# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Audit and citation data items may have been added by the CCDC. 
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data_Ho2benzoicNO3
_database_code_depnum_ccdc_archive 'CCDC 1477857'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2016-02-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H34 Ho2 N6 O14'
_chemical_formula_sum            'C52 H34 Ho2 N6 O14'
_chemical_formula_weight         1296.71
_chemical_melting_point          ?
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'
Ho Ho -0.2175 4.6783 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6380(3)
_cell_length_b                   11.0224(4)
_cell_length_c                   11.0417(4)
_cell_angle_alpha                85.008(2)
_cell_angle_beta                 68.905(2)
_cell_angle_gamma                81.393(2)
_cell_volume                     1193.57(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    17680
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.7256
_exptl_absorpt_correction_T_max  0.8625
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.063
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.028
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            4890
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         2.961
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  template
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3397
_reflns_number_total             4890
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_refine_diff_density_max         3.057
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.0148(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1272
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C22(H22), C23(H23),
  C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.2034(7) 1.1120(7) -0.1773(7) 0.0368(17) Uani 1 1 d . . . . .
C2 C 0.3125(7) 1.1661(7) -0.2888(7) 0.0424(18) Uani 1 1 d . . . . .
C3 C 0.2913(8) 1.2870(8) -0.3319(8) 0.051(2) Uani 1 1 d . . . . .
H3 H 0.2086 1.3343 -0.2918 0.062 Uiso 1 1 calc R . . . .
C4 C 0.3915(10) 1.3384(10) -0.4341(9) 0.069(3) Uani 1 1 d . . . . .
H4 H 0.3751 1.4187 -0.4636 0.083 Uiso 1 1 calc R . . . .
C5 C 0.5143(10) 1.2698(10) -0.4908(10) 0.072(3) Uani 1 1 d . . . . .
H5 H 0.5826 1.3043 -0.5577 0.087 Uiso 1 1 calc R . . . .
C6 C 0.5373(10) 1.1513(11) -0.4501(11) 0.089(4) Uani 1 1 d . . . . .
H6 H 0.6207 1.1051 -0.4902 0.107 Uiso 1 1 calc R . . . .
C7 C 0.4383(9) 1.0990(9) -0.3499(9) 0.068(3) Uani 1 1 d . . . . .
H7 H 0.4557 1.0180 -0.3230 0.081 Uiso 1 1 calc R . . . .
C8 C 0.0691(7) 1.0231(7) 0.2003(7) 0.0350(16) Uani 1 1 d . . . . .
C9 C 0.0460(8) 1.0914(7) 0.3181(8) 0.0453(19) Uani 1 1 d . . . . .
C10 C 0.1483(9) 1.0752(9) 0.3704(9) 0.060(2) Uani 1 1 d . . . . .
H10 H 0.2267 1.0214 0.3329 0.072 Uiso 1 1 calc R . . . .
C11 C 0.1341(13) 1.1389(11) 0.4783(10) 0.081(3) Uani 1 1 d . . . . .
H11 H 0.2025 1.1266 0.5136 0.097 Uiso 1 1 calc R . . . .
C12 C 0.0204(15) 1.2196(11) 0.5332(11) 0.087(4) Uani 1 1 d . . . . .
H12 H 0.0137 1.2661 0.6021 0.105 Uiso 1 1 calc R . . . .
C13 C -0.0853(13) 1.2315(10) 0.4853(11) 0.084(3) Uani 1 1 d . . . . .
H13 H -0.1656 1.2818 0.5261 0.101 Uiso 1 1 calc R . . . .
C14 C -0.0708(10) 1.1675(8) 0.3747(9) 0.062(2) Uani 1 1 d . . . . .
H14 H -0.1402 1.1771 0.3409 0.074 Uiso 1 1 calc R . . . .
C15 C 0.4709(8) 0.8737(9) -0.0718(9) 0.057(2) Uani 1 1 d . . . . .
H15 H 0.4509 0.9411 -0.1216 0.068 Uiso 1 1 calc R . . . .
C16 C 0.6025(8) 0.8511(9) -0.0644(9) 0.060(2) Uani 1 1 d . . . . .
H16 H 0.6662 0.9045 -0.1059 0.073 Uiso 1 1 calc R . . . .
C17 C 0.6341(8) 0.7524(10) 0.0029(10) 0.064(3) Uani 1 1 d . . . . .
H17 H 0.7215 0.7355 0.0052 0.076 Uiso 1 1 calc R . . . .
C18 C 0.5374(8) 0.6732(8) 0.0703(8) 0.048(2) Uani 1 1 d . . . . .
C19 C 0.5661(10) 0.5677(10) 0.1440(10) 0.063(3) Uani 1 1 d . . . . .
C20 C 0.4681(11) 0.4967(10) 0.2066(10) 0.076(3) Uani 1 1 d . . . . .
H20 H 0.4883 0.4286 0.2554 0.091 Uiso 1 1 calc R . . . .
C21 C 0.3342(9) 0.5212(8) 0.2016(8) 0.053(2) Uani 1 1 d . . . . .
C22 C 0.2327(10) 0.4457(9) 0.2595(10) 0.069(3) Uani 1 1 d . . . . .
H22 H 0.2485 0.3770 0.3098 0.083 Uiso 1 1 calc R . . . .
C23 C 0.1103(10) 0.4720(8) 0.2429(9) 0.062(2) Uani 1 1 d . . . . .
H23 H 0.0427 0.4216 0.2811 0.075 Uiso 1 1 calc R . . . .
C24 C 0.0881(9) 0.5758(7) 0.1678(8) 0.050(2) Uani 1 1 d . . . . .
H24 H 0.0049 0.5922 0.1559 0.060 Uiso 1 1 calc R . . . .
C25 C 0.3053(7) 0.6238(7) 0.1263(8) 0.0428(19) Uani 1 1 d . . . . .
C26 C 0.4066(7) 0.7016(7) 0.0612(8) 0.046(2) Uani 1 1 d . . . . .
Ho1 Ho 0.12786(3) 0.85087(3) -0.00542(4) 0.03893(19) Uani 1 1 d . . . . .
N1 N 0.3756(6) 0.8035(6) -0.0113(6) 0.0419(15) Uani 1 1 d . . . . .
N2 N 0.1803(6) 0.6526(5) 0.1122(6) 0.0419(15) Uani 1 1 d . . . . .
N3 N 0.1679(8) 0.6564(6) -0.1784(7) 0.0503(18) Uani 1 1 d . . . . .
O1 O 0.2365(5) 1.0091(5) -0.1320(5) 0.0447(13) Uani 1 1 d . . . . .
O2 O 0.0870(5) 1.1738(5) -0.1389(5) 0.0430(13) Uani 1 1 d . . . . .
O3 O 0.1505(5) 0.9261(5) 0.1774(5) 0.0496(14) Uani 1 1 d . . . . .
O4 O -0.0023(5) 0.9417(5) -0.1267(5) 0.0505(14) Uani 1 1 d . . . . .
O5 O 0.0562(6) 0.6754(5) -0.0866(6) 0.0518(14) Uani 1 1 d . . . . .
O6 O 0.2569(6) 0.7257(6) -0.1878(6) 0.0546(15) Uani 1 1 d . . . . .
O7 O 0.1934(7) 0.5722(6) -0.2533(7) 0.0712(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.506(10) . ?
C1 O1 1.253(8) . ?
C1 O2 1.264(8) . ?
C2 C3 1.389(11) . ?
C2 C7 1.391(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.391(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.367(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.360(14) . ?
C6 H6 0.9300 . ?
C6 C7 1.377(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.484(11) . ?
C8 Ho1 2.920(7) . ?
C8 O3 1.253(9) . ?
C8 O4 1.264(8) 2_575 ?
C9 C10 1.388(11) . ?
C9 C14 1.363(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.385(13) . ?
C11 H11 0.9300 . ?
C11 C12 1.366(16) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(16) . ?
C13 H13 0.9300 . ?
C13 C14 1.412(14) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.416(11) . ?
C15 N1 1.315(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.333(13) . ?
C17 H17 0.9300 . ?
C17 C18 1.406(12) . ?
C18 C19 1.420(12) . ?
C18 C26 1.417(10) . ?
C19 C20 1.345(14) . ?
C20 H20 0.9300 . ?
C20 C21 1.430(12) . ?
C21 C22 1.395(12) . ?
C21 C25 1.408(11) . ?
C22 H22 0.9300 . ?
C22 C23 1.365(13) . ?
C23 H23 0.9300 . ?
C23 C24 1.395(11) . ?
C24 H24 0.9300 . ?
C24 N2 1.334(10) . ?
C25 C26 1.423(11) . ?
C25 N2 1.381(9) . ?
C26 N1 1.391(9) . ?
Ho1 Ho1 3.9217(7) 2_575 ?
Ho1 N1 2.587(6) . ?
Ho1 N2 2.537(6) . ?
Ho1 N3 2.877(7) . ?
Ho1 O1 2.312(5) . ?
Ho1 O2 2.308(5) 2_575 ?
Ho1 O3 2.349(5) . ?
Ho1 O4 2.323(5) . ?
Ho1 O4 2.721(6) 2_575 ?
Ho1 O5 2.522(6) . ?
Ho1 O6 2.402(6) . ?
N3 O5 1.257(9) . ?
N3 O6 1.273(9) . ?
N3 O7 1.231(9) . ?
O2 Ho1 2.308(5) 2_575 ?
O4 C8 1.264(8) 2_575 ?
O4 Ho1 2.721(6) 2_575 ?

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
O1 C1 C2 116.8(6) . . ?
O1 C1 O2 126.1(7) . . ?
O2 C1 C2 117.2(6) . . ?
C3 C2 C1 120.6(7) . . ?
C3 C2 C7 117.6(7) . . ?
C7 C2 C1 121.8(7) . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.2(8) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(9) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(9) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.7(10) . . ?
C7 C6 H6 119.6 . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.7(9) . . ?
C6 C7 H7 119.7 . . ?
C9 C8 Ho1 169.8(5) . . ?
O3 C8 C9 119.7(6) . . ?
O3 C8 Ho1 51.2(4) . . ?
O3 C8 O4 119.6(7) . 2_575 ?
O4 C8 C9 120.6(7) 2_575 . ?
O4 C8 Ho1 68.4(4) 2_575 . ?
C10 C9 C8 117.6(8) . . ?
C14 C9 C8 122.2(8) . . ?
C14 C9 C10 120.2(8) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.3(10) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.5(11) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 120.3 . . ?
C11 C12 C13 119.4(11) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.1(10) . . ?
C14 C13 H13 120.0 . . ?
C9 C14 C13 119.4(9) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 H15 118.6 . . ?
N1 C15 H15 118.6 . . ?
N1 C15 C16 122.8(8) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.3(8) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.5 . . ?
C16 C17 C18 121.1(7) . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C19 123.0(7) . . ?
C17 C18 C26 117.2(8) . . ?
C26 C18 C19 119.8(8) . . ?
C20 C19 C18 119.7(8) . . ?
C19 C20 H20 118.5 . . ?
C19 C20 C21 123.0(9) . . ?
C21 C20 H20 118.5 . . ?
C22 C21 C20 124.3(8) . . ?
C22 C21 C25 117.6(8) . . ?
C25 C21 C20 118.0(8) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.4(8) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 120.5 . . ?
C22 C23 C24 119.0(9) . . ?
C24 C23 H23 120.5 . . ?
C23 C24 H24 118.4 . . ?
N2 C24 C23 123.3(8) . . ?
N2 C24 H24 118.4 . . ?
C21 C25 C26 120.0(7) . . ?
N2 C25 C21 122.2(7) . . ?
N2 C25 C26 117.8(7) . . ?
C18 C26 C25 119.5(7) . . ?
N1 C26 C18 121.2(7) . . ?
N1 C26 C25 119.2(6) . . ?
C8 Ho1 Ho1 61.01(14) . 2_575 ?
N1 Ho1 C8 89.5(2) . . ?
N1 Ho1 Ho1 135.46(13) . 2_575 ?
N1 Ho1 N3 91.8(2) . . ?
N1 Ho1 O4 110.53(18) . 2_575 ?
N2 Ho1 C8 99.6(2) . . ?
N2 Ho1 Ho1 146.35(14) . 2_575 ?
N2 Ho1 N1 64.82(19) . . ?
N2 Ho1 N3 73.6(2) . . ?
N2 Ho1 O4 121.17(18) . 2_575 ?
N3 Ho1 C8 171.7(2) . . ?
N3 Ho1 Ho1 122.32(12) . 2_575 ?
O1 Ho1 C8 81.9(2) . . ?
O1 Ho1 Ho1 68.54(13) . 2_575 ?
O1 Ho1 N1 75.23(18) . . ?
O1 Ho1 N2 139.97(19) . . ?
O1 Ho1 N3 106.3(2) . . ?
O1 Ho1 O3 89.66(19) . . ?
O1 Ho1 O4 74.57(18) . 2_575 ?
O1 Ho1 O4 72.19(18) . . ?
O1 Ho1 O5 125.96(19) . . ?
O1 Ho1 O6 85.4(2) . . ?
O2 Ho1 C8 73.73(19) 2_575 . ?
O2 Ho1 Ho1 68.65(12) 2_575 2_575 ?
O2 Ho1 N1 137.77(18) 2_575 . ?
O2 Ho1 N2 79.86(18) 2_575 . ?
O2 Ho1 N3 100.0(2) 2_575 . ?
O2 Ho1 O1 136.94(18) 2_575 . ?
O2 Ho1 O3 82.67(18) 2_575 . ?
O2 Ho1 O4 68.08(17) 2_575 2_575 ?
O2 Ho1 O4 79.78(18) 2_575 . ?
O2 Ho1 O5 74.17(18) 2_575 . ?
O2 Ho1 O6 125.94(19) 2_575 . ?
O3 Ho1 C8 24.58(18) . . ?
O3 Ho1 Ho1 85.56(13) . 2_575 ?
O3 Ho1 N1 68.9(2) . . ?
O3 Ho1 N2 78.8(2) . . ?
O3 Ho1 N3 151.21(19) . . ?
O3 Ho1 O4 50.15(17) . 2_575 ?
O3 Ho1 O5 144.04(19) . . ?
O3 Ho1 O6 139.99(19) . . ?
O4 Ho1 C8 25.57(17) 2_575 . ?
O4 Ho1 C8 103.8(2) . . ?
O4 Ho1 Ho1 35.44(11) 2_575 2_575 ?
O4 Ho1 Ho1 42.78(15) . 2_575 ?
O4 Ho1 N1 142.42(19) . . ?
O4 Ho1 N2 143.0(2) . . ?
O4 Ho1 N3 80.01(19) . . ?
O4 Ho1 N3 156.73(17) 2_575 . ?
O4 Ho1 O3 128.3(2) . . ?
O4 Ho1 O4 78.2(2) . 2_575 ?
O4 Ho1 O5 74.48(19) . . ?
O4 Ho1 O6 87.6(2) . . ?
O5 Ho1 C8 147.61(19) . . ?
O5 Ho1 Ho1 110.17(13) . 2_575 ?
O5 Ho1 N1 111.83(19) . . ?
O5 Ho1 N2 70.44(19) . . ?
O5 Ho1 N3 25.87(18) . . ?
O5 Ho1 O4 136.50(17) . 2_575 ?
O6 Ho1 C8 159.31(19) . . ?
O6 Ho1 Ho1 128.26(14) . 2_575 ?
O6 Ho1 N1 71.5(2) . . ?
O6 Ho1 N2 79.9(2) . . ?
O6 Ho1 N3 25.97(19) . . ?
O6 Ho1 O4 158.16(19) . 2_575 ?
O6 Ho1 O5 51.84(19) . . ?
C15 N1 C26 118.4(6) . . ?
C15 N1 Ho1 124.0(5) . . ?
C26 N1 Ho1 117.4(5) . . ?
C24 N2 C25 117.5(7) . . ?
C24 N2 Ho1 122.2(5) . . ?
C25 N2 Ho1 120.2(5) . . ?
O5 N3 Ho1 61.1(4) . . ?
O5 N3 O6 116.8(7) . . ?
O6 N3 Ho1 55.7(4) . . ?
O7 N3 Ho1 176.1(6) . . ?
O7 N3 O5 122.2(7) . . ?
O7 N3 O6 120.9(8) . . ?
C1 O1 Ho1 137.3(5) . . ?
C1 O2 Ho1 137.9(5) . 2_575 ?
C8 O3 Ho1 104.2(4) . . ?
C8 O4 Ho1 172.0(5) 2_575 . ?
C8 O4 Ho1 86.1(5) 2_575 2_575 ?
Ho1 O4 Ho1 101.8(2) . 2_575 ?
N3 O5 Ho1 93.1(4) . . ?
N3 O6 Ho1 98.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 179.5(8) . . . . ?
C1 C2 C7 C6 -178.7(10) . . . . ?
C2 C1 O1 Ho1 -161.6(5) . . . . ?
C2 C1 O2 Ho1 173.1(5) . . . 2_575 ?
C2 C3 C4 C5 -1.8(15) . . . . ?
C3 C2 C7 C6 -0.3(15) . . . . ?
C3 C4 C5 C6 1.7(17) . . . . ?
C4 C5 C6 C7 -1.0(19) . . . . ?
C5 C6 C7 C2 0.3(19) . . . . ?
C7 C2 C3 C4 1.1(13) . . . . ?
C8 C9 C10 C11 178.3(8) . . . . ?
C8 C9 C14 C13 -178.8(8) . . . . ?
C9 C8 O3 Ho1 174.4(5) . . . . ?
C9 C10 C11 C12 -1.0(16) . . . . ?
C10 C9 C14 C13 1.4(13) . . . . ?
C10 C11 C12 C13 4.2(17) . . . . ?
C11 C12 C13 C14 -4.6(17) . . . . ?
C12 C13 C14 C9 1.9(15) . . . . ?
C14 C9 C10 C11 -1.8(14) . . . . ?
C15 C16 C17 C18 -2.4(14) . . . . ?
C16 C15 N1 C26 -1.1(13) . . . . ?
C16 C15 N1 Ho1 174.5(7) . . . . ?
C16 C17 C18 C19 -179.4(9) . . . . ?
C16 C17 C18 C26 1.3(13) . . . . ?
C17 C18 C19 C20 179.6(9) . . . . ?
C17 C18 C26 C25 179.3(8) . . . . ?
C17 C18 C26 N1 -0.1(12) . . . . ?
C18 C19 C20 C21 0.9(16) . . . . ?
C18 C26 N1 C15 0.0(12) . . . . ?
C18 C26 N1 Ho1 -176.0(6) . . . . ?
C19 C18 C26 C25 0.0(12) . . . . ?
C19 C18 C26 N1 -179.3(8) . . . . ?
C19 C20 C21 C22 176.4(10) . . . . ?
C19 C20 C21 C25 0.6(15) . . . . ?
C20 C21 C22 C23 -175.8(10) . . . . ?
C20 C21 C25 C26 -1.8(12) . . . . ?
C20 C21 C25 N2 177.9(8) . . . . ?
C21 C22 C23 C24 -0.3(15) . . . . ?
C21 C25 C26 C18 1.5(12) . . . . ?
C21 C25 C26 N1 -179.2(7) . . . . ?
C21 C25 N2 C24 -3.1(12) . . . . ?
C21 C25 N2 Ho1 173.6(6) . . . . ?
C22 C21 C25 C26 -177.8(8) . . . . ?
C22 C21 C25 N2 1.9(13) . . . . ?
C22 C23 C24 N2 -1.0(14) . . . . ?
C23 C24 N2 C25 2.7(12) . . . . ?
C23 C24 N2 Ho1 -174.0(6) . . . . ?
C25 C21 C22 C23 -0.1(15) . . . . ?
C25 C26 N1 C15 -179.4(8) . . . . ?
