# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_zht-3-3
_database_code_depnum_ccdc_archive 'CCDC 1544848'
_audit_update_record             
;
2017-04-19 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H136 N14 O82 S16 Sm10'
_chemical_formula_weight         3997.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   16.0748(4)
_cell_length_b                   16.0748(4)
_cell_length_c                   22.7327(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5874.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4047
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      23.45

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.260
_exptl_crystal_F_000             3868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.307
_shelx_estimated_absorpt_T_min   0.545
_shelx_estimated_absorpt_T_max   0.593
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25854
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.552
_diffrn_reflns_theta_max         24.056
_diffrn_reflns_theta_full        24.056
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4622
_reflns_number_gt                3400
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0621P)²+14.2659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4622
_refine_ls_number_parameters     358
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.095
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.42109(3) 0.20174(3) 0.24534(2) 0.02668(17) Uani 1 1 d . . . . .
Sm2 Sm 0.42507(3) 0.41792(3) 0.09271(2) 0.03124(17) Uani 1 1 d . . . . .
Sm3 Sm 0.2500 0.2500 0.12930(3) 0.02254(19) Uani 1 2 d S T P . .
S1 S 0.45721(17) 0.19853(17) 0.09142(12) 0.0364(6) Uani 1 1 d . . . . .
S2 S 0.51481(18) 0.39723(19) 0.23565(13) 0.0431(7) Uani 1 1 d . . . . .
S3 S 0.38627(17) 0.47962(19) -0.03196(13) 0.0431(7) Uani 1 1 d . . . . .
S4 S 0.3479(2) 0.56553(18) 0.16369(13) 0.0493(8) Uani 1 1 d . . . . .
O1 O 0.2972(3) 0.1605(4) 0.2021(2) 0.0204(13) Uani 1 1 d . . . . .
O2 O 0.3596(4) 0.3111(3) 0.1852(3) 0.0218(14) Uani 1 1 d . . . . .
O3 O 0.3026(4) 0.3528(4) 0.0761(2) 0.0211(13) Uani 1 1 d . . . . .
O4 O 0.3667(4) 0.1848(4) 0.0851(3) 0.0413(18) Uani 1 1 d . . . . .
O5 O 0.4759(4) 0.2850(4) 0.0750(3) 0.0449(19) Uani 1 1 d . . . . .
O6 O 0.3187(5) 0.4754(4) 0.1571(3) 0.0447(19) Uani 1 1 d . . . . .
O7 O 0.4795(4) 0.1852(5) 0.1534(3) 0.0424(19) Uani 1 1 d . . . . .
O8 O 0.4408(5) 0.4382(5) 0.2603(3) 0.046(2) Uani 1 1 d . . . . .
O9 O 0.5018(5) 0.1429(5) 0.0536(3) 0.051(2) Uani 1 1 d . . . . .
O10 O 0.5136(5) 0.3082(5) 0.2523(3) 0.048(2) Uani 1 1 d . . . . .
O11 O 0.4234(5) 0.3979(5) -0.0154(4) 0.056(2) Uani 1 1 d . . . . .
O12 O 0.5138(5) 0.4035(5) 0.1714(3) 0.048(2) Uani 1 1 d . . . . .
O13 O 0.3595(5) 0.5154(4) 0.0256(3) 0.0461(19) Uani 1 1 d . . . . .
O14 O 0.5896(5) 0.4360(5) 0.2589(3) 0.056(2) Uani 1 1 d . . . . .
O15 O 0.3159(5) 0.4730(5) -0.0693(4) 0.070(3) Uani 1 1 d D . . . .
O16 O 0.2905(6) 0.6205(5) 0.1319(4) 0.064(3) Uani 1 1 d . . . . .
O17 O 0.4307(5) 0.5654(5) 0.1357(4) 0.059(2) Uani 1 1 d . . . . .
O18 O 0.4478(5) 0.5350(5) -0.0587(3) 0.052(2) Uani 1 1 d . . . . .
O19 O 0.3501(6) 0.5803(5) 0.2272(4) 0.061(2) Uani 1 1 d . . . . .
C1 C 0.3708(11) -0.0191(9) 0.0998(7) 0.087(5) Uani 1 1 d . . . . .
H1A H 0.3455 -0.0074 0.1371 0.131 Uiso 1 1 calc R U . . .
H1B H 0.3762 -0.0782 0.0950 0.131 Uiso 1 1 calc R U . . .
H1C H 0.4249 0.0062 0.0983 0.131 Uiso 1 1 calc R U . . .
C2 C 0.3560(10) -0.0025(12) -0.0035(6) 0.095(6) Uani 1 1 d . . . . .
H2A H 0.3205 0.0203 -0.0334 0.143 Uiso 1 1 calc R U . . .
H2B H 0.4099 0.0230 -0.0059 0.143 Uiso 1 1 calc R U . . .
H2C H 0.3613 -0.0614 -0.0092 0.143 Uiso 1 1 calc R U . . .
C3 C 0.5307(12) 0.2496(11) -0.0791(8) 0.110(6) Uani 1 1 d . U . . .
H3A H 0.4827 0.2744 -0.0972 0.165 Uiso 1 1 calc R U . . .
H3B H 0.5693 0.2328 -0.1091 0.165 Uiso 1 1 calc R U . . .
H3C H 0.5139 0.2018 -0.0567 0.165 Uiso 1 1 calc R U . . .
C4 C 0.6438(10) 0.2815(11) -0.0099(8) 0.108(6) Uani 1 1 d . U . . .
H4A H 0.6652 0.3254 0.0144 0.162 Uiso 1 1 calc R U . . .
H4B H 0.6297 0.2346 0.0142 0.162 Uiso 1 1 calc R U . . .
H4C H 0.6851 0.2655 -0.0382 0.162 Uiso 1 1 calc R U . . .
C5 C 0.5661(17) 0.6445(17) 0.2392(12) 0.179(11) Uani 1 1 d . U . . .
H5A H 0.5400 0.6647 0.2040 0.268 Uiso 1 1 calc R U . . .
H5B H 0.6039 0.6858 0.2539 0.268 Uiso 1 1 calc R U . . .
H5C H 0.5961 0.5944 0.2305 0.268 Uiso 1 1 calc R U . . .
C6 C 0.5222(14) 0.5947(13) 0.3441(10) 0.136(8) Uani 1 1 d . U . . .
H6A H 0.4715 0.5879 0.3659 0.204 Uiso 1 1 calc R U . . .
H6B H 0.5499 0.5420 0.3408 0.204 Uiso 1 1 calc R U . . .
H6C H 0.5577 0.6335 0.3641 0.204 Uiso 1 1 calc R U . . .
C7 C 0.2403(16) 0.8251(12) 0.3438(10) 0.058(6) Uani 0.5 1 d D U P . .
H7A H 0.2342 0.8729 0.3188 0.087 Uiso 0.5 1 calc R U P . .
H7B H 0.1919 0.8195 0.3682 0.087 Uiso 0.5 1 calc R U P . .
H7C H 0.2886 0.8320 0.3682 0.087 Uiso 0.5 1 calc R U P . .
C8 C 0.208(2) 0.275(2) -0.0568(14) 0.120(11) Uani 0.5 1 d D U P . .
H8A H 0.1600 0.3002 -0.0742 0.180 Uiso 0.5 1 d R U P . .
H8B H 0.2358 0.3152 -0.0320 0.180 Uiso 0.5 1 d R U P . .
H8C H 0.1920 0.2280 -0.0336 0.180 Uiso 0.5 1 d R U P . .
N1 N 0.3203(6) 0.0136(7) 0.0539(5) 0.061(3) Uani 1 1 d . . . . .
H1D H 0.3147 0.0683 0.0588 0.073 Uiso 1 1 calc R U . . .
H1E H 0.2700 -0.0092 0.0558 0.073 Uiso 1 1 calc R U . . .
N2 N 0.5706(8) 0.3103(7) -0.0401(6) 0.084(4) Uani 1 1 d . . . . .
H2D H 0.5842 0.3548 -0.0614 0.100 Uiso 1 1 calc R U . . .
H2E H 0.5335 0.3265 -0.0134 0.100 Uiso 1 1 calc R U . . .
N3 N 0.5025(12) 0.6272(11) 0.2837(9) 0.141(7) Uani 1 1 d . . . . .
H3D H 0.4672 0.5912 0.2675 0.169 Uiso 1 1 calc R U . . .
H3E H 0.4743 0.6743 0.2888 0.169 Uiso 1 1 calc R U . . .
N4 N 0.2500 0.7500 0.3074(13) 0.078(8) Uani 0.5 2 d DS TU P . .
H4D H 0.2967 0.7551 0.2858 0.093 Uiso 0.5 1 d R U P . .
O1W O 0.2854(8) 0.5499(10) -0.1730(6) 0.146(5) Uani 1 1 d . U . . .
N5 N 0.2500 0.2500 -0.1117(15) 0.113(11) Uani 0.5 2 d DS TU P . .
H5D H 0.2715 0.2909 -0.1342 0.136 Uiso 0.5 1 d R U P . .
O2W O 0.1601(12) 0.7082(11) 0.2019(8) 0.072(5) Uani 0.5 1 d . U P . .


_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 O10 2.272(8) . ?
Sm1 O7 2.305(7) . ?
Sm1 O8 2.311(7) 7_566 ?
Sm1 O1 2.317(6) . ?
Sm1 O1 2.346(6) 8_656 ?
Sm1 O6 2.407(7) 7_566 ?
Sm1 O2 2.437(6) . ?
Sm1 O2 2.568(6) 7_566 ?
Sm1 O19 2.763(9) 7_566 ?
Sm1 S4 3.210(3) 7_566 ?
Sm1 Sm3 3.8890(7) . ?
Sm1 Sm3 4.0357(7) 7_566 ?
Sm2 O3 2.262(6) . ?
Sm2 O12 2.300(7) . ?
Sm2 O18 2.312(7) 5_665 ?
Sm2 O5 2.323(7) . ?
Sm2 O13 2.428(7) . ?
Sm2 O6 2.432(7) . ?
Sm2 O11 2.479(9) . ?
Sm2 O17 2.567(8) . ?
Sm2 O2 2.910(6) . ?
Sm2 S3 3.067(3) . ?
Sm2 S4 3.126(3) . ?
Sm2 Sm3 3.9873(5) . ?
Sm3 O3 2.215(5) 2 ?
Sm3 O3 2.215(5) . ?
Sm3 O1 2.321(6) 2 ?
Sm3 O1 2.321(6) . ?
Sm3 O4 2.372(7) . ?
Sm3 O4 2.372(7) 2 ?
Sm3 O2 2.384(6) 2 ?
Sm3 O2 2.384(6) . ?
Sm3 Sm1 3.8890(7) 2 ?
Sm3 Sm2 3.9873(5) 2 ?
S1 O9 1.433(7) . ?
S1 O7 1.470(7) . ?
S1 O5 1.470(7) . ?
S1 O4 1.478(7) . ?
S2 O14 1.453(8) . ?
S2 O12 1.464(7) . ?
S2 O8 1.471(8) . ?
S2 O10 1.481(8) . ?
S3 O15 1.418(8) . ?
S3 O18 1.463(7) . ?
S3 O11 1.491(8) . ?
S3 O13 1.492(8) . ?
S4 O19 1.463(8) . ?
S4 O16 1.468(9) . ?
S4 O17 1.474(8) . ?
S4 O6 1.531(7) . ?
S4 Sm1 3.210(3) 8_656 ?
O1 Sm1 2.346(6) 7_566 ?
O2 Sm1 2.568(6) 8_656 ?
O6 Sm1 2.406(7) 8_656 ?
O8 Sm1 2.311(7) 8_656 ?
O18 Sm2 2.312(7) 5_665 ?
O19 Sm1 2.762(9) 8_656 ?
C1 N1 1.423(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.448(16) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N2 1.466(19) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N2 1.438(18) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N3 1.47(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.50(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N4 1.473(17) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N5 1.474(19) . ?
C8 C8 1.56(7) 2 ?
C8 H8A 0.9611 . ?
C8 H8B 0.9609 . ?
C8 H8C 0.9610 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N4 C7 1.473(17) 2_565 ?
N4 H4D 0.9009 . ?
N5 C8 1.474(19) 2 ?
N5 H5D 0.9010 . ?

