0387(8) Uani 1 1 d D . .
H3W1 H 0.892(7) 0.823(4) -0.1081(18) 0.058 Uiso 1 1 d D . .
H3W2 H 0.807(7) 0.903(3) -0.052(3) 0.058 Uiso 1 1 d D . .
O4 O 0.5625(4) 0.8496(2) 0.2791(2) 0.0274(7) Uani 1 1 d D . .
H4O H 0.518(6) 0.910(3) 0.288(4) 0.041 Uiso 1 1 d D . .
O4W O 0.9458(4) 0.6249(3) -0.1109(2) 0.0392(8) Uani 1 1 d D . .
H4W1 H 1.048(3) 0.660(4) -0.102(3) 0.059 Uiso 1 1 d D . .
H4W2 H 0.900(5) 0.606(5) -0.1682(13) 0.059 Uiso 1 1 d D . .
O5 O 0.7412(4) 1.1230(3) 0.6047(2) 0.0338(7) Uani 1 1 d D . .
H5O H 0.762(7) 1.178(3) 0.656(2) 0.051 Uiso 1 1 d D . .
O5W O 1.0555(4) 0.6458(3) 0.0674(2) 0.0396(8) Uani 1 1 d D . .
H5W1 H 1.109(6) 0.594(3) 0.038(3) 0.059 Uiso 1 1 d D . .
H5W2 H 1.092(6) 0.665(4) 0.1261(9) 0.059 Uiso 1 1 d D . .
O6 O 0.9241(4) 1.0421(3) 0.6806(2) 0.0387(8) Uani 1 1 d . . .
O6W O 0.5990(4) 0.6472(3) -0.1351(2) 0.0325(7) Uani 1 1 d D . .
H6W1 H 0.541(6) 0.5815(18) -0.165(3) 0.049 Uiso 1 1 d D . .
H6W2 H 0.577(6) 0.694(3) -0.165(3) 0.049 Uiso 1 1 d D . .
O7 O 0.4775(5) 0.1708(3) 0.1927(3) 0.0584(11) Uani 1 1 d . . .
O7W O 1.2628(5) 0.9576(4) 0.0499(4) 0.0638(12) Uani 1 1 d D . .
H7W1 H 1.261(7) 0.906(5) -0.003(3) 0.096 Uiso 1 1 d D . .
H7W2 H 1.364(4) 0.970(6) 0.082(4) 0.096 Uiso 1 1 d D . .
O8 O 0.7253(5) 0.0951(3) 0.2434(3) 0.0507(10) Uani 1 1 d . . .
O8W O 0.7307(5) 0.2501(4) 0.0757(3) 0.0463(9) Uani 1 1 d D . .
H8W1 H 0.658(6) 0.280(5) 0.047(3) 0.069 Uiso 1 1 d D . .
H8W2 H 0.692(6) 0.239(5) 0.123(3) 0.069 Uiso 1 1 d D . .
O9 O 0.4538(4) 0.0530(3) 0.2942(2) 0.0360(8) Uani 1 1 d . . .
O9W O 1.2283(4) 0.6829(3) 0.2491(2) 0.0330(7) Uani 1 1 d D . .
H9W1 H 1.182(5) 0.631(3) 0.269(4) 0.050 Uiso 1 1 d D . .
H9W2 H 1.324(4) 0.668(4) 0.232(4) 0.050 Uiso 1 1 d D . .
O10 O 0.7635(5) 0.3601(3) 0.2802(2) 0.0389(9) Uani 1 1 d D . .
H10O H 0.803(7) 0.426(2) 0.278(4) 0.058 Uiso 1 1 d D . .
O10W O 0.9283(5) 0.8297(3) 0.7567(3) 0.0421(9) Uani 1 1 d D . .
HAW H 0.876(5) 0.879(4) 0.740(4) 0.063 Uiso 1 1 d D . .
HBW H 1.0366(16) 0.847(4) 0.760(4) 0.063 Uiso 1 1 d D . .
O11 O 0.8278(5) 0.6430(3) 0.6056(2) 0.0474(10) Uani 1 1 d D . .
H11O H 0.860(8) 0.694(4) 0.659(2) 0.071 Uiso 1 1 d D . .
O12 O 0.7765(5) 0.5352(3) 0.6963(2) 0.0465(10) Uani 1 1 d . . .
O13 O 0.4885(4) 0.6460(2) 0.0305(2) 0.0264(7) Uani 1 1 d . . .
O14 O 0.2843(4) 0.4969(2) 0.0138(2) 0.0271(7) Uani 1 1 d . . .