C25 C26 N1 Ho1 4.7(10) . . . . ?
C26 C18 C19 C20 -1.2(14) . . . . ?
C26 C25 N2 C24 176.6(7) . . . . ?
C26 C25 N2 Ho1 -6.7(9) . . . . ?
Ho1 C8 C9 C10 50(3) . . . . ?
Ho1 C8 C9 C14 -130(3) . . . . ?
N1 C15 C16 C17 2.4(15) . . . . ?
N2 C25 C26 C18 -178.2(7) . . . . ?
N2 C25 C26 N1 1.1(11) . . . . ?
O1 C1 C2 C3 -170.1(7) . . . . ?
O1 C1 C2 C7 8.2(12) . . . . ?
O1 C1 O2 Ho1 -6.2(13) . . . 2_575 ?
O2 C1 C2 C3 10.5(11) . . . . ?
O2 C1 C2 C7 -171.1(8) . . . . ?
O2 C1 O1 Ho1 17.7(13) . . . . ?
O3 C8 C9 C10 24.5(11) . . . . ?
O3 C8 C9 C14 -155.4(8) . . . . ?
O4 C8 C9 C10 -159.3(7) 2_575 . . . ?
O4 C8 C9 C14 20.8(12) 2_575 . . . ?
O4 C8 O3 Ho1 -1.8(8) 2_575 . . . ?
O5 N3 O6 Ho1 -0.3(7) . . . . ?
O6 N3 O5 Ho1 0.3(6) . . . . ?
O7 N3 O5 Ho1 177.5(6) . . . . ?
O7 N3 O6 Ho1 -177.6(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Phase1Eu
_database_code_depnum_ccdc_archive 'CCDC 1477858'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2015-10-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H14 Eu N2 O8 S2, 3(H2 O)'
_chemical_formula_sum            'C22 H20 Eu N2 O11 S2'
_chemical_formula_weight         704.48
_chemical_melting_point          ?
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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2352(6)
_cell_length_b                   11.8774(7)
_cell_length_c                   12.6755(8)
_cell_angle_alpha                106.681(3)
_cell_angle_beta                 110.149(3)
_cell_angle_gamma                99.171(3)
_cell_volume                     1197.69(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5482
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.38
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.860
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0715 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8805.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             698
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21024
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_min         1.841
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4056
_reflns_number_total             4955
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.284
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²+0.4362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0894
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O11(0.57469)
3.a Free rotating group:
 O9(H9A,H9B,O10,H10A,H10B,O11,H11A,H11B)
3.b Rotating group:
 O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14),
 C16(H16), C19(H19), C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.7022(7) 0.0688(6) 0.9169(5) 0.0372(14) Uani 1 1 d . . . . .
H1 H 0.7568 0.1432 0.9197 0.045 Uiso 1 1 calc R . . . .
C2 C 0.7757(8) 0.0245(7) 1.0057(5) 0.0482(17) Uani 1 1 d . . . . .
H2 H 0.8788 0.0675 1.0653 0.058 Uiso 1 1 calc R . . . .
C3 C 0.6943(8) -0.0831(6) 1.0042(5) 0.0473(16) Uani 1 1 d . . . . .
H3 H 0.7427 -0.1147 1.0621 0.057 Uiso 1 1 calc R . . . .
C4 C 0.5397(7) -0.1449(5) 0.9166(5) 0.0352(13) Uani 1 1 d . . . . .
C5 C 0.4439(9) -0.2552(6) 0.9131(6) 0.0483(17) Uani 1 1 d . . . . .
H5 H 0.4867 -0.2880 0.9712 0.058 Uiso 1 1 calc R . . . .
C6 C 0.2954(9) -0.3110(6) 0.8282(6) 0.0465(16) Uani 1 1 d . . . . .
H6 H 0.2350 -0.3807 0.8298 0.056 Uiso 1 1 calc R . . . .
C7 C 0.2259(7) -0.2667(5) 0.7345(5) 0.0348(13) Uani 1 1 d . . . . .
C8 C 0.0739(7) -0.3267(5) 0.6397(6) 0.0431(15) Uani 1 1 d . . . . .
H8 H 0.0107 -0.3978 0.6368 0.052 Uiso 1 1 calc R . . . .
C9 C 0.0184(7) -0.2807(6) 0.5513(6) 0.0457(16) Uani 1 1 d . . . . .
H9 H -0.0829 -0.3200 0.4880 0.055 Uiso 1 1 calc R . . . .
C10 C 0.1155(7) -0.1738(5) 0.5570(5) 0.0352(13) Uani 1 1 d . . . . .
H10 H 0.0762 -0.1434 0.4961 0.042 Uiso 1 1 calc R . . . .
C11 C 0.3161(6) -0.1591(4) 0.7334(5) 0.0251(11) Uani 1 1 d . . . . .
C12 C 0.4737(7) -0.0966(5) 0.8272(5) 0.0275(11) Uani 1 1 d . . . . .
C13 C 0.3073(6) 0.1585(4) 0.3586(4) 0.0210(10) Uani 1 1 d . . . . .
C14 C 0.2486(6) 0.2282(4) 0.2941(4) 0.0250(11) Uani 1 1 d . . . . .
H14 H 0.1404 0.2038 0.2414 0.030 Uiso 1 1 calc R . . . .
C15 C 0.3539(6) 0.3382(4) 0.3083(4) 0.0223(10) Uani 1 1 d . . . . .
C16 C 0.3000(6) 0.4098(4) 0.2389(5) 0.0257(11) Uani 1 1 d . . . . .
H16 H 0.1931 0.3867 0.1840 0.031 Uiso 1 1 calc R . . . .
C17 C 0.4070(6) 0.5134(4) 0.2534(4) 0.0249(11) Uani 1 1 d . . . . .
C18 C 0.5701(6) 0.5529(5) 0.3380(5) 0.0288(12) Uani 1 1 d . . . . .
C19 C 0.6213(6) 0.4845(4) 0.4054(5) 0.0269(11) Uani 1 1 d . . . . .
H19 H 0.7280 0.5099 0.4611 0.032 Uiso 1 1 calc R . . . .
C20 C 0.5165(6) 0.3754(4) 0.3928(4) 0.0207(10) Uani 1 1 d . . . . .
C21 C 0.5718(6) 0.3023(4) 0.4588(4) 0.0210(10) Uani 1 1 d . . . . .
H21 H 0.6777 0.3286 0.5162 0.025 Uiso 1 1 calc R . . . .
C22 C 0.4721(6) 0.1925(4) 0.4401(4) 0.0186(10) Uani 1 1 d . . . . .
Eu1 Eu 0.45419(3) 0.06682(2) 0.64039(2) 0.02031(9) Uani 1 1 d . . . . .
N1 N 0.5571(5) 0.0092(4) 0.8280(4) 0.0290(10) Uani 1 1 d . . . . .
N2 N 0.2597(5) -0.1142(4) 0.6443(4) 0.0242(9) Uani 1 1 d . . . . .
O1 O 0.2084(4) 0.0371(3) 0.4713(3) 0.0251(8) Uani 1 1 d . . . . .
O2 O 0.2523(4) -0.0771(3) 0.2989(3) 0.0255(8) Uani 1 1 d . . . . .
O3 O 0.0212(4) 0.0023(3) 0.2685(3) 0.0302(8) Uani 1 1 d . . . . .
O4 O 0.4109(6) 0.5706(4) 0.0722(4) 0.0542(13) Uani 1 1 d . . . . .
O5 O 0.4173(5) 0.7278(3) 0.2434(3) 0.0365(9) Uani 1 1 d . . . . .
O6 O 0.1730(5) 0.5654(4) 0.1125(5) 0.0587(14) Uani 1 1 d . . . . .
O7 O 0.5257(4) 0.1138(3) 0.4912(3) 0.0193(7) Uani 1 1 d . . . . .
O8 O 0.2726(5) 0.1390(4) 0.7259(4) 0.0388(10) Uani 1 1 d . . . . .
H8A H 0.1740 0.0999 0.6762 0.058 Uiso 1 1 d GR . . . .
H8B H 0.2868 0.2162 0.7395 0.058 Uiso 1 1 d GR . . . .
O9 O 0.9716(5) 0.7208(5) 0.0701(5) 0.0901(19) Uani 1 1 d . . . . .
H9A H 1.0496 0.7669 0.1368 0.135 Uiso 1 1 d G . . . .
H9B H 0.9911 0.6532 0.0433 0.135 Uiso 1 1 d G . . . .
O10 O 0.7589(5) 0.6477(4) 0.1615(5) 0.087(2) Uani 1 1 d G . . . .
H10A H 0.6598 0.6100 0.1178 0.131 Uiso 1 1 d G . . . .
H10B H 0.8077 0.6532 0.1165 0.131 Uiso 1 1 d G . . . .
O11 O 0.0313(8) 0.5802(9) 0.2949(8) 0.076(3) Uani 0.5747 1 d G . P . .
H11A H 0.0655 0.6489 0.2908 0.114 Uiso 1 1 d G . . . .
H11B H -0.0301 0.5285 0.2244 0.114 Uiso 1 1 d G . . . .
S1 S 0.18598(14) 0.02071(11) 0.34650(11) 0.0212(3) Uani 1 1 d . . . . .
S2 S 0.34493(16) 0.59860(11) 0.16077(12) 0.0287(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9300 . ?
C1 C2 1.390(8) . ?
C1 N1 1.328(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.367(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(8) . ?
C4 C5 1.439(8) . ?
C4 C12 1.413(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.327(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.429(8) . ?
C7 C8 1.397(8) . ?
C7 C11 1.416(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.364(9) . ?
C9 H9 0.9300 . ?
C9 C10 1.401(8) . ?
C10 H10 0.9300 . ?
C10 N2 1.317(7) . ?
C11 C12 1.428(7) . ?
C11 N2 1.364(6) . ?
C12 N1 1.360(6) . ?
C13 C14 1.369(6) . ?
C13 C22 1.424(6) . ?
C13 S1 1.764(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.424(6) . ?
C15 C16 1.416(6) . ?
C15 C20 1.416(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.372(7) . ?
C17 C18 1.419(7) . ?
C17 S2 1.770(5) . ?
C18 C19 1.362(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.420(6) . ?
C20 C21 1.407(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.375(6) . ?
C22 Eu1 3.214(5) 2_656 ?
C22 O7 1.347(5) . ?
Eu1 C22 3.214(5) 2_656 ?
Eu1 Eu1 3.8938(5) 2_656 ?
Eu1 N1 2.572(4) . ?
Eu1 N2 2.596(4) . ?
Eu1 O1 2.414(3) . ?
Eu1 O2 2.522(3) 2_656 ?
Eu1 O5 2.310(3) 2_666 ?
Eu1 O7 2.381(3) . ?
Eu1 O7 2.388(3) 2_656 ?
Eu1 O8 2.429(4) . ?
Eu1 S1 3.5146(12) . ?
O1 S1 1.473(3) . ?
O2 Eu1 2.522(3) 2_656 ?
O2 S1 1.472(3) . ?
O3 S1 1.441(3) . ?
O4 S2 1.437(4) . ?
O5 Eu1 2.310(3) 2_666 ?
O5 S2 1.473(4) . ?
O6 S2 1.430(4) . ?
O7 Eu1 2.388(3) 2_656 ?
O8 H8A 0.8627 . ?
O8 H8B 0.8625 . ?
O9 H9A 0.8497 . ?
O9 H9B 0.8504 . ?
O10 H10A 0.8501 . ?
O10 H10B 0.8500 . ?
O11 H11A 0.8500 . ?
O11 H11B 0.8498 . ?

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
C2 C1 H1 118.6 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(6) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 119.0(6) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0(6) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 123.1(5) . . ?
C3 C4 C12 118.0(5) . . ?
C12 C4 C5 118.9(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.2(6) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 119.2 . . ?
C5 C6 C7 121.6(6) . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 123.3(5) . . ?
C8 C7 C11 117.3(5) . . ?
C11 C7 C6 119.4(6) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.8(5) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.3(6) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C10 C9 123.2(5) . . ?
N2 C10 H10 118.4 . . ?
C7 C11 C12 119.0(5) . . ?
N2 C11 C7 122.5(5) . . ?
N2 C11 C12 118.4(4) . . ?
C4 C12 C11 119.9(5) . . ?
N1 C12 C4 121.4(5) . . ?
N1 C12 C11 118.7(4) . . ?
C14 C13 C22 121.9(4) . . ?
C14 C13 S1 122.8(4) . . ?
C22 C13 S1 115.3(3) . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.6(4) . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 121.5(4) . . ?
C16 C15 C20 119.7(4) . . ?
C20 C15 C14 118.8(4) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 C15 119.4(5) . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 121.9(5) . . ?
C16 C17 S2 120.0(4) . . ?
C18 C17 S2 118.0(4) . . ?
C19 C18 C17 118.6(5) . . ?
C18 C19 H19 119.0 . . ?
C18 C19 C20 121.9(5) . . ?
C20 C19 H19 119.0 . . ?
C15 C20 C19 118.5(4) . . ?
C21 C20 C15 119.8(4) . . ?
C21 C20 C19 121.6(4) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.2(4) . . ?
C22 C21 H21 119.4 . . ?
C13 C22 Eu1 99.7(3) . 2_656 ?
C21 C22 C13 118.4(4) . . ?
C21 C22 Eu1 123.8(3) . 2_656 ?
O7 C22 C13 118.9(4) . . ?
O7 C22 C21 122.7(4) . . ?
O7 C22 Eu1 41.94(19) . 2_656 ?
C22 Eu1 Eu1 54.88(8) 2_656 2_656 ?
C22 Eu1 S1 94.10(8) 2_656 . ?
N1 Eu1 C22 72.03(13) . 2_656 ?
N1 Eu1 Eu1 122.53(10) . 2_656 ?
N1 Eu1 N2 63.83(13) . . ?
N1 Eu1 S1 154.18(10) . . ?
N2 Eu1 C22 65.41(12) . 2_656 ?
N2 Eu1 Eu1 106.30(9) . 2_656 ?
N2 Eu1 S1 90.74(9) . . ?
O1 Eu1 C22 102.20(12) . 2_656 ?
O1 Eu1 Eu1 76.19(8) . 2_656 ?
O1 Eu1 N1 140.99(13) . . ?
O1 Eu1 N2 78.52(12) . . ?
O1 Eu1 O2 143.48(11) . 2_656 ?
O1 Eu1 O8 73.72(13) . . ?
O1 Eu1 S1 19.35(8) . . ?
O2 Eu1 C22 64.51(11) 2_656 2_656 ?
O2 Eu1 Eu1 68.45(8) 2_656 2_656 ?
O2 Eu1 N1 70.23(13) 2_656 . ?
O2 Eu1 N2 119.54(12) 2_656 . ?
O2 Eu1 S1 124.15(8) 2_656 . ?
O5 Eu1 C22 141.37(13) 2_666 2_656 ?
O5 Eu1 Eu1 116.04(10) 2_666 2_656 ?
O5 Eu1 N1 91.06(14) 2_666 . ?
O5 Eu1 N2 137.64(14) 2_666 . ?
O5 Eu1 O1 111.96(12) 2_666 . ?
O5 Eu1 O2 77.19(13) 2_666 2_656 ?
O5 Eu1 O7 84.54(12) 2_666 . ?
O5 Eu1 O7 144.14(13) 2_666 2_656 ?
O5 Eu1 O8 74.78(14) 2_666 . ?
O5 Eu1 S1 112.26(10) 2_666 . ?
O7 Eu1 C22 22.15(11) 2_656 2_656 ?
O7 Eu1 C22 89.32(11) . 2_656 ?
O7 Eu1 Eu1 35.33(7) . 2_656 ?
O7 Eu1 Eu1 35.21(7) 2_656 2_656 ?
O7 Eu1 N1 94.19(12) 2_656 . ?
O7 Eu1 N1 143.73(13) . . ?
O7 Eu1 N2 74.95(12) 2_656 . ?
O7 Eu1 N2 136.01(12) . . ?
O7 Eu1 O1 72.24(11) . . ?
O7 Eu1 O1 85.12(11) 2_656 . ?
O7 Eu1 O2 71.40(11) 2_656 2_656 ?
O7 Eu1 O2 73.70(11) . 2_656 ?
O7 Eu1 O7 70.54(12) . 2_656 ?
O7 Eu1 O8 129.36(12) . . ?
O7 Eu1 O8 141.07(12) 2_656 . ?
O7 Eu1 S1 73.68(8) 2_656 . ?
O7 Eu1 S1 54.05(8) . . ?
O8 Eu1 C22 134.14(13) . 2_656 ?
O8 Eu1 Eu1 149.87(10) . 2_656 ?
O8 Eu1 N1 83.28(14) . . ?
O8 Eu1 N2 69.11(13) . . ?
O8 Eu1 O2 140.71(13) . 2_656 ?
O8 Eu1 S1 92.02(10) . . ?
S1 Eu1 Eu1 57.90(2) . 2_656 ?
C1 N1 C12 118.7(5) . . ?
C1 N1 Eu1 121.3(4) . . ?
C12 N1 Eu1 119.0(3) . . ?
C10 N2 C11 118.0(4) . . ?
C10 N2 Eu1 123.1(3) . . ?
C11 N2 Eu1 118.5(3) . . ?
S1 O1 Eu1 127.75(19) . . ?
S1 O2 Eu1 126.77(19) . 2_656 ?
S2 O5 Eu1 173.6(3) . 2_666 ?
C22 O7 Eu1 115.9(3) . 2_656 ?
C22 O7 Eu1 124.2(3) . . ?
Eu1 O7 Eu1 109.46(12) . 2_656 ?
Eu1 O8 H8A 110.2 . . ?
Eu1 O8 H8B 109.7 . . ?
H8A O8 H8B 108.8 . . ?
H9A O9 H9B 109.5 . . ?
H10A O10 H10B 109.5 . . ?
H11A O11 H11B 109.5 . . ?
C13 S1 Eu1 88.55(16) . . ?
O1 S1 C13 104.9(2) . . ?
O1 S1 Eu1 32.90(13) . . ?
O2 S1 C13 106.2(2) . . ?
O2 S1 Eu1 88.83(14) . . ?
O2 S1 O1 110.6(2) . . ?
O3 S1 C13 109.4(2) . . ?
O3 S1 Eu1 145.41(16) . . ?
O3 S1 O1 112.5(2) . . ?
O3 S1 O2 112.7(2) . . ?
O4 S2 C17 107.0(2) . . ?
O4 S2 O5 111.0(3) . . ?
O5 S2 C17 104.7(2) . . ?
O6 S2 C17 106.8(2) . . ?
O6 S2 O4 115.0(3) . . ?
O6 S2 O5 111.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.3(10) . . . . ?
C2 C1 N1 C12 3.3(9) . . . . ?
C2 C1 N1 Eu1 -165.5(5) . . . . ?
C2 C3 C4 C5 -176.8(6) . . . . ?
C2 C3 C4 C12 2.9(9) . . . . ?
C3 C4 C5 C6 179.2(6) . . . . ?
C3 C4 C12 C11 178.5(5) . . . . ?
C3 C4 C12 N1 -1.6(8) . . . . ?
C4 C5 C6 C7 2.1(10) . . . . ?
C4 C12 N1 C1 -1.5(8) . . . . ?
C4 C12 N1 Eu1 167.6(4) . . . . ?
C5 C4 C12 C11 -1.7(8) . . . . ?
C5 C4 C12 N1 178.2(5) . . . . ?
C5 C6 C7 C8 176.1(6) . . . . ?
C5 C6 C7 C11 -1.4(9) . . . . ?
C6 C7 C8 C9 -177.7(6) . . . . ?
C6 C7 C11 C12 -0.8(8) . . . . ?
C6 C7 C11 N2 177.5(5) . . . . ?
C7 C8 C9 C10 0.2(10) . . . . ?