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
O10 Sm1 O7 83.3(3) . . ?
O10 Sm1 O8 132.2(3) . 7_566 ?
O7 Sm1 O8 77.7(3) . 7_566 ?
O10 Sm1 O1 143.8(2) . . ?
O7 Sm1 O1 86.1(2) . . ?
O8 Sm1 O1 78.2(2) 7_566 . ?
O10 Sm1 O1 80.7(2) . 8_656 ?
O7 Sm1 O1 139.8(2) . 8_656 ?
O8 Sm1 O1 138.0(2) 7_566 8_656 ?
O1 Sm1 O1 85.6(3) . 8_656 ?
O10 Sm1 O6 78.5(2) . 7_566 ?
O7 Sm1 O6 132.2(3) . 7_566 ?
O8 Sm1 O6 82.7(3) 7_566 7_566 ?
O1 Sm1 O6 131.5(2) . 7_566 ?
O1 Sm1 O6 79.8(2) 8_656 7_566 ?
O10 Sm1 O2 76.2(2) . . ?
O7 Sm1 O2 74.9(2) . . ?
O8 Sm1 O2 137.1(2) 7_566 . ?
O1 Sm1 O2 67.68(19) . . ?
O1 Sm1 O2 65.61(19) 8_656 . ?
O6 Sm1 O2 139.7(2) 7_566 . ?
O10 Sm1 O2 134.2(2) . 7_566 ?
O7 Sm1 O2 142.5(2) . 7_566 ?
O8 Sm1 O2 74.6(2) 7_566 7_566 ?
O1 Sm1 O2 63.86(19) . 7_566 ?
O1 Sm1 O2 63.47(19) 8_656 7_566 ?
O6 Sm1 O2 68.3(2) 7_566 7_566 ?
O2 Sm1 O2 110.1(3) . 7_566 ?
O10 Sm1 O19 66.7(3) . 7_566 ?
O7 Sm1 O19 78.1(2) . 7_566 ?
O8 Sm1 O19 66.6(3) 7_566 7_566 ?
O1 Sm1 O19 143.7(2) . 7_566 ?
O1 Sm1 O19 126.9(2) 8_656 7_566 ?
O6 Sm1 O19 54.2(2) 7_566 7_566 ?
O2 Sm1 O19 136.0(2) . 7_566 ?
O2 Sm1 O19 112.5(2) 7_566 7_566 ?
O10 Sm1 S4 70.68(19) . 7_566 ?
O7 Sm1 S4 105.12(18) . 7_566 ?
O8 Sm1 S4 72.7(2) 7_566 7_566 ?
O1 Sm1 S4 145.43(15) . 7_566 ?
O1 Sm1 S4 103.84(15) 8_656 7_566 ?
O6 Sm1 S4 27.12(18) 7_566 7_566 ?
O2 Sm1 S4 146.53(15) . 7_566 ?
O2 Sm1 S4 90.34(14) 7_566 7_566 ?
O19 Sm1 S4 27.05(17) 7_566 7_566 ?
O10 Sm1 Sm3 111.09(18) . . ?
O7 Sm1 Sm3 72.31(17) . . ?
O8 Sm1 Sm3 104.2(2) 7_566 . ?
O1 Sm1 Sm3 33.05(14) . . ?
O1 Sm1 Sm3 79.59(14) 8_656 . ?
O6 Sm1 Sm3 155.35(17) 7_566 . ?
O2 Sm1 Sm3 35.78(13) . . ?
O2 Sm1 Sm3 90.41(13) 7_566 . ?
O19 Sm1 Sm3 150.29(17) 7_566 . ?
S4 Sm1 Sm3 176.45(6) 7_566 . ?
O10 Sm1 Sm3 104.6(2) . 7_566 ?
O7 Sm1 Sm3 159.94(17) . 7_566 ?
O8 Sm1 Sm3 108.11(19) 7_566 7_566 ?
O1 Sm1 Sm3 76.62(14) . 7_566 ?
O1 Sm1 Sm3 29.96(14) 8_656 7_566 ?
O6 Sm1 Sm3 67.80(17) 7_566 7_566 ?
O2 Sm1 Sm3 88.93(14) . 7_566 ?
O2 Sm1 Sm3 33.94(13) 7_566 7_566 ?
O19 Sm1 Sm3 121.98(17) 7_566 7_566 ?
S4 Sm1 Sm3 94.92(6) 7_566 7_566 ?
Sm3 Sm1 Sm3 87.631(17) . 7_566 ?
O3 Sm2 O12 128.5(2) . . ?
O3 Sm2 O18 149.9(2) . 5_665 ?
O12 Sm2 O18 75.2(3) . 5_665 ?
O3 Sm2 O5 81.5(2) . . ?
O12 Sm2 O5 79.8(3) . . ?
O18 Sm2 O5 86.1(3) 5_665 . ?
O3 Sm2 O13 79.4(2) . . ?
O12 Sm2 O13 145.4(3) . . ?
O18 Sm2 O13 87.8(3) 5_665 . ?
O5 Sm2 O13 129.6(3) . . ?
O3 Sm2 O6 70.4(2) . . ?
O12 Sm2 O6 90.4(3) . . ?
O18 Sm2 O6 134.3(3) 5_665 . ?
O5 Sm2 O6 134.5(2) . . ?
O13 Sm2 O6 80.1(2) . . ?
O3 Sm2 O11 76.4(2) . . ?
O12 Sm2 O11 139.9(3) . . ?
O18 Sm2 O11 73.7(3) 5_665 . ?
O5 Sm2 O11 73.3(3) . . ?
O13 Sm2 O11 57.0(3) . . ?
O6 Sm2 O11 129.6(3) . . ?
O3 Sm2 O17 121.5(2) . . ?
O12 Sm2 O17 77.0(3) . . ?
O18 Sm2 O17 78.1(3) 5_665 . ?
O5 Sm2 O17 154.6(3) . . ?
O13 Sm2 O17 70.1(3) . . ?
O6 Sm2 O17 56.3(2) . . ?
O11 Sm2 O17 119.9(3) . . ?
O3 Sm2 O2 62.15(18) . . ?
O12 Sm2 O2 66.6(2) . . ?
O18 Sm2 O2 138.9(2) 5_665 . ?
O5 Sm2 O2 73.1(2) . . ?
O13 Sm2 O2 132.7(2) . . ?
O6 Sm2 O2 62.3(2) . . ?
O11 Sm2 O2 129.5(2) . . ?
O17 Sm2 O2 106.4(2) . . ?
O3 Sm2 S3 79.54(15) . . ?
O12 Sm2 S3 151.36(18) . . ?
O18 Sm2 S3 76.4(2) 5_665 . ?
O5 Sm2 S3 102.1(2) . . ?
O13 Sm2 S3 28.60(18) . . ?
O6 Sm2 S3 106.86(18) . . ?
O11 Sm2 S3 28.78(19) . . ?
O17 Sm2 S3 93.47(19) . . ?
O2 Sm2 S3 141.68(13) . . ?
O3 Sm2 S4 95.29(16) . . ?
O12 Sm2 S4 85.5(2) . . ?
O18 Sm2 S4 106.0(2) 5_665 . ?
O5 Sm2 S4 158.01(19) . . ?
O13 Sm2 S4 70.29(18) . . ?
O6 Sm2 S4 28.66(17) . . ?
O11 Sm2 S4 127.31(19) . . ?
O17 Sm2 S4 27.87(18) . . ?
O2 Sm2 S4 86.07(12) . . ?
S3 Sm2 S4 98.68(8) . . ?
O3 Sm2 Sm3 26.74(14) . . ?
O12 Sm2 Sm3 101.96(18) . . ?
O18 Sm2 Sm3 156.2(2) 5_665 . ?
O5 Sm2 Sm3 70.23(18) . . ?
O13 Sm2 Sm3 105.16(18) . . ?
O6 Sm2 Sm3 68.61(17) . . ?
O11 Sm2 Sm3 96.40(19) . . ?
O17 Sm2 Sm3 124.81(17) . . ?
O2 Sm2 Sm3 36.39(11) . . ?
S3 Sm2 Sm3 105.55(6) . . ?
S4 Sm2 Sm3 97.25(6) . . ?
O3 Sm3 O3 113.8(3) 2 . ?
O3 Sm3 O1 136.6(2) 2 2 ?
O3 Sm3 O1 93.0(2) . 2 ?
O3 Sm3 O1 93.0(2) 2 . ?
O3 Sm3 O1 136.6(2) . . ?
O1 Sm3 O1 89.0(3) 2 . ?
O3 Sm3 O4 75.0(2) 2 . ?
O3 Sm3 O4 78.3(2) . . ?
O1 Sm3 O4 146.6(2) 2 . ?
O1 Sm3 O4 76.7(2) . . ?
O3 Sm3 O4 78.3(2) 2 2 ?
O3 Sm3 O4 75.0(2) . 2 ?
O1 Sm3 O4 76.7(2) 2 2 ?
O1 Sm3 O4 146.6(2) . 2 ?
O4 Sm3 O4 129.9(4) . 2 ?
O3 Sm3 O2 72.6(2) 2 2 ?
O3 Sm3 O2 151.7(2) . 2 ?
O1 Sm3 O2 68.5(2) 2 2 ?
O1 Sm3 O2 66.81(19) . 2 ?
O4 Sm3 O2 128.9(2) . 2 ?
O4 Sm3 O2 79.8(2) 2 2 ?
O3 Sm3 O2 151.7(2) 2 . ?
O3 Sm3 O2 72.6(2) . . ?
O1 Sm3 O2 66.81(19) 2 . ?
O1 Sm3 O2 68.5(2) . . ?
O4 Sm3 O2 79.8(2) . . ?
O4 Sm3 O2 128.9(2) 2 . ?
O2 Sm3 O2 115.6(3) 2 . ?
O3 Sm3 Sm1 119.43(15) 2 . ?
O3 Sm3 Sm1 104.44(15) . . ?
O1 Sm3 Sm1 82.59(14) 2 . ?
O1 Sm3 Sm1 32.99(14) . . ?
O4 Sm3 Sm1 68.89(17) . . ?
O4 Sm3 Sm1 159.18(18) 2 . ?
O2 Sm3 Sm1 94.55(14) 2 . ?
O2 Sm3 Sm1 36.70(13) . . ?
O3 Sm3 Sm1 104.44(15) 2 2 ?
O3 Sm3 Sm1 119.43(15) . 2 ?
O1 Sm3 Sm1 32.99(14) 2 2 ?
O1 Sm3 Sm1 82.59(14) . 2 ?
O4 Sm3 Sm1 159.19(18) . 2 ?
O4 Sm3 Sm1 68.89(17) 2 2 ?
O2 Sm3 Sm1 36.70(13) 2 2 ?
O2 Sm3 Sm1 94.55(14) . 2 ?
Sm1 Sm3 Sm1 94.58(2) . 2 ?
O3 Sm3 Sm2 27.36(15) 2 2 ?
O3 Sm3 Sm2 131.32(16) . 2 ?
O1 Sm3 Sm2 109.74(14) 2 2 ?
O1 Sm3 Sm2 87.70(14) . 2 ?
O4 Sm3 Sm2 99.84(17) . 2 ?
O4 Sm3 Sm2 69.66(18) 2 2 ?
O2 Sm3 Sm2 46.39(14) 2 2 ?
O2 Sm3 Sm2 155.77(14) . 2 ?
Sm1 Sm3 Sm2 120.371(13) . 2 ?
Sm1 Sm3 Sm2 77.138(11) 2 2 ?
O3 Sm3 Sm2 131.32(16) 2 . ?
O3 Sm3 Sm2 27.36(15) . . ?
O1 Sm3 Sm2 87.70(14) 2 . ?
O1 Sm3 Sm2 109.74(14) . . ?
O4 Sm3 Sm2 69.66(18) . . ?
O4 Sm3 Sm2 99.84(17) 2 . ?
O2 Sm3 Sm2 155.77(14) 2 . ?
O2 Sm3 Sm2 46.40(14) . . ?
Sm1 Sm3 Sm2 77.138(11) . . ?
Sm1 Sm3 Sm2 120.372(13) 2 . ?
Sm2 Sm3 Sm2 155.92(2) 2 . ?
O9 S1 O7 111.3(5) . . ?
O9 S1 O5 109.6(5) . . ?
O7 S1 O5 109.3(5) . . ?
O9 S1 O4 109.9(5) . . ?
O7 S1 O4 108.1(4) . . ?
O5 S1 O4 108.5(4) . . ?
O14 S2 O12 110.0(5) . . ?
O14 S2 O8 109.8(5) . . ?
O12 S2 O8 109.9(5) . . ?
O14 S2 O10 109.4(5) . . ?
O12 S2 O10 108.7(5) . . ?
O8 S2 O10 109.0(5) . . ?
O15 S3 O18 109.6(5) . . ?
O15 S3 O11 113.9(5) . . ?
O18 S3 O11 111.7(5) . . ?
O15 S3 O13 108.9(5) . . ?
O18 S3 O13 108.9(5) . . ?
O11 S3 O13 103.5(5) . . ?
O15 S3 Sm2 133.8(4) . . ?
O18 S3 Sm2 116.3(3) . . ?
O11 S3 Sm2 53.2(3) . . ?
O13 S3 Sm2 51.2(3) . . ?
O19 S4 O16 113.7(5) . . ?
O19 S4 O17 113.8(5) . . ?
O16 S4 O17 110.9(5) . . ?
O19 S4 O6 104.9(5) . . ?
O16 S4 O6 109.2(5) . . ?
O17 S4 O6 103.5(5) . . ?
O19 S4 Sm2 128.5(4) . . ?
O16 S4 Sm2 116.9(4) . . ?
O17 S4 Sm2 54.5(3) . . ?
O6 S4 Sm2 49.6(3) . . ?
O19 S4 Sm1 59.2(4) . 8_656 ?
O16 S4 Sm1 126.5(4) . 8_656 ?
O17 S4 Sm1 120.1(3) . 8_656 ?
O6 S4 Sm1 45.8(3) . 8_656 ?
Sm2 S4 Sm1 83.24(7) . 8_656 ?
Sm1 O1 Sm3 114.0(2) . . ?
Sm1 O1 Sm1 120.4(2) . 7_566 ?
Sm3 O1 Sm1 119.7(2) . 7_566 ?
Sm3 O2 Sm1 107.5(2) . . ?
Sm3 O2 Sm1 109.1(2) . 8_656 ?
Sm1 O2 Sm1 107.9(2) . 8_656 ?
Sm3 O2 Sm2 97.22(19) . . ?
Sm1 O2 Sm2 133.2(2) . . ?
Sm1 O2 Sm2 100.21(18) 8_656 . ?
Sm3 O3 Sm2 125.9(3) . . ?
S1 O4 Sm3 132.2(4) . . ?
S1 O5 Sm2 138.9(4) . . ?
S4 O6 Sm1 107.1(4) . 8_656 ?
S4 O6 Sm2 101.7(4) . . ?
Sm1 O6 Sm2 120.9(3) 8_656 . ?
S1 O7 Sm1 138.9(4) . . ?
S2 O8 Sm1 136.7(5) . 8_656 ?
S2 O10 Sm1 135.9(5) . . ?
S3 O11 Sm2 98.1(4) . . ?
S2 O12 Sm2 142.2(5) . . ?
S3 O13 Sm2 100.2(4) . . ?
S4 O17 Sm2 97.7(4) . . ?
S3 O18 Sm2 159.3(5) . 5_665 ?
S4 O19 Sm1 93.8(4) . 8_656 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 C8 57.9(16) . 2 ?
N5 C8 H8A 97.7 . . ?
C8 C8 H8A 155.4 2 . ?
N5 C8 H8B 118.2 . . ?
C8 C8 H8B 87.4 2 . ?
H8A C8 H8B 109.5 . . ?
N5 C8 H8C 111.7 . . ?
C8 C8 H8C 79.9 2 . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 N1 C2 111.6(11) . . ?
C1 N1 H1D 109.3 . . ?
C2 N1 H1D 109.3 . . ?
C1 N1 H1E 109.3 . . ?
C2 N1 H1E 109.3 . . ?
H1D N1 H1E 108.0 . . ?
C4 N2 C3 115.6(14) . . ?
C4 N2 H2D 108.4 . . ?
C3 N2 H2D 108.4 . . ?
C4 N2 H2E 108.4 . . ?
C3 N2 H2E 108.4 . . ?
H2D N2 H2E 107.4 . . ?
C5 N3 C6 123(2) . . ?
C5 N3 H3D 106.5 . . ?
C6 N3 H3D 106.5 . . ?
C5 N3 H3E 106.5 . . ?
C6 N3 H3E 106.5 . . ?
H3D N3 H3E 106.5 . . ?
C7 N4 C7 112(3) . 2_565 ?
C7 N4 H4D 108.7 . . ?
C7 N4 H4D 107.0 2_565 . ?
C8 N5 C8 64(3) 2 . ?
C8 N5 H5D 120.5 2 . ?
C8 N5 H5D 116.9 . . ?

_refine_diff_density_max         1.817
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.244

####################################################################### 
# 
# 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_a01
_database_code_depnum_ccdc_archive 'CCDC 1544849'
_audit_update_record             
;
2017-04-19 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H138 N14 O82 S16 Tb10'
_chemical_formula_weight         4085.68

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   16.144(6)
_cell_length_b                   16.144(6)
_cell_length_c                   22.809(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5945(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1904
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      22.36