C1 C 0.7660(5) 0.7616(3) 0.3536(3) 0.0194(8) Uani 1 1 d . . .
C2 C 0.6723(5) 0.8519(3) 0.3575(3) 0.0217(8) Uani 1 1 d . . .
C3 C 0.6932(5) 0.9426(3) 0.4415(3) 0.0226(9) Uani 1 1 d . . .
H3A H 0.6311 1.0031 0.4448 0.027 Uiso 1 1 calc R . .
C4 C 0.8060(5) 0.9432(4) 0.5201(3) 0.0241(9) Uani 1 1 d . . .
C5 C 0.8997(6) 0.8534(4) 0.5155(3) 0.0261(9) Uani 1 1 d . . .
H5A H 0.9757 0.8538 0.5681 0.031 Uiso 1 1 calc R . .
C6 C 0.8792(6) 0.7635(4) 0.4322(3) 0.0252(9) Uani 1 1 d . . .
H6A H 0.9423 0.7035 0.4290 0.030 Uiso 1 1 calc R . .
C7 C 0.8316(6) 1.0407(4) 0.6104(3) 0.0261(9) Uani 1 1 d . . .
C8 C 0.6229(5) 0.2594(3) 0.3684(3) 0.0245(9) Uani 1 1 d . . .
C9 C 0.7176(6) 0.3598(4) 0.3642(3) 0.0256(9) Uani 1 1 d . . .
C10 C 0.7635(6) 0.4540(4) 0.4453(3) 0.0273(10) Uani 1 1 d . . .
H10A H 0.8257 0.5213 0.4429 0.033 Uiso 1 1 calc R . .
C11 C 0.7167(6) 0.4479(4) 0.5305(3) 0.0260(9) Uani 1 1 d . . .
C12 C 0.6181(6) 0.3489(4) 0.5336(3) 0.0323(11) Uani 1 1 d . . .
H12A H 0.5834 0.3456 0.5898 0.039 Uiso 1 1 calc R . .
C13 C 0.5721(6) 0.2557(4) 0.4527(3) 0.0322(10) Uani 1 1 d . . .
H13A H 0.5061 0.1895 0.4546 0.039 Uiso 1 1 calc R . .
C14 C 0.7752(6) 0.5453(4) 0.6194(3) 0.0283(10) Uani 1 1 d . . .
C15 C 0.4349(5) 0.5419(3) 0.0129(3) 0.0217(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 O5W 2.360(3) . ?
Tb1 O14 2.380(3) 2_665 ?
Tb1 O3W 2.400(3) . ?
Tb1 O1 2.409(3) . ?
Tb1 O4W 2.431(3) . ?
Tb1 O2W 2.459(3) . ?
Tb1 O13 2.474(3) . ?
Tb1 O6W 2.478(3) . ?
Tb1 O1W 2.502(3) . ?
S1 O1 1.456(3) . ?
S1 O3 1.456(3) . ?
S1 O2 1.460(3) . ?
S1 C1 1.775(4) . ?
S2 O7 1.442(4) . ?
S2 O8 1.452(4) . ?
S2 O9 1.461(3) . ?
S2 C8 1.773(4) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O2W H2W1 0.85(5) . ?
O2W H2W2 0.85(5) . ?
O3W H3W1 0.85(5) . ?
O3W H3W2 0.85(5) . ?
O4 C2 1.364(5) . ?
O4 H4O 0.85(5) . ?
O4W H4W1 0.85(5) . ?
O4W H4W2 0.85(5) . ?
O5 C7 1.321(6) . ?
O5 H5O 0.85(5) . ?
O5W H5W1 0.85(5) . ?
O5W H5W2 0.85(5) . ?
O6 C7 1.201(5) . ?
O6W H6W1 0.85(5) . ?
O6W H6W2 0.85(5) . ?
O7W H7W1 0.85(5) . ?
O7W H7W2 0.85(5) . ?
O8W H8W1 0.85(5) . ?
O8W H8W2 0.85(5) . ?
O9W H9W1 0.85(5) . ?
O9W H9W2 0.85(5) . ?
O10 C9 1.358(5) . ?
O10 H10O 0.85(5) . ?
O10W HAW 0.85(5) . ?
O10W HBW 0.85(5) . ?
O11 C14 1.316(5) . ?
O11 H11O 0.85(5) . ?
O12 C14 1.200(5) . ?
O13 C15 1.246(5) . ?
O14 C15 1.255(5) . ?
O14 Tb1 2.380(3) 2_665 ?
C1 C6 1.383(6) . ?
C1 C2 1.396(6) . ?