C7 C11 C12 C4 2.4(8) . . . . ?
C7 C11 C12 N1 -177.6(5) . . . . ?
C7 C11 N2 C10 0.3(7) . . . . ?
C7 C11 N2 Eu1 -172.1(4) . . . . ?
C8 C7 C11 C12 -178.5(5) . . . . ?
C8 C7 C11 N2 -0.2(8) . . . . ?
C8 C9 C10 N2 0.0(10) . . . . ?
C9 C10 N2 C11 -0.2(8) . . . . ?
C9 C10 N2 Eu1 171.8(5) . . . . ?
C11 C7 C8 C9 -0.1(9) . . . . ?
C11 C12 N1 C1 178.5(5) . . . . ?
C11 C12 N1 Eu1 -12.5(6) . . . . ?
C12 C4 C5 C6 -0.5(9) . . . . ?
C12 C11 N2 C10 178.7(5) . . . . ?
C12 C11 N2 Eu1 6.3(6) . . . . ?
C13 C14 C15 C16 176.8(5) . . . . ?
C13 C14 C15 C20 -2.5(7) . . . . ?
C13 C22 O7 Eu1 70.9(5) . . . 2_656 ?
C13 C22 O7 Eu1 -70.2(5) . . . . ?
C14 C13 C22 C21 3.8(7) . . . . ?
C14 C13 C22 Eu1 -133.4(4) . . . 2_656 ?
C14 C13 C22 O7 -173.2(4) . . . . ?
C14 C13 S1 Eu1 -154.3(4) . . . . ?
C14 C13 S1 O1 -125.5(4) . . . . ?
C14 C13 S1 O2 117.3(4) . . . . ?
C14 C13 S1 O3 -4.5(5) . . . . ?
C14 C15 C16 C17 -178.3(5) . . . . ?
C14 C15 C20 C19 179.3(5) . . . . ?
C14 C15 C20 C21 1.5(7) . . . . ?
C15 C16 C17 C18 -1.4(8) . . . . ?
C15 C16 C17 S2 176.0(4) . . . . ?
C15 C20 C21 C22 2.2(7) . . . . ?
C16 C15 C20 C19 0.0(7) . . . . ?
C16 C15 C20 C21 -177.8(4) . . . . ?
C16 C17 C18 C19 0.8(8) . . . . ?
C16 C17 S2 O4 -103.8(5) . . . . ?
C16 C17 S2 O5 138.3(4) . . . . ?
C16 C17 S2 O6 19.8(5) . . . . ?
C17 C18 C19 C20 0.1(8) . . . . ?
C18 C17 S2 O4 73.7(5) . . . . ?
C18 C17 S2 O5 -44.2(5) . . . . ?
C18 C17 S2 O6 -162.7(4) . . . . ?
C18 C19 C20 C15 -0.5(7) . . . . ?
C18 C19 C20 C21 177.2(5) . . . . ?
C19 C20 C21 C22 -175.5(5) . . . . ?
C20 C15 C16 C17 0.9(7) . . . . ?
C20 C21 C22 C13 -4.8(7) . . . . ?
C20 C21 C22 Eu1 121.5(4) . . . 2_656 ?
C20 C21 C22 O7 172.1(4) . . . . ?
C21 C22 O7 Eu1 112.9(4) . . . . ?
C21 C22 O7 Eu1 -106.0(4) . . . 2_656 ?
C22 C13 C14 C15 -0.2(7) . . . . ?
C22 C13 S1 Eu1 26.1(3) . . . . ?
C22 C13 S1 O1 54.9(4) . . . . ?
C22 C13 S1 O2 -62.3(4) . . . . ?
C22 C13 S1 O3 175.9(3) . . . . ?
Eu1 C22 O7 Eu1 -141.1(4) 2_656 . . . ?
Eu1 O1 S1 C13 -62.6(3) . . . . ?
Eu1 O1 S1 O2 51.6(3) . . . . ?
Eu1 O1 S1 O3 178.6(2) . . . . ?
Eu1 O2 S1 C13 41.4(3) 2_656 . . . ?
Eu1 O2 S1 Eu1 -46.7(2) 2_656 . . . ?
Eu1 O2 S1 O1 -71.9(3) 2_656 . . . ?
Eu1 O2 S1 O3 161.2(2) 2_656 . . . ?
N1 C1 C2 C3 -1.9(10) . . . . ?
N2 C11 C12 C4 -176.1(5) . . . . ?
N2 C11 C12 N1 4.0(7) . . . . ?
S1 C13 C14 C15 -179.8(4) . . . . ?
S1 C13 C22 C21 -176.6(4) . . . . ?
S1 C13 C22 Eu1 46.2(3) . . . 2_656 ?
S1 C13 C22 O7 6.4(6) . . . . ?
S2 C17 C18 C19 -176.6(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Phase3-Er
_database_code_depnum_ccdc_archive 'CCDC 1477859'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2015-10-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H28 Er2 N4 O15 S4, 3(H2 O)'
_chemical_formula_sum            'C44 H34 Er2 N4 O18 S4'
_chemical_formula_weight         1369.51
_chemical_melting_point          ?
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'
Er Er -0.2586 4.9576 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2425(8)
_cell_length_b                   17.0358(9)
_cell_length_c                   18.8857(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.030(2)
_cell_angle_gamma                90
_cell_volume                     4525.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9276
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      1.6
_cell_measurement_theta_min      26.4
_shelx_estimated_absorpt_T_max   0.858
_shelx_estimated_absorpt_T_min   0.415
_exptl_absorpt_coefficient_mu    3.953
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0687 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.8255.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2680
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            129298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         1.619
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7853
_reflns_number_total             9276
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 20015)'
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0214P)²+10.2461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0588
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B,O17,H17A,H17B,O18,H18A,H18B)
2.b Rotating group:
 O15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C -0.2368(3) 0.2603(2) 0.25319(19) 0.0185(7) Uani 1 1 d . . . . .
C2 C -0.2080(3) 0.2686(2) 0.32498(19) 0.0197(7) Uani 1 1 d . . . . .
H2 H -0.1928 0.3178 0.3447 0.024 Uiso 1 1 calc R . . . .
C3 C -0.2014(3) 0.2009(2) 0.36915(18) 0.0201(7) Uani 1 1 d . . . . .
C4 C -0.6739(3) 0.2932(2) -0.05534(19) 0.0219(8) Uani 1 1 d . . . . .
H4 H -0.6632 0.2442 -0.0338 0.026 Uiso 1 1 calc R . . . .
C5 C -0.6635(3) 0.3596(2) -0.01477(19) 0.0228(8) Uani 1 1 d . . . . .
C6 C -0.6779(3) 0.4345(2) -0.0465(2) 0.0322(9) Uani 1 1 d . . . . .
H6 H -0.6680 0.4793 -0.0181 0.039 Uiso 1 1 calc R . . . .
C7 C -0.2062(3) 0.0586(2) 0.3815(2) 0.0326(10) Uani 1 1 d . . . . .
H7 H -0.2164 0.0091 0.3611 0.039 Uiso 1 1 calc R . . . .
C8 C -0.2205(3) 0.1260(2) 0.33724(19) 0.0222(8) Uani 1 1 d . . . . .
C9 C -0.2551(3) 0.1201(2) 0.26246(18) 0.0219(8) Uani 1 1 d . . . . .
H9 H -0.2692 0.0712 0.2417 0.026 Uiso 1 1 calc R . . . .
C10 C -0.2677(2) 0.1865(2) 0.22112(18) 0.0186(7) Uani 1 1 d . . . . .
C11 C -0.4099(2) 0.2853(2) -0.03885(18) 0.0183(7) Uani 1 1 d . . . . .
C12 C -0.4121(3) 0.3541(2) -0.07695(19) 0.0234(8) Uani 1 1 d . . . . .
H12 H -0.3955 0.4010 -0.0530 0.028 Uiso 1 1 calc R . . . .
C13 C -0.4393(3) 0.3544(2) -0.15226(19) 0.0219(8) Uani 1 1 d . . . . .
C14 C 0.0692(3) 0.0774(2) 0.3061(2) 0.0305(9) Uani 1 1 d . . . . .
H14 H 0.0853 0.0297 0.3289 0.037 Uiso 1 1 calc R . . . .
C15 C 0.0541(3) 0.0809(2) 0.2329(2) 0.0292(9) Uani 1 1 d . . . . .
H15 H 0.0617 0.0361 0.2062 0.035 Uiso 1 1 calc R . . . .
C16 C 0.0270(3) 0.1518(2) 0.19780(19) 0.0233(8) Uani 1 1 d . . . . .
C17 C 0.0129(3) 0.2182(2) 0.23533(19) 0.0240(8) Uani 1 1 d . . . . .
H17 H -0.0083 0.2640 0.2112 0.029 Uiso 1 1 calc R . . . .
C18 C -0.4693(3) 0.2831(2) -0.18862(19) 0.0207(8) Uani 1 1 d . . . . .
C19 C -0.4783(3) 0.2149(2) -0.14753(19) 0.0220(8) Uani 1 1 d . . . . .
H19 H -0.5037 0.1692 -0.1697 0.026 Uiso 1 1 calc R . . . .
C20 C -0.4494(2) 0.2165(2) -0.07518(18) 0.0187(7) Uani 1 1 d . . . . .
C21 C -0.4651(3) 0.3703(3) 0.2718(2) 0.0358(10) Uani 1 1 d . . . . .
H21 H -0.4675 0.4105 0.2382 0.043 Uiso 1 1 calc R . . . .
C22 C -0.4551(4) 0.3898(3) 0.3448(2) 0.0464(12) Uani 1 1 d . . . . .
H22 H -0.4528 0.4420 0.3591 0.056 Uiso 1 1 calc R . . . .
C23 C -0.4489(4) 0.3315(3) 0.3944(2) 0.0483(13) Uani 1 1 d . . . . .
H23 H -0.4413 0.3439 0.4430 0.058 Uiso 1 1 calc R . . . .
C24 C -0.4540(3) 0.2531(3) 0.3730(2) 0.0335(10) Uani 1 1 d . . . . .
C25 C -0.4469(3) 0.1889(3) 0.4222(2) 0.0449(12) Uani 1 1 d . . . . .
H25 H -0.4370 0.1989 0.4712 0.054 Uiso 1 1 calc R . . . .
C26 C -0.4543(3) 0.1142(3) 0.3986(2) 0.0436(12) Uani 1 1 d . . . . .
H26 H -0.4481 0.0733 0.4317 0.052 Uiso 1 1 calc R . . . .
C27 C -0.4717(3) 0.0964(3) 0.3233(2) 0.0327(10) Uani 1 1 d . . . . .
C28 C -0.4861(4) 0.0198(3) 0.2959(3) 0.0451(12) Uani 1 1 d . . . . .
H28 H -0.4834 -0.0229 0.3268 0.054 Uiso 1 1 calc R . . . .
C29 C -0.5039(4) 0.0090(3) 0.2239(3) 0.0489(13) Uani 1 1 d . . . . .
H29 H -0.5152 -0.0412 0.2052 0.059 Uiso 1 1 calc R . . . .
C30 C -0.5054(3) 0.0730(2) 0.1781(2) 0.0332(10) Uani 1 1 d . . . . .
H30 H -0.5169 0.0639 0.1289 0.040 Uiso 1 1 calc R . . . .
C31 C -0.4762(3) 0.1583(2) 0.27342(19) 0.0244(8) Uani 1 1 d . . . . .
C32 C -0.4668(3) 0.2377(2) 0.2987(2) 0.0245(8) Uani 1 1 d . . . . .
C33 C -0.1754(3) 0.3856(2) -0.0062(2) 0.0309(9) Uani 1 1 d . . . . .
H33 H -0.1668 0.3972 0.0425 0.037 Uiso 1 1 calc R . . . .
C34 C -0.1732(3) 0.4473(3) -0.0545(2) 0.0368(10) Uani 1 1 d . . . . .
H34 H -0.1632 0.4985 -0.0379 0.044 Uiso 1 1 calc R . . . .
C35 C -0.1858(3) 0.4318(3) -0.1261(2) 0.0379(11) Uani 1 1 d . . . . .
H35 H -0.1864 0.4726 -0.1589 0.045 Uiso 1 1 calc R . . . .
C36 C -0.1980(3) 0.3543(2) -0.1502(2) 0.0291(9) Uani 1 1 d . . . . .
C37 C -0.2097(3) 0.3326(3) -0.2240(2) 0.0396(11) Uani 1 1 d . . . . .
H37 H -0.2102 0.3715 -0.2586 0.047 Uiso 1 1 calc R . . . .
C38 C -0.2201(3) 0.2573(3) -0.2447(2) 0.0437(12) Uani 1 1 d . . . . .
H38 H -0.2278 0.2451 -0.2932 0.052 Uiso 1 1 calc R . . . .
C39 C -0.2195(3) 0.1957(3) -0.1933(2) 0.0331(10) Uani 1 1 d . . . . .
C40 C -0.2279(4) 0.1156(3) -0.2117(2) 0.0480(13) Uani 1 1 d . . . . .
H40 H -0.2331 0.1005 -0.2594 0.058 Uiso 1 1 calc R . . . .
C41 C -0.2285(4) 0.0605(3) -0.1598(3) 0.0485(13) Uani 1 1 d . . . . .
H41 H -0.2337 0.0075 -0.1717 0.058 Uiso 1 1 calc R . . . .
C42 C -0.2212(3) 0.0844(2) -0.0885(2) 0.0362(10) Uani 1 1 d . . . . .
H42 H -0.2228 0.0462 -0.0536 0.043 Uiso 1 1 calc R . . . .
C43 C -0.2101(3) 0.2145(2) -0.1196(2) 0.0256(8) Uani 1 1 d . . . . .
C44 C -0.1981(3) 0.2949(2) -0.0978(2) 0.0238(8) Uani 1 1 d . . . . .
O1 O -0.18625(18) 0.30908(15) 0.13631(13) 0.0250(6) Uani 1 1 d . . . . .
O2 O -0.1893(2) 0.40511(15) 0.23076(14) 0.0301(6) Uani 1 1 d . . . . .
O3 O -0.33713(18) 0.35478(14) 0.16461(13) 0.0233(6) Uani 1 1 d . . . . .
O4 O -0.52639(19) 0.38044(16) 0.09246(14) 0.0306(6) Uani 1 1 d . . . . .
O5 O -0.62416(19) 0.26994(15) 0.09897(14) 0.0262(6) Uani 1 1 d . . . . .
O6 O -0.6891(2) 0.40156(18) 0.11275(15) 0.0402(8) Uani 1 1 d . . . . .
O7 O -0.31053(17) 0.18676(14) 0.15148(12) 0.0200(5) Uani 1 1 d . . . . .
O8 O -0.35828(18) 0.11504(15) 0.01069(13) 0.0244(6) Uani 1 1 d . . . . .
O9 O -0.50575(19) 0.07256(15) -0.06196(13) 0.0274(6) Uani 1 1 d . . . . .
O10 O -0.50802(18) 0.16294(15) 0.03756(13) 0.0245(6) Uani 1 1 d . . . . .
O11 O 0.1030(2) 0.19526(19) 0.08775(16) 0.0393(7) Uani 1 1 d . . . . .
O12 O -0.06595(18) 0.20464(16) 0.07818(14) 0.0277(6) Uani 1 1 d . . . . .
O13 O 0.0076(2) 0.07642(17) 0.07746(15) 0.0370(7) Uani 1 1 d . . . . .
O14 O -0.37043(17) 0.27914(14) 0.03076(12) 0.0201(5) Uani 1 1 d . . . . .
O15 O -0.1859(2) 0.07502(16) 0.08507(16) 0.0362(7) Uani 1 1 d . . . . .
H15A H -0.1897 0.0650 0.1297 0.054 Uiso 1 1 d GR . . . .
H15B H -0.1275 0.0673 0.0786 0.054 Uiso 1 1 d GR . . . .
O16 O 0.0914(2) 0.37135(17) 0.1072(3) 0.146(3) Uani 1 1 d . . . . .
H16A H 0.0955 0.3770 0.1523 0.219 Uiso 1 1 d G . . . .
H16B H 0.1351 0.3976 0.0923 0.219 Uiso 1 1 d G . . . .
O17 O 0.7118(2) 0.94251(16) 0.0648(2) 0.0686(12) Uani 1 1 d G . . . .
H17A H 0.6878 0.9575 0.1010 0.103 Uiso 1 1 d G . . . .
H17B H 0.6914 0.9716 0.0291 0.103 Uiso 1 1 d G . . . .
O18 O 0.2739(2) 0.11592(15) 0.0726(3) 0.0756(13) Uani 1 1 d G . . . .
H18A H 0.2189 0.1322 0.0777 0.113 Uiso 1 1 d G . . . .
H18B H 0.3101 0.1550 0.0692 0.113 Uiso 1 1 d G . . . .
S1 S -0.23676(7) 0.33951(5) 0.19337(5) 0.02041(19) Uani 1 1 d . . . . .
S2 S -0.62642(7) 0.35390(6) 0.07878(5) 0.0244(2) Uani 1 1 d . . . . .
S3 S -0.45642(6) 0.13408(5) -0.01967(5) 0.01918(18) Uani 1 1 d . . . . .
S4 S 0.01826(7) 0.15642(6) 0.10328(5) 0.0253(2) Uani 1 1 d . . . . .
Er1 Er -0.22987(2) 0.20376(2) 0.05596(2) 0.01926(5) Uani 1 1 d . . . . .
Er2 Er -0.45127(2) 0.25762(2) 0.12482(2) 0.01850(5) Uani 1 1 d . . . . .
N1 N -0.4711(2) 0.29602(18) 0.24902(16) 0.0248(7) Uani 1 1 d . . . . .
N2 N -0.4912(2) 0.14619(18) 0.20077(16) 0.0234(7) Uani 1 1 d . . . . .
N3 N -0.1890(2) 0.31100(18) -0.02619(16) 0.0239(7) Uani 1 1 d . . . . .
N4 N -0.2122(2) 0.15906(19) -0.06810(16) 0.0274(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.361(5) . ?
C1 C10 1.434(5) . ?
C1 S1 1.760(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.417(5) . ?
C3 C4 1.422(5) 4_666 ?
C3 C8 1.418(5) . ?
C4 C3 1.422(5) 4_565 ?
C4 H4 0.9300 . ?
C4 C5 1.362(5) . ?
C5 C6 1.410(5) . ?
C5 S2 1.765(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.362(5) 4_565 ?
C7 C6 1.362(5) 4_666 ?
C7 H7 0.9300 . ?
C7 C8 1.416(5) . ?
C8 C9 1.424(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.370(5) . ?
C10 O7 1.360(4) . ?
C11 C12 1.373(5) . ?
C11 C20 1.428(5) . ?
C11 O14 1.350(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.414(5) . ?
C13 C14 1.420(5) 4_565 ?
C13 C18 1.427(5) . ?
C14 C13 1.420(5) 4_666 ?
C14 H14 0.9300 . ?
C14 C15 1.367(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.402(5) . ?
C16 C17 1.367(5) . ?
C16 S4 1.771(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.419(5) 4_666 ?
C18 C17 1.419(5) 4_565 ?
C18 C19 1.415(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.364(5) . ?
C20 S3 1.765(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.404(6) . ?
C21 N1 1.336(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.359(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.394(7) . ?
C24 C25 1.428(6) . ?
C24 C32 1.410(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.348(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.437(6) . ?
C27 C28 1.407(7) . ?
C27 C31 1.409(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.356(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.390(6) . ?
C30 H30 0.9300 . ?
C30 N2 1.324(5) . ?
C31 C32 1.434(5) . ?
C31 N2 1.371(5) . ?
C32 N1 1.361(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.395(6) . ?
C33 N3 1.332(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.362(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.398(6) . ?
C36 C37 1.426(6) . ?