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.282
_exptl_crystal_F_000             3932
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    6.253
_shelx_estimated_absorpt_T_min   0.497
_shelx_estimated_absorpt_T_max   0.521
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19281
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.545
_diffrn_reflns_theta_max         25.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             5437
_reflns_number_gt                3336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5437
_refine_ls_number_parameters     353
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.57800(4) 0.70156(4) 0.24509(2) 0.02930(19) Uani 1 1 d . . . . .
Tb2 Tb 0.92530(4) 0.58296(4) 0.09281(3) 0.0338(2) Uani 1 1 d . . . . .
Tb3 Tb 0.7500 0.7500 0.12906(3) 0.0246(2) Uani 1 2 d S T P . .
S1 S 0.9577(2) 0.8020(2) 0.09103(13) 0.0316(8) Uani 1 1 d . . . . .
S2 S 1.0159(2) 0.6030(2) 0.23565(14) 0.0389(9) Uani 1 1 d . . . . .
S3 S 0.8862(2) 0.5218(2) -0.03235(14) 0.0382(9) Uani 1 1 d . . . . .
S4 S 0.4350(2) 0.6526(3) 0.33660(15) 0.0441(9) Uani 1 1 d . . . . .
O1 O 0.7037(4) 0.6607(4) 0.2025(3) 0.0138(16) Uani 1 1 d . . . . .
O2 O 0.6379(4) 0.8116(4) 0.1835(3) 0.0164(17) Uani 1 1 d . . . . .
O3 O 0.8021(4) 0.6473(4) 0.0753(3) 0.0162(16) Uani 1 1 d . . . . .
O4 O 0.9777(5) 0.7159(6) 0.0754(3) 0.038(2) Uani 1 1 d . . . . .
O5 O 0.8674(5) 0.8146(6) 0.0852(4) 0.040(2) Uani 1 1 d . . . . .
O6 O 0.9806(5) 0.8155(6) 0.1530(3) 0.040(2) Uani 1 1 d . . . . .
O7 O 1.0023(6) 0.8580(5) 0.0529(3) 0.041(2) Uani 1 1 d . . . . .
O8 O 0.9406(5) 0.5621(6) 0.2601(4) 0.040(2) Uani 1 1 d . . . . .
O9 O 0.5254(5) 0.6820(6) 0.3431(4) 0.042(2) Uani 1 1 d . . . . .
O10 O 1.0146(5) 0.6921(6) 0.2523(4) 0.040(2) Uani 1 1 d . . . . .
O11 O 0.8594(6) 0.4854(5) 0.0248(4) 0.040(2) Uani 1 1 d . . . . .
O12 O 0.9237(6) 0.6018(6) -0.0166(4) 0.051(3) Uani 1 1 d . . . . .
O13 O 1.0150(6) 0.5976(6) 0.1710(3) 0.043(2) Uani 1 1 d . . . . .
O14 O 0.3805(6) 0.7087(7) 0.3673(5) 0.060(3) Uani 1 1 d . . . . .
O15 O 1.0904(6) 0.5648(7) 0.2588(4) 0.055(3) Uani 1 1 d . . . . .
O16 O 0.4362(6) 0.5711(6) 0.3638(4) 0.052(3) Uani 1 1 d . . . . .
O17 O 0.4208(6) 0.6507(7) 0.2727(4) 0.054(3) Uani 1 1 d . . . . .
O18 O 0.8168(6) 0.5348(7) -0.0709(4) 0.061(3) Uani 1 1 d . . . . .
O19 O 0.9466(6) 0.4650(6) -0.0594(4) 0.051(3) Uani 1 1 d . . . . .
N1 N 0.8211(8) 0.9868(8) 0.0558(6) 0.062(4) Uani 1 1 d . . . . .
H1D H 0.7707 1.0089 0.0582 0.074 Uiso 1 1 calc R U . . .
H1E H 0.8159 0.9323 0.0601 0.074 Uiso 1 1 calc R U . . .
N2 N 1.0753(9) 0.6872(8) -0.0385(6) 0.070(4) Uani 1 1 d . . . . .
H2D H 1.0353 0.6683 -0.0153 0.084 Uiso 1 1 calc R U . . .
H2E H 1.0932 0.6447 -0.0599 0.084 Uiso 1 1 calc R U . . .
C2 C 0.8714(12) 1.0190(12) 0.1043(7) 0.077(6) Uani 1 1 d . . . . .
H2A H 0.8454 1.0056 0.1409 0.115 Uiso 1 1 calc R U . . .
H2B H 0.9256 0.9945 0.1030 0.115 Uiso 1 1 calc R U . . .
H2C H 0.8762 1.0781 0.1008 0.115 Uiso 1 1 calc R U . . .
C1 C 0.8546(11) 1.0036(13) -0.0029(7) 0.085(6) Uani 1 1 d . U . . .
H1A H 0.8183 0.9807 -0.0320 0.127 Uiso 1 1 calc R U . . .
H1B H 0.8591 1.0624 -0.0086 0.127 Uiso 1 1 calc R U . . .
H1C H 0.9084 0.9788 -0.0065 0.127 Uiso 1 1 calc R U . . .
C4 C 1.0385(15) 0.7491(13) -0.0788(8) 0.105(7) Uani 1 1 d . U . . .
H4A H 0.9945 0.7239 -0.1007 0.158 Uiso 1 1 calc R U . . .
H4B H 1.0169 0.7947 -0.0564 0.158 Uiso 1 1 calc R U . . .
H4C H 1.0802 0.7690 -0.1053 0.158 Uiso 1 1 calc R U . . .
C3 C 1.1412(7) 0.7142(13) -0.0029(9) 0.119(8) Uani 1 1 d . U . . .
H3C H 1.1599 0.6691 0.0212 0.179 Uiso 1 1 calc R U . . .
H3D H 1.1860 0.7330 -0.0271 0.179 Uiso 1 1 calc DR U . . .
H3E H 1.1227 0.7588 0.0217 0.179 Uiso 1 1 calc R U . . .
N3 N 0.4886(15) 0.1309(17) 0.2757(11) 0.197(9) Uani 1 1 d D U . . .
H3A H 0.5178 0.0931 0.2562 0.237 Uiso 1 1 calc R U . . .
H3B H 0.5182 0.1774 0.2758 0.237 Uiso 1 1 calc R U . . .
C5 C 0.480(2) 0.1020(19) 0.3380(12) 0.188(11) Uani 1 1 d D U . . .
H5A H 0.5343 0.0941 0.3546 0.282 Uiso 1 1 calc R U . . .
H5B H 0.4508 0.1429 0.3603 0.282 Uiso 1 1 calc R U . . .
H5C H 0.4504 0.0507 0.3389 0.282 Uiso 1 1 calc R U . . .
O1W O 0.2103(11) 0.5613(13) 0.1701(8) 0.173(8) Uani 1 1 d . U . . .
O2W O 1.1637(16) 0.7924(14) -0.2027(10) 0.083(7) Uani 0.5 1 d . U P . .
N5 N 0.2500 0.2500 0.1050(18) 0.095(17) Uani 0.5 2 d DS T P . .
H5D H 0.2727 0.2106 0.1279 0.114 Uiso 0.5 1 d R U P . .
N4 N 1.2500 0.7500 -0.3021(16) 0.080(13) Uani 0.5 2 d DS TU P . .
H4D H 1.2048 0.7523 -0.2791 0.096 Uiso 0.5 1 d R U P . .
C7 C 1.257(2) 0.8234(17) -0.3406(12) 0.078(11) Uani 0.5 1 d D U P . .
H7A H 1.2611 0.8725 -0.3170 0.117 Uiso 0.5 1 calc R U P . .
H7B H 1.3049 0.8183 -0.3649 0.117 Uiso 0.5 1 calc R U P . .
H7C H 1.2082 0.8271 -0.3649 0.117 Uiso 0.5 1 calc R U P . .
C8 C 0.192(2) 0.214(3) 0.0649(16) 0.110(14) Uani 0.5 1 d D U P . .
H8A H 0.1484 0.1865 0.0867 0.165 Uiso 0.5 1 calc R U P . .
H8B H 0.1680 0.2560 0.0407 0.165 Uiso 0.5 1 calc R U P . .
H8C H 0.2195 0.1737 0.0407 0.165 Uiso 0.5 1 calc R U P . .
C6 C 0.4097(19) 0.147(2) 0.2417(14) 0.225(12) Uiso 1 1 d D U . . .
H6A H 0.4233 0.1650 0.2028 0.338 Uiso 1 1 calc R U . . .
H6B H 0.3777 0.0969 0.2397 0.338 Uiso 1 1 calc R U . . .
H6C H 0.3780 0.1892 0.2611 0.338 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O10 2.283(9) 2_665 ?
Tb1 O8 2.312(9) 7_576 ?
Tb1 O6 2.320(8) 2_665 ?
Tb1 O1 2.345(7) . ?
Tb1 O1 2.357(7) 7_576 ?
Tb1 O9 2.411(8) . ?
Tb1 O2 2.463(7) . ?
Tb1 O2 2.625(7) 8_756 ?
Tb1 O17 2.741(10) . ?
Tb1 S4 3.211(4) . ?
Tb1 Tb3 3.9148(13) . ?
Tb2 O3 2.279(7) . ?
Tb2 O13 2.309(9) . ?
Tb2 O19 2.336(9) 5_765 ?
Tb2 O4 2.340(9) . ?
Tb2 O9 2.450(9) 8_756 ?
Tb2 O11 2.454(8) . ?
Tb2 O12 2.514(9) . ?
Tb2 O16 2.569(10) 8_756 ?
Tb2 O2 2.866(7) 2_665 ?
Tb2 S3 3.086(3) . ?
Tb2 S4 3.143(4) 8_756 ?
Tb2 Tb3 3.9958(15) . ?
Tb3 O3 2.228(7) . ?
Tb3 O3 2.228(7) 2_665 ?
Tb3 O1 2.332(6) 2_665 ?
Tb3 O1 2.332(6) . ?
Tb3 O5 2.384(9) 2_665 ?
Tb3 O5 2.384(9) . ?
Tb3 O2 2.409(7) . ?
Tb3 O2 2.409(7) 2_665 ?
Tb3 Tb1 3.9149(13) 2_665 ?
Tb3 Tb2 3.9958(15) 2_665 ?
S1 O7 1.447(9) . ?
S1 O4 1.471(9) . ?
S1 O5 1.478(9) . ?
S1 O6 1.478(8) . ?
S2 O15 1.451(9) . ?
S2 O13 1.478(8) . ?
S2 O10 1.488(9) . ?
S2 O8 1.491(9) . ?
S3 O18 1.439(10) . ?
S3 O12 1.470(10) . ?
S3 O19 1.474(9) . ?
S3 O11 1.495(9) . ?
S4 O14 1.443(10) . ?
S4 O16 1.456(10) . ?
S4 O17 1.477(9) . ?
S4 O9 1.542(9) . ?
S4 Tb2 3.143(4) 7_576 ?
O1 Tb1 2.356(7) 8_756 ?
O2 Tb1 2.625(7) 7_576 ?
O2 Tb2 2.866(7) 2_665 ?
O6 Tb1 2.320(8) 2_665 ?
O8 Tb1 2.312(9) 8_756 ?
O9 Tb2 2.450(9) 7_576 ?
O10 Tb1 2.283(9) 2_665 ?
O16 Tb2 2.569(10) 7_576 ?
O19 Tb2 2.336(9) 5_765 ?
N1 C2 1.468(19) . ?
N1 C1 1.470(18) . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 C3 1.408(18) . ?
N2 C4 1.48(2) . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?
N3 C5 1.500(17) . ?
N3 C6 1.515(18) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
N5 C8 1.439(19) . ?
N5 C8 1.439(19) 2 ?
N5 H5D 0.8999 . ?
N4 C7 1.479(18) 2_765 ?
N4 C7 1.479(18) . ?
N4 H4D 0.9000 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
O10 Tb1 O8 132.7(3) 2_665 7_576 ?
O10 Tb1 O6 83.6(3) 2_665 2_665 ?
O8 Tb1 O6 77.9(3) 7_576 2_665 ?
O10 Tb1 O1 143.9(3) 2_665 . ?
O8 Tb1 O1 78.2(3) 7_576 . ?
O6 Tb1 O1 86.8(3) 2_665 . ?
O10 Tb1 O1 81.2(3) 2_665 7_576 ?
O8 Tb1 O1 137.1(3) 7_576 7_576 ?
O6 Tb1 O1 140.2(3) 2_665 7_576 ?
O1 Tb1 O1 84.4(3) . 7_576 ?
O10 Tb1 O9 78.5(3) 2_665 . ?
O8 Tb1 O9 83.0(3) 7_576 . ?
O6 Tb1 O9 132.8(3) 2_665 . ?
O1 Tb1 O9 130.7(3) . . ?
O1 Tb1 O9 79.3(3) 7_576 . ?
O10 Tb1 O2 75.9(3) 2_665 . ?
O8 Tb1 O2 136.9(3) 7_576 . ?
O6 Tb1 O2 74.3(3) 2_665 . ?
O1 Tb1 O2 68.1(2) . . ?
O1 Tb1 O2 66.4(2) 7_576 . ?
O9 Tb1 O2 139.6(3) . . ?
O10 Tb1 O2 134.0(3) 2_665 8_756 ?
O8 Tb1 O2 73.6(3) 7_576 8_756 ?
O6 Tb1 O2 142.4(3) 2_665 8_756 ?
O1 Tb1 O2 63.9(2) . 8_756 ?
O1 Tb1 O2 63.5(2) 7_576 8_756 ?
O9 Tb1 O2 67.2(3) . 8_756 ?
O2 Tb1 O2 111.7(3) . 8_756 ?
O10 Tb1 O17 66.6(3) 2_665 . ?
O8 Tb1 O17 67.1(3) 7_576 . ?
O6 Tb1 O17 78.1(3) 2_665 . ?
O1 Tb1 O17 144.3(3) . . ?
O1 Tb1 O17 127.1(3) 7_576 . ?
O9 Tb1 O17 54.7(3) . . ?
O2 Tb1 O17 135.3(3) . . ?
O2 Tb1 O17 111.6(2) 8_756 . ?
O10 Tb1 S4 70.6(2) 2_665 . ?
O8 Tb1 S4 73.1(2) 7_576 . ?
O6 Tb1 S4 105.4(2) 2_665 . ?
O1 Tb1 S4 145.34(18) . . ?
O1 Tb1 S4 103.73(18) 7_576 . ?
O9 Tb1 S4 27.4(2) . . ?
O2 Tb1 S4 146.17(17) . . ?
O2 Tb1 S4 89.32(16) 8_756 . ?
O17 Tb1 S4 27.29(19) . . ?
O10 Tb1 Tb3 111.3(2) 2_665 . ?
O8 Tb1 Tb3 104.0(2) 7_576 . ?
O6 Tb1 Tb3 72.6(2) 2_665 . ?
O1 Tb1 Tb3 33.07(16) . . ?
O1 Tb1 Tb3 79.13(16) 7_576 . ?
O9 Tb1 Tb3 154.5(2) . . ?
O2 Tb1 Tb3 36.07(16) . . ?
O2 Tb1 Tb3 90.94(15) 8_756 . ?
O17 Tb1 Tb3 150.68(19) . . ?
S4 Tb1 Tb3 176.91(8) . . ?
O3 Tb2 O13 129.5(3) . . ?
O3 Tb2 O19 150.1(3) . 5_765 ?
O13 Tb2 O19 74.4(3) . 5_765 ?
O3 Tb2 O4 82.4(3) . . ?
O13 Tb2 O4 79.1(3) . . ?
O19 Tb2 O4 85.9(3) 5_765 . ?
O3 Tb2 O9 70.1(3) . 8_756 ?
O13 Tb2 O9 91.2(3) . 8_756 ?
O19 Tb2 O9 134.0(3) 5_765 8_756 ?
O4 Tb2 O9 134.8(3) . 8_756 ?
O3 Tb2 O11 78.6(3) . . ?
O13 Tb2 O11 145.7(3) . . ?
O19 Tb2 O11 88.0(3) 5_765 . ?
O4 Tb2 O11 129.6(3) . . ?
O9 Tb2 O11 80.1(3) 8_756 . ?
O3 Tb2 O12 76.2(3) . . ?
O13 Tb2 O12 139.5(3) . . ?
O19 Tb2 O12 74.1(3) 5_765 . ?
O4 Tb2 O12 74.0(3) . . ?
O9 Tb2 O12 129.1(3) 8_756 . ?
O11 Tb2 O12 56.3(3) . . ?
O3 Tb2 O16 120.5(3) . 8_756 ?
O13 Tb2 O16 77.4(3) . 8_756 ?
O19 Tb2 O16 78.4(3) 5_765 8_756 ?
O4 Tb2 O16 154.6(3) . 8_756 ?
O9 Tb2 O16 55.7(3) 8_756 8_756 ?
O11 Tb2 O16 70.2(3) . 8_756 ?
O12 Tb2 O16 119.6(3) . 8_756 ?
O3 Tb2 O2 62.9(2) . 2_665 ?
O13 Tb2 O2 66.8(2) . 2_665 ?
O19 Tb2 O2 138.4(3) 5_765 2_665 ?
O4 Tb2 O2 72.9(2) . 2_665 ?
O9 Tb2 O2 62.8(2) 8_756 2_665 ?
O11 Tb2 O2 133.1(2) . 2_665 ?
O12 Tb2 O2 129.8(3) . 2_665 ?
O16 Tb2 O2 106.1(2) 8_756 2_665 ?
O3 Tb2 S3 78.75(17) . . ?
O13 Tb2 S3 151.1(2) . . ?
O19 Tb2 S3 76.9(2) 5_765 . ?
O4 Tb2 S3 102.1(2) . . ?
O9 Tb2 S3 106.6(2) 8_756 . ?
O11 Tb2 S3 28.5(2) . . ?
O12 Tb2 S3 28.1(2) . . ?
O16 Tb2 S3 93.8(2) 8_756 . ?
O2 Tb2 S3 141.68(15) 2_665 . ?
O3 Tb2 S4 94.97(19) . 8_756 ?
O13 Tb2 S4 86.2(2) . 8_756 ?
O19 Tb2 S4 105.6(3) 5_765 8_756 ?
O4 Tb2 S4 158.2(2) . 8_756 ?
O9 Tb2 S4 28.7(2) 8_756 8_756 ?
O11 Tb2 S4 70.3(2) . 8_756 ?
O12 Tb2 S4 126.6(2) . 8_756 ?
O16 Tb2 S4 27.2(2) 8_756 8_756 ?
O2 Tb2 S4 86.51(15) 2_665 8_756 ?
S3 Tb2 S4 98.57(10) . 8_756 ?
O3 Tb2 Tb3 27.21(16) . . ?
O13 Tb2 Tb3 102.4(2) . . ?
O19 Tb2 Tb3 156.7(3) 5_765 . ?
O4 Tb2 Tb3 70.9(2) . . ?
O9 Tb2 Tb3 68.4(2) 8_756 . ?
O11 Tb2 Tb3 104.9(2) . . ?
O12 Tb2 Tb3 96.7(2) . . ?
O16 Tb2 Tb3 124.0(2) 8_756 . ?
O2 Tb2 Tb3 36.65(13) 2_665 . ?
S3 Tb2 Tb3 105.21(7) . . ?
S4 Tb2 Tb3 97.08(7) 8_756 . ?
O3 Tb3 O3 113.2(3) . 2_665 ?
O3 Tb3 O1 137.3(2) . 2_665 ?
O3 Tb3 O1 93.2(2) 2_665 2_665 ?
O3 Tb3 O1 93.2(2) . . ?
O3 Tb3 O1 137.3(2) 2_665 . ?
O1 Tb3 O1 88.2(3) 2_665 . ?
O3 Tb3 O5 75.1(3) . 2_665 ?
O3 Tb3 O5 78.1(3) 2_665 2_665 ?
O1 Tb3 O5 145.7(3) 2_665 2_665 ?
O1 Tb3 O5 77.1(3) . 2_665 ?
O3 Tb3 O5 78.1(3) . . ?
O3 Tb3 O5 75.1(3) 2_665 . ?
O1 Tb3 O5 77.1(3) 2_665 . ?
O1 Tb3 O5 145.7(3) . . ?
O5 Tb3 O5 130.3(4) 2_665 . ?
O3 Tb3 O2 151.0(2) . . ?
O3 Tb3 O2 72.1(2) 2_665 . ?
O1 Tb3 O2 67.4(2) 2_665 . ?
O1 Tb3 O2 69.2(2) . . ?
O5 Tb3 O2 78.4(3) 2_665 . ?
O5 Tb3 O2 129.3(3) . . ?
O3 Tb3 O2 72.1(2) . 2_665 ?
O3 Tb3 O2 151.0(2) 2_665 2_665 ?
O1 Tb3 O2 69.2(2) 2_665 2_665 ?
O1 Tb3 O2 67.4(2) . 2_665 ?
O5 Tb3 O2 129.3(3) 2_665 2_665 ?
O5 Tb3 O2 78.4(3) . 2_665 ?
O2 Tb3 O2 118.0(3) . 2_665 ?
O3 Tb3 Tb1 119.42(18) . . ?
O3 Tb3 Tb1 104.66(18) 2_665 . ?
O1 Tb3 Tb1 82.26(16) 2_665 . ?
O1 Tb3 Tb1 33.27(17) . . ?
O5 Tb3 Tb1 68.4(2) 2_665 . ?
O5 Tb3 Tb1 159.3(2) . . ?
O2 Tb3 Tb1 37.01(16) . . ?
O2 Tb3 Tb1 95.87(16) 2_665 . ?
O3 Tb3 Tb1 104.66(18) . 2_665 ?
O3 Tb3 Tb1 119.42(18) 2_665 2_665 ?
O1 Tb3 Tb1 33.27(17) 2_665 2_665 ?
O1 Tb3 Tb1 82.26(16) . 2_665 ?
O5 Tb3 Tb1 159.3(2) 2_665 2_665 ?
O5 Tb3 Tb1 68.4(2) . 2_665 ?
O2 Tb3 Tb1 95.87(16) . 2_665 ?
O2 Tb3 Tb1 37.01(16) 2_665 2_665 ?
Tb1 Tb3 Tb1 94.94(4) . 2_665 ?
O3 Tb3 Tb2 130.99(17) . 2_665 ?
O3 Tb3 Tb2 27.89(17) 2_665 2_665 ?
O1 Tb3 Tb2 87.62(17) 2_665 2_665 ?
O1 Tb3 Tb2 109.80(17) . 2_665 ?
O5 Tb3 Tb2 69.2(2) 2_665 2_665 ?
O5 Tb3 Tb2 100.4(2) . 2_665 ?
O2 Tb3 Tb2 45.24(16) . 2_665 ?
O2 Tb3 Tb2 156.53(16) 2_665 2_665 ?
Tb1 Tb3 Tb2 76.841(18) . 2_665 ?
Tb1 Tb3 Tb2 120.497(16) 2_665 2_665 ?
O3 Tb3 Tb2 27.89(17) . . ?
O3 Tb3 Tb2 130.99(17) 2_665 . ?
O1 Tb3 Tb2 109.80(17) 2_665 . ?
O1 Tb3 Tb2 87.62(17) . . ?
O5 Tb3 Tb2 100.4(2) 2_665 . ?
O5 Tb3 Tb2 69.2(2) . . ?
O2 Tb3 Tb2 156.54(16) . . ?
O2 Tb3 Tb2 45.24(16) 2_665 . ?
Tb1 Tb3 Tb2 120.497(16) . . ?
Tb1 Tb3 Tb2 76.840(18) 2_665 . ?
Tb2 Tb3 Tb2 156.11(3) 2_665 . ?
O7 S1 O4 109.6(5) . . ?
O7 S1 O5 110.5(6) . . ?
O4 S1 O5 108.9(5) . . ?
O7 S1 O6 111.0(5) . . ?
O4 S1 O6 108.5(5) . . ?
O5 S1 O6 108.2(5) . . ?
O15 S2 O13 110.2(5) . . ?
O15 S2 O10 109.2(6) . . ?
O13 S2 O10 108.2(5) . . ?
O15 S2 O8 110.6(6) . . ?
O13 S2 O8 109.8(5) . . ?
O10 S2 O8 108.7(5) . . ?
O18 S3 O12 110.0(7) . . ?
O18 S3 O19 110.4(6) . . ?
O12 S3 O19 112.1(6) . . ?
O18 S3 O11 111.4(6) . . ?
O12 S3 O11 104.6(5) . . ?
O19 S3 O11 108.1(6) . . ?
O18 S3 Tb2 132.7(4) . . ?
O12 S3 Tb2 53.8(4) . . ?
O19 S3 Tb2 116.8(4) . . ?
O11 S3 Tb2 51.6(3) . . ?
O14 S4 O16 111.6(6) . . ?
O14 S4 O17 113.4(6) . . ?
O16 S4 O17 113.8(6) . . ?
O14 S4 O9 109.7(6) . . ?
O16 S4 O9 103.0(5) . . ?
O17 S4 O9 104.4(5) . . ?
O14 S4 Tb2 117.8(5) . 7_576 ?
O16 S4 Tb2 53.8(4) . 7_576 ?
O17 S4 Tb2 128.0(4) . 7_576 ?
O9 S4 Tb2 49.8(3) . 7_576 ?
O14 S4 Tb1 126.8(5) . . ?
O16 S4 Tb1 119.4(4) . . ?
O17 S4 Tb1 58.3(4) . . ?
O9 S4 Tb1 46.1(3) . . ?
Tb2 S4 Tb1 83.42(9) 7_576 . ?
Tb3 O1 Tb1 113.7(3) . . ?
Tb3 O1 Tb1 120.4(3) . 8_756 ?
Tb1 O1 Tb1 120.7(3) . 8_756 ?
Tb3 O2 Tb1 106.9(3) . . ?
Tb3 O2 Tb1 107.8(3) . 7_576 ?
Tb1 O2 Tb1 106.8(2) . 7_576 ?
Tb3 O2 Tb2 98.1(2) . 2_665 ?
Tb1 O2 Tb2 134.5(3) . 2_665 ?
Tb1 O2 Tb2 100.6(2) 7_576 2_665 ?
Tb3 O3 Tb2 124.9(3) . . ?
S1 O4 Tb2 138.3(5) . . ?
S1 O5 Tb3 133.4(5) . . ?
S1 O6 Tb1 138.3(5) . 2_665 ?
S2 O8 Tb1 137.8(5) . 8_756 ?
S4 O9 Tb1 106.5(4) . . ?
S4 O9 Tb2 101.4(4) . 7_576 ?
Tb1 O9 Tb2 120.8(4) . 7_576 ?
S2 O10 Tb1 135.9(5) . 2_665 ?
S3 O11 Tb2 99.9(4) . . ?
S3 O12 Tb2 98.1(5) . . ?
S2 O13 Tb2 141.5(6) . . ?
S4 O16 Tb2 98.9(5) . 7_576 ?
S4 O17 Tb1 94.4(5) . . ?
S3 O19 Tb2 158.2(6) . 5_765 ?
C2 N1 C1 114.7(13) . . ?
C2 N1 H1D 108.6 . . ?
C1 N1 H1D 108.6 . . ?
C2 N1 H1E 108.6 . . ?
C1 N1 H1E 108.6 . . ?
H1D N1 H1E 107.6 . . ?
C3 N2 C4 116.9(16) . . ?
C3 N2 H2D 108.1 . . ?
C4 N2 H2D 108.1 . . ?
C3 N2 H2E 108.1 . . ?
C4 N2 H2E 108.1 . . ?
H2D N2 H2E 107.3 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C3 H3C 109.5 . . ?
N2 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
N2 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
C5 N3 C6 118(3) . . ?
C5 N3 H3A 107.9 . . ?
C6 N3 H3A 107.9 . . ?
C5 N3 H3B 107.9 . . ?
C6 N3 H3B 107.9 . . ?
H3A N3 H3B 107.2 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C8 N5 C8 101(5) . 2 ?
C8 N5 H5D 110.2 . . ?
C8 N5 H5D 113.0 2 . ?
C7 N4 C7 107(3) 2_765 . ?
C7 N4 H4D 108.7 2_765 . ?
C7 N4 H4D 111.9 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 H8A 109.5 . . ?
N5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_refine_diff_density_max         2.665
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.341