C2 C3 1.394(5) . ?
C3 C4 1.387(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(6) . ?
C4 C7 1.497(6) . ?
C5 C6 1.382(6) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C8 C13 1.387(6) . ?
C8 C9 1.397(5) . ?
C9 C10 1.387(6) . ?
C10 C11 1.397(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.391(6) . ?
C11 C14 1.488(6) . ?
C12 C13 1.380(6) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C15 C15 1.539(8) 2_665 ?

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
O5W Tb1 O14 76.54(12) . 2_665 ?
O5W Tb1 O3W 107.72(14) . . ?
O14 Tb1 O3W 142.58(11) 2_665 . ?
O5W Tb1 O1 72.81(11) . . ?
O14 Tb1 O1 80.13(10) 2_665 . ?
O3W Tb1 O1 137.17(10) . . ?
O5W Tb1 O4W 66.88(12) . . ?
O14 Tb1 O4W 77.36(11) 2_665 . ?
O3W Tb1 O4W 71.05(12) . . ?
O1 Tb1 O4W 137.27(12) . . ?
O5W Tb1 O2W 71.31(13) . . ?
O14 Tb1 O2W 142.58(12) 2_665 . ?
O3W Tb1 O2W 67.70(12) . . ?
O1 Tb1 O2W 72.57(10) . . ?
O4W Tb1 O2W 106.14(12) . . ?
O5W Tb1 O13 132.78(12) . . ?
O14 Tb1 O13 66.31(9) 2_665 . ?
O3W Tb1 O13 119.49(12) . . ?
O1 Tb1 O13 73.01(10) . . ?
O4W Tb1 O13 127.28(11) . . ?
O2W Tb1 O13 126.06(10) . . ?
O5W Tb1 O6W 132.06(11) . . ?
O14 Tb1 O6W 77.45(11) 2_665 . ?
O3W Tb1 O6W 72.75(11) . . ?
O1 Tb1 O6W 139.55(10) . . ?
O4W Tb1 O6W 68.54(12) . . ?
O2W Tb1 O6W 139.27(11) . . ?
O13 Tb1 O6W 67.25(11) . . ?
O5W Tb1 O1W 134.50(11) . . ?
O14 Tb1 O1W 129.13(10) 2_665 . ?
O3W Tb1 O1W 75.06(11) . . ?
O1 Tb1 O1W 75.98(11) . . ?
O4W Tb1 O1W 144.84(12) . . ?
O2W Tb1 O1W 68.22(12) . . ?
O13 Tb1 O1W 63.97(10) . . ?
O6W Tb1 O1W 92.86(11) . . ?
O1 S1 O3 112.67(19) . . ?
O1 S1 O2 112.30(18) . . ?
O3 S1 O2 112.78(18) . . ?
O1 S1 C1 105.20(17) . . ?
O3 S1 C1 107.57(18) . . ?
O2 S1 C1 105.65(19) . . ?
O7 S2 O8 111.6(3) . . ?
O7 S2 O9 112.5(2) . . ?
O8 S2 O9 111.8(2) . . ?
O7 S2 C8 107.4(2) . . ?
O8 S2 C8 107.1(2) . . ?
O9 S2 C8 106.02(19) . . ?
S1 O1 Tb1 154.94(18) . . ?
Tb1 O1W H1W1 108(4) . . ?
H1W1 O1W H1W2 109.7(17) . . ?
Tb1 O2W H2W1 125(4) . . ?
Tb1 O2W H2W2 110(3) . . ?
H2W1 O2W H2W2 108.6(17) . . ?
Tb1 O3W H3W1 115(3) . . ?
Tb1 O3W H3W2 123(3) . . ?
H3W1 O3W H3W2 110.5(18) . . ?
C2 O4 H4O 112(4) . . ?
Tb1 O4W H4W1 112(3) . . ?
Tb1 O4W H4W2 123(4) . . ?
H4W1 O4W H4W2 110.7(18) . . ?
C7 O5 H5O 111(4) . . ?
Tb1 O5W H5W1 131(3) . . ?
Tb1 O5W H5W2 117(3) . . ?
H5W1 O5W H5W2 109.3(17) . . ?
Tb1 O6W H6W1 127(3) . . ?
Tb1 O6W H6W2 123(3) . . ?
H6W1 O6W H6W2 109.3(17) . . ?
H7W1 O7W H7W2 108.6(18) . . ?
H8W1 O8W H8W2 109.5(18) . . ?
H9W1 O9W H9W2 111.1(18) . . ?
C9 O10 H10O 114(4) . . ?