C36 C44 1.416(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.341(7) . ?
C38 H38 0.9300 . ?
C38 C39 1.428(6) . ?
C39 C40 1.408(6) . ?
C39 C43 1.414(5) . ?
C40 H40 0.9300 . ?
C40 C41 1.358(7) . ?
C41 H41 0.9300 . ?
C41 C42 1.394(6) . ?
C42 H42 0.9300 . ?
C42 N4 1.330(5) . ?
C43 C44 1.433(6) . ?
C43 N4 1.360(5) . ?
C44 N3 1.365(5) . ?
O1 S1 1.480(3) . ?
O1 Er1 2.369(3) . ?
O2 S1 1.433(3) . ?
O3 S1 1.470(3) . ?
O3 Er2 2.359(2) . ?
O4 S2 1.478(3) . ?
O4 Er2 2.386(3) . ?
O5 S2 1.479(3) . ?
O5 Er2 2.443(3) . ?
O6 S2 1.431(3) . ?
O7 Er1 2.304(2) . ?
O7 Er2 2.326(2) . ?
O8 S3 1.462(3) . ?
O8 Er1 2.423(2) . ?
O9 S3 1.433(3) . ?
O10 S3 1.483(3) . ?
O10 Er2 2.356(2) . ?
O11 S4 1.446(3) . ?
O12 S4 1.469(3) . ?
O12 Er1 2.306(3) . ?
O13 S4 1.447(3) . ?
O14 Er1 2.363(2) . ?
O14 Er2 2.293(2) . ?
O15 H15A 0.8703 . ?
O15 H15B 0.8701 . ?
O15 Er1 2.323(3) . ?
O16 H16A 0.8500 . ?
O16 H16B 0.8507 . ?
O17 H17A 0.8508 . ?
O17 H17B 0.8501 . ?
O18 H18A 0.8505 . ?
O18 H18B 0.8506 . ?
S2 Er2 2.9980(9) . ?
Er1 Er2 3.7099(3) . ?
Er1 N3 2.523(3) . ?
Er1 N4 2.514(3) . ?
Er2 N1 2.494(3) . ?
Er2 N2 2.498(3) . ?

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
C2 C1 C10 122.4(3) . . ?
C2 C1 S1 122.0(3) . . ?
C10 C1 S1 115.6(3) . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 118.9(3) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 121.0(3) . 4_666 ?
C2 C3 C8 119.4(3) . . ?
C8 C3 C4 119.6(3) . 4_666 ?
C3 C4 H4 120.2 4_565 . ?
C5 C4 C3 119.6(3) . 4_565 ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 S2 120.4(3) . . ?
C6 C5 S2 118.4(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(4) 4_565 . ?
C7 C6 H6 119.9 4_565 . ?
C6 C7 H7 119.6 4_666 . ?
C6 C7 C8 120.8(4) 4_666 . ?
C8 C7 H7 119.6 . . ?
C3 C8 C9 119.9(3) . . ?
C7 C8 C3 118.5(3) . . ?
C7 C8 C9 121.5(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C1 118.6(3) . . ?
O7 C10 C1 117.9(3) . . ?
O7 C10 C9 123.5(3) . . ?
C12 C11 C20 118.3(3) . . ?
O14 C11 C12 123.3(3) . . ?
O14 C11 C20 118.5(3) . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.7(3) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 121.8(3) . 4_565 ?
C12 C13 C18 119.7(3) . . ?
C14 C13 C18 118.4(3) 4_565 . ?
C13 C14 H14 119.6 4_666 . ?
C15 C14 C13 120.7(4) . 4_666 ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.3(4) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 S4 119.0(3) . . ?
C17 C16 C15 121.3(3) . . ?
C17 C16 S4 119.5(3) . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.6(3) . 4_666 ?
C18 C17 H17 120.2 4_666 . ?
C17 C18 C13 119.6(3) 4_565 . ?
C19 C18 C13 118.8(3) . . ?
C19 C18 C17 121.7(3) . 4_565 ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C11 C20 S3 115.0(3) . . ?
C19 C20 C11 122.2(3) . . ?
C19 C20 S3 122.8(3) . . ?
C22 C21 H21 119.0 . . ?
N1 C21 H21 119.0 . . ?
N1 C21 C22 122.1(4) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 C21 119.4(4) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.3(4) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 123.3(4) . . ?
C23 C24 C32 117.4(4) . . ?
C32 C24 C25 119.4(4) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.0(4) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.2(4) . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 123.5(4) . . ?
C28 C27 C31 117.4(4) . . ?
C31 C27 C26 119.2(4) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 C27 119.2(4) . . ?
C29 C28 H28 120.4 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(4) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 118.3 . . ?
N2 C30 C29 123.4(4) . . ?
N2 C30 H30 118.3 . . ?
C27 C31 C32 119.4(4) . . ?
N2 C31 C27 122.7(4) . . ?
N2 C31 C32 117.9(3) . . ?
C24 C32 C31 119.8(4) . . ?
N1 C32 C24 122.4(4) . . ?
N1 C32 C31 117.8(3) . . ?
C34 C33 H33 118.3 . . ?
N3 C33 H33 118.3 . . ?
N3 C33 C34 123.4(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 C33 119.4(4) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.8(4) . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C37 123.6(4) . . ?
C35 C36 C44 117.4(4) . . ?
C44 C36 C37 119.0(4) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 C36 121.6(4) . . ?
C38 C37 H37 119.2 . . ?
C37 C38 H38 119.5 . . ?
C37 C38 C39 121.1(4) . . ?
C39 C38 H38 119.5 . . ?
C40 C39 C38 123.6(4) . . ?
C40 C39 C43 117.0(4) . . ?
C43 C39 C38 119.4(4) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 C39 120.2(4) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 120.4 . . ?
C40 C41 C42 119.1(4) . . ?
C42 C41 H41 120.4 . . ?
C41 C42 H42 118.4 . . ?
N4 C42 C41 123.3(4) . . ?
N4 C42 H42 118.4 . . ?
C39 C43 C44 119.3(4) . . ?
N4 C43 C39 122.5(4) . . ?
N4 C43 C44 118.2(3) . . ?
C36 C44 C43 119.6(4) . . ?
N3 C44 C36 122.6(4) . . ?
N3 C44 C43 117.8(3) . . ?
S1 O1 Er1 128.53(15) . . ?
S1 O3 Er2 125.10(14) . . ?
S2 O4 Er2 99.07(14) . . ?
S2 O5 Er2 96.61(13) . . ?
C10 O7 Er1 123.7(2) . . ?
C10 O7 Er2 116.8(2) . . ?
Er1 O7 Er2 106.49(9) . . ?
S3 O8 Er1 128.50(15) . . ?
S3 O10 Er2 125.58(15) . . ?
S4 O12 Er1 143.77(17) . . ?
C11 O14 Er1 116.6(2) . . ?
C11 O14 Er2 125.7(2) . . ?
Er2 O14 Er1 105.64(9) . . ?
H15A O15 H15B 108.3 . . ?
Er1 O15 H15A 111.0 . . ?
Er1 O15 H15B 109.7 . . ?
H16A O16 H16B 109.5 . . ?
H17A O17 H17B 109.4 . . ?
H18A O18 H18B 109.5 . . ?
O1 S1 C1 104.35(16) . . ?
O2 S1 C1 109.22(16) . . ?
O2 S1 O1 112.74(16) . . ?
O2 S1 O3 113.55(16) . . ?
O3 S1 C1 105.95(16) . . ?
O3 S1 O1 110.39(15) . . ?
C5 S2 Er2 115.13(13) . . ?
O4 S2 C5 106.64(17) . . ?
O4 S2 O5 105.62(16) . . ?
O4 S2 Er2 51.79(11) . . ?
O5 S2 C5 107.58(17) . . ?
O5 S2 Er2 54.04(11) . . ?
O6 S2 C5 107.93(17) . . ?
O6 S2 O4 113.61(18) . . ?
O6 S2 O5 115.01(18) . . ?
O6 S2 Er2 136.87(12) . . ?
O8 S3 C20 105.64(16) . . ?
O8 S3 O10 109.91(15) . . ?
O9 S3 C20 108.64(16) . . ?
O9 S3 O8 114.29(16) . . ?
O9 S3 O10 113.14(16) . . ?
O10 S3 C20 104.47(16) . . ?
O11 S4 C16 107.19(18) . . ?
O11 S4 O12 110.10(17) . . ?
O11 S4 O13 114.17(19) . . ?
O12 S4 C16 105.95(17) . . ?
O13 S4 C16 106.54(18) . . ?
O13 S4 O12 112.34(17) . . ?
O1 Er1 O8 143.72(9) . . ?
O1 Er1 Er2 74.93(6) . . ?
O1 Er1 N3 77.46(9) . . ?
O1 Er1 N4 140.53(10) . . ?
O7 Er1 O1 72.94(8) . . ?
O7 Er1 O8 75.90(8) . . ?
O7 Er1 O12 118.25(9) . . ?
O7 Er1 O14 73.46(8) . . ?
O7 Er1 O15 81.08(10) . . ?
O7 Er1 Er2 36.96(6) . . ?
O7 Er1 N3 139.80(9) . . ?
O7 Er1 N4 145.79(10) . . ?
O8 Er1 Er2 69.02(6) . . ?
O8 Er1 N3 117.96(9) . . ?
O8 Er1 N4 70.28(10) . . ?
O12 Er1 O1 73.88(9) . . ?
O12 Er1 O8 139.01(9) . . ?
O12 Er1 O14 146.56(9) . . ?
O12 Er1 O15 74.67(10) . . ?
O12 Er1 Er2 145.73(6) . . ?
O12 Er1 N3 77.45(10) . . ?
O12 Er1 N4 85.69(10) . . ?
O14 Er1 O1 81.15(9) . . ?
O14 Er1 O8 72.50(8) . . ?
O14 Er1 Er2 36.53(6) . . ?
O14 Er1 N3 75.66(9) . . ?
O14 Er1 N4 100.52(9) . . ?
O15 Er1 O1 121.98(10) . . ?
O15 Er1 O8 69.82(9) . . ?
O15 Er1 O14 138.51(9) . . ?
O15 Er1 Er2 111.28(8) . . ?
O15 Er1 N3 138.55(11) . . ?
O15 Er1 N4 82.64(11) . . ?
N3 Er1 Er2 109.09(7) . . ?
N4 Er1 Er2 128.08(8) . . ?
N4 Er1 N3 65.15(10) . . ?
O3 Er2 O4 74.04(9) . . ?
O3 Er2 O5 128.76(9) . . ?
O3 Er2 S2 102.06(6) . . ?
O3 Er2 Er1 72.78(6) . . ?
O3 Er2 N1 71.96(10) . . ?
O3 Er2 N2 123.91(9) . . ?
O4 Er2 O5 58.40(9) . . ?
O4 Er2 S2 29.14(7) . . ?
O4 Er2 Er1 119.92(7) . . ?
O4 Er2 N1 84.17(10) . . ?
O4 Er2 N2 132.86(10) . . ?
O5 Er2 S2 29.35(6) . . ?
O5 Er2 Er1 146.79(6) . . ?
O5 Er2 N1 84.61(9) . . ?
O5 Er2 N2 82.35(9) . . ?
O7 Er2 O3 76.57(8) . . ?
O7 Er2 O4 147.90(9) . . ?
O7 Er2 O5 153.51(9) . . ?
O7 Er2 O10 89.17(9) . . ?
O7 Er2 S2 174.95(6) . . ?
O7 Er2 Er1 36.55(6) . . ?
O7 Er2 N1 98.83(9) . . ?
O7 Er2 N2 75.37(9) . . ?
O10 Er2 O3 147.86(9) . . ?
O10 Er2 O4 109.29(9) . . ?
O10 Er2 O5 72.23(9) . . ?
O10 Er2 S2 89.61(7) . . ?
O10 Er2 Er1 78.62(6) . . ?
O10 Er2 N1 139.50(9) . . ?
O10 Er2 N2 78.31(9) . . ?
O14 Er2 O3 74.32(9) . . ?
O14 Er2 O4 85.46(9) . . ?
O14 Er2 O5 116.38(9) . . ?
O14 Er2 O7 74.35(8) . . ?
O14 Er2 O10 74.13(8) . . ?
O14 Er2 S2 100.60(6) . . ?
O14 Er2 Er1 37.84(6) . . ?
O14 Er2 N1 146.26(9) . . ?
O14 Er2 N2 138.90(9) . . ?
S2 Er2 Er1 138.415(19) . . ?
N1 Er2 S2 85.26(7) . . ?
N1 Er2 Er1 128.51(7) . . ?
N1 Er2 N2 65.77(10) . . ?
N2 Er2 S2 109.16(7) . . ?
N2 Er2 Er1 107.21(7) . . ?
C21 N1 C32 118.4(3) . . ?
C21 N1 Er2 122.7(3) . . ?
C32 N1 Er2 117.2(2) . . ?
C30 N2 C31 117.2(3) . . ?
C30 N2 Er2 124.5(3) . . ?
C31 N2 Er2 116.5(2) . . ?
C33 N3 C44 117.4(3) . . ?
C33 N3 Er1 123.7(3) . . ?
C44 N3 Er1 117.9(2) . . ?
C42 N4 C43 118.0(3) . . ?
C42 N4 Er1 122.8(3) . . ?
C43 N4 Er1 118.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -178.4(3) . . . 4_666 ?
C1 C2 C3 C8 3.0(5) . . . . ?
C1 C10 O7 Er1 74.5(4) . . . . ?
C1 C10 O7 Er2 -61.5(4) . . . . ?
C2 C1 C10 C9 -9.5(5) . . . . ?
C2 C1 C10 O7 168.8(3) . . . . ?
C2 C1 S1 O1 129.7(3) . . . . ?
C2 C1 S1 O2 9.0(4) . . . . ?
C2 C1 S1 O3 -113.7(3) . . . . ?
C2 C3 C8 C7 175.0(4) . . . . ?
C2 C3 C8 C9 -6.3(5) . . . . ?
C3 C4 C5 C6 -1.0(6) 4_565 . . . ?
C3 C4 C5 S2 -178.3(3) 4_565 . . . ?
C3 C8 C9 C10 1.6(6) . . . . ?
C4 C3 C8 C7 -3.6(5) 4_666 . . . ?
C4 C3 C8 C9 175.1(3) 4_666 . . . ?
C4 C5 C6 C7 2.5(6) . . . 4_565 ?
C4 C5 S2 O4 105.8(3) . . . . ?
C4 C5 S2 O5 -7.1(4) . . . . ?
C4 C5 S2 O6 -131.8(3) . . . . ?
C4 C5 S2 Er2 50.8(4) . . . . ?
C6 C5 S2 O4 -71.6(4) . . . . ?
C6 C5 S2 O5 175.5(3) . . . . ?
C6 C5 S2 O6 50.8(4) . . . . ?
C6 C5 S2 Er2 -126.6(3) . . . . ?
C6 C7 C8 C3 2.2(6) 4_666 . . . ?
C6 C7 C8 C9 -176.5(4) 4_666 . . . ?
C7 C8 C9 C10 -179.7(4) . . . . ?
C8 C9 C10 C1 6.0(5) . . . . ?
C8 C9 C10 O7 -172.2(3) . . . . ?
C9 C10 O7 Er1 -107.3(3) . . . . ?
C9 C10 O7 Er2 116.7(3) . . . . ?
C10 C1 C2 C3 4.9(5) . . . . ?
C10 C1 S1 O1 -49.4(3) . . . . ?
C10 C1 S1 O2 -170.2(3) . . . . ?
C10 C1 S1 O3 67.2(3) . . . . ?
C11 C12 C13 C14 -171.9(4) . . . 4_565 ?
C11 C12 C13 C18 3.1(6) . . . . ?
C11 C20 S3 O8 -62.7(3) . . . . ?
C11 C20 S3 O9 174.3(3) . . . . ?
C11 C20 S3 O10 53.3(3) . . . . ?
C12 C11 C20 C19 8.0(5) . . . . ?
C12 C11 C20 S3 -172.7(3) . . . . ?
C12 C11 O14 Er1 -111.4(3) . . . . ?
C12 C11 O14 Er2 111.6(3) . . . . ?
C12 C13 C18 C17 -173.5(3) . . . 4_565 ?
C12 C13 C18 C19 5.0(5) . . . . ?
C13 C14 C15 C16 -1.9(6) 4_666 . . . ?
C13 C18 C19 C20 -6.4(5) . . . . ?
C14 C13 C18 C17 1.7(5) 4_565 . . 4_565 ?
C14 C13 C18 C19 -179.8(4) 4_565 . . . ?
C14 C15 C16 C17 -1.7(6) . . . . ?
C14 C15 C16 S4 174.4(3) . . . . ?
C15 C16 C17 C18 3.4(6) . . . 4_666 ?
C15 C16 S4 O11 -101.8(3) . . . . ?
C15 C16 S4 O12 140.7(3) . . . . ?
C15 C16 S4 O13 20.9(4) . . . . ?
C17 C16 S4 O11 74.4(3) . . . . ?
C17 C16 S4 O12 -43.1(4) . . . . ?
C17 C16 S4 O13 -163.0(3) . . . . ?
C17 C18 C19 C20 172.0(3) 4_565 . . . ?
C18 C19 C20 C11 0.0(6) . . . . ?
C18 C19 C20 S3 -179.2(3) . . . . ?
C19 C20 S3 O8 116.6(3) . . . . ?
C19 C20 S3 O9 -6.5(4) . . . . ?
C19 C20 S3 O10 -127.5(3) . . . . ?
C20 C11 C12 C13 -9.4(5) . . . . ?
C20 C11 O14 Er1 67.1(4) . . . . ?
C20 C11 O14 Er2 -69.9(4) . . . . ?
C21 C22 C23 C24 -1.0(8) . . . . ?
C22 C21 N1 C32 -0.4(6) . . . . ?
C22 C21 N1 Er2 -165.5(3) . . . . ?
C22 C23 C24 C25 179.2(5) . . . . ?
C22 C23 C24 C32 -0.8(7) . . . . ?
C23 C24 C25 C26 178.5(5) . . . . ?
C23 C24 C32 C31 -177.6(4) . . . . ?
C23 C24 C32 N1 2.1(6) . . . . ?
C24 C25 C26 C27 -1.4(7) . . . . ?
C24 C32 N1 C21 -1.5(6) . . . . ?
C24 C32 N1 Er2 164.4(3) . . . . ?
C25 C24 C32 C31 2.4(6) . . . . ?
C25 C24 C32 N1 -177.9(4) . . . . ?
C25 C26 C27 C28 -175.8(5) . . . . ?
C25 C26 C27 C31 3.3(7) . . . . ?
C26 C27 C28 C29 178.7(4) . . . . ?
C26 C27 C31 C32 -2.2(6) . . . . ?
C26 C27 C31 N2 179.1(4) . . . . ?
C27 C28 C29 C30 1.7(8) . . . . ?
C27 C31 C32 C24 -0.6(6) . . . . ?
C27 C31 C32 N1 179.8(4) . . . . ?
C27 C31 N2 C30 2.6(6) . . . . ?
C27 C31 N2 Er2 -163.2(3) . . . . ?
C28 C27 C31 C32 176.9(4) . . . . ?
C28 C27 C31 N2 -1.8(6) . . . . ?
C28 C29 C30 N2 -0.9(8) . . . . ?
C29 C30 N2 C31 -1.2(6) . . . . ?
C29 C30 N2 Er2 163.4(4) . . . . ?
C31 C27 C28 C29 -0.4(7) . . . . ?
C31 C32 N1 C21 178.2(4) . . . . ?
C31 C32 N1 Er2 -15.9(4) . . . . ?
C32 C24 C25 C26 -1.5(7) . . . . ?
C32 C31 N2 C30 -176.1(4) . . . . ?