####################################################################### 
# 
# 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_zht-3-4
_database_code_depnum_ccdc_archive 'CCDC 1544846'
_audit_update_record             
;
2017-04-19 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H136 Er10 N14 O82 S16'
_chemical_formula_weight         4167.06

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   15.9800(7)
_cell_length_b                   15.9800(7)
_cell_length_c                   22.646(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5783.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4123
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      21.41

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_F_000             3988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    7.569
_shelx_estimated_absorpt_T_min   0.377
_shelx_estimated_absorpt_T_max   0.464
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41342
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_av_R_equivalents  0.1322
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.560
_diffrn_reflns_theta_max         25.493
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5365
_reflns_number_gt                3850
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+340.1336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5365
_refine_ls_number_parameters     358
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0981
_refine_ls_wR_factor_ref         0.1900
_refine_ls_wR_factor_gt          0.1810
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.163
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.41918(6) 0.19992(7) 0.24513(4) 0.0421(3) Uani 1 1 d . . . . .
Er2 Er 0.42612(7) 0.41812(8) 0.09277(4) 0.0503(3) Uani 1 1 d . . . . .
Er3 Er 0.2500 0.2500 0.12988(5) 0.0374(4) Uani 1 2 d S T P . .
S1 S 0.4561(4) 0.1984(4) 0.0917(2) 0.0463(15) Uani 1 1 d . . . . .
S2 S 0.5156(4) 0.3946(4) 0.2353(2) 0.0526(16) Uani 1 1 d . . . . .
S3 S 0.3862(4) 0.4790(5) -0.0318(3) 0.0578(19) Uani 1 1 d . . . . .
S4 S 0.3514(5) 0.5654(5) 0.1644(3) 0.065(2) Uani 1 1 d . . . . .
O1 O 0.2946(8) 0.1596(7) 0.2019(5) 0.024(3) Uani 1 1 d . . . . .
O2 O 0.3594(8) 0.3080(8) 0.1865(5) 0.026(3) Uani 1 1 d . . . . .
O3 O 0.3038(8) 0.3514(8) 0.0782(5) 0.028(3) Uani 1 1 d . U . . .
O4 O 0.3634(9) 0.1863(10) 0.0855(6) 0.047(4) Uani 1 1 d . . . . .
O5 O 0.4757(9) 0.2847(10) 0.0762(6) 0.047(4) Uani 1 1 d . . . . .
O6 O 0.3247(11) 0.4751(11) 0.1595(7) 0.061(5) Uani 1 1 d . . . . .
O7 O 0.4791(10) 0.1831(11) 0.1543(6) 0.056(5) Uani 1 1 d . . . . .
O8 O 0.4418(10) 0.4363(10) 0.2615(6) 0.053(4) Uani 1 1 d . . . . .
O9 O 0.5011(11) 0.1416(12) 0.0535(7) 0.067(5) Uani 1 1 d . . . . .
O10 O 0.5122(9) 0.3059(10) 0.2521(7) 0.052(4) Uani 1 1 d . . . . .
O11 O 0.4248(10) 0.3985(12) -0.0155(7) 0.063(5) Uani 1 1 d . . . . .
O12 O 0.5133(10) 0.4001(11) 0.1707(6) 0.058(5) Uani 1 1 d . . . . .
O13 O 0.3616(10) 0.5157(11) 0.0268(7) 0.063(5) Uani 1 1 d . . . . .
O14 O 0.5923(11) 0.4327(11) 0.2580(7) 0.067(5) Uani 1 1 d . . . . .
O15 O 0.3147(11) 0.4697(12) -0.0708(8) 0.082(7) Uani 1 1 d D . . . .
O16 O 0.2934(11) 0.6199(9) 0.1325(8) 0.064(5) Uani 1 1 d . . . . .
O17 O 0.4340(12) 0.5642(12) 0.1364(8) 0.072(6) Uani 1 1 d . . . . .
O18 O 0.4483(10) 0.5353(12) -0.0581(7) 0.066(5) Uani 1 1 d . . . . .
O19 O 0.3565(13) 0.5818(12) 0.2276(8) 0.079(6) Uani 1 1 d . . . . .
C1 C 0.372(2) -0.021(2) 0.1027(13) 0.100(12) Uani 1 1 d . . . . .
H1A H 0.3469 -0.0090 0.1402 0.150 Uiso 1 1 calc R U . . .
H1B H 0.3763 -0.0803 0.0975 0.150 Uiso 1 1 calc R U . . .
H1C H 0.4271 0.0034 0.1013 0.150 Uiso 1 1 calc R U . . .
C2 C 0.359(2) -0.003(2) -0.0032(12) 0.091(11) Uani 1 1 d . . . . .
H2A H 0.3248 0.0206 -0.0340 0.137 Uiso 1 1 calc R U . . .
H2B H 0.4137 0.0214 -0.0048 0.137 Uiso 1 1 calc R U . . .
H2C H 0.3629 -0.0623 -0.0087 0.137 Uiso 1 1 calc R U . . .
C3 C 0.539(3) 0.248(2) -0.0818(16) 0.113(13) Uani 1 1 d . U . . .
H3A H 0.4906 0.2699 -0.1014 0.170 Uiso 1 1 calc R U . . .
H3B H 0.5811 0.2343 -0.1106 0.170 Uiso 1 1 calc R U . . .
H3C H 0.5240 0.1984 -0.0603 0.170 Uiso 1 1 calc R U . . .
C4 C 0.644(3) 0.284(3) -0.0099(19) 0.132(15) Uani 1 1 d . U . . .
H4A H 0.6623 0.3275 0.0161 0.197 Uiso 1 1 calc R U . . .
H4B H 0.6307 0.2347 0.0129 0.197 Uiso 1 1 calc R U . . .
H4C H 0.6878 0.2707 -0.0374 0.197 Uiso 1 1 calc R U . . .
C5 C 0.568(3) 0.642(4) 0.243(2) 0.18(2) Uani 1 1 d . U . . .
H5A H 0.5428 0.6639 0.2075 0.264 Uiso 1 1 calc R U . . .
H5B H 0.6070 0.6815 0.2584 0.264 Uiso 1 1 calc R U . . .
H5C H 0.5970 0.5907 0.2332 0.264 Uiso 1 1 calc R U . . .
C6 C 0.529(3) 0.591(3) 0.3419(19) 0.138(16) Uani 1 1 d . U . . .
H6A H 0.4799 0.5829 0.3655 0.206 Uiso 1 1 calc R U . . .
H6B H 0.5566 0.5377 0.3363 0.206 Uiso 1 1 calc R U . . .
H6C H 0.5666 0.6286 0.3615 0.206 Uiso 1 1 calc R U . . .
C7 C 0.243(5) 0.817(4) 0.341(3) 0.102(19) Uani 0.5 1 d D U P . .
H7A H 0.2381 0.8705 0.3221 0.153 Uiso 0.5 1 calc R U P . .
H7B H 0.1951 0.8067 0.3650 0.153 Uiso 0.5 1 calc R U P . .
H7C H 0.2928 0.8163 0.3650 0.153 Uiso 0.5 1 calc R U P . .
C8 C 0.215(6) 0.254(9) -0.071(3) 0.18(4) Uani 0.5 1 d D U P . .
H8A H 0.1669 0.2795 -0.0884 0.277 Uiso 0.5 1 d R U P . .
H8B H 0.2427 0.2944 -0.0463 0.277 Uiso 0.5 1 d R U P . .
H8C H 0.1989 0.2072 -0.0479 0.277 Uiso 0.5 1 d R U P . .
N1 N 0.3203(14) 0.0151(15) 0.0551(9) 0.071(7) Uani 1 1 d . . . . .
H1D H 0.3159 0.0702 0.0600 0.085 Uiso 1 1 calc R U . . .
H1E H 0.2691 -0.0068 0.0565 0.085 Uiso 1 1 calc R U . . .
N2 N 0.5719(17) 0.3103(17) -0.0411(11) 0.087(8) Uani 1 1 d . U . . .
H2D H 0.5845 0.3564 -0.0613 0.105 Uiso 1 1 calc R U . . .
H2E H 0.5322 0.3235 -0.0152 0.105 Uiso 1 1 calc R U . . .
N3 N 0.506(3) 0.625(3) 0.2847(17) 0.162(17) Uani 1 1 d . . . . .
H3D H 0.4694 0.5898 0.2683 0.194 Uiso 1 1 calc R U . . .
H3E H 0.4785 0.6727 0.2913 0.194 Uiso 1 1 calc R U . . .
N4 N 0.2500 0.7500 0.295(3) 0.109(19) Uani 0.5 2 d DS TU P . .
H4D H 0.2967 0.7551 0.2730 0.131 Uiso 0.5 1 d R U P . .
O1W O 0.2826(16) 0.5468(18) -0.1754(12) 0.128(9) Uani 1 1 d . U . . .
N5 N 0.2500 0.2500 -0.132(3) 0.19(4) Uani 0.5 2 d DS TU P . .
H5D H 0.2715 0.2909 -0.1543 0.223 Uiso 0.5 1 d R U P . .
O2W O 0.161(4) 0.712(4) 0.201(3) 0.16(2) Uani 0.5 1 d . U P . .


_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 O10 2.258(16) . ?
Er1 O7 2.285(14) . ?
Er1 O8 2.286(16) 7_566 ?
Er1 O1 2.305(12) 8_656 ?
Er1 O1 2.311(12) . ?
Er1 O6 2.370(14) 7_566 ?
Er1 O2 2.379(11) . ?
Er1 O2 2.540(12) 7_566 ?
Er1 O19 2.818(19) 7_566 ?
Er1 S4 3.214(6) 7_566 ?
Er1 Er3 3.8421(12) . ?
Er2 O3 2.250(13) . ?
Er2 O12 2.266(16) . ?
Er2 O18 2.279(16) 5_665 ?
Er2 O5 2.306(15) . ?
Er2 O13 2.393(15) . ?
Er2 O6 2.396(15) . ?
Er2 O11 2.472(16) . ?
Er2 O17 2.54(2) . ?
Er2 S3 3.051(6) . ?
Er2 S4 3.097(7) . ?
Er3 O3 2.176(11) 2 ?
Er3 O3 2.176(11) . ?
Er3 O1 2.291(11) 2 ?
Er3 O1 2.292(11) . ?
Er3 O4 2.309(13) . ?
Er3 O4 2.309(13) 2 ?
Er3 O2 2.359(13) 2 ?
Er3 O2 2.359(13) . ?
Er3 Er1 3.8421(12) 2 ?
S1 O9 1.444(16) . ?
S1 O5 1.457(16) . ?
S1 O7 1.485(14) . ?
S1 O4 1.501(16) . ?
S2 O14 1.463(19) . ?
S2 O12 1.466(15) . ?
S2 O10 1.469(16) . ?
S2 O8 1.479(17) . ?
S3 O15 1.453(18) . ?
S3 O18 1.467(17) . ?
S3 O11 1.473(18) . ?
S3 O13 1.503(17) . ?
S4 O19 1.459(19) . ?
S4 O16 1.464(18) . ?
S4 O17 1.465(18) . ?
S4 O6 1.508(19) . ?
S4 Er1 3.214(6) 8_656 ?
O1 Er1 2.305(12) 7_566 ?
O2 Er1 2.540(12) 8_656 ?
O6 Er1 2.370(14) 8_656 ?
O8 Er1 2.286(16) 8_656 ?
O18 Er2 2.279(16) 5_665 ?
O19 Er1 2.818(19) 8_656 ?
C1 N1 1.48(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.49(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N2 1.46(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N2 1.42(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N3 1.40(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.46(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N4 1.50(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C8 1.12(18) 2 ?
C8 N5 1.49(2) . ?
C8 H8A 0.9558 . ?
C8 H8B 0.9560 . ?
C8 H8C 0.9559 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N4 C7 1.50(2) 2_565 ?
N4 H4D 0.8961 . ?
N5 C8 1.49(2) 2 ?
N5 H5D 0.8963 . ?