HAW O10W HBW 110.2(18) . . ?
C14 O11 H11O 108(4) . . ?
C15 O13 Tb1 118.3(2) . . ?
C15 O14 Tb1 122.3(3) . 2_665 ?
C6 C1 C2 120.0(4) . . ?
C6 C1 S1 119.9(3) . . ?
C2 C1 S1 120.2(3) . . ?
O4 C2 C3 121.4(4) . . ?
O4 C2 C1 119.4(4) . . ?
C3 C2 C1 119.2(4) . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 C7 121.0(4) . . ?
C5 C4 C7 118.9(4) . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
O6 C7 O5 124.2(4) . . ?
O6 C7 C4 122.6(4) . . ?
O5 C7 C4 113.2(4) . . ?
C13 C8 C9 119.9(4) . . ?
C13 C8 S2 119.3(3) . . ?
C9 C8 S2 120.9(3) . . ?
O10 C9 C10 122.6(4) . . ?
O10 C9 C8 118.0(4) . . ?
C10 C9 C8 119.4(4) . . ?
C9 C10 C11 120.2(4) . . ?
C9 C10 H10A 119.9 . . ?
C11 C10 H10A 119.9 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 C14 119.0(4) . . ?
C10 C11 C14 120.8(4) . . ?
C13 C12 C11 119.3(4) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C12 C13 C8 121.0(4) . . ?
C12 C13 H13A 119.5 . . ?
C8 C13 H13A 119.5 . . ?
O12 C14 O11 123.3(4) . . ?
O12 C14 C11 123.0(4) . . ?
O11 C14 C11 113.7(4) . . ?
O13 C15 O14 126.9(4) . . ?
O13 C15 C15 117.4(4) . 2_665 ?
O14 C15 C15 115.7(4) . 2_665 ?

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
O3 S1 O1 Tb1 -41.9(5) . . . . ?
O2 S1 O1 Tb1 86.8(5) . . . . ?
C1 S1 O1 Tb1 -158.8(4) . . . . ?
O5W Tb1 O1 S1 -98.3(5) . . . . ?
O14 Tb1 O1 S1 -19.5(4) 2_665 . . . ?
O3W Tb1 O1 S1 163.9(4) . . . . ?
O4W Tb1 O1 S1 -78.4(5) . . . . ?
O2W Tb1 O1 S1 -173.6(5) . . . . ?
O13 Tb1 O1 S1 48.6(4) . . . . ?
O6W Tb1 O1 S1 37.6(5) . . . . ?
O1W Tb1 O1 S1 115.2(5) . . . . ?
O5W Tb1 O13 C15 -42.4(3) . . . . ?
O14 Tb1 O13 C15 -1.2(3) 2_665 . . . ?
O3W Tb1 O13 C15 137.2(3) . . . . ?
O1 Tb1 O13 C15 -87.7(3) . . . . ?
O4W Tb1 O13 C15 49.4(3) . . . . ?
O2W Tb1 O13 C15 -140.1(3) . . . . ?
O6W Tb1 O13 C15 84.6(3) . . . . ?
O1W Tb1 O13 C15 -170.0(3) . . . . ?
O1 S1 C1 C6 -120.9(3) . . . . ?
O3 S1 C1 C6 118.8(3) . . . . ?
O2 S1 C1 C6 -1.9(4) . . . . ?
O1 S1 C1 C2 58.1(4) . . . . ?
O3 S1 C1 C2 -62.3(4) . . . . ?
O2 S1 C1 C2 177.0(3) . . . . ?
C6 C1 C2 O4 179.3(3) . . . . ?
S1 C1 C2 O4 0.3(5) . . . . ?
C6 C1 C2 C3 -0.7(6) . . . . ?
S1 C1 C2 C3 -179.7(3) . . . . ?
O4 C2 C3 C4 -179.8(4) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
C2 C3 C4 C5 0.3(6) . . . . ?
C2 C3 C4 C7 179.2(3) . . . . ?
C3 C4 C5 C6 -0.3(6) . . . . ?
C7 C4 C5 C6 -179.2(4) . . . . ?
C4 C5 C6 C1 -0.3(6) . . . . ?
C2 C1 C6 C5 0.8(6) . . . . ?
S1 C1 C6 C5 179.7(3) . . . . ?
C3 C4 C7 O6 177.6(4) . . . . ?
C5 C4 C7 O6 -3.5(6) . . . . ?
C3 C4 C7 O5 -1.7(6) . . . . ?
C5 C4 C7 O5 177.2(4) . . . . ?
O7 S2 C8 C13 126.0(4) . . . . ?