C32 C31 N2 Er2 18.0(4) . . . . ?
C33 C34 C35 C36 -1.9(7) . . . . ?
C34 C33 N3 C44 2.2(6) . . . . ?
C34 C33 N3 Er1 -165.7(3) . . . . ?
C34 C35 C36 C37 -178.7(4) . . . . ?
C34 C35 C36 C44 1.1(6) . . . . ?
C35 C36 C37 C38 179.2(4) . . . . ?
C35 C36 C44 C43 -179.8(4) . . . . ?
C35 C36 C44 N3 1.4(6) . . . . ?
C36 C37 C38 C39 -0.2(7) . . . . ?
C36 C44 N3 C33 -3.0(5) . . . . ?
C36 C44 N3 Er1 165.6(3) . . . . ?
C37 C36 C44 C43 -0.1(6) . . . . ?
C37 C36 C44 N3 -178.8(4) . . . . ?
C37 C38 C39 C40 -178.5(5) . . . . ?
C37 C38 C39 C43 1.5(7) . . . . ?
C38 C39 C40 C41 -178.8(5) . . . . ?
C38 C39 C43 C44 -2.1(6) . . . . ?
C38 C39 C43 N4 177.7(4) . . . . ?
C39 C40 C41 C42 0.4(8) . . . . ?
C39 C43 C44 C36 1.4(5) . . . . ?
C39 C43 C44 N3 -179.8(3) . . . . ?
C39 C43 N4 C42 1.6(6) . . . . ?
C39 C43 N4 Er1 -167.0(3) . . . . ?
C40 C39 C43 C44 178.0(4) . . . . ?
C40 C39 C43 N4 -2.2(6) . . . . ?
C40 C41 C42 N4 -1.1(8) . . . . ?
C41 C42 N4 C43 0.1(7) . . . . ?
C41 C42 N4 Er1 168.2(4) . . . . ?
C43 C39 C40 C41 1.2(7) . . . . ?
C43 C44 N3 C33 178.2(3) . . . . ?
C43 C44 N3 Er1 -13.2(4) . . . . ?
C44 C36 C37 C38 -0.6(6) . . . . ?
C44 C43 N4 C42 -178.6(4) . . . . ?
C44 C43 N4 Er1 12.8(4) . . . . ?
O14 C11 C12 C13 169.0(3) . . . . ?
O14 C11 C20 C19 -170.5(3) . . . . ?
O14 C11 C20 S3 8.8(4) . . . . ?
S1 C1 C2 C3 -174.2(3) . . . . ?
S1 C1 C10 C9 169.6(3) . . . . ?
S1 C1 C10 O7 -12.1(4) . . . . ?
S2 C5 C6 C7 179.9(3) . . . 4_565 ?
S4 C16 C17 C18 -172.6(3) . . . 4_666 ?
Er1 O1 S1 C1 62.5(2) . . . . ?
Er1 O1 S1 O2 -179.15(17) . . . . ?
Er1 O1 S1 O3 -51.0(2) . . . . ?
Er1 O8 S3 C20 41.5(2) . . . . ?
Er1 O8 S3 O9 160.82(16) . . . . ?
Er1 O8 S3 O10 -70.7(2) . . . . ?
Er1 O12 S4 C16 -76.8(3) . . . . ?
Er1 O12 S4 O11 167.6(2) . . . . ?
Er1 O12 S4 O13 39.1(3) . . . . ?
Er2 O3 S1 C1 -44.5(2) . . . . ?
Er2 O3 S1 O1 67.9(2) . . . . ?
Er2 O3 S1 O2 -164.38(16) . . . . ?
Er2 O4 S2 C5 -109.19(15) . . . . ?
Er2 O4 S2 O5 5.07(16) . . . . ?
Er2 O4 S2 O6 132.04(15) . . . . ?
Er2 O5 S2 C5 108.69(15) . . . . ?
Er2 O5 S2 O4 -4.92(16) . . . . ?
Er2 O5 S2 O6 -131.03(15) . . . . ?
Er2 O10 S3 C20 -66.0(2) . . . . ?
Er2 O10 S3 O8 46.9(2) . . . . ?
Er2 O10 S3 O9 175.99(16) . . . . ?
N1 C21 C22 C23 1.7(7) . . . . ?
N2 C31 C32 C24 178.2(3) . . . . ?
N2 C31 C32 N1 -1.5(5) . . . . ?
N3 C33 C34 C35 0.2(7) . . . . ?
N4 C43 C44 C36 -178.5(3) . . . . ?
N4 C43 C44 N3 0.3(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Phase3-Ho
_database_code_depnum_ccdc_archive 'CCDC 1477860'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2015-10-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H28 Ho2 N4 O15 S4, 3(H2 O)'
_chemical_formula_sum            'C44 H34 Ho2 N4 O18 S4'
_chemical_formula_weight         1364.85
_chemical_melting_point          ?
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'
Ho Ho -0.2175 4.6783 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2341(3)
_cell_length_b                   17.0149(4)
_cell_length_c                   18.8852(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.9910(10)
_cell_angle_gamma                90
_cell_volume                     4517.64(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8464
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.877
_shelx_estimated_absorpt_T_min   0.451
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0898 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.8359.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2672
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.036
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32602
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.410
_diffrn_reflns_theta_min         1.620
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7378
_reflns_number_total             9231
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 20015)'
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+0.5006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0658
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B,O17,H17A,H17B,O18,H18A,H18B)
2.b Rotating group:
 O15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C -0.2375(3) 0.2605(2) 0.2533(2) 0.0186(9) Uani 1 1 d . . . . .
C2 C -0.2086(3) 0.2678(2) 0.3251(2) 0.0205(9) Uani 1 1 d . . . . .
H2 H -0.1932 0.3170 0.3450 0.025 Uiso 1 1 calc R . . . .
C3 C -0.2021(3) 0.2008(2) 0.3694(2) 0.0190(9) Uani 1 1 d . . . . .
C4 C -0.6750(3) 0.2930(2) -0.0555(2) 0.0208(9) Uani 1 1 d . . . . .
H4 H -0.6646 0.2439 -0.0342 0.025 Uiso 1 1 calc R . . . .
C5 C -0.6644(3) 0.3595(2) -0.0145(2) 0.0218(9) Uani 1 1 d . . . . .
C6 C -0.6781(3) 0.4344(3) -0.0461(2) 0.0308(11) Uani 1 1 d . . . . .
H6 H -0.6678 0.4793 -0.0179 0.037 Uiso 1 1 calc R . . . .
C7 C -0.2066(3) 0.0588(3) 0.3820(2) 0.0304(11) Uani 1 1 d . . . . .
H7 H -0.2169 0.0091 0.3617 0.036 Uiso 1 1 calc R . . . .
C8 C -0.2207(3) 0.1259(2) 0.3374(2) 0.0209(9) Uani 1 1 d . . . . .
C9 C -0.2557(3) 0.1201(2) 0.2632(2) 0.0211(9) Uani 1 1 d . . . . .
H9 H -0.2702 0.0711 0.2426 0.025 Uiso 1 1 calc R . . . .
C10 C -0.2683(3) 0.1866(2) 0.2213(2) 0.0171(9) Uani 1 1 d . . . . .
C11 C -0.4103(3) 0.2856(2) -0.0387(2) 0.0185(9) Uani 1 1 d . . . . .
C12 C -0.4122(3) 0.3537(2) -0.0768(2) 0.0218(9) Uani 1 1 d . . . . .
H12 H -0.3951 0.4005 -0.0529 0.026 Uiso 1 1 calc R . . . .
C13 C -0.4397(3) 0.3544(2) -0.1518(2) 0.0208(9) Uani 1 1 d . . . . .
C14 C 0.0693(3) 0.0774(3) 0.3065(2) 0.0313(11) Uani 1 1 d . . . . .
H14 H 0.0853 0.0297 0.3293 0.038 Uiso 1 1 calc R . . . .
C15 C 0.0547(3) 0.0809(3) 0.2331(2) 0.0288(10) Uani 1 1 d . . . . .
H15 H 0.0630 0.0362 0.2065 0.035 Uiso 1 1 calc R . . . .
C16 C 0.0273(3) 0.1518(2) 0.1984(2) 0.0230(9) Uani 1 1 d . . . . .
C17 C 0.0128(3) 0.2180(2) 0.2361(2) 0.0223(9) Uani 1 1 d . . . . .
H17 H -0.0087 0.2638 0.2120 0.027 Uiso 1 1 calc R . . . .
C18 C -0.4697(3) 0.2831(2) -0.1885(2) 0.0203(9) Uani 1 1 d . . . . .
C19 C -0.4785(3) 0.2150(2) -0.1472(2) 0.0219(9) Uani 1 1 d . . . . .
H19 H -0.5041 0.1693 -0.1693 0.026 Uiso 1 1 calc R . . . .
C20 C -0.4494(3) 0.2163(2) -0.0751(2) 0.0165(8) Uani 1 1 d . . . . .
C21 C -0.4663(3) 0.3695(3) 0.2728(2) 0.0363(12) Uani 1 1 d . . . . .
H21 H -0.4694 0.4097 0.2392 0.044 Uiso 1 1 calc R . . . .
C22 C -0.4556(4) 0.3894(3) 0.3455(3) 0.0478(14) Uani 1 1 d . . . . .
H22 H -0.4530 0.4418 0.3597 0.057 Uiso 1 1 calc R . . . .
C23 C -0.4490(4) 0.3310(4) 0.3949(3) 0.0488(14) Uani 1 1 d . . . . .
H23 H -0.4408 0.3433 0.4434 0.059 Uiso 1 1 calc R . . . .
C24 C -0.4544(3) 0.2520(3) 0.3733(2) 0.0333(12) Uani 1 1 d . . . . .
C25 C -0.4468(3) 0.1884(3) 0.4229(3) 0.0429(13) Uani 1 1 d . . . . .
H25 H -0.4364 0.1984 0.4719 0.051 Uiso 1 1 calc R . . . .
C26 C -0.4546(3) 0.1137(3) 0.3987(3) 0.0421(13) Uani 1 1 d . . . . .
H26 H -0.4486 0.0727 0.4317 0.051 Uiso 1 1 calc R . . . .
C27 C -0.4716(3) 0.0958(3) 0.3240(2) 0.0312(11) Uani 1 1 d . . . . .
C28 C -0.4864(4) 0.0196(3) 0.2964(3) 0.0441(14) Uani 1 1 d . . . . .
H28 H -0.4845 -0.0231 0.3273 0.053 Uiso 1 1 calc R . . . .
C29 C -0.5036(4) 0.0082(3) 0.2246(3) 0.0444(13) Uani 1 1 d . . . . .
H29 H -0.5143 -0.0421 0.2058 0.053 Uiso 1 1 calc R . . . .
C30 C -0.5048(3) 0.0723(3) 0.1794(3) 0.0322(11) Uani 1 1 d . . . . .
H30 H -0.5156 0.0631 0.1303 0.039 Uiso 1 1 calc R . . . .
C31 C -0.4771(3) 0.1580(3) 0.2740(2) 0.0226(9) Uani 1 1 d . . . . .
C32 C -0.4673(3) 0.2372(3) 0.2991(2) 0.0233(10) Uani 1 1 d . . . . .
C33 C -0.1748(3) 0.3854(3) -0.0064(3) 0.0319(11) Uani 1 1 d . . . . .
H33 H -0.1662 0.3969 0.0423 0.038 Uiso 1 1 calc R . . . .
C34 C -0.1726(3) 0.4474(3) -0.0544(3) 0.0367(12) Uani 1 1 d . . . . .
H34 H -0.1621 0.4986 -0.0378 0.044 Uiso 1 1 calc R . . . .
C35 C -0.1860(3) 0.4318(3) -0.1263(3) 0.0380(13) Uani 1 1 d . . . . .
H35 H -0.1874 0.4726 -0.1593 0.046 Uiso 1 1 calc R . . . .
C36 C -0.1975(3) 0.3542(3) -0.1499(2) 0.0276(10) Uani 1 1 d . . . . .
C37 C -0.2104(3) 0.3324(3) -0.2242(3) 0.0401(13) Uani 1 1 d . . . . .
H37 H -0.2118 0.3715 -0.2588 0.048 Uiso 1 1 calc R . . . .
C38 C -0.2203(3) 0.2576(3) -0.2449(3) 0.0417(13) Uani 1 1 d . . . . .
H38 H -0.2273 0.2454 -0.2935 0.050 Uiso 1 1 calc R . . . .
C39 C -0.2203(3) 0.1955(3) -0.1934(2) 0.0314(11) Uani 1 1 d . . . . .
C40 C -0.2297(4) 0.1158(3) -0.2119(3) 0.0501(15) Uani 1 1 d . . . . .
H40 H -0.2361 0.1008 -0.2598 0.060 Uiso 1 1 calc R . . . .
C41 C -0.2295(4) 0.0610(3) -0.1607(3) 0.0500(15) Uani 1 1 d . . . . .
H41 H -0.2346 0.0080 -0.1727 0.060 Uiso 1 1 calc R . . . .
C42 C -0.2216(3) 0.0848(3) -0.0894(3) 0.0387(12) Uani 1 1 d . . . . .
H42 H -0.2229 0.0463 -0.0545 0.046 Uiso 1 1 calc R . . . .
C43 C -0.2106(3) 0.2147(3) -0.1202(2) 0.0233(10) Uani 1 1 d . . . . .
C44 C -0.1985(3) 0.2948(3) -0.0977(2) 0.0237(10) Uani 1 1 d . . . . .
O1 O -0.18679(19) 0.30970(16) 0.13671(14) 0.0242(7) Uani 1 1 d . . . . .
O2 O -0.1897(2) 0.40513(17) 0.23161(15) 0.0294(7) Uani 1 1 d . . . . .
O3 O -0.33765(18) 0.35492(16) 0.16556(14) 0.0227(6) Uani 1 1 d . . . . .
O4 O -0.52783(19) 0.38050(17) 0.09287(15) 0.0307(7) Uani 1 1 d . . . . .
O5 O -0.62524(19) 0.27021(17) 0.09893(15) 0.0251(7) Uani 1 1 d . . . . .
O6 O -0.6913(2) 0.40123(19) 0.11253(16) 0.0400(9) Uani 1 1 d . . . . .
O7 O -0.31041(18) 0.18663(16) 0.15222(13) 0.0190(6) Uani 1 1 d . . . . .
O8 O -0.35902(18) 0.11480(16) 0.01041(14) 0.0225(6) Uani 1 1 d . . . . .
O9 O -0.50594(19) 0.07265(16) -0.06240(15) 0.0265(7) Uani 1 1 d . . . . .
O10 O -0.50862(18) 0.16262(16) 0.03725(14) 0.0223(6) Uani 1 1 d . . . . .
O11 O 0.1039(2) 0.1949(2) 0.08841(16) 0.0394(8) Uani 1 1 d . . . . .
O12 O -0.06558(18) 0.20481(17) 0.07870(15) 0.0270(7) Uani 1 1 d . . . . .
O13 O 0.0076(2) 0.07588(18) 0.07774(16) 0.0359(8) Uani 1 1 d . . . . .
O14 O -0.37084(18) 0.27950(16) 0.03068(14) 0.0202(6) Uani 1 1 d . . . . .
O15 O -0.1858(2) 0.07425(17) 0.08455(17) 0.0357(8) Uani 1 1 d . . . . .
H15A H -0.1905 0.0640 0.1290 0.054 Uiso 1 1 d GR . . . .
H15B H -0.1270 0.0668 0.0788 0.054 Uiso 1 1 d GR . . . .
O16 O 0.0912(2) 0.37082(17) 0.1075(3) 0.146(3) Uani 1 1 d . . . . .
H16A H 0.0954 0.3765 0.1526 0.219 Uiso 1 1 d G . . . .
H16B H 0.1350 0.3971 0.0925 0.219 Uiso 1 1 d G . . . .
O17 O 0.7116(2) 0.94183(16) 0.0644(2) 0.0716(13) Uani 1 1 d G . . . .
H17A H 0.6877 0.9569 0.1007 0.107 Uiso 1 1 d G . . . .
H17B H 0.6912 0.9709 0.0287 0.107 Uiso 1 1 d G . . . .
O18 O 0.2737(2) 0.11533(14) 0.0730(2) 0.0742(13) Uani 1 1 d G . . . .
H18A H 0.2187 0.1316 0.0781 0.111 Uiso 1 1 d G . . . .
H18B H 0.3099 0.1544 0.0695 0.111 Uiso 1 1 d G . . . .
S1 S -0.23717(7) 0.33977(6) 0.19392(5) 0.0201(2) Uani 1 1 d . . . . .
S2 S -0.62789(7) 0.35390(6) 0.07868(5) 0.0242(2) Uani 1 1 d . . . . .
S3 S -0.45684(7) 0.13402(6) -0.01977(5) 0.0193(2) Uani 1 1 d . . . . .
S4 S 0.01880(7) 0.15605(7) 0.10400(6) 0.0256(2) Uani 1 1 d . . . . .
Ho1 Ho -0.22982(2) 0.20360(2) 0.05611(2) 0.01891(6) Uani 1 1 d . . . . .
Ho2 Ho -0.45201(2) 0.25765(2) 0.12514(2) 0.01824(6) Uani 1 1 d . . . . .
N1 N -0.4722(2) 0.2954(2) 0.24962(18) 0.0241(8) Uani 1 1 d . . . . .
N2 N -0.4917(2) 0.1460(2) 0.20157(18) 0.0228(8) Uani 1 1 d . . . . .
N3 N -0.1886(2) 0.3112(2) -0.02622(18) 0.0228(8) Uani 1 1 d . . . . .
N4 N -0.2123(2) 0.1591(2) -0.06854(19) 0.0279(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.359(5) . ?
C1 C10 1.434(5) . ?
C1 S1 1.755(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.408(5) . ?
C3 C4 1.413(5) 4_666 ?
C3 C8 1.417(6) . ?
C4 C3 1.413(5) 4_565 ?
C4 H4 0.9300 . ?
C4 C5 1.367(5) . ?
C5 C6 1.408(6) . ?
C5 S2 1.758(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.360(6) 4_565 ?
C7 C6 1.360(6) 4_666 ?
C7 H7 0.9300 . ?
C7 C8 1.413(6) . ?
C8 C9 1.416(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.376(5) . ?
C10 O7 1.348(4) . ?
C11 C12 1.362(5) . ?
C11 C20 1.433(6) . ?
C11 O14 1.346(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.409(5) . ?
C13 C14 1.419(6) 4_565 ?
C13 C18 1.430(6) . ?
C14 C13 1.419(6) 4_666 ?
C14 H14 0.9300 . ?
C14 C15 1.370(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(6) . ?
C16 C17 1.366(6) . ?
C16 S4 1.769(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.406(5) 4_666 ?
C18 C17 1.405(5) 4_565 ?
C18 C19 1.414(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.360(5) . ?
C20 S3 1.759(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.399(6) . ?
C21 N1 1.333(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.357(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.403(7) . ?
C24 C25 1.423(7) . ?
C24 C32 1.407(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.350(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.426(7) . ?
C27 C28 1.402(7) . ?
C27 C31 1.412(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.353(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.382(6) . ?
C30 H30 0.9300 . ?
C30 N2 1.327(5) . ?
C31 C32 1.427(6) . ?
C31 N2 1.367(5) . ?
C32 N1 1.356(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.394(6) . ?
C33 N3 1.323(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.368(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.394(7) . ?
C36 C37 1.435(6) . ?
C36 C44 1.413(6) . ?
C37 H37 0.9300 . ?
C37 C38 1.333(7) . ?
C38 H38 0.9300 . ?
C38 C39 1.436(7) . ?
C39 C40 1.401(7) . ?
C39 C43 1.406(6) . ?
C40 H40 0.9300 . ?
C40 C41 1.342(7) . ?