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
O10 Er1 O7 82.9(6) . . ?
O10 Er1 O8 131.9(6) . 7_566 ?
O7 Er1 O8 76.9(6) . 7_566 ?
O10 Er1 O1 80.3(5) . 8_656 ?
O7 Er1 O1 140.8(5) . 8_656 ?
O8 Er1 O1 138.6(5) 7_566 8_656 ?
O10 Er1 O1 143.7(5) . . ?
O7 Er1 O1 86.9(5) . . ?
O8 Er1 O1 78.4(5) 7_566 . ?
O1 Er1 O1 86.1(5) 8_656 . ?
O10 Er1 O6 79.2(5) . 7_566 ?
O7 Er1 O6 130.0(6) . 7_566 ?
O8 Er1 O6 81.4(6) 7_566 7_566 ?
O1 Er1 O6 80.8(5) 8_656 7_566 ?
O1 Er1 O6 131.7(5) . 7_566 ?
O10 Er1 O2 76.0(5) . . ?
O7 Er1 O2 75.6(4) . . ?
O8 Er1 O2 137.0(5) 7_566 . ?
O1 Er1 O2 66.1(4) 8_656 . ?
O1 Er1 O2 67.7(4) . . ?
O6 Er1 O2 141.3(5) 7_566 . ?
O10 Er1 O2 134.2(5) . 7_566 ?
O7 Er1 O2 142.9(5) . 7_566 ?
O8 Er1 O2 75.8(5) 7_566 7_566 ?
O1 Er1 O2 63.0(4) 8_656 7_566 ?
O1 Er1 O2 63.4(4) . 7_566 ?
O6 Er1 O2 69.3(5) 7_566 7_566 ?
O2 Er1 O2 109.3(5) . 7_566 ?
O10 Er1 O19 67.5(6) . 7_566 ?
O7 Er1 O19 76.9(5) . 7_566 ?
O8 Er1 O19 65.6(6) 7_566 7_566 ?
O1 Er1 O19 126.8(5) 8_656 7_566 ?
O1 Er1 O19 143.0(5) . 7_566 ?
O6 Er1 O19 53.1(6) 7_566 7_566 ?
O2 Er1 O19 136.4(5) . 7_566 ?
O2 Er1 O19 113.1(4) 7_566 7_566 ?
O10 Er1 S4 70.6(4) . 7_566 ?
O7 Er1 S4 103.9(4) . 7_566 ?
O8 Er1 S4 72.7(4) 7_566 7_566 ?
O1 Er1 S4 103.4(3) 8_656 7_566 ?
O1 Er1 S4 145.6(3) . 7_566 ?
O6 Er1 S4 26.2(5) 7_566 7_566 ?
O2 Er1 S4 146.4(3) . 7_566 ?
O2 Er1 S4 91.4(3) 7_566 7_566 ?
O19 Er1 S4 27.0(4) 7_566 7_566 ?
O10 Er1 Er3 110.8(4) . . ?
O7 Er1 Er3 73.0(4) . . ?
O8 Er1 Er3 104.2(4) 7_566 . ?
O1 Er1 Er3 80.4(3) 8_656 . ?
O1 Er1 Er3 33.2(3) . . ?
O6 Er1 Er3 156.8(4) 7_566 . ?
O2 Er1 Er3 35.6(3) . . ?
O2 Er1 Er3 90.0(3) 7_566 . ?
O19 Er1 Er3 149.8(4) 7_566 . ?
S4 Er1 Er3 176.17(16) 7_566 . ?
O3 Er2 O12 126.0(5) . . ?
O3 Er2 O18 150.3(5) . 5_665 ?
O12 Er2 O18 76.6(5) . 5_665 ?
O3 Er2 O5 80.6(5) . . ?
O12 Er2 O5 78.3(6) . . ?
O18 Er2 O5 86.7(6) 5_665 . ?
O3 Er2 O13 81.0(5) . . ?
O12 Er2 O13 146.5(7) . . ?
O18 Er2 O13 87.2(5) 5_665 . ?
O5 Er2 O13 130.5(6) . . ?
O3 Er2 O6 71.7(6) . . ?
O12 Er2 O6 88.5(6) . . ?
O18 Er2 O6 133.5(7) 5_665 . ?
O5 Er2 O6 133.4(5) . . ?
O13 Er2 O6 81.6(5) . . ?
O3 Er2 O11 77.7(5) . . ?
O12 Er2 O11 139.6(6) . . ?
O18 Er2 O11 73.0(6) 5_665 . ?
O5 Er2 O11 74.0(5) . . ?
O13 Er2 O11 57.3(6) . . ?
O6 Er2 O11 131.9(6) . . ?
O3 Er2 O17 122.4(5) . . ?
O12 Er2 O17 77.5(6) . . ?
O18 Er2 O17 77.9(6) 5_665 . ?
O5 Er2 O17 153.8(6) . . ?
O13 Er2 O17 70.4(6) . . ?
O6 Er2 O17 55.9(6) . . ?
O11 Er2 O17 120.2(6) . . ?
O3 Er2 S3 80.4(3) . . ?
O12 Er2 S3 152.7(4) . . ?
O18 Er2 S3 76.2(4) 5_665 . ?
O5 Er2 S3 102.5(4) . . ?
O13 Er2 S3 29.0(4) . . ?
O6 Er2 S3 108.7(4) . . ?
O11 Er2 S3 28.6(4) . . ?
O17 Er2 S3 94.4(4) . . ?
O3 Er2 S4 95.9(3) . . ?
O12 Er2 S4 85.8(5) . . ?
O18 Er2 S4 105.8(5) 5_665 . ?
O5 Er2 S4 157.0(3) . . ?
O13 Er2 S4 70.5(4) . . ?
O6 Er2 S4 28.4(4) . . ?
O11 Er2 S4 127.8(4) . . ?
O17 Er2 S4 28.0(4) . . ?
S3 Er2 S4 99.28(18) . . ?
O3 Er3 O3 114.9(7) 2 . ?
O3 Er3 O1 136.8(5) 2 2 ?
O3 Er3 O1 92.1(4) . 2 ?
O3 Er3 O1 92.1(4) 2 . ?
O3 Er3 O1 136.8(5) . . ?
O1 Er3 O1 89.3(5) 2 . ?
O3 Er3 O4 75.4(5) 2 . ?
O3 Er3 O4 77.5(5) . . ?
O1 Er3 O4 146.3(5) 2 . ?
O1 Er3 O4 77.8(4) . . ?
O3 Er3 O4 77.5(5) 2 2 ?
O3 Er3 O4 75.4(5) . 2 ?
O1 Er3 O4 77.8(4) 2 2 ?
O1 Er3 O4 146.3(5) . 2 ?
O4 Er3 O4 128.4(7) . 2 ?
O3 Er3 O2 72.9(4) 2 2 ?
O3 Er3 O2 151.5(4) . 2 ?
O1 Er3 O2 68.3(4) 2 2 ?
O1 Er3 O2 66.2(4) . 2 ?
O4 Er3 O2 130.2(5) . 2 ?
O4 Er3 O2 80.1(5) 2 2 ?
O3 Er3 O2 151.5(4) 2 . ?
O3 Er3 O2 72.9(4) . . ?
O1 Er3 O2 66.2(4) 2 . ?
O1 Er3 O2 68.3(4) . . ?
O4 Er3 O2 80.1(5) . . ?
O4 Er3 O2 130.2(5) 2 . ?
O2 Er3 O2 114.1(5) 2 . ?
O3 Er3 Er1 119.2(3) 2 . ?
O3 Er3 Er1 104.0(3) . . ?
O1 Er3 Er1 82.3(3) 2 . ?
O1 Er3 Er1 33.6(3) . . ?
O4 Er3 Er1 69.6(3) . . ?
O4 Er3 Er1 160.0(3) 2 . ?
O2 Er3 Er1 94.0(3) 2 . ?
O2 Er3 Er1 36.0(3) . . ?
O3 Er3 Er1 104.0(3) 2 2 ?
O3 Er3 Er1 119.2(3) . 2 ?
O1 Er3 Er1 33.6(3) 2 2 ?
O1 Er3 Er1 82.3(3) . 2 ?
O4 Er3 Er1 160.0(3) . 2 ?
O4 Er3 Er1 69.6(3) 2 2 ?
O2 Er3 Er1 36.0(3) 2 2 ?
O2 Er3 Er1 94.0(3) . 2 ?
Er1 Er3 Er1 94.42(4) . 2 ?
O9 S1 O5 110.1(10) . . ?
O9 S1 O7 110.3(9) . . ?
O5 S1 O7 109.4(10) . . ?
O9 S1 O4 110.8(11) . . ?
O5 S1 O4 108.1(9) . . ?
O7 S1 O4 108.2(9) . . ?
O14 S2 O12 110.3(10) . . ?
O14 S2 O10 110.0(10) . . ?
O12 S2 O10 108.4(10) . . ?
O14 S2 O8 109.8(10) . . ?
O12 S2 O8 110.7(10) . . ?
O10 S2 O8 107.6(9) . . ?
O15 S3 O18 110.3(10) . . ?
O15 S3 O11 113.1(12) . . ?
O18 S3 O11 110.8(10) . . ?
O15 S3 O13 111.8(11) . . ?
O18 S3 O13 107.2(11) . . ?
O11 S3 O13 103.3(9) . . ?
O15 S3 Er2 134.0(8) . . ?
O18 S3 Er2 115.5(7) . . ?
O11 S3 Er2 53.3(7) . . ?
O13 S3 Er2 50.4(6) . . ?
O19 S4 O16 114.4(12) . . ?
O19 S4 O17 112.2(13) . . ?
O16 S4 O17 111.4(10) . . ?
O19 S4 O6 105.0(10) . . ?
O16 S4 O6 110.8(11) . . ?
O17 S4 O6 102.2(10) . . ?
O19 S4 Er2 129.0(9) . . ?
O16 S4 Er2 116.0(8) . . ?
O17 S4 Er2 54.3(8) . . ?
O6 S4 Er2 49.0(6) . . ?
O19 S4 Er1 61.2(8) . 8_656 ?
O16 S4 Er1 125.9(7) . 8_656 ?
O17 S4 Er1 119.8(8) . 8_656 ?
O6 S4 Er1 43.9(6) . 8_656 ?
Er2 S4 Er1 83.10(17) . 8_656 ?
Er3 O1 Er1 120.7(5) . 7_566 ?
Er3 O1 Er1 113.2(5) . . ?
Er1 O1 Er1 119.8(4) 7_566 . ?
Er3 O2 Er1 108.4(5) . . ?
Er3 O2 Er1 109.2(4) . 8_656 ?
Er1 O2 Er1 108.5(4) . 8_656 ?
Er3 O3 Er2 128.1(5) . . ?
S1 O4 Er3 132.7(9) . . ?
S1 O5 Er2 139.7(8) . . ?
S4 O6 Er1 109.9(9) . 8_656 ?
S4 O6 Er2 102.6(8) . . ?
Er1 O6 Er2 122.9(7) 8_656 . ?
S1 O7 Er1 137.5(9) . . ?
S2 O8 Er1 135.1(10) . 8_656 ?
S2 O10 Er1 136.9(10) . . ?
S3 O11 Er2 98.1(9) . . ?
S2 O12 Er2 143.1(10) . . ?
S3 O13 Er2 100.6(8) . . ?
S4 O17 Er2 97.8(10) . . ?
S3 O18 Er2 159.4(11) . 5_665 ?
S4 O19 Er1 91.8(9) . 8_656 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C8 N5 68(4) 2 . ?
C8 C8 H8A 149.0 2 . ?
N5 C8 H8A 86.6 . . ?
C8 C8 H8B 68.4 2 . ?
N5 C8 H8B 113.9 . . ?
H8A C8 H8B 109.5 . . ?
C8 C8 H8C 99.8 2 . ?
N5 C8 H8C 124.9 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.4 . . ?
C1 N1 C2 110(2) . . ?
C1 N1 H1D 109.7 . . ?
C2 N1 H1D 109.7 . . ?
C1 N1 H1E 109.7 . . ?
C2 N1 H1E 109.7 . . ?
H1D N1 H1E 108.2 . . ?
C4 N2 C3 114(3) . . ?
C4 N2 H2D 108.8 . . ?
C3 N2 H2D 108.8 . . ?
C4 N2 H2E 108.8 . . ?
C3 N2 H2E 108.8 . . ?
H2D N2 H2E 107.7 . . ?
C5 N3 C6 119(4) . . ?
C5 N3 H3D 107.5 . . ?
C6 N3 H3D 107.5 . . ?
C5 N3 H3E 107.5 . . ?
C6 N3 H3E 107.5 . . ?
H3D N3 H3E 107.0 . . ?
C7 N4 C7 91(7) . 2_565 ?
C7 N4 H4D 112.0 . . ?
C7 N4 H4D 112.8 2_565 . ?
C8 N5 C8 44(7) . 2 ?
C8 N5 H5D 129.3 . . ?
C8 N5 H5D 114.7 2 . ?

_refine_diff_density_max         2.248
_refine_diff_density_min         -2.121
_refine_diff_density_rms         0.265

####################################################################### 
# 
# 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_a01_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1544847'
_audit_update_record             
;
2017-04-20 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H136 Eu10 N14 O82 S16'
_chemical_formula_weight         4014.06

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   16.0974(13)
_cell_length_b                   16.0974(13)
_cell_length_c                   22.8640(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5924.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7780
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      24.27