O8 S2 C8 C13 -114.0(4) . . . . ?
O9 S2 C8 C13 5.5(4) . . . . ?
O7 S2 C8 C9 -53.8(4) . . . . ?
O8 S2 C8 C9 66.2(4) . . . . ?
O9 S2 C8 C9 -174.3(4) . . . . ?
C13 C8 C9 O10 -179.5(4) . . . . ?
S2 C8 C9 O10 0.3(6) . . . . ?
C13 C8 C9 C10 1.6(7) . . . . ?
S2 C8 C9 C10 -178.6(4) . . . . ?
O10 C9 C10 C11 -178.3(4) . . . . ?
C8 C9 C10 C11 0.6(7) . . . . ?
C9 C10 C11 C12 -2.5(7) . . . . ?
C9 C10 C11 C14 175.8(4) . . . . ?
C10 C11 C12 C13 2.2(7) . . . . ?
C14 C11 C12 C13 -176.1(4) . . . . ?
C11 C12 C13 C8 0.0(7) . . . . ?
C9 C8 C13 C12 -1.9(7) . . . . ?
S2 C8 C13 C12 178.3(4) . . . . ?
C12 C11 C14 O12 17.4(7) . . . . ?
C10 C11 C14 O12 -161.0(5) . . . . ?
C12 C11 C14 O11 -163.6(4) . . . . ?
C10 C11 C14 O11 18.0(6) . . . . ?
Tb1 O13 C15 O14 -178.9(3) . . . . ?
Tb1 O13 C15 C15 1.1(6) . . . 2_665 ?
Tb1 O14 C15 O13 -178.8(3) 2_665 . . . ?
Tb1 O14 C15 C15 1.3(6) 2_665 . . 2_665 ?

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
O1W H1W1 O8 0.85(5) 2.33(4) 3.029(5) 140(5) 1_565
O1W H1W2 O4 0.85(5) 2.26(3) 2.992(5) 145(4) .
O1W H1W2 O1 0.85(5) 2.59(5) 3.024(5) 113(4) .
O2W H2W1 O6 0.85(5) 1.92(2) 2.730(4) 157(6) 2_776
O2W H2W2 O7W 0.85(5) 1.961(16) 2.805(6) 169(6) .
O3W H3W1 O10W 0.85(5) 2.12(2) 2.902(5) 154(4) 1_554
O3W H3W2 O7W 0.85(5) 1.860(19) 2.687(6) 165(6) 2_775
O4 H4O O9 0.85(5) 1.868(15) 2.700(4) 168(5) 1_565
O4W H4W1 O8W 0.85(5) 1.889(12) 2.731(5) 174(6) 2_765
O4W H4W2 O12 0.85(5) 2.032(14) 2.868(5) 170(5) 1_554
O5 H5O O9W 0.85(5) 1.867(18) 2.691(4) 165(6) 2_776
O5W H5W1 O14 0.85(5) 1.92(2) 2.736(4) 160(5) 1_655
O5W H5W2 O9W 0.85(5) 1.958(18) 2.781(5) 163(4) .
O6W H6W1 O3 0.85(5) 2.059(12) 2.899(4) 169(4) 2_665
O6W H6W2 O7 0.85(5) 1.918(17) 2.740(5) 162(5) 2_665
O7W H7W1 O8W 0.85(5) 1.92(4) 2.705(6) 151(7) 2_765
O7W H7W2 O7 0.85(5) 2.53(6) 3.026(5) 118(5) 1_665
O8W H8W1 O13 0.85(5) 2.020(12) 2.868(5) 172(5) 2_665
O8W H8W2 O7 0.85(5) 2.30(3) 3.081(5) 152(5) .
O8W H8W2 O10 0.85(5) 2.35(5) 2.935(5) 126(5) .
O9W H9W1 O12 0.85(5) 2.32(3) 3.042(5) 144(4) 2_766
O9W H9W1 O2 0.85(5) 2.52(4) 3.117(4) 128(4) .
O9W H9W2 O3 0.85(5) 2.22(2) 3.013(4) 158(4) 1_655
O9W H9W2 O4 0.85(5) 2.62(4) 3.053(4) 113(4) 1_655
O10 H10O O2 0.85(5) 1.871(13) 2.712(4) 173(6) .
O10W HAW O6 0.85(5) 2.45(3) 3.164(5) 142(4) .
O10W HBW O8 0.85(5) 1.944(15) 2.781(5) 170(5) 2_766
O11 H11O O10W 0.85(5) 1.85(2) 2.671(5) 165(6) .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.131