C41 H41 0.9300 . ?
C41 C42 1.394(6) . ?
C42 H42 0.9300 . ?
C42 N4 1.324(6) . ?
C43 C44 1.429(6) . ?
C43 N4 1.363(5) . ?
C44 N3 1.365(5) . ?
O1 S1 1.478(3) . ?
O1 Ho1 2.379(3) . ?
O2 S1 1.432(3) . ?
O3 S1 1.470(3) . ?
O3 Ho2 2.363(3) . ?
O4 S2 1.479(3) . ?
O4 Ho2 2.387(3) . ?
O5 S2 1.474(3) . ?
O5 Ho2 2.447(3) . ?
O6 S2 1.432(3) . ?
O7 Ho1 2.312(3) . ?
O7 Ho2 2.337(3) . ?
O8 S3 1.457(3) . ?
O8 Ho1 2.432(3) . ?
O9 S3 1.432(3) . ?
O10 S3 1.479(3) . ?
O10 Ho2 2.367(3) . ?
O11 S4 1.449(3) . ?
O12 S4 1.476(3) . ?
O12 Ho1 2.310(3) . ?
O13 S4 1.452(3) . ?
O14 Ho1 2.372(3) . ?
O14 Ho2 2.302(3) . ?
O15 H15A 0.8708 . ?
O15 H15B 0.8693 . ?
O15 Ho1 2.328(3) . ?
O16 H16A 0.8498 . ?
O16 H16B 0.8502 . ?
O17 H17A 0.8505 . ?
O17 H17B 0.8500 . ?
O18 H18A 0.8498 . ?
O18 H18B 0.8497 . ?
S2 Ho2 3.0055(10) . ?
Ho1 Ho2 3.7197(3) . ?
Ho1 N3 2.530(3) . ?
Ho1 N4 2.522(4) . ?
Ho2 N1 2.496(3) . ?
Ho2 N2 2.503(3) . ?

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
C2 C1 C10 121.7(4) . . ?
C2 C1 S1 122.5(3) . . ?
C10 C1 S1 115.8(3) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.1(4) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 121.2(4) . 4_666 ?
C2 C3 C8 118.9(4) . . ?
C4 C3 C8 119.9(4) 4_666 . ?
C3 C4 H4 120.2 4_565 . ?
C5 C4 C3 119.7(4) . 4_565 ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.9(4) . . ?
C4 C5 S2 120.8(3) . . ?
C6 C5 S2 118.3(3) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0(4) 4_565 . ?
C7 C6 H6 120.0 4_565 . ?
C6 C7 H7 119.4 4_666 . ?
C6 C7 C8 121.2(4) 4_666 . ?
C8 C7 H7 119.4 . . ?
C7 C8 C3 118.2(4) . . ?
C7 C8 C9 121.9(4) . . ?
C9 C8 C3 119.8(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(4) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C1 118.3(4) . . ?
O7 C10 C1 118.0(3) . . ?
O7 C10 C9 123.7(4) . . ?
C12 C11 C20 118.2(4) . . ?
O14 C11 C12 123.4(4) . . ?
O14 C11 C20 118.4(3) . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.3(4) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C14 122.0(4) . 4_565 ?
C12 C13 C18 119.6(4) . . ?
C14 C13 C18 118.1(4) 4_565 . ?
C13 C14 H14 119.6 4_666 . ?
C15 C14 C13 120.8(4) . 4_666 ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.0(4) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 S4 118.6(3) . . ?
C17 C16 C15 121.3(4) . . ?
C17 C16 S4 120.0(3) . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(4) . 4_666 ?
C18 C17 H17 120.0 4_666 . ?
C17 C18 C13 119.6(4) 4_565 . ?
C17 C18 C19 122.1(4) 4_565 . ?
C19 C18 C13 118.2(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19 120.0 . . ?
C11 C20 S3 115.1(3) . . ?
C19 C20 C11 121.9(4) . . ?
C19 C20 S3 123.0(3) . . ?
C22 C21 H21 118.5 . . ?
N1 C21 H21 118.5 . . ?
N1 C21 C22 122.9(5) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.8(5) . . ?
C23 C22 H22 120.6 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.5(5) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 122.7(5) . . ?
C23 C24 C32 117.0(4) . . ?
C32 C24 C25 120.3(5) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 119.9(5) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.1 . . ?
C25 C26 C27 121.9(5) . . ?
C27 C26 H26 119.1 . . ?
C28 C27 C26 124.0(4) . . ?
C28 C27 C31 117.0(4) . . ?
C31 C27 C26 119.0(4) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 119.9(5) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 120.4 . . ?
C28 C29 C30 119.2(5) . . ?
C30 C29 H29 120.4 . . ?
C29 C30 H30 117.9 . . ?
N2 C30 C29 124.3(5) . . ?
N2 C30 H30 117.9 . . ?
C27 C31 C32 119.5(4) . . ?
N2 C31 C27 122.8(4) . . ?
N2 C31 C32 117.7(4) . . ?
C24 C32 C31 119.3(4) . . ?
N1 C32 C24 122.7(4) . . ?
N1 C32 C31 117.9(4) . . ?
C34 C33 H33 118.1 . . ?
N3 C33 H33 118.1 . . ?
N3 C33 C34 123.7(5) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.0(5) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 120.3 . . ?
C34 C35 C36 119.5(4) . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C37 123.2(4) . . ?
C35 C36 C44 117.9(4) . . ?
C44 C36 C37 118.9(4) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 C36 121.7(5) . . ?
C38 C37 H37 119.2 . . ?
C37 C38 H38 119.5 . . ?
C37 C38 C39 121.0(5) . . ?
C39 C38 H38 119.5 . . ?
C40 C39 C38 123.6(4) . . ?
C40 C39 C43 117.4(4) . . ?
C43 C39 C38 119.0(4) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 C39 120.2(5) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 120.5 . . ?
C40 C41 C42 119.0(5) . . ?
C42 C41 H41 120.5 . . ?
C41 C42 H42 118.2 . . ?
N4 C42 C41 123.6(5) . . ?
N4 C42 H42 118.2 . . ?
C39 C43 C44 120.1(4) . . ?
N4 C43 C39 122.2(4) . . ?
N4 C43 C44 117.7(4) . . ?
C36 C44 C43 119.2(4) . . ?
N3 C44 C36 122.2(4) . . ?
N3 C44 C43 118.6(4) . . ?
S1 O1 Ho1 128.63(16) . . ?
S1 O3 Ho2 125.24(16) . . ?
S2 O4 Ho2 99.36(15) . . ?
S2 O5 Ho2 96.95(14) . . ?
C10 O7 Ho1 124.0(2) . . ?
C10 O7 Ho2 116.7(2) . . ?
Ho1 O7 Ho2 106.29(10) . . ?
S3 O8 Ho1 128.53(16) . . ?
S3 O10 Ho2 125.57(15) . . ?
S4 O12 Ho1 143.46(18) . . ?
C11 O14 Ho1 116.8(2) . . ?
C11 O14 Ho2 125.6(2) . . ?
Ho2 O14 Ho1 105.46(10) . . ?
H15A O15 H15B 108.3 . . ?
Ho1 O15 H15A 110.7 . . ?
Ho1 O15 H15B 109.8 . . ?
H16A O16 H16B 109.5 . . ?
H17A O17 H17B 109.5 . . ?
H18A O18 H18B 109.5 . . ?
O1 S1 C1 104.56(18) . . ?
O2 S1 C1 109.09(18) . . ?
O2 S1 O1 112.75(17) . . ?
O2 S1 O3 113.70(17) . . ?
O3 S1 C1 105.57(17) . . ?
O3 S1 O1 110.49(16) . . ?
C5 S2 Ho2 115.09(14) . . ?
O4 S2 C5 106.87(19) . . ?
O4 S2 Ho2 51.60(11) . . ?
O5 S2 C5 107.70(18) . . ?
O5 S2 O4 105.30(16) . . ?
O5 S2 Ho2 53.93(11) . . ?
O6 S2 C5 107.95(18) . . ?
O6 S2 O4 113.79(19) . . ?
O6 S2 O5 114.82(19) . . ?
O6 S2 Ho2 136.90(13) . . ?
O8 S3 C20 105.57(17) . . ?
O8 S3 O10 110.09(16) . . ?
O9 S3 C20 108.40(18) . . ?
O9 S3 O8 114.13(17) . . ?
O9 S3 O10 113.22(16) . . ?
O10 S3 C20 104.67(17) . . ?
O11 S4 C16 107.19(19) . . ?
O11 S4 O12 109.96(18) . . ?
O11 S4 O13 114.17(19) . . ?
O12 S4 C16 105.85(18) . . ?
O13 S4 C16 107.0(2) . . ?
O13 S4 O12 112.16(17) . . ?
O1 Ho1 O8 143.46(9) . . ?
O1 Ho1 Ho2 74.70(6) . . ?
O1 Ho1 N3 77.45(10) . . ?
O1 Ho1 N4 140.53(11) . . ?
O7 Ho1 O1 72.68(9) . . ?
O7 Ho1 O8 76.14(9) . . ?
O7 Ho1 O14 73.67(9) . . ?
O7 Ho1 O15 81.35(11) . . ?
O7 Ho1 Ho2 37.09(6) . . ?
O7 Ho1 N3 139.84(10) . . ?
O7 Ho1 N4 145.98(10) . . ?
O8 Ho1 Ho2 68.95(6) . . ?
O8 Ho1 N3 117.83(10) . . ?
O8 Ho1 N4 70.23(10) . . ?
O12 Ho1 O1 73.93(10) . . ?
O12 Ho1 O7 117.92(9) . . ?
O12 Ho1 O8 139.33(9) . . ?
O12 Ho1 O14 146.36(10) . . ?
O12 Ho1 O15 74.78(10) . . ?
O12 Ho1 Ho2 145.54(7) . . ?
O12 Ho1 N3 77.38(10) . . ?
O12 Ho1 N4 85.99(10) . . ?
O14 Ho1 O1 80.88(9) . . ?
O14 Ho1 O8 72.38(9) . . ?
O14 Ho1 Ho2 36.62(6) . . ?
O14 Ho1 N3 75.64(10) . . ?
O14 Ho1 N4 100.29(10) . . ?
O15 Ho1 O1 122.46(10) . . ?
O15 Ho1 O8 69.88(9) . . ?
O15 Ho1 O14 138.61(10) . . ?
O15 Ho1 Ho2 111.47(8) . . ?
O15 Ho1 N3 138.24(11) . . ?
O15 Ho1 N4 82.47(11) . . ?
N3 Ho1 Ho2 109.16(7) . . ?
N4 Ho1 Ho2 127.95(8) . . ?
N4 Ho1 N3 65.01(11) . . ?
O3 Ho2 O4 74.35(9) . . ?
O3 Ho2 O5 128.73(9) . . ?
O3 Ho2 O10 147.89(9) . . ?
O3 Ho2 S2 102.30(7) . . ?
O3 Ho2 Ho1 72.89(7) . . ?
O3 Ho2 N1 71.97(10) . . ?
O3 Ho2 N2 123.47(10) . . ?
O4 Ho2 O5 58.06(9) . . ?
O4 Ho2 S2 29.04(7) . . ?
O4 Ho2 Ho1 120.15(7) . . ?
O4 Ho2 N1 84.34(11) . . ?
O4 Ho2 N2 132.68(10) . . ?
O5 Ho2 S2 29.12(7) . . ?
O5 Ho2 Ho1 146.69(7) . . ?
O5 Ho2 N1 84.70(10) . . ?
O5 Ho2 N2 82.64(10) . . ?
O7 Ho2 O3 76.38(9) . . ?
O7 Ho2 O4 148.06(9) . . ?
O7 Ho2 O5 153.71(9) . . ?
O7 Ho2 O10 89.29(9) . . ?
O7 Ho2 S2 174.98(7) . . ?
O7 Ho2 Ho1 36.62(6) . . ?
O7 Ho2 N1 98.57(10) . . ?
O7 Ho2 N2 75.28(10) . . ?
O10 Ho2 O4 109.17(9) . . ?
O10 Ho2 O5 72.30(9) . . ?
O10 Ho2 S2 89.47(7) . . ?
O10 Ho2 Ho1 78.48(6) . . ?
O10 Ho2 N1 139.42(10) . . ?
O10 Ho2 N2 78.64(10) . . ?
O14 Ho2 O3 74.54(9) . . ?
O14 Ho2 O4 85.55(10) . . ?
O14 Ho2 O5 116.17(9) . . ?
O14 Ho2 O7 74.51(9) . . ?
O14 Ho2 O10 73.98(9) . . ?
O14 Ho2 S2 100.48(7) . . ?
O14 Ho2 Ho1 37.92(6) . . ?
O14 Ho2 N1 146.48(10) . . ?
O14 Ho2 N2 139.04(10) . . ?
S2 Ho2 Ho1 138.37(2) . . ?
N1 Ho2 S2 85.51(8) . . ?
N1 Ho2 Ho1 128.51(8) . . ?
N1 Ho2 N2 65.33(11) . . ?
N2 Ho2 S2 109.22(8) . . ?
N2 Ho2 Ho1 107.17(7) . . ?
C21 N1 C32 118.1(4) . . ?
C21 N1 Ho2 122.8(3) . . ?
C32 N1 Ho2 117.4(3) . . ?
C30 N2 C31 116.7(4) . . ?
C30 N2 Ho2 124.7(3) . . ?
C31 N2 Ho2 116.8(3) . . ?
C33 N3 C44 117.6(4) . . ?
C33 N3 Ho1 123.7(3) . . ?
C44 N3 Ho1 117.5(3) . . ?
C42 N4 C43 117.5(4) . . ?
C42 N4 Ho1 123.0(3) . . ?
C43 N4 Ho1 118.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -178.1(4) . . . 4_666 ?
C1 C2 C3 C8 3.5(6) . . . . ?
C1 C10 O7 Ho1 74.3(4) . . . . ?
C1 C10 O7 Ho2 -61.6(4) . . . . ?
C2 C1 C10 C9 -9.1(6) . . . . ?
C2 C1 C10 O7 169.2(4) . . . . ?
C2 C1 S1 O1 129.6(3) . . . . ?
C2 C1 S1 O2 8.7(4) . . . . ?
C2 C1 S1 O3 -113.8(3) . . . . ?
C2 C3 C8 C7 175.1(4) . . . . ?
C2 C3 C8 C9 -7.0(6) . . . . ?
C3 C4 C5 C6 -1.2(6) 4_565 . . . ?
C3 C4 C5 S2 -178.4(3) 4_565 . . . ?
C3 C8 C9 C10 2.5(6) . . . . ?
C4 C3 C8 C7 -3.3(6) 4_666 . . . ?
C4 C3 C8 C9 174.5(4) 4_666 . . . ?
C4 C5 C6 C7 3.0(7) . . . 4_565 ?
C4 C5 S2 O4 106.0(4) . . . . ?
C4 C5 S2 O5 -6.7(4) . . . . ?
C4 C5 S2 O6 -131.2(4) . . . . ?
C4 C5 S2 Ho2 51.1(4) . . . . ?
C6 C5 S2 O4 -71.2(4) . . . . ?
C6 C5 S2 O5 176.0(3) . . . . ?
C6 C5 S2 O6 51.5(4) . . . . ?
C6 C5 S2 Ho2 -126.2(3) . . . . ?
C6 C7 C8 C3 1.6(6) 4_666 . . . ?
C6 C7 C8 C9 -176.2(4) 4_666 . . . ?
C7 C8 C9 C10 -179.8(4) . . . . ?
C8 C9 C10 C1 5.4(6) . . . . ?
C8 C9 C10 O7 -172.8(3) . . . . ?
C9 C10 O7 Ho1 -107.5(4) . . . . ?
C9 C10 O7 Ho2 116.6(4) . . . . ?
C10 C1 C2 C3 4.5(6) . . . . ?
C10 C1 S1 O1 -49.2(3) . . . . ?
C10 C1 S1 O2 -170.0(3) . . . . ?
C10 C1 S1 O3 67.4(3) . . . . ?
C11 C12 C13 C14 -171.8(4) . . . 4_565 ?
C11 C12 C13 C18 2.4(6) . . . . ?
C11 C20 S3 O8 -63.2(3) . . . . ?
C11 C20 S3 O9 174.1(3) . . . . ?
C11 C20 S3 O10 53.0(3) . . . . ?
C12 C11 C20 C19 7.2(6) . . . . ?
C12 C11 C20 S3 -172.8(3) . . . . ?
C12 C11 O14 Ho1 -111.1(4) . . . . ?
C12 C11 O14 Ho2 112.1(4) . . . . ?
C12 C13 C18 C17 -173.1(4) . . . 4_565 ?
C12 C13 C18 C19 5.3(6) . . . . ?
C13 C14 C15 C16 -2.3(7) 4_666 . . . ?
C13 C18 C19 C20 -6.7(6) . . . . ?
C14 C13 C18 C17 1.3(6) 4_565 . . 4_565 ?
C14 C13 C18 C19 179.8(4) 4_565 . . . ?
C14 C15 C16 C17 -1.2(6) . . . . ?
C14 C15 C16 S4 174.8(3) . . . . ?
C15 C16 C17 C18 3.4(6) . . . 4_666 ?
C15 C16 S4 O11 -101.4(4) . . . . ?
C15 C16 S4 O12 141.2(3) . . . . ?
C15 C16 S4 O13 21.4(4) . . . . ?
C17 C16 S4 O11 74.7(4) . . . . ?
C17 C16 S4 O12 -42.6(4) . . . . ?
C17 C16 S4 O13 -162.4(3) . . . . ?
C17 C18 C19 C20 171.7(4) 4_565 . . . ?
C18 C19 C20 C11 0.6(6) . . . . ?
C18 C19 C20 S3 -179.5(3) . . . . ?
C19 C20 S3 O8 116.8(3) . . . . ?
C19 C20 S3 O9 -5.9(4) . . . . ?
C19 C20 S3 O10 -127.0(3) . . . . ?
C20 C11 C12 C13 -8.5(6) . . . . ?
C20 C11 O14 Ho1 66.6(4) . . . . ?
C20 C11 O14 Ho2 -70.2(4) . . . . ?
C21 C22 C23 C24 -1.1(8) . . . . ?
C22 C21 N1 C32 -0.1(7) . . . . ?
C22 C21 N1 Ho2 -164.8(4) . . . . ?
C22 C23 C24 C25 179.2(5) . . . . ?
C22 C23 C24 C32 -0.3(7) . . . . ?
C23 C24 C25 C26 178.6(5) . . . . ?
C23 C24 C32 C31 -177.6(4) . . . . ?
C23 C24 C32 N1 1.6(6) . . . . ?
C24 C25 C26 C27 -0.8(7) . . . . ?
C24 C32 N1 C21 -1.4(6) . . . . ?
C24 C32 N1 Ho2 164.2(3) . . . . ?
C25 C24 C32 C31 2.8(6) . . . . ?
C25 C24 C32 N1 -178.0(4) . . . . ?
C25 C26 C27 C28 -175.6(5) . . . . ?
C25 C26 C27 C31 2.4(7) . . . . ?
C26 C27 C28 C29 179.0(4) . . . . ?
C26 C27 C31 C32 -1.3(6) . . . . ?
C26 C27 C31 N2 178.9(4) . . . . ?
C27 C28 C29 C30 0.9(8) . . . . ?
C27 C31 C32 C24 -1.3(6) . . . . ?
C27 C31 C32 N1 179.5(4) . . . . ?
C27 C31 N2 C30 2.8(6) . . . . ?
C27 C31 N2 Ho2 -162.7(3) . . . . ?
C28 C27 C31 C32 176.9(4) . . . . ?
C28 C27 C31 N2 -2.9(6) . . . . ?
C28 C29 C30 N2 -1.1(8) . . . . ?