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_F_000             3888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    5.599
_shelx_estimated_absorpt_T_min   0.487
_shelx_estimated_absorpt_T_max   0.530
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43204
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_av_R_equivalents  0.1772
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.547
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5498
_reflns_number_gt                4192
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²+174.8680P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5498
_refine_ls_number_parameters     358
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_ref         0.1959
_refine_ls_wR_factor_gt          0.1888
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.177
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.42729(6) 0.41691(6) 0.09407(4) 0.0478(3) Uani 1 1 d . . . . .
Eu2 Eu 0.2500 0.2500 0.12862(4) 0.0342(3) Uani 1 2 d S T P . .
Eu3 Eu 0.42393(6) 0.19992(6) 0.24455(3) 0.0404(3) Uani 1 1 d . . . . .
S1 S 0.4593(3) 0.1959(3) 0.09036(18) 0.0441(11) Uani 1 1 d . . . . .
S2 S 0.5197(3) 0.3968(3) 0.23644(19) 0.0508(12) Uani 1 1 d . . . . .
S3 S 0.3850(3) 0.4787(3) -0.0312(2) 0.0542(13) Uani 1 1 d . . . . .
S4 S 0.3498(4) 0.5669(3) 0.1644(2) 0.0620(15) Uani 1 1 d . . . . .
O1 O 0.2954(6) 0.1611(6) 0.2033(4) 0.026(2) Uani 1 1 d . . . . .
O2 O 0.3641(6) 0.3125(6) 0.1827(4) 0.024(2) Uani 1 1 d . . . . .
O3 O 0.3024(6) 0.3526(6) 0.0752(4) 0.029(2) Uani 1 1 d . . . . .
O4 O 0.3685(8) 0.1838(8) 0.0856(5) 0.050(3) Uani 1 1 d . . . . .
O5 O 0.4787(8) 0.2820(8) 0.0746(5) 0.053(3) Uani 1 1 d . . . . .
O6 O 0.3195(9) 0.4796(8) 0.1566(5) 0.060(4) Uani 1 1 d . . . . .
O7 O 0.4839(8) 0.1815(9) 0.1523(5) 0.054(4) Uani 1 1 d . . . . .
O8 O 0.4454(8) 0.4393(9) 0.2608(5) 0.057(4) Uani 1 1 d . . . . .
O9 O 0.5035(8) 0.1389(8) 0.0527(5) 0.057(4) Uani 1 1 d . . . . .
O10 O 0.5162(8) 0.3094(9) 0.2532(5) 0.059(4) Uani 1 1 d . . . . .
O11 O 0.4260(8) 0.4008(9) -0.0156(5) 0.060(4) Uani 1 1 d . . . . .
O12 O 0.5195(9) 0.4029(9) 0.1723(5) 0.061(4) Uani 1 1 d . . . . .
O13 O 0.3596(9) 0.5164(9) 0.0262(5) 0.061(4) Uani 1 1 d . . . . .
O14 O 0.5939(10) 0.4353(10) 0.2605(6) 0.074(5) Uani 1 1 d . . . . .
O15 O 0.3142(9) 0.4675(10) -0.0683(6) 0.082(5) Uani 1 1 d D . . . .
O16 O 0.2945(9) 0.6230(8) 0.1343(7) 0.069(4) Uani 1 1 d . . . . .
O17 O 0.4328(9) 0.5663(9) 0.1376(6) 0.067(4) Uani 1 1 d . . . . .
O18 O 0.4464(8) 0.5364(9) -0.0580(5) 0.060(4) Uani 1 1 d . . . . .
O19 O 0.3537(11) 0.5795(9) 0.2282(6) 0.074(5) Uani 1 1 d . . . . .
C1 C 0.3710(19) -0.0248(17) 0.1009(11) 0.096(9) Uani 1 1 d . . . . .
H1A H 0.3472 -0.0109 0.1382 0.144 Uiso 1 1 calc R U . . .
H1B H 0.3707 -0.0840 0.0960 0.144 Uiso 1 1 calc R U . . .
H1C H 0.4271 -0.0048 0.0992 0.144 Uiso 1 1 calc R U . . .
C2 C 0.3577(15) -0.007(2) -0.0031(10) 0.098(10) Uani 1 1 d . . . . .
H2A H 0.3263 0.0180 -0.0342 0.147 Uiso 1 1 calc R U . . .
H2B H 0.4138 0.0131 -0.0044 0.147 Uiso 1 1 calc R U . . .
H2C H 0.3574 -0.0661 -0.0076 0.147 Uiso 1 1 calc R U . . .
C3 C 0.533(2) 0.251(2) -0.0805(14) 0.119(11) Uani 1 1 d . U . . .
H3A H 0.4855 0.2751 -0.0989 0.179 Uiso 1 1 calc R U . . .
H3B H 0.5725 0.2342 -0.1098 0.179 Uiso 1 1 calc R U . . .
H3C H 0.5170 0.2037 -0.0578 0.179 Uiso 1 1 calc R U . . .
C4 C 0.6432(19) 0.2804(19) -0.0139(13) 0.113(10) Uani 1 1 d . U . . .
H4A H 0.6665 0.3227 0.0108 0.170 Uiso 1 1 calc R U . . .
H4B H 0.6279 0.2333 0.0095 0.170 Uiso 1 1 calc R U . . .
H4C H 0.6835 0.2638 -0.0425 0.170 Uiso 1 1 calc R U . . .
C5 C 0.570(3) 0.639(3) 0.2438(19) 0.166(17) Uani 1 1 d . U . . .
H5A H 0.5464 0.6618 0.2086 0.249 Uiso 1 1 calc R U . . .
H5B H 0.6092 0.6778 0.2597 0.249 Uiso 1 1 calc R U . . .
H5C H 0.5973 0.5877 0.2350 0.249 Uiso 1 1 calc R U . . .
C6 C 0.525(2) 0.592(2) 0.3407(14) 0.122(11) Uani 1 1 d . U . . .
H6A H 0.4744 0.5858 0.3629 0.184 Uiso 1 1 calc R U . . .
H6B H 0.5502 0.5380 0.3361 0.184 Uiso 1 1 calc R U . . .
H6C H 0.5621 0.6281 0.3608 0.184 Uiso 1 1 calc R U . . .
C7 C 0.240(4) 0.820(3) 0.343(2) 0.116(18) Uani 0.5 1 d D U P . .
H7A H 0.2333 0.8714 0.3221 0.174 Uiso 0.5 1 calc R U P . .
H7B H 0.1925 0.8108 0.3673 0.174 Uiso 0.5 1 calc R U P . .
H7C H 0.2890 0.8240 0.3673 0.174 Uiso 0.5 1 calc R U P . .
C8 C 0.216(5) 0.260(6) -0.069(2) 0.17(3) Uani 0.5 1 d D U P . .
H8A H 0.1677 0.2853 -0.0863 0.256 Uiso 0.5 1 d R U P . .
H8B H 0.2436 0.3002 -0.0442 0.256 Uiso 0.5 1 d R U P . .
H8C H 0.1998 0.2130 -0.0458 0.256 Uiso 0.5 1 d R U P . .
N1 N 0.3205(11) 0.0151(12) 0.0528(7) 0.069(5) Uani 1 1 d . . . . .
H1D H 0.2683 -0.0030 0.0543 0.082 Uiso 1 1 calc R U . . .
H1E H 0.3202 0.0700 0.0572 0.082 Uiso 1 1 calc R U . . .
N2 N 0.5718(14) 0.3121(13) -0.0425(10) 0.092(8) Uani 1 1 d . . . . .
H2D H 0.5860 0.3564 -0.0635 0.111 Uiso 1 1 calc R U . . .
H2E H 0.5350 0.3284 -0.0158 0.111 Uiso 1 1 calc R U . . .
N3 N 0.506(2) 0.625(2) 0.2849(14) 0.150(12) Uani 1 1 d . . . . .
H3D H 0.4801 0.6731 0.2907 0.179 Uiso 1 1 calc R U . . .
H3E H 0.4693 0.5910 0.2682 0.179 Uiso 1 1 calc R U . . .
N4 N 0.2500 0.7500 0.301(3) 0.123(19) Uani 0.5 2 d DS TU P . .
H4D H 0.2967 0.7551 0.2792 0.148 Uiso 0.5 1 d R U P . .
O1W O 0.2819(15) 0.5476(16) -0.1725(11) 0.147(9) Uani 1 1 d . U . . .
N5 N 0.2500 0.2500 -0.129(2) 0.17(3) Uani 0.5 2 d DS TU P . .
H5D H 0.2715 0.2909 -0.1514 0.207 Uiso 0.5 1 d R U P . .
O2W O 0.158(4) 0.714(3) 0.204(2) 0.156(19) Uani 0.5 1 d . U P . .


_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 O3 2.302(11) . ?
Eu1 O18 2.319(12) 5_665 ?
Eu1 O12 2.335(13) . ?
Eu1 O5 2.366(12) . ?
Eu1 O6 2.465(11) . ?
Eu1 O13 2.482(12) . ?
Eu1 O11 2.521(12) . ?
Eu1 O17 2.604(15) . ?
Eu1 O2 2.823(9) . ?
Eu1 S3 3.107(5) . ?
Eu1 S4 3.158(5) . ?
Eu1 Eu2 3.9984(11) . ?
Eu2 O3 2.220(9) 2 ?
Eu2 O3 2.221(9) . ?
Eu2 O1 2.345(8) . ?
Eu2 O1 2.345(8) 2 ?
Eu2 O4 2.396(12) 2 ?
Eu2 O4 2.396(12) . ?
Eu2 O2 2.432(10) 2 ?
Eu2 O2 2.432(10) . ?
Eu2 Eu3 3.9389(11) . ?
Eu2 Eu3 3.9389(11) 2 ?
Eu2 Eu1 3.9984(11) 2 ?
Eu3 O10 2.313(15) . ?
Eu3 O7 2.338(11) . ?
Eu3 O1 2.358(10) . ?
Eu3 O8 2.356(14) 7_566 ?
Eu3 O1 2.379(10) 8_656 ?
Eu3 O6 2.452(11) 7_566 ?
Eu3 O2 2.492(9) . ?
Eu3 O2 2.655(9) 7_566 ?
Eu3 O19 2.721(15) 7_566 ?
Eu3 S4 3.205(5) 7_566 ?
Eu3 S2 3.529(5) . ?
S1 O9 1.446(12) . ?
S1 O5 1.465(14) . ?
S1 O4 1.478(14) . ?
S1 O7 1.489(11) . ?
S2 O14 1.454(16) . ?
S2 O10 1.460(15) . ?
S2 O12 1.470(12) . ?
S2 O8 1.485(14) . ?
S3 O15 1.432(16) . ?
S3 O11 1.461(14) . ?
S3 O18 1.489(13) . ?
S3 O13 1.503(13) . ?
S4 O16 1.443(15) . ?
S4 O17 1.470(14) . ?
S4 O19 1.473(15) . ?
S4 O6 1.498(15) . ?
S4 Eu3 3.205(5) 8_656 ?
O1 Eu3 2.379(10) 7_566 ?
O2 Eu3 2.655(9) 8_656 ?
O6 Eu3 2.452(11) 8_656 ?
O8 Eu3 2.356(14) 8_656 ?
O18 Eu1 2.319(12) 5_665 ?
O19 Eu3 2.721(15) 8_656 ?
C1 N1 1.51(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.46(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N2 1.45(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N2 1.42(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N3 1.41(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.42(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N4 1.50(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C8 1.14(14) 2 ?
C8 N5 1.48(2) . ?
C8 H8A 0.9631 . ?
C8 H8B 0.9637 . ?
C8 H8C 0.9636 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N4 C7 1.50(2) 2_565 ?
N4 H4D 0.9033 . ?
N5 C8 1.48(2) 2 ?
N5 H5D 0.9035 . ?

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
O3 Eu1 O18 147.7(4) . 5_665 ?
O3 Eu1 O12 130.9(4) . . ?
O18 Eu1 O12 75.3(4) 5_665 . ?
O3 Eu1 O5 81.8(4) . . ?
O18 Eu1 O5 85.7(5) 5_665 . ?
O12 Eu1 O5 80.4(5) . . ?
O3 Eu1 O6 71.2(4) . . ?
O18 Eu1 O6 133.7(5) 5_665 . ?
O12 Eu1 O6 92.5(5) . . ?
O5 Eu1 O6 137.0(4) . . ?
O3 Eu1 O13 77.9(4) . . ?
O18 Eu1 O13 87.3(4) 5_665 . ?
O12 Eu1 O13 145.1(5) . . ?
O5 Eu1 O13 128.9(4) . . ?
O6 Eu1 O13 77.8(4) . . ?
O3 Eu1 O11 76.1(4) . . ?
O18 Eu1 O11 71.8(5) 5_665 . ?
O12 Eu1 O11 139.2(4) . . ?
O5 Eu1 O11 73.8(4) . . ?
O6 Eu1 O11 127.8(4) . . ?
O13 Eu1 O11 56.0(4) . . ?
O3 Eu1 O17 121.1(4) . . ?
O18 Eu1 O17 78.9(5) 5_665 . ?
O12 Eu1 O17 77.0(5) . . ?
O5 Eu1 O17 155.1(5) . . ?
O6 Eu1 O17 54.8(4) . . ?
O13 Eu1 O17 70.0(5) . . ?
O11 Eu1 O17 118.4(4) . . ?
O3 Eu1 O2 63.4(3) . . ?
O18 Eu1 O2 139.8(4) 5_665 . ?
O12 Eu1 O2 67.8(4) . . ?
O5 Eu1 O2 73.4(3) . . ?
O6 Eu1 O2 64.8(3) . . ?
O13 Eu1 O2 132.5(4) . . ?
O11 Eu1 O2 130.5(4) . . ?
O17 Eu1 O2 106.7(3) . . ?
O3 Eu1 S3 77.3(2) . . ?
O18 Eu1 S3 76.2(3) 5_665 . ?
O12 Eu1 S3 151.2(3) . . ?
O5 Eu1 S3 101.4(3) . . ?
O6 Eu1 S3 104.4(3) . . ?
O13 Eu1 S3 28.5(3) . . ?
O11 Eu1 S3 27.7(3) . . ?
O17 Eu1 S3 93.7(3) . . ?
O2 Eu1 S3 140.7(2) . . ?
O3 Eu1 S4 95.4(3) . . ?
O18 Eu1 S4 106.2(4) 5_665 . ?
O12 Eu1 S4 86.3(4) . . ?
O5 Eu1 S4 159.3(3) . . ?
O6 Eu1 S4 27.5(3) . . ?
O13 Eu1 S4 69.6(3) . . ?
O11 Eu1 S4 125.6(3) . . ?
O17 Eu1 S4 27.5(3) . . ?
O2 Eu1 S4 87.0(2) . . ?
S3 Eu1 S4 97.94(14) . . ?
O3 Eu1 Eu2 27.3(2) . . ?
O18 Eu1 Eu2 156.0(4) 5_665 . ?
O12 Eu1 Eu2 103.7(3) . . ?
O5 Eu1 Eu2 70.7(3) . . ?
O6 Eu1 Eu2 70.0(3) . . ?
O13 Eu1 Eu2 104.1(4) . . ?
O11 Eu1 Eu2 97.0(3) . . ?
O17 Eu1 Eu2 124.7(3) . . ?
O2 Eu1 Eu2 36.94(19) . . ?
S3 Eu1 Eu2 103.93(11) . . ?
S4 Eu1 Eu2 97.54(10) . . ?
O3 Eu2 O3 113.3(5) 2 . ?
O3 Eu2 O1 93.7(3) 2 . ?
O3 Eu2 O1 137.4(4) . . ?
O3 Eu2 O1 137.4(4) 2 2 ?
O3 Eu2 O1 93.7(3) . 2 ?
O1 Eu2 O1 86.5(4) . 2 ?
O3 Eu2 O4 78.6(4) 2 2 ?
O3 Eu2 O4 75.3(4) . 2 ?
O1 Eu2 O4 144.9(4) . 2 ?
O1 Eu2 O4 77.2(4) 2 2 ?
O3 Eu2 O4 75.3(4) 2 . ?
O3 Eu2 O4 78.6(4) . . ?
O1 Eu2 O4 77.2(4) . . ?
O1 Eu2 O4 144.9(4) 2 . ?
O4 Eu2 O4 131.6(5) 2 . ?
O3 Eu2 O2 71.7(3) 2 2 ?
O3 Eu2 O2 150.9(3) . 2 ?
O1 Eu2 O2 67.2(3) . 2 ?
O1 Eu2 O2 69.3(3) 2 2 ?
O4 Eu2 O2 77.9(4) 2 2 ?
O4 Eu2 O2 128.8(4) . 2 ?
O3 Eu2 O2 150.9(3) 2 . ?
O3 Eu2 O2 71.7(3) . . ?
O1 Eu2 O2 69.3(3) . . ?
O1 Eu2 O2 67.2(3) 2 . ?
O4 Eu2 O2 128.8(4) 2 . ?
O4 Eu2 O2 77.9(4) . . ?
O2 Eu2 O2 118.9(4) 2 . ?
O3 Eu2 Eu3 119.2(2) 2 . ?
O3 Eu2 Eu3 104.6(3) . . ?
O1 Eu2 Eu3 33.2(3) . . ?
O1 Eu2 Eu3 81.8(2) 2 . ?
O4 Eu2 Eu3 158.9(3) 2 . ?
O4 Eu2 Eu3 67.6(3) . . ?
O2 Eu2 Eu3 96.3(2) 2 . ?
O2 Eu2 Eu3 37.4(2) . . ?
O3 Eu2 Eu3 104.6(3) 2 2 ?
O3 Eu2 Eu3 119.2(2) . 2 ?
O1 Eu2 Eu3 81.8(2) . 2 ?
O1 Eu2 Eu3 33.2(3) 2 2 ?
O4 Eu2 Eu3 67.6(3) 2 2 ?
O4 Eu2 Eu3 158.9(3) . 2 ?
O2 Eu2 Eu3 37.4(2) 2 2 ?
O2 Eu2 Eu3 96.3(2) . 2 ?
Eu3 Eu2 Eu3 95.41(3) . 2 ?
O3 Eu2 Eu1 131.5(3) 2 . ?
O3 Eu2 Eu1 28.4(3) . . ?
O1 Eu2 Eu1 109.3(3) . . ?
O1 Eu2 Eu1 87.5(3) 2 . ?
O4 Eu2 Eu1 100.9(3) 2 . ?
O4 Eu2 Eu1 69.5(3) . . ?
O2 Eu2 Eu1 156.5(2) 2 . ?
O2 Eu2 Eu1 44.2(2) . . ?
Eu3 Eu2 Eu1 76.30(2) . . ?
Eu3 Eu2 Eu1 120.18(2) 2 . ?
O3 Eu2 Eu1 28.4(3) 2 2 ?
O3 Eu2 Eu1 131.5(3) . 2 ?
O1 Eu2 Eu1 87.5(3) . 2 ?
O1 Eu2 Eu1 109.3(3) 2 2 ?
O4 Eu2 Eu1 69.5(3) 2 2 ?
O4 Eu2 Eu1 100.9(3) . 2 ?
O2 Eu2 Eu1 44.2(2) 2 2 ?
O2 Eu2 Eu1 156.5(2) . 2 ?
Eu3 Eu2 Eu1 120.18(2) . 2 ?
Eu3 Eu2 Eu1 76.30(2) 2 2 ?
Eu1 Eu2 Eu1 157.21(4) . 2 ?
O10 Eu3 O7 84.7(5) . . ?
O10 Eu3 O1 143.1(4) . . ?
O7 Eu3 O1 88.1(4) . . ?
O10 Eu3 O8 133.9(5) . 7_566 ?
O7 Eu3 O8 77.5(4) . 7_566 ?
O1 Eu3 O8 78.9(4) . 7_566 ?
O10 Eu3 O1 80.5(4) . 8_656 ?
O7 Eu3 O1 140.5(4) . 8_656 ?
O1 Eu3 O1 82.4(4) . 8_656 ?
O8 Eu3 O1 136.8(4) 7_566 8_656 ?
O10 Eu3 O6 77.5(4) . 7_566 ?
O7 Eu3 O6 131.7(4) . 7_566 ?
O1 Eu3 O6 131.0(4) . 7_566 ?
O8 Eu3 O6 83.3(4) 7_566 7_566 ?
O1 Eu3 O6 80.2(4) 8_656 7_566 ?
O10 Eu3 O2 75.1(4) . . ?
O7 Eu3 O2 74.9(3) . . ?
O1 Eu3 O2 68.1(3) . . ?
O8 Eu3 O2 137.1(4) 7_566 . ?
O1 Eu3 O2 65.9(3) 8_656 . ?
O6 Eu3 O2 139.2(4) 7_566 . ?
O10 Eu3 O2 132.6(4) . 7_566 ?
O7 Eu3 O2 142.6(4) . 7_566 ?
O1 Eu3 O2 63.6(3) . 7_566 ?
O8 Eu3 O2 73.6(4) 7_566 7_566 ?
O1 Eu3 O2 63.1(3) 8_656 7_566 ?
O6 Eu3 O2 67.7(4) 7_566 7_566 ?
O2 Eu3 O2 112.1(4) . 7_566 ?
O10 Eu3 O19 68.4(5) . 7_566 ?
O7 Eu3 O19 77.7(4) . 7_566 ?
O1 Eu3 O19 144.6(4) . 7_566 ?
O8 Eu3 O19 66.4(5) 7_566 7_566 ?
O1 Eu3 O19 128.3(4) 8_656 7_566 ?
O6 Eu3 O19 54.0(5) 7_566 7_566 ?
O2 Eu3 O19 135.8(4) . 7_566 ?
O2 Eu3 O19 110.8(4) 7_566 7_566 ?
O10 Eu3 S4 70.9(3) . 7_566 ?
O7 Eu3 S4 105.0(3) . 7_566 ?
O1 Eu3 S4 145.5(2) . 7_566 ?
O8 Eu3 S4 73.2(3) 7_566 7_566 ?
O1 Eu3 S4 104.4(2) 8_656 7_566 ?
O6 Eu3 S4 26.7(4) 7_566 7_566 ?
O2 Eu3 S4 145.9(3) . 7_566 ?
O2 Eu3 S4 88.9(2) 7_566 7_566 ?
O19 Eu3 S4 27.3(3) 7_566 7_566 ?
O10 Eu3 S2 16.3(3) . . ?
O7 Eu3 S2 83.5(4) . . ?
O1 Eu3 S2 126.9(2) . . ?
O8 Eu3 S2 147.5(4) 7_566 . ?
O1 Eu3 S2 72.4(2) 8_656 . ?
O6 Eu3 S2 90.2(3) 7_566 . ?
O2 Eu3 S2 59.1(2) . . ?
O2 Eu3 S2 132.6(2) 7_566 . ?
O19 Eu3 S2 84.0(4) 7_566 . ?
S4 Eu3 S2 86.84(13) 7_566 . ?
O10 Eu3 Eu2 111.0(3) . . ?
O7 Eu3 Eu2 73.3(3) . . ?
O1 Eu3 Eu2 33.0(2) . . ?
O8 Eu3 Eu2 104.0(3) 7_566 . ?
O1 Eu3 Eu2 78.2(2) 8_656 . ?
O6 Eu3 Eu2 155.0(3) 7_566 . ?
O2 Eu3 Eu2 36.3(2) . . ?
O2 Eu3 Eu2 91.18(19) 7_566 . ?
O19 Eu3 Eu2 150.8(3) 7_566 . ?
S4 Eu3 Eu2 177.06(12) 7_566 . ?
S2 Eu3 Eu2 95.23(8) . . ?
O9 S1 O5 110.4(7) . . ?
O9 S1 O4 111.1(8) . . ?
O5 S1 O4 108.5(8) . . ?
O9 S1 O7 109.7(7) . . ?
O5 S1 O7 108.9(8) . . ?
O4 S1 O7 108.2(7) . . ?
O14 S2 O10 110.0(9) . . ?
O14 S2 O12 110.6(8) . . ?
O10 S2 O12 109.0(8) . . ?
O14 S2 O8 108.8(9) . . ?
O10 S2 O8 108.3(8) . . ?
O12 S2 O8 110.1(8) . . ?
O14 S2 Eu3 136.2(7) . . ?
O10 S2 Eu3 26.3(5) . . ?
O12 S2 Eu3 96.4(6) . . ?
O8 S2 Eu3 92.4(6) . . ?
O15 S3 O11 113.3(10) . . ?
O15 S3 O18 111.2(8) . . ?
O11 S3 O18 109.7(8) . . ?
O15 S3 O13 110.6(9) . . ?
O11 S3 O13 104.9(7) . . ?
O18 S3 O13 106.7(9) . . ?
O15 S3 Eu1 132.9(7) . . ?
O11 S3 Eu1 53.2(5) . . ?
O18 S3 Eu1 115.7(6) . . ?
O13 S3 Eu1 52.0(5) . . ?
O16 S4 O17 111.5(8) . . ?
O16 S4 O19 114.4(9) . . ?
O17 S4 O19 111.9(10) . . ?
O16 S4 O6 109.2(9) . . ?
O17 S4 O6 103.9(8) . . ?
O19 S4 O6 105.1(8) . . ?
O16 S4 Eu1 118.6(7) . . ?
O17 S4 Eu1 54.8(6) . . ?
O19 S4 Eu1 126.3(7) . . ?
O6 S4 Eu1 49.5(5) . . ?
O16 S4 Eu3 127.3(6) . 8_656 ?
O17 S4 Eu3 119.5(6) . 8_656 ?
O19 S4 Eu3 57.8(6) . 8_656 ?
O6 S4 Eu3 47.4(5) . 8_656 ?
Eu1 S4 Eu3 83.13(13) . 8_656 ?
Eu2 O1 Eu3 113.8(4) . . ?
Eu2 O1 Eu3 121.0(4) . 7_566 ?
Eu3 O1 Eu3 121.3(3) . 7_566 ?
Eu2 O2 Eu3 106.3(4) . . ?
Eu2 O2 Eu3 107.8(3) . 8_656 ?
Eu3 O2 Eu3 106.6(3) . 8_656 ?
Eu2 O2 Eu1 98.8(3) . . ?
Eu3 O2 Eu1 134.5(4) . . ?
Eu3 O2 Eu1 100.8(3) 8_656 . ?
Eu2 O3 Eu1 124.3(4) . . ?
S1 O4 Eu2 134.3(7) . . ?
S1 O5 Eu1 138.4(7) . . ?
S4 O6 Eu3 105.9(7) . 8_656 ?
S4 O6 Eu1 102.9(6) . . ?
Eu3 O6 Eu1 118.3(5) 8_656 . ?
S1 O7 Eu3 136.8(7) . . ?
S2 O8 Eu3 137.0(8) . 8_656 ?
S2 O10 Eu3 137.4(8) . . ?
S3 O11 Eu1 99.1(7) . . ?
S2 O12 Eu1 140.5(8) . . ?
S3 O13 Eu1 99.5(6) . . ?
S4 O17 Eu1 97.7(7) . . ?
S3 O18 Eu1 158.5(9) . 5_665 ?
S4 O19 Eu3 95.0(7) . 8_656 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C8 N5 67(3) 2 . ?
C8 C8 H8A 153.6 2 . ?
N5 C8 H8A 87.8 . . ?
C8 C8 H8B 75.9 2 . ?
N5 C8 H8B 116.7 . . ?
H8A C8 H8B 109.5 . . ?
C8 C8 H8C 91.9 2 . ?
N5 C8 H8C 121.3 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.3 . . ?
C2 N1 C1 108.4(18) . . ?
C2 N1 H1D 110.0 . . ?
C1 N1 H1D 110.0 . . ?
C2 N1 H1E 110.0 . . ?
C1 N1 H1E 110.0 . . ?
H1D N1 H1E 108.4 . . ?
C4 N2 C3 112(2) . . ?
C4 N2 H2D 109.2 . . ?
C3 N2 H2D 109.2 . . ?
C4 N2 H2E 109.2 . . ?
C3 N2 H2E 109.2 . . ?
H2D N2 H2E 107.9 . . ?
C6 N3 C5 120(4) . . ?
C6 N3 H3D 107.2 . . ?
C5 N3 H3D 107.2 . . ?
C6 N3 H3E 107.2 . . ?
C5 N3 H3E 107.2 . . ?
H3D N3 H3E 106.9 . . ?
C7 N4 C7 99(6) . 2_565 ?
C7 N4 H4D 111.8 . . ?
C7 N4 H4D 109.6 2_565 . ?
C8 N5 C8 45(6) 2 . ?
C8 N5 H5D 117.7 2 . ?
C8 N5 H5D 125.7 . . ?

_refine_diff_density_max         2.176
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.270

####################################################################### 
# 
# 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_zht-3-1
_database_code_depnum_ccdc_archive 'CCDC 1544845'
_audit_update_record             
;
2017-04-19 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H136 Dy10 N14 O82 S16'
_chemical_formula_weight         4119.46

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   16.0542(5)
_cell_length_b                   16.0542(5)
_cell_length_c                   22.7238(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5856.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6366
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      24.42

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_F_000             3948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    6.688
_shelx_estimated_absorpt_T_min   0.414
_shelx_estimated_absorpt_T_max   0.501
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42736
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.553
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5482
_reflns_number_gt                4059
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+47.8672P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5482
_refine_ls_number_parameters     358
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.42107(2) 0.20062(2) 0.24507(2) 0.03457(9) Uani 1 1 d . . . . .
Dy2 Dy 0.42592(2) 0.41749(2) 0.09292(2) 0.04065(10) Uani 1 1 d . . . . .
Dy3 Dy 0.2500 0.2500 0.12941(2) 0.02979(12) Uani 1 2 d S T P . .
S1 S 0.45732(12) 0.19772(12) 0.09123(8) 0.0377(5) Uani 1 1 d . . . . .
S2 S 0.51620(13) 0.39612(14) 0.23549(8) 0.0445(5) Uani 1 1 d . . . . .
S3 S 0.38593(13) 0.47908(14) -0.03164(8) 0.0472(6) Uani 1 1 d . . . . .
S4 S 0.34927(15) 0.56525(13) 0.16404(9) 0.0523(6) Uani 1 1 d . . . . .
O1 O 0.2958(3) 0.1607(3) 0.20231(16) 0.0205(10) Uani 1 1 d . . . . .
O2 O 0.3603(3) 0.3095(3) 0.18484(17) 0.0227(11) Uani 1 1 d . . . . .
O3 O 0.3032(3) 0.3518(3) 0.07680(16) 0.0232(11) Uani 1 1 d . . . . .
O4 O 0.3663(3) 0.1854(3) 0.0855(2) 0.0424(14) Uani 1 1 d . . . . .
O5 O 0.4767(3) 0.2838(3) 0.0752(2) 0.0439(14) Uani 1 1 d . . . . .
O6 O 0.3204(3) 0.4756(3) 0.1576(2) 0.0490(15) Uani 1 1 d . . . . .
O7 O 0.4798(3) 0.1847(3) 0.1535(2) 0.0454(15) Uani 1 1 d . . . . .
O8 O 0.4424(3) 0.4376(4) 0.2608(2) 0.0478(15) Uani 1 1 d . . . . .
O9 O 0.5012(3) 0.1411(4) 0.0531(2) 0.0529(16) Uani 1 1 d . . . . .
O10 O 0.5139(3) 0.3068(4) 0.2521(2) 0.0478(15) Uani 1 1 d . . . . .
O11 O 0.4250(4) 0.3988(4) -0.0159(2) 0.0548(17) Uani 1 1 d . . . . .
O12 O 0.5149(3) 0.4031(3) 0.1712(2) 0.0470(15) Uani 1 1 d . . . . .
O13 O 0.3604(3) 0.5148(3) 0.0260(2) 0.0486(15) Uani 1 1 d . . . . .
O14 O 0.5908(4) 0.4350(4) 0.2592(2) 0.0588(18) Uani 1 1 d . . . . .
O15 O 0.3153(4) 0.4694(3) -0.0701(3) 0.067(2) Uani 1 1 d D . . . .
O16 O 0.2929(4) 0.6200(4) 0.1330(3) 0.0627(19) Uani 1 1 d . . . . .
O17 O 0.4320(4) 0.5646(4) 0.1365(2) 0.0572(17) Uani 1 1 d . . . . .
O18 O 0.4475(4) 0.5353(4) -0.0581(2) 0.0605(18) Uani 1 1 d . . . . .
O19 O 0.3527(4) 0.5804(4) 0.2277(3) 0.0634(19) Uani 1 1 d . . . . .
C1 C 0.3722(8) -0.0181(7) 0.1031(4) 0.082(4) Uani 1 1 d . . . . .
H1A H 0.3460 -0.0050 0.1400 0.122 Uiso 1 1 calc R U . . .
H1B H 0.3778 -0.0774 0.0995 0.122 Uiso 1 1 calc R U . . .
H1C H 0.4263 0.0073 0.1017 0.122 Uiso 1 1 calc R U . . .
C2 C 0.3564(7) -0.0036(8) -0.0030(4) 0.092(4) Uani 1 1 d . . . . .
H2A H 0.3202 0.0187 -0.0327 0.138 Uiso 1 1 calc R U . . .
H2B H 0.4103 0.0221 -0.0061 0.138 Uiso 1 1 calc R U . . .
H2C H 0.3618 -0.0626 -0.0083 0.138 Uiso 1 1 calc R U . . .
C3 C 0.5354(9) 0.2502(8) -0.0816(5) 0.107(5) Uani 1 1 d . U . . .
H3A H 0.4872 0.2742 -0.0999 0.161 Uiso 1 1 calc R U . . .
H3B H 0.5754 0.2356 -0.1112 0.161 Uiso 1 1 calc R U . . .
H3C H 0.5194 0.2012 -0.0602 0.161 Uiso 1 1 calc R U . . .
C4 C 0.6453(8) 0.2828(8) -0.0103(6) 0.121(5) Uani 1 1 d . U . . .
H4A H 0.6650 0.3262 0.0152 0.182 Uiso 1 1 calc R U . . .
H4B H 0.6318 0.2345 0.0127 0.182 Uiso 1 1 calc R U . . .
H4C H 0.6878 0.2689 -0.0383 0.182 Uiso 1 1 calc R U . . .
C5 C 0.5704(12) 0.6404(13) 0.2415(8) 0.181(8) Uani 1 1 d . U . . .
H5A H 0.5457 0.6602 0.2056 0.271 Uiso 1 1 calc R U . . .
H5B H 0.6075 0.6820 0.2568 0.271 Uiso 1 1 calc R U . . .
H5C H 0.6010 0.5902 0.2337 0.271 Uiso 1 1 calc R U . . .
C6 C 0.5251(11) 0.5934(9) 0.3408(6) 0.130(6) Uani 1 1 d . U . . .
H6A H 0.4746 0.5859 0.3628 0.196 Uiso 1 1 calc R U . . .
H6B H 0.5537 0.5411 0.3376 0.196 Uiso 1 1 calc R U . . .
H6C H 0.5601 0.6329 0.3607 0.196 Uiso 1 1 calc R U . . .
C7 C 0.2404(14) 0.8202(9) 0.3419(7) 0.082(6) Uani 0.5 1 d D U P . .
H7A H 0.2334 0.8711 0.3203 0.123 Uiso 0.5 1 calc R U P . .
H7B H 0.1924 0.8109 0.3662 0.123 Uiso 0.5 1 calc R U P . .
H7C H 0.2891 0.8241 0.3662 0.123 Uiso 0.5 1 calc R U P . .
C8 C 0.2189(17) 0.263(2) -0.0697(7) 0.166(5) Uani 0.5 1 d D U P . .
H8A H 0.1704 0.2875 -0.0871 0.248 Uiso 0.5 1 d R U P . .
H8B H 0.2463 0.3025 -0.0449 0.248 Uiso 0.5 1 d R U P . .
H8C H 0.2025 0.2153 -0.0466 0.248 Uiso 0.5 1 d R U P . .
N1 N 0.3215(5) 0.0134(5) 0.0551(3) 0.059(2) Uani 1 1 d . . . . .
H1D H 0.3155 0.0682 0.0593 0.071 Uiso 1 1 calc R U . . .
H1E H 0.2711 -0.0095 0.0573 0.071 Uiso 1 1 calc R U . . .
N2 N 0.5724(5) 0.3109(5) -0.0408(4) 0.084(3) Uani 1 1 d . . . . .
H2D H 0.5854 0.3566 -0.0610 0.101 Uiso 1 1 calc R U . . .
H2E H 0.5341 0.3250 -0.0143 0.101 Uiso 1 1 calc R U . . .
N3 N 0.5057(9) 0.6235(8) 0.2840(5) 0.155(6) Uani 1 1 d . . . . .
H3D H 0.4771 0.6704 0.2887 0.186 Uiso 1 1 calc R U . . .
H3E H 0.4712 0.5868 0.2676 0.186 Uiso 1 1 calc R U . . .
N4 N 0.2500 0.7500 0.3002(9) 0.104(7) Uani 0.5 2 d DS TU P . .
H4D H 0.2967 0.7551 0.2786 0.125 Uiso 0.5 1 d R U P . .
O1W O 0.2834(6) 0.5507(7) -0.1739(5) 0.147(4) Uani 1 1 d . U . . .
N5 N 0.2500 0.2500 -0.1290(6) 0.168(5) Uani 0.5 2 d DS TU P . .
H5D H 0.2715 0.2909 -0.1515 0.202 Uiso 0.5 1 d R U P . .
O2W O 0.1611(13) 0.7110(11) 0.2040(8) 0.120(6) Uani 0.5 1 d . U P . .