C29 C30 N2 C31 -0.7(6) . . . . ?
C29 C30 N2 Ho2 163.4(4) . . . . ?
C31 C27 C28 C29 1.0(7) . . . . ?
C31 C32 N1 C21 177.8(4) . . . . ?
C31 C32 N1 Ho2 -16.6(5) . . . . ?
C32 C24 C25 C26 -1.8(7) . . . . ?
C32 C31 N2 C30 -177.0(4) . . . . ?
C32 C31 N2 Ho2 17.5(4) . . . . ?
C33 C34 C35 C36 -2.7(7) . . . . ?
C34 C33 N3 C44 1.8(6) . . . . ?
C34 C33 N3 Ho1 -165.6(3) . . . . ?
C34 C35 C36 C37 -178.9(4) . . . . ?
C34 C35 C36 C44 2.4(6) . . . . ?
C35 C36 C37 C38 179.3(4) . . . . ?
C35 C36 C44 C43 179.7(4) . . . . ?
C35 C36 C44 N3 0.0(6) . . . . ?
C36 C37 C38 C39 1.2(7) . . . . ?
C36 C44 N3 C33 -2.1(6) . . . . ?
C36 C44 N3 Ho1 166.1(3) . . . . ?
C37 C36 C44 C43 1.0(6) . . . . ?
C37 C36 C44 N3 -178.7(4) . . . . ?
C37 C38 C39 C40 -179.5(5) . . . . ?
C37 C38 C39 C43 0.6(7) . . . . ?
C38 C39 C40 C41 -179.7(5) . . . . ?
C38 C39 C43 C44 -1.6(6) . . . . ?
C38 C39 C43 N4 178.4(4) . . . . ?
C39 C40 C41 C42 1.2(8) . . . . ?
C39 C43 C44 C36 0.8(6) . . . . ?
C39 C43 C44 N3 -179.5(4) . . . . ?
C39 C43 N4 C42 1.3(6) . . . . ?
C39 C43 N4 Ho1 -167.0(3) . . . . ?
C40 C39 C43 C44 178.5(4) . . . . ?
C40 C39 C43 N4 -1.4(6) . . . . ?
C40 C41 C42 N4 -1.3(8) . . . . ?
C41 C42 N4 C43 0.1(7) . . . . ?
C41 C42 N4 Ho1 167.8(4) . . . . ?
C43 C39 C40 C41 0.1(7) . . . . ?
C43 C44 N3 C33 178.2(4) . . . . ?
C43 C44 N3 Ho1 -13.6(4) . . . . ?
C44 C36 C37 C38 -2.0(7) . . . . ?
C44 C43 N4 C42 -178.7(4) . . . . ?
C44 C43 N4 Ho1 13.1(4) . . . . ?
O14 C11 C12 C13 169.3(3) . . . . ?
O14 C11 C20 C19 -170.7(3) . . . . ?
O14 C11 C20 S3 9.3(5) . . . . ?
S1 C1 C2 C3 -174.2(3) . . . . ?
S1 C1 C10 C9 169.7(3) . . . . ?
S1 C1 C10 O7 -12.0(5) . . . . ?
S2 C5 C6 C7 -179.8(3) . . . 4_565 ?
S4 C16 C17 C18 -172.6(3) . . . 4_666 ?
Ho1 O1 S1 C1 61.8(2) . . . . ?
Ho1 O1 S1 O2 -179.80(18) . . . . ?
Ho1 O1 S1 O3 -51.3(2) . . . . ?
Ho1 O8 S3 C20 41.7(2) . . . . ?
Ho1 O8 S3 O9 160.60(18) . . . . ?
Ho1 O8 S3 O10 -70.8(2) . . . . ?
Ho1 O12 S4 C16 -77.3(3) . . . . ?
Ho1 O12 S4 O11 167.2(3) . . . . ?
Ho1 O12 S4 O13 39.0(4) . . . . ?
Ho2 O3 S1 C1 -44.9(2) . . . . ?
Ho2 O3 S1 O1 67.6(2) . . . . ?
Ho2 O3 S1 O2 -164.49(17) . . . . ?
Ho2 O4 S2 C5 -108.97(17) . . . . ?
Ho2 O4 S2 O5 5.38(18) . . . . ?
Ho2 O4 S2 O6 131.98(17) . . . . ?
Ho2 O5 S2 C5 108.56(16) . . . . ?
Ho2 O5 S2 O4 -5.22(17) . . . . ?
Ho2 O5 S2 O6 -131.18(16) . . . . ?
Ho2 O10 S3 C20 -66.0(2) . . . . ?
Ho2 O10 S3 O8 47.0(2) . . . . ?
Ho2 O10 S3 O9 176.14(17) . . . . ?
N1 C21 C22 C23 1.4(8) . . . . ?
N2 C31 C32 C24 178.5(4) . . . . ?
N2 C31 C32 N1 -0.7(5) . . . . ?
N3 C33 C34 C35 0.6(7) . . . . ?
N4 C43 C44 C36 -179.2(4) . . . . ?
N4 C43 C44 N3 0.5(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Phase3-Dy
_database_code_depnum_ccdc_archive 'CCDC 1477861'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2016-02-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H28 Dy2 N4 O15 S4, O0.9, 2(H2 O)'
_chemical_formula_sum            'C44 H32 Dy2 N4 O17.90 S4'
_chemical_formula_weight         1356.45
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2586(6)
_cell_length_b                   17.0438(7)
_cell_length_c                   18.9287(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.0710(10)
_cell_angle_gamma                90
_cell_volume                     4542.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   0.914
_shelx_estimated_absorpt_T_min   0.493
_exptl_absorpt_coefficient_mu    3.532
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0698 after correction.
The Ratio of minimum to maximum transmission is 0.9255.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2653
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.026
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            89917
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         1.617
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6786
_reflns_number_total             9287
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 20015)'
_refine_diff_density_max         1.793
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²+8.6578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0870
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O16(0.76012) O0AA(0.14476)
3.a Free rotating group:
 O16(O17,H17A,H17B)
3.b Rotating group:
 O15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C -0.2378(4) 0.2605(3) 0.2539(3) 0.0189(12) Uani 1 1 d . . . . .
C2 C -0.2087(4) 0.2677(3) 0.3252(3) 0.0203(12) Uani 1 1 d . . . . .
H2 H -0.1927 0.3168 0.3450 0.024 Uiso 1 1 calc R . . . .
C3 C -0.2028(4) 0.2014(3) 0.3692(2) 0.0182(11) Uani 1 1 d . . . . .
C4 C -0.6755(4) 0.2928(3) -0.0548(3) 0.0239(13) Uani 1 1 d . . . . .
H4 H -0.6652 0.2440 -0.0331 0.029 Uiso 1 1 calc R . . . .
C5 C -0.6651(4) 0.3592(3) -0.0149(3) 0.0244(13) Uani 1 1 d . . . . .
C6 C -0.6787(4) 0.4343(4) -0.0462(3) 0.0327(15) Uani 1 1 d . . . . .
H6 H -0.6686 0.4790 -0.0179 0.039 Uiso 1 1 calc R . . . .
C7 C -0.2070(4) 0.0593(3) 0.3817(3) 0.0309(15) Uani 1 1 d . . . . .
H7 H -0.2174 0.0097 0.3614 0.037 Uiso 1 1 calc R . . . .
C8 C -0.2208(4) 0.1260(3) 0.3374(3) 0.0217(12) Uani 1 1 d . . . . .
C9 C -0.2551(4) 0.1201(3) 0.2628(3) 0.0235(13) Uani 1 1 d . . . . .
H9 H -0.2690 0.0712 0.2420 0.028 Uiso 1 1 calc R . . . .
C10 C -0.2676(4) 0.1868(3) 0.2219(2) 0.0194(12) Uani 1 1 d . . . . .
C11 C -0.4102(4) 0.2853(3) -0.0388(2) 0.0189(12) Uani 1 1 d . . . . .
C12 C -0.4122(4) 0.3537(3) -0.0766(3) 0.0236(13) Uani 1 1 d . . . . .
H12 H -0.3956 0.4005 -0.0525 0.028 Uiso 1 1 calc R . . . .
C13 C -0.4394(4) 0.3543(3) -0.1522(3) 0.0223(12) Uani 1 1 d . . . . .
C14 C 0.0690(4) 0.0778(4) 0.3068(3) 0.0327(15) Uani 1 1 d . . . . .
H14 H 0.0846 0.0302 0.3297 0.039 Uiso 1 1 calc R . . . .
C15 C 0.0546(4) 0.0812(3) 0.2340(3) 0.0292(14) Uani 1 1 d . . . . .
H15 H 0.0626 0.0362 0.2077 0.035 Uiso 1 1 calc R . . . .
C16 C 0.0281(4) 0.1512(3) 0.1984(3) 0.0242(13) Uani 1 1 d . . . . .
C17 C 0.0126(4) 0.2176(3) 0.2363(3) 0.0255(13) Uani 1 1 d . . . . .
H17 H -0.0099 0.2632 0.2123 0.031 Uiso 1 1 calc R . . . .
C18 C -0.4688(4) 0.2838(3) -0.1876(3) 0.0225(12) Uani 1 1 d . . . . .
C19 C -0.4778(4) 0.2152(3) -0.1468(3) 0.0222(12) Uani 1 1 d . . . . .
H19 H -0.5023 0.1694 -0.1693 0.027 Uiso 1 1 calc R . . . .
C20 C -0.4504(4) 0.2167(3) -0.0744(3) 0.0188(12) Uani 1 1 d . . . . .
C21 C -0.4669(5) 0.3690(4) 0.2735(3) 0.0394(16) Uani 1 1 d . . . . .
H21 H -0.4695 0.4091 0.2399 0.047 Uiso 1 1 calc R . . . .
C22 C -0.4570(5) 0.3892(4) 0.3461(3) 0.050(2) Uani 1 1 d . . . . .
H22 H -0.4559 0.4415 0.3602 0.060 Uiso 1 1 calc R . . . .
C23 C -0.4492(5) 0.3305(5) 0.3955(3) 0.052(2) Uani 1 1 d . . . . .
H23 H -0.4397 0.3428 0.4440 0.063 Uiso 1 1 calc R . . . .
C24 C -0.4552(5) 0.2523(4) 0.3742(3) 0.0363(16) Uani 1 1 d . . . . .
C25 C -0.4464(5) 0.1878(5) 0.4229(3) 0.0449(19) Uani 1 1 d . . . . .
H25 H -0.4351 0.1975 0.4719 0.054 Uiso 1 1 calc R . . . .
C26 C -0.4543(5) 0.1132(5) 0.3994(3) 0.0452(19) Uani 1 1 d . . . . .
H26 H -0.4484 0.0723 0.4324 0.054 Uiso 1 1 calc R . . . .
C27 C -0.4717(4) 0.0956(4) 0.3246(3) 0.0333(15) Uani 1 1 d . . . . .
C28 C -0.4857(5) 0.0193(4) 0.2973(4) 0.0450(18) Uani 1 1 d . . . . .
H28 H -0.4833 -0.0233 0.3282 0.054 Uiso 1 1 calc R . . . .
C29 C -0.5029(5) 0.0080(4) 0.2250(4) 0.0477(19) Uani 1 1 d . . . . .
H29 H -0.5127 -0.0423 0.2062 0.057 Uiso 1 1 calc R . . . .
C30 C -0.5056(5) 0.0726(3) 0.1797(3) 0.0330(15) Uani 1 1 d . . . . .
H30 H -0.5177 0.0638 0.1307 0.040 Uiso 1 1 calc R . . . .
C31 C -0.4765(4) 0.1578(3) 0.2746(3) 0.0257(13) Uani 1 1 d . . . . .
C32 C -0.4675(4) 0.2372(3) 0.2992(3) 0.0252(13) Uani 1 1 d . . . . .
C33 C -0.1747(4) 0.3855(4) -0.0065(3) 0.0339(15) Uani 1 1 d . . . . .
H33 H -0.1654 0.3970 0.0421 0.041 Uiso 1 1 calc R . . . .
C34 C -0.1731(5) 0.4477(4) -0.0550(3) 0.0404(16) Uani 1 1 d . . . . .
H34 H -0.1635 0.4990 -0.0386 0.048 Uiso 1 1 calc R . . . .
C35 C -0.1858(4) 0.4319(4) -0.1265(3) 0.0383(16) Uani 1 1 d . . . . .
H35 H -0.1860 0.4725 -0.1594 0.046 Uiso 1 1 calc R . . . .
C36 C -0.1985(4) 0.3544(4) -0.1501(3) 0.0285(14) Uani 1 1 d . . . . .
C37 C -0.2104(4) 0.3327(4) -0.2248(3) 0.0399(17) Uani 1 1 d . . . . .
H37 H -0.2109 0.3716 -0.2593 0.048 Uiso 1 1 calc R . . . .
C38 C -0.2209(5) 0.2583(4) -0.2450(3) 0.0433(18) Uani 1 1 d . . . . .
H38 H -0.2283 0.2461 -0.2934 0.052 Uiso 1 1 calc R . . . .
C39 C -0.2209(4) 0.1962(4) -0.1937(3) 0.0347(15) Uani 1 1 d . . . . .
C40 C -0.2304(5) 0.1167(4) -0.2121(3) 0.050(2) Uani 1 1 d . . . . .
H40 H -0.2367 0.1019 -0.2599 0.060 Uiso 1 1 calc R . . . .
C41 C -0.2304(5) 0.0611(4) -0.1611(3) 0.050(2) Uani 1 1 d . . . . .
H41 H -0.2359 0.0083 -0.1733 0.061 Uiso 1 1 calc R . . . .
C42 C -0.2221(5) 0.0847(4) -0.0896(3) 0.0379(16) Uani 1 1 d . . . . .
H42 H -0.2234 0.0464 -0.0548 0.046 Uiso 1 1 calc R . . . .
C43 C -0.2101(4) 0.2154(4) -0.1201(3) 0.0288(14) Uani 1 1 d . . . . .
C44 C -0.1980(4) 0.2955(4) -0.0985(3) 0.0276(13) Uani 1 1 d . . . . .
O1 O -0.1871(3) 0.3098(2) 0.13734(18) 0.0268(9) Uani 1 1 d . . . . .
O2 O -0.1903(3) 0.4050(2) 0.23206(19) 0.0308(10) Uani 1 1 d . . . . .
O3 O -0.3376(3) 0.3551(2) 0.16569(17) 0.0241(9) Uani 1 1 d . . . . .
O4 O -0.5295(3) 0.3813(2) 0.09324(19) 0.0314(10) Uani 1 1 d . . . . .
O5 O -0.6270(3) 0.2702(2) 0.09862(18) 0.0261(9) Uani 1 1 d . . . . .
O6 O -0.6931(3) 0.4008(3) 0.11189(19) 0.0419(12) Uani 1 1 d . . . . .
O7 O -0.3112(3) 0.1865(2) 0.15204(17) 0.0201(8) Uani 1 1 d . . . . .
O8 O -0.3594(3) 0.1148(2) 0.01061(19) 0.0266(9) Uani 1 1 d . . . . .
O9 O -0.5062(3) 0.0728(2) -0.06279(18) 0.0275(9) Uani 1 1 d . . . . .
O10 O -0.5094(3) 0.1619(2) 0.03706(17) 0.0245(9) Uani 1 1 d . . . . .
O11 O 0.1040(3) 0.1947(3) 0.0892(2) 0.0419(11) Uani 1 1 d . . . . .
O12 O -0.0647(3) 0.2047(2) 0.07944(19) 0.0293(9) Uani 1 1 d . . . . .
O13 O 0.0081(3) 0.0761(2) 0.0786(2) 0.0389(11) Uani 1 1 d . . . . .
O14 O -0.3710(3) 0.2793(2) 0.03079(17) 0.0223(9) Uani 1 1 d . . . . .
O15 O -0.1842(3) 0.0732(2) 0.0841(2) 0.0384(11) Uani 1 1 d . . . . .
H15A H -0.2326 0.0470 0.0911 0.058 Uiso 1 1 d GR . . . .
H15B H -0.1432 0.0729 0.1220 0.058 Uiso 1 1 d GR . . . .
O16 O 0.0972(6) 0.3688(4) 0.1097(5) 0.091(3) Uiso 0.7601 1 d . . P . .
O17 O 0.7130(4) 0.9428(3) 0.0649(3) 0.0719(17) Uani 1 1 d G . . . .
H17A H 0.7045 0.9291 0.0212 0.108 Uiso 1 1 d G . . . .
H17B H 0.6632 0.9651 0.0744 0.108 Uiso 1 1 d G . . . .
O18 O 0.2737(4) 0.1155(4) 0.0729(4) 0.079(2) Uani 1 1 d . . . . .
H18A H 0.217(7) 0.123(6) 0.073(6) 0.118 Uiso 1 1 d R . . . .
H18B H 0.313(8) 0.147(6) 0.078(6) 0.118 Uiso 1 1 d R . . . .
S1 S -0.23746(10) 0.33980(8) 0.19449(7) 0.0225(3) Uani 1 1 d . . . . .
S2 S -0.62930(11) 0.35405(9) 0.07872(7) 0.0265(3) Uani 1 1 d . . . . .
S3 S -0.45713(10) 0.13366(8) -0.01998(6) 0.0208(3) Uani 1 1 d . . . . .
S4 S 0.01948(11) 0.15629(9) 0.10468(7) 0.0273(3) Uani 1 1 d . . . . .
Dy1 Dy -0.22966(2) 0.20338(2) 0.05631(2) 0.02083(8) Uani 1 1 d . . . . .
Dy2 Dy -0.45279(2) 0.25770(2) 0.12531(2) 0.02028(8) Uani 1 1 d . . . . .
N1 N -0.4728(3) 0.2956(3) 0.2506(2) 0.0257(11) Uani 1 1 d . . . . .
N2 N -0.4920(3) 0.1456(3) 0.2023(2) 0.0252(11) Uani 1 1 d . . . . .
N3 N -0.1886(3) 0.3111(3) -0.0263(2) 0.0245(11) Uani 1 1 d . . . . .
N4 N -0.2124(3) 0.1598(3) -0.0689(2) 0.0297(12) Uani 1 1 d . . . . .
O0AA O 0.045(3) 0.3760(18) 0.0982(17) 0.041(8) Uiso 0.1448 1 d . . 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
C1 C2 1.354(7) . ?
C1 C10 1.429(7) . ?
C1 S1 1.759(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.398(7) . ?
C3 C4 1.433(7) 4_666 ?
C3 C8 1.424(7) . ?
C4 C3 1.433(7) 4_565 ?
C4 H4 0.9300 . ?
C4 C5 1.356(7) . ?
C5 C6 1.410(8) . ?
C5 S2 1.768(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.365(7) 4_565 ?
C7 C6 1.365(7) 4_666 ?
C7 H7 0.9300 . ?
C7 C8 1.409(7) . ?
C8 C9 1.423(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.372(7) . ?
C10 O7 1.369(5) . ?
C11 C12 1.366(7) . ?
C11 C20 1.424(7) . ?
C11 O14 1.351(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.422(7) . ?
C13 C14 1.409(8) 4_565 ?
C13 C18 1.408(8) . ?
C14 C13 1.409(8) 4_666 ?
C14 H14 0.9300 . ?
C14 C15 1.363(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.392(8) . ?
C16 C17 1.377(8) . ?
C16 S4 1.762(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.423(7) 4_666 ?
C18 C17 1.423(7) 4_565 ?
C18 C19 1.419(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.364(7) . ?
C20 S3 1.762(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.402(8) . ?
C21 N1 1.322(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.362(10) . ?
C23 H23 0.9300 . ?
C23 C24 1.391(10) . ?
C24 C25 1.429(9) . ?
C24 C32 1.425(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.346(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.431(9) . ?
C27 C28 1.402(9) . ?
C27 C31 1.415(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.364(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.392(8) . ?