_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 O10 2.270(6) . ?
Dy1 O7 2.299(5) . ?
Dy1 O8 2.316(5) 7_566 ?
Dy1 O1 2.323(4) . ?
Dy1 O1 2.343(4) 8_656 ?
Dy1 O6 2.402(5) 7_566 ?
Dy1 O2 2.425(4) . ?
Dy1 O2 2.589(4) 7_566 ?
Dy1 O19 2.767(6) 7_566 ?
Dy1 S4 3.204(2) 7_566 ?
Dy1 Dy3 3.8830(4) . ?
Dy2 O3 2.265(4) . ?
Dy2 O12 2.294(5) . ?
Dy2 O18 2.309(6) 5_665 ?
Dy2 O5 2.331(5) . ?
Dy2 O13 2.421(5) . ?
Dy2 O6 2.430(5) . ?
Dy2 O11 2.491(5) . ?
Dy2 O17 2.563(6) . ?
Dy2 S3 3.0661(19) . ?
Dy2 S4 3.123(2) . ?
Dy2 Dy3 3.9868(4) . ?
Dy3 O3 2.197(4) . ?
Dy3 O3 2.197(4) 2 ?
Dy3 O1 2.310(4) . ?
Dy3 O1 2.310(4) 2 ?
Dy3 O4 2.357(5) . ?
Dy3 O4 2.357(5) 2 ?
Dy3 O2 2.373(4) 2 ?
Dy3 O2 2.373(4) . ?
Dy3 Dy1 3.8831(4) 2 ?
Dy3 Dy2 3.9868(4) 2 ?
S1 O9 1.439(6) . ?
S1 O5 1.462(6) . ?
S1 O7 1.476(5) . ?
S1 O4 1.481(6) . ?
S2 O14 1.454(6) . ?
S2 O12 1.464(5) . ?
S2 O8 1.475(6) . ?
S2 O10 1.483(6) . ?
S3 O15 1.439(6) . ?
S3 O18 1.467(6) . ?
S3 O11 1.477(6) . ?
S3 O13 1.487(5) . ?
S4 O16 1.446(6) . ?
S4 O17 1.468(6) . ?
S4 O19 1.468(6) . ?
S4 O6 1.518(6) . ?
S4 Dy1 3.204(2) 8_656 ?
O1 Dy1 2.343(4) 7_566 ?
O2 Dy1 2.589(4) 8_656 ?
O6 Dy1 2.402(5) 8_656 ?
O8 Dy1 2.316(5) 8_656 ?
O18 Dy2 2.309(6) 5_665 ?
O19 Dy1 2.767(6) 8_656 ?
C1 N1 1.453(12) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.459(12) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N2 1.470(15) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N2 1.433(14) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N3 1.44(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.412(18) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N4 1.479(15) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C8 1.08(5) 2 ?
C8 N5 1.451(16) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N4 C7 1.479(15) 2_565 ?
N4 H4D 0.9000 . ?
N5 C8 1.451(16) 2 ?
N5 H5D 0.9001 . ?

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
O10 Dy1 O7 83.01(19) . . ?
O10 Dy1 O8 132.4(2) . 7_566 ?
O7 Dy1 O8 77.92(19) . 7_566 ?
O10 Dy1 O1 143.59(17) . . ?
O7 Dy1 O1 86.90(16) . . ?
O8 Dy1 O1 78.57(17) 7_566 . ?
O10 Dy1 O1 80.91(17) . 8_656 ?
O7 Dy1 O1 139.86(16) . 8_656 ?
O8 Dy1 O1 137.76(17) 7_566 8_656 ?
O1 Dy1 O1 84.7(2) . 8_656 ?
O10 Dy1 O6 78.51(18) . 7_566 ?
O7 Dy1 O6 131.90(19) . 7_566 ?
O8 Dy1 O6 82.64(18) 7_566 7_566 ?
O1 Dy1 O6 131.45(16) . 7_566 ?
O1 Dy1 O6 79.99(16) 8_656 7_566 ?
O10 Dy1 O2 76.28(17) . . ?
O7 Dy1 O2 74.60(16) . . ?
O8 Dy1 O2 136.76(16) 7_566 . ?
O1 Dy1 O2 67.31(14) . . ?
O1 Dy1 O2 65.94(13) 8_656 . ?
O6 Dy1 O2 140.13(16) 7_566 . ?
O10 Dy1 O2 133.97(16) . 7_566 ?
O7 Dy1 O2 143.02(16) . 7_566 ?
O8 Dy1 O2 74.94(16) 7_566 7_566 ?
O1 Dy1 O2 63.54(13) . 7_566 ?
O1 Dy1 O2 62.90(13) 8_656 7_566 ?
O6 Dy1 O2 68.47(16) 7_566 7_566 ?
O2 Dy1 O2 109.93(18) . 7_566 ?
O10 Dy1 O19 67.0(2) . 7_566 ?
O7 Dy1 O19 77.80(18) . 7_566 ?
O8 Dy1 O19 66.5(2) 7_566 7_566 ?
O1 Dy1 O19 143.94(17) . 7_566 ?
O1 Dy1 O19 127.27(16) 8_656 7_566 ?
O6 Dy1 O19 54.10(18) 7_566 7_566 ?
O2 Dy1 O19 136.14(16) . 7_566 ?
O2 Dy1 O19 112.67(15) 7_566 7_566 ?
O10 Dy1 S4 70.60(14) . 7_566 ?
O7 Dy1 S4 105.02(13) . 7_566 ?
O8 Dy1 S4 72.93(14) 7_566 7_566 ?
O1 Dy1 S4 145.70(11) . 7_566 ?
O1 Dy1 S4 103.83(10) 8_656 7_566 ?
O6 Dy1 S4 26.88(14) 7_566 7_566 ?
O2 Dy1 S4 146.59(11) . 7_566 ?
O2 Dy1 S4 90.51(10) 7_566 7_566 ?
O19 Dy1 S4 27.22(13) 7_566 7_566 ?
O10 Dy1 Dy3 111.03(13) . . ?
O7 Dy1 Dy3 72.56(13) . . ?
O8 Dy1 Dy3 104.16(13) 7_566 . ?
O1 Dy1 Dy3 32.97(10) . . ?
O1 Dy1 Dy3 79.39(9) 8_656 . ?
O6 Dy1 Dy3 155.45(13) 7_566 . ?
O2 Dy1 Dy3 35.53(10) . . ?
O2 Dy1 Dy3 90.24(9) 7_566 . ?
O19 Dy1 Dy3 150.25(12) 7_566 . ?
S4 Dy1 Dy3 176.68(5) 7_566 . ?
O3 Dy2 O12 128.33(16) . . ?
O3 Dy2 O18 149.66(17) . 5_665 ?
O12 Dy2 O18 75.59(19) . 5_665 ?
O3 Dy2 O5 81.20(17) . . ?
O12 Dy2 O5 79.81(19) . . ?
O18 Dy2 O5 86.3(2) 5_665 . ?
O3 Dy2 O13 79.69(17) . . ?
O12 Dy2 O13 145.41(19) . . ?
O18 Dy2 O13 87.43(19) 5_665 . ?
O5 Dy2 O13 129.62(17) . . ?
O3 Dy2 O6 70.75(17) . . ?
O12 Dy2 O6 90.21(18) . . ?
O18 Dy2 O6 134.0(2) 5_665 . ?
O5 Dy2 O6 134.58(18) . . ?
O13 Dy2 O6 80.17(17) . . ?
O3 Dy2 O11 77.17(16) . . ?
O12 Dy2 O11 139.61(18) . . ?
O18 Dy2 O11 72.80(19) 5_665 . ?
O5 Dy2 O11 73.73(18) . . ?
O13 Dy2 O11 56.74(18) . . ?
O6 Dy2 O11 130.00(18) . . ?
O3 Dy2 O17 121.68(17) . . ?
O12 Dy2 O17 76.66(19) . . ?
O18 Dy2 O17 78.3(2) 5_665 . ?
O5 Dy2 O17 154.41(19) . . ?
O13 Dy2 O17 70.43(18) . . ?
O6 Dy2 O17 55.85(18) . . ?
O11 Dy2 O17 119.68(18) . . ?
O3 Dy2 S3 79.56(10) . . ?
O12 Dy2 S3 151.54(14) . . ?
O18 Dy2 S3 76.22(14) 5_665 . ?
O5 Dy2 S3 102.17(12) . . ?
O13 Dy2 S3 28.47(13) . . ?
O6 Dy2 S3 106.78(13) . . ?
O11 Dy2 S3 28.51(14) . . ?
O17 Dy2 S3 93.89(13) . . ?
O3 Dy2 S4 95.44(11) . . ?
O12 Dy2 S4 85.45(14) . . ?
O18 Dy2 S4 105.97(17) 5_665 . ?
O5 Dy2 S4 157.90(12) . . ?
O13 Dy2 S4 70.35(13) . . ?
O6 Dy2 S4 28.39(14) . . ?
O11 Dy2 S4 127.08(14) . . ?
O17 Dy2 S4 27.76(14) . . ?
S3 Dy2 S4 98.65(6) . . ?
O3 Dy2 Dy3 26.25(10) . . ?
O12 Dy2 Dy3 102.23(13) . . ?
O18 Dy2 Dy3 156.37(16) 5_665 . ?
O5 Dy2 Dy3 70.27(13) . . ?
O13 Dy2 Dy3 104.96(13) . . ?
O6 Dy2 Dy3 68.86(13) . . ?
O11 Dy2 Dy3 96.94(14) . . ?
O17 Dy2 Dy3 124.62(13) . . ?
S3 Dy2 Dy3 105.14(4) . . ?
S4 Dy2 Dy3 97.21(4) . . ?
O3 Dy3 O3 114.1(2) . 2 ?
O3 Dy3 O1 136.68(15) . . ?
O3 Dy3 O1 93.02(14) 2 . ?
O3 Dy3 O1 93.02(14) . 2 ?
O3 Dy3 O1 136.68(15) 2 2 ?
O1 Dy3 O1 88.40(19) . 2 ?
O3 Dy3 O4 77.83(17) . . ?
O3 Dy3 O4 75.52(17) 2 . ?
O1 Dy3 O4 77.20(15) . . ?
O1 Dy3 O4 145.97(16) 2 . ?
O3 Dy3 O4 75.52(17) . 2 ?
O3 Dy3 O4 77.83(17) 2 2 ?
O1 Dy3 O4 145.97(16) . 2 ?
O1 Dy3 O4 77.20(15) 2 2 ?
O4 Dy3 O4 129.9(2) . 2 ?
O3 Dy3 O2 151.39(15) . 2 ?
O3 Dy3 O2 72.52(14) 2 2 ?
O1 Dy3 O2 66.89(14) . 2 ?
O1 Dy3 O2 68.39(14) 2 2 ?
O4 Dy3 O2 129.65(16) . 2 ?
O4 Dy3 O2 79.13(16) 2 2 ?
O3 Dy3 O2 72.52(14) . . ?
O3 Dy3 O2 151.39(15) 2 . ?
O1 Dy3 O2 68.39(14) . . ?
O1 Dy3 O2 66.89(14) 2 . ?
O4 Dy3 O2 79.13(16) . . ?
O4 Dy3 O2 129.65(16) 2 . ?
O2 Dy3 O2 115.90(19) 2 . ?
O3 Dy3 Dy1 104.19(11) . . ?
O3 Dy3 Dy1 119.43(11) 2 . ?
O1 Dy3 Dy1 33.17(10) . . ?
O1 Dy3 Dy1 82.33(10) 2 . ?
O4 Dy3 Dy1 68.70(12) . . ?
O4 Dy3 Dy1 159.47(12) 2 . ?
O2 Dy3 Dy1 94.95(10) 2 . ?
O2 Dy3 Dy1 36.43(10) . . ?
O3 Dy3 Dy1 119.43(11) . 2 ?
O3 Dy3 Dy1 104.20(11) 2 2 ?
O1 Dy3 Dy1 82.33(10) . 2 ?
O1 Dy3 Dy1 33.17(10) 2 2 ?
O4 Dy3 Dy1 159.47(12) . 2 ?
O4 Dy3 Dy1 68.70(12) 2 2 ?
O2 Dy3 Dy1 36.43(10) 2 2 ?
O2 Dy3 Dy1 94.95(10) . 2 ?
Dy1 Dy3 Dy1 94.808(14) . 2 ?
O3 Dy3 Dy2 27.13(11) . . ?
O3 Dy3 Dy2 131.57(11) 2 . ?
O1 Dy3 Dy2 109.99(10) . . ?
O1 Dy3 Dy2 87.50(10) 2 . ?
O4 Dy3 Dy2 69.39(13) . . ?
O4 Dy3 Dy2 100.13(13) 2 . ?
O2 Dy3 Dy2 155.54(10) 2 . ?
O2 Dy3 Dy2 46.41(9) . . ?
Dy1 Dy3 Dy2 77.141(8) . . ?
Dy1 Dy3 Dy2 120.272(9) 2 . ?
O3 Dy3 Dy2 131.58(11) . 2 ?
O3 Dy3 Dy2 27.13(11) 2 2 ?
O1 Dy3 Dy2 87.50(10) . 2 ?
O1 Dy3 Dy2 109.99(10) 2 2 ?
O4 Dy3 Dy2 100.13(13) . 2 ?
O4 Dy3 Dy2 69.39(13) 2 2 ?
O2 Dy3 Dy2 46.41(9) 2 2 ?
O2 Dy3 Dy2 155.54(10) . 2 ?
Dy1 Dy3 Dy2 120.271(9) . 2 ?
Dy1 Dy3 Dy2 77.140(8) 2 2 ?
Dy2 Dy3 Dy2 155.991(15) . 2 ?
O9 S1 O5 110.0(3) . . ?
O9 S1 O7 111.6(3) . . ?
O5 S1 O7 108.7(3) . . ?
O9 S1 O4 110.2(3) . . ?
O5 S1 O4 108.3(3) . . ?
O7 S1 O4 107.9(3) . . ?
O14 S2 O12 110.3(3) . . ?
O14 S2 O8 108.9(4) . . ?
O12 S2 O8 110.1(3) . . ?
O14 S2 O10 109.9(4) . . ?
O12 S2 O10 109.1(3) . . ?
O8 S2 O10 108.5(3) . . ?
O15 S3 O18 110.4(3) . . ?
O15 S3 O11 112.7(4) . . ?
O18 S3 O11 110.5(3) . . ?
O15 S3 O13 111.0(3) . . ?
O18 S3 O13 108.0(3) . . ?
O11 S3 O13 103.9(3) . . ?
O15 S3 Dy2 133.6(3) . . ?
O18 S3 Dy2 115.8(2) . . ?
O11 S3 Dy2 53.6(2) . . ?
O13 S3 Dy2 50.9(2) . . ?
O16 S4 O17 111.3(4) . . ?
O16 S4 O19 113.7(4) . . ?
O17 S4 O19 112.8(4) . . ?
O16 S4 O6 109.8(4) . . ?
O17 S4 O6 103.2(3) . . ?
O19 S4 O6 105.2(3) . . ?
O16 S4 Dy2 117.2(3) . . ?
O17 S4 Dy2 54.4(2) . . ?
O19 S4 Dy2 128.4(3) . . ?
O6 S4 Dy2 49.5(2) . . ?
O16 S4 Dy1 126.7(3) . 8_656 ?
O17 S4 Dy1 119.7(2) . 8_656 ?
O19 S4 Dy1 59.6(3) . 8_656 ?
O6 S4 Dy1 45.66(19) . 8_656 ?
Dy2 S4 Dy1 83.30(5) . 8_656 ?
Dy3 O1 Dy1 113.86(17) . . ?
Dy3 O1 Dy1 120.38(18) . 7_566 ?
Dy1 O1 Dy1 120.37(15) . 7_566 ?
Dy3 O2 Dy1 108.04(16) . . ?
Dy3 O2 Dy1 108.86(15) . 8_656 ?
Dy1 O2 Dy1 107.66(14) . 8_656 ?
Dy3 O3 Dy2 126.62(18) . . ?
S1 O4 Dy3 133.2(3) . . ?
S1 O5 Dy2 138.9(3) . . ?
S4 O6 Dy1 107.5(3) . 8_656 ?
S4 O6 Dy2 102.1(3) . . ?
Dy1 O6 Dy2 121.0(2) 8_656 . ?
S1 O7 Dy1 138.8(3) . . ?
S2 O8 Dy1 136.2(3) . 8_656 ?
S2 O10 Dy1 136.4(3) . . ?
S3 O11 Dy2 97.9(3) . . ?
S2 O12 Dy2 142.2(3) . . ?
S3 O13 Dy2 100.6(3) . . ?
S4 O17 Dy2 97.9(3) . . ?
S3 O18 Dy2 159.3(4) . 5_665 ?
S4 O19 Dy1 93.2(3) . 8_656 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C8 N5 68.2(11) 2 . ?
C8 C8 H8A 155.2 2 . ?
N5 C8 H8A 87.4 . . ?
C8 C8 H8B 79.9 2 . ?
N5 C8 H8B 118.6 . . ?
H8A C8 H8B 109.5 . . ?
C8 C8 H8C 87.7 2 . ?
N5 C8 H8C 119.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 N1 C2 113.5(8) . . ?
C1 N1 H1D 108.9 . . ?
C2 N1 H1D 108.9 . . ?
C1 N1 H1E 108.9 . . ?
C2 N1 H1E 108.9 . . ?
H1D N1 H1E 107.7 . . ?
C4 N2 C3 115.2(10) . . ?
C4 N2 H2D 108.5 . . ?
C3 N2 H2D 108.5 . . ?
C4 N2 H2E 108.5 . . ?
C3 N2 H2E 108.5 . . ?
H2D N2 H2E 107.5 . . ?
C6 N3 C5 121.2(15) . . ?
C6 N3 H3D 107.0 . . ?
C5 N3 H3D 107.0 . . ?
C6 N3 H3E 107.0 . . ?
C5 N3 H3E 107.0 . . ?
H3D N3 H3E 106.8 . . ?
C7 N4 C7 100.5(18) 2_565 . ?
C7 N4 H4D 109.4 2_565 . ?
C7 N4 H4D 111.5 . . ?
C8 N5 C8 44(2) . 2 ?
C8 N5 H5D 123.9 . . ?
C8 N5 H5D 119.7 2 . ?

_refine_diff_density_max         1.823
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.205