C30 H30 0.9300 . ?
C30 N2 1.321(7) . ?
C31 C32 1.429(8) . ?
C31 N2 1.368(6) . ?
C32 N1 1.350(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.405(8) . ?
C33 N3 1.328(7) . ?
C34 H34 0.9300 . ?
C34 C35 1.365(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.397(9) . ?
C36 C37 1.446(8) . ?
C36 C44 1.399(8) . ?
C37 H37 0.9300 . ?
C37 C38 1.326(9) . ?
C38 H38 0.9300 . ?
C38 C39 1.436(9) . ?
C39 C40 1.400(9) . ?
C39 C43 1.416(8) . ?
C40 H40 0.9300 . ?
C40 C41 1.352(9) . ?
C41 H41 0.9300 . ?
C41 C42 1.399(8) . ?
C42 H42 0.9300 . ?
C42 N4 1.339(7) . ?
C43 C44 1.427(8) . ?
C43 N4 1.360(7) . ?
C44 N3 1.379(7) . ?
O1 S1 1.481(4) . ?
O1 Dy1 2.391(4) . ?
O2 S1 1.428(4) . ?
O3 S1 1.470(4) . ?
O3 Dy2 2.375(4) . ?
O4 S2 1.480(4) . ?
O4 Dy2 2.406(4) . ?
O5 S2 1.477(4) . ?
O5 Dy2 2.464(4) . ?
O6 S2 1.427(4) . ?
O7 Dy1 2.320(3) . ?
O7 Dy2 2.341(4) . ?
O8 S3 1.458(4) . ?
O8 Dy1 2.439(4) . ?
O9 S3 1.429(4) . ?
O10 S3 1.485(4) . ?
O10 Dy2 2.384(3) . ?
O11 S4 1.442(4) . ?
O12 S4 1.472(4) . ?
O12 Dy1 2.324(4) . ?
O13 S4 1.454(4) . ?
O14 Dy1 2.380(4) . ?
O14 Dy2 2.314(4) . ?
O15 H15A 0.8496 . ?
O15 H15B 0.8503 . ?
O15 Dy1 2.348(4) . ?
O16 O0AA 0.75(3) . ?
O17 H17A 0.8498 . ?
O17 H17B 0.8494 . ?
O18 H18A 0.81(10) . ?
O18 H18B 0.77(10) . ?
S2 Dy2 3.0180(15) . ?
Dy1 Dy2 3.7411(4) . ?
Dy1 N3 2.539(5) . ?
Dy1 N4 2.532(4) . ?
Dy2 N1 2.517(4) . ?
Dy2 N2 2.518(4) . ?

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
C2 C1 C10 121.8(5) . . ?
C2 C1 S1 122.4(4) . . ?
C10 C1 S1 115.8(4) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0(5) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 121.5(5) . 4_666 ?
C2 C3 C8 119.2(4) . . ?
C8 C3 C4 119.2(5) . 4_666 ?
C3 C4 H4 120.3 4_565 . ?
C5 C4 C3 119.3(5) . 4_565 ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 121.8(5) . . ?
C4 C5 S2 120.4(4) . . ?
C6 C5 S2 117.7(4) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.5(5) 4_565 . ?
C7 C6 H6 120.3 4_565 . ?
C6 C7 H7 119.3 4_666 . ?
C6 C7 C8 121.4(5) 4_666 . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 118.6(4) . . ?
C7 C8 C9 121.8(5) . . ?
C9 C8 C3 119.6(5) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.7(5) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C1 119.0(4) . . ?
O7 C10 C1 118.2(4) . . ?
O7 C10 C9 122.8(5) . . ?
C12 C11 C20 118.6(4) . . ?
O14 C11 C12 123.1(5) . . ?
O14 C11 C20 118.3(4) . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.9(5) . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 121.8(5) 4_565 . ?
C18 C13 C12 119.1(5) . . ?
C18 C13 C14 118.9(5) . 4_565 ?
C13 C14 H14 119.7 4_666 . ?
C15 C14 C13 120.7(5) . 4_666 ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.7(5) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 S4 120.0(4) . . ?
C17 C16 C15 120.5(5) . . ?
C17 C16 S4 119.5(4) . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.5(5) . 4_666 ?
C18 C17 H17 120.2 4_666 . ?
C13 C18 C17 119.4(5) . 4_565 ?
C13 C18 C19 119.4(5) . . ?
C19 C18 C17 121.2(5) . 4_565 ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.7(5) . . ?
C20 C19 H19 120.2 . . ?
C11 C20 S3 115.9(4) . . ?
C19 C20 C11 121.4(5) . . ?
C19 C20 S3 122.6(4) . . ?
C22 C21 H21 118.5 . . ?
N1 C21 H21 118.5 . . ?
N1 C21 C22 123.1(6) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 C21 118.5(7) . . ?
C23 C22 H22 120.8 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.6(6) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 123.7(6) . . ?
C23 C24 C32 117.1(6) . . ?
C32 C24 C25 119.2(6) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.3(6) . . ?
C26 C25 H25 119.4 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.2(6) . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 123.5(6) . . ?
C28 C27 C31 117.4(6) . . ?
C31 C27 C26 119.1(6) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 C27 119.5(6) . . ?
C29 C28 H28 120.2 . . ?
C28 C29 H29 120.4 . . ?
C28 C29 C30 119.3(6) . . ?
C30 C29 H29 120.4 . . ?
C29 C30 H30 118.0 . . ?
N2 C30 C29 123.9(6) . . ?
N2 C30 H30 118.0 . . ?
C27 C31 C32 120.0(5) . . ?
N2 C31 C27 122.5(5) . . ?
N2 C31 C32 117.5(5) . . ?
C24 C32 C31 119.1(5) . . ?
N1 C32 C24 122.0(5) . . ?
N1 C32 C31 118.9(5) . . ?
C34 C33 H33 118.2 . . ?
N3 C33 H33 118.2 . . ?
N3 C33 C34 123.6(6) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.1(6) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 120.2 . . ?
C34 C35 C36 119.6(6) . . ?
C36 C35 H35 120.2 . . ?
C35 C36 C37 122.9(6) . . ?
C35 C36 C44 118.0(5) . . ?
C44 C36 C37 119.1(6) . . ?
C36 C37 H37 119.4 . . ?
C38 C37 C36 121.1(6) . . ?
C38 C37 H37 119.4 . . ?
C37 C38 H38 119.3 . . ?
C37 C38 C39 121.5(6) . . ?
C39 C38 H38 119.3 . . ?
C40 C39 C38 123.8(6) . . ?
C40 C39 C43 117.3(6) . . ?
C43 C39 C38 118.8(6) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 C39 120.8(6) . . ?
C41 C40 H40 119.6 . . ?
C40 C41 H41 120.7 . . ?
C40 C41 C42 118.6(6) . . ?
C42 C41 H41 120.7 . . ?
C41 C42 H42 118.4 . . ?
N4 C42 C41 123.2(6) . . ?
N4 C42 H42 118.4 . . ?
C39 C43 C44 119.5(5) . . ?
N4 C43 C39 121.9(6) . . ?
N4 C43 C44 118.5(5) . . ?
C36 C44 C43 119.9(5) . . ?
N3 C44 C36 122.8(5) . . ?
N3 C44 C43 117.2(5) . . ?
S1 O1 Dy1 128.8(2) . . ?
S1 O3 Dy2 125.3(2) . . ?
S2 O4 Dy2 99.1(2) . . ?
S2 O5 Dy2 96.73(19) . . ?
C10 O7 Dy1 123.1(3) . . ?
C10 O7 Dy2 116.9(3) . . ?
Dy1 O7 Dy2 106.75(13) . . ?
S3 O8 Dy1 128.9(2) . . ?
S3 O10 Dy2 125.3(2) . . ?
S4 O12 Dy1 143.6(2) . . ?
C11 O14 Dy1 116.4(3) . . ?
C11 O14 Dy2 125.8(3) . . ?
Dy2 O14 Dy1 105.67(13) . . ?
H15A O15 H15B 109.5 . . ?
Dy1 O15 H15A 109.2 . . ?
Dy1 O15 H15B 108.9 . . ?
H17A O17 H17B 109.5 . . ?
H18A O18 H18B 126(10) . . ?
O1 S1 C1 104.6(2) . . ?
O2 S1 C1 109.1(2) . . ?
O2 S1 O1 112.8(2) . . ?
O2 S1 O3 113.6(2) . . ?
O3 S1 C1 105.8(2) . . ?
O3 S1 O1 110.2(2) . . ?
C5 S2 Dy2 114.55(19) . . ?
O4 S2 C5 106.7(3) . . ?
O4 S2 Dy2 51.94(15) . . ?
O5 S2 C5 107.2(2) . . ?
O5 S2 O4 105.9(2) . . ?
O5 S2 Dy2 54.19(16) . . ?
O6 S2 C5 108.1(2) . . ?
O6 S2 O4 113.8(3) . . ?
O6 S2 O5 114.7(3) . . ?
O6 S2 Dy2 137.33(17) . . ?
O8 S3 C20 105.8(2) . . ?
O8 S3 O10 109.9(2) . . ?
O9 S3 C20 108.5(2) . . ?
O9 S3 O8 114.6(2) . . ?
O9 S3 O10 112.9(2) . . ?
O10 S3 C20 104.2(2) . . ?
O11 S4 C16 107.5(3) . . ?
O11 S4 O12 110.1(3) . . ?
O11 S4 O13 114.2(3) . . ?
O12 S4 C16 106.2(2) . . ?
O13 S4 C16 106.4(3) . . ?
O13 S4 O12 112.0(2) . . ?
O1 Dy1 O8 143.05(13) . . ?
O1 Dy1 Dy2 74.48(9) . . ?
O1 Dy1 N3 77.66(13) . . ?
O1 Dy1 N4 140.39(14) . . ?
O7 Dy1 O1 72.60(12) . . ?
O7 Dy1 O8 75.80(12) . . ?
O7 Dy1 O12 118.11(12) . . ?
O7 Dy1 O14 73.33(12) . . ?
O7 Dy1 O15 82.10(14) . . ?
O7 Dy1 Dy2 36.81(9) . . ?
O7 Dy1 N3 139.73(14) . . ?
O7 Dy1 N4 146.02(14) . . ?
O8 Dy1 Dy2 68.76(9) . . ?
O8 Dy1 N3 117.72(13) . . ?
O8 Dy1 N4 70.53(14) . . ?
O12 Dy1 O1 74.02(13) . . ?
O12 Dy1 O8 139.59(13) . . ?
O12 Dy1 O14 146.38(13) . . ?
O12 Dy1 O15 74.41(14) . . ?
O12 Dy1 Dy2 145.40(9) . . ?
O12 Dy1 N3 77.55(14) . . ?
O12 Dy1 N4 86.22(14) . . ?
O14 Dy1 O1 80.74(12) . . ?
O14 Dy1 O8 72.18(12) . . ?
O14 Dy1 Dy2 36.55(8) . . ?
O14 Dy1 N3 75.62(14) . . ?
O14 Dy1 N4 100.01(14) . . ?
O15 Dy1 O1 122.66(13) . . ?
O15 Dy1 O8 70.22(13) . . ?
O15 Dy1 O14 138.99(14) . . ?
O15 Dy1 Dy2 112.07(11) . . ?
O15 Dy1 N3 137.66(15) . . ?
O15 Dy1 N4 82.44(15) . . ?
N3 Dy1 Dy2 109.09(10) . . ?
N4 Dy1 Dy2 127.80(11) . . ?
N4 Dy1 N3 64.54(15) . . ?
O3 Dy2 O4 74.52(12) . . ?
O3 Dy2 O5 128.97(12) . . ?
O3 Dy2 O10 147.66(12) . . ?
O3 Dy2 S2 102.48(9) . . ?
O3 Dy2 Dy1 72.69(9) . . ?
O3 Dy2 N1 72.09(14) . . ?
O3 Dy2 N2 123.30(13) . . ?
O4 Dy2 O5 57.95(13) . . ?
O4 Dy2 S2 28.97(10) . . ?
O4 Dy2 Dy1 120.42(10) . . ?
O4 Dy2 N1 84.17(14) . . ?
O4 Dy2 N2 132.56(14) . . ?
O5 Dy2 S2 29.09(9) . . ?
O5 Dy2 Dy1 146.60(8) . . ?
O5 Dy2 N1 84.88(13) . . ?
O5 Dy2 N2 82.87(14) . . ?
O7 Dy2 O3 76.34(12) . . ?
O7 Dy2 O4 148.24(13) . . ?
O7 Dy2 O5 153.61(12) . . ?
O7 Dy2 O10 88.95(12) . . ?
O7 Dy2 S2 174.89(9) . . ?
O7 Dy2 Dy1 36.43(8) . . ?
O7 Dy2 N1 98.70(13) . . ?
O7 Dy2 N2 75.17(14) . . ?
O10 Dy2 O4 109.42(12) . . ?
O10 Dy2 O5 72.33(12) . . ?
O10 Dy2 S2 89.62(9) . . ?
O10 Dy2 Dy1 78.38(9) . . ?
O10 Dy2 N1 139.45(14) . . ?
O10 Dy2 N2 78.72(13) . . ?
O14 Dy2 O3 74.36(12) . . ?
O14 Dy2 O4 85.98(13) . . ?
O14 Dy2 O5 116.23(12) . . ?
O14 Dy2 O7 74.18(12) . . ?
O14 Dy2 O10 73.96(12) . . ?
O14 Dy2 S2 100.71(9) . . ?
O14 Dy2 Dy1 37.78(9) . . ?
O14 Dy2 N1 146.43(14) . . ?
O14 Dy2 N2 138.87(14) . . ?
S2 Dy2 Dy1 138.46(3) . . ?
N1 Dy2 S2 85.56(11) . . ?
N1 Dy2 Dy1 128.41(11) . . ?
N1 Dy2 N2 65.24(15) . . ?
N2 Dy2 S2 109.34(11) . . ?
N2 Dy2 Dy1 107.02(10) . . ?
C21 N1 C32 118.7(5) . . ?
C21 N1 Dy2 122.8(4) . . ?
C32 N1 Dy2 116.8(4) . . ?
C30 N2 C31 117.4(5) . . ?
C30 N2 Dy2 124.2(4) . . ?
C31 N2 Dy2 116.7(4) . . ?
C33 N3 C44 116.8(5) . . ?
C33 N3 Dy1 123.8(4) . . ?
C44 N3 Dy1 118.4(4) . . ?
C42 N4 C43 118.0(5) . . ?
C42 N4 Dy1 122.2(4) . . ?
C43 N4 Dy1 118.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -177.7(5) . . . 4_666 ?
C1 C2 C3 C8 4.6(8) . . . . ?
C1 C10 O7 Dy1 75.3(5) . . . . ?
C1 C10 O7 Dy2 -60.4(5) . . . . ?
C2 C1 C10 C9 -8.4(8) . . . . ?
C2 C1 C10 O7 168.9(5) . . . . ?
C2 C1 S1 O1 129.3(5) . . . . ?
C2 C1 S1 O2 8.3(6) . . . . ?
C2 C1 S1 O3 -114.3(5) . . . . ?
C2 C3 C8 C7 174.9(5) . . . . ?
C2 C3 C8 C9 -7.3(8) . . . . ?
C3 C4 C5 C6 -1.0(9) 4_565 . . . ?
C3 C4 C5 S2 -178.8(4) 4_565 . . . ?
C3 C8 C9 C10 2.1(8) . . . . ?
C4 C3 C8 C7 -2.8(8) 4_666 . . . ?
C4 C3 C8 C9 175.0(5) 4_666 . . . ?
C4 C5 C6 C7 2.6(10) . . . 4_565 ?
C4 C5 S2 O4 106.7(5) . . . . ?
C4 C5 S2 O5 -6.3(6) . . . . ?
C4 C5 S2 O6 -130.4(5) . . . . ?
C4 C5 S2 Dy2 51.5(5) . . . . ?
C6 C5 S2 O4 -71.1(5) . . . . ?
C6 C5 S2 O5 175.8(5) . . . . ?
C6 C5 S2 O6 51.7(6) . . . . ?
C6 C5 S2 Dy2 -126.3(4) . . . . ?
C6 C7 C8 C3 1.2(9) 4_666 . . . ?
C6 C7 C8 C9 -176.6(6) 4_666 . . . ?
C7 C8 C9 C10 179.9(6) . . . . ?
C8 C9 C10 C1 5.5(8) . . . . ?
C8 C9 C10 O7 -171.6(5) . . . . ?
C9 C10 O7 Dy1 -107.5(5) . . . . ?
C9 C10 O7 Dy2 116.8(5) . . . . ?
C10 C1 C2 C3 3.2(8) . . . . ?
C10 C1 S1 O1 -48.6(5) . . . . ?
C10 C1 S1 O2 -169.6(4) . . . . ?
C10 C1 S1 O3 67.8(5) . . . . ?
C11 C12 C13 C14 -172.1(6) . . . 4_565 ?
C11 C12 C13 C18 3.0(8) . . . . ?
C11 C20 S3 O8 -61.4(5) . . . . ?
C11 C20 S3 O9 175.0(4) . . . . ?
C11 C20 S3 O10 54.5(5) . . . . ?
C12 C11 C20 C19 9.6(8) . . . . ?
C12 C11 C20 S3 -173.1(4) . . . . ?
C12 C11 O14 Dy1 -111.5(5) . . . . ?
C12 C11 O14 Dy2 111.6(5) . . . . ?
C12 C13 C18 C17 -174.0(5) . . . 4_565 ?
C12 C13 C18 C19 5.0(8) . . . . ?
C13 C14 C15 C16 -2.2(10) 4_666 . . . ?
C13 C18 C19 C20 -5.5(8) . . . . ?
C14 C13 C18 C17 1.2(8) 4_565 . . 4_565 ?
C14 C13 C18 C19 -179.8(5) 4_565 . . . ?
C14 C15 C16 C17 -2.4(9) . . . . ?
C14 C15 C16 S4 174.7(5) . . . . ?
C15 C16 C17 C18 5.0(9) . . . 4_666 ?
C15 C16 S4 O11 -101.5(5) . . . . ?
C15 C16 S4 O12 140.6(5) . . . . ?
C15 C16 S4 O13 21.1(6) . . . . ?
C17 C16 S4 O11 75.6(5) . . . . ?
C17 C16 S4 O12 -42.3(5) . . . . ?
C17 C16 S4 O13 -161.8(5) . . . . ?
C17 C18 C19 C20 173.5(5) 4_565 . . . ?
C18 C19 C20 C11 -1.8(8) . . . . ?
C18 C19 C20 S3 -178.8(4) . . . . ?
C19 C20 S3 O8 115.8(5) . . . . ?
C19 C20 S3 O9 -7.7(6) . . . . ?
C19 C20 S3 O10 -128.3(5) . . . . ?
C20 C11 C12 C13 -10.1(8) . . . . ?
C20 C11 O14 Dy1 67.9(5) . . . . ?
C20 C11 O14 Dy2 -69.0(6) . . . . ?
C21 C22 C23 C24 -2.9(11) . . . . ?
C22 C21 N1 C32 -1.1(10) . . . . ?
C22 C21 N1 Dy2 -165.5(5) . . . . ?
C22 C23 C24 C25 179.2(7) . . . . ?
C22 C23 C24 C32 1.4(11) . . . . ?
C23 C24 C25 C26 178.9(7) . . . . ?
C23 C24 C32 C31 -178.4(6) . . . . ?
C23 C24 C32 N1 0.4(9) . . . . ?
C24 C25 C26 C27 0.1(11) . . . . ?
C24 C32 N1 C21 -0.5(9) . . . . ?
C24 C32 N1 Dy2 164.9(4) . . . . ?
C25 C24 C32 C31 3.7(9) . . . . ?
C25 C24 C32 N1 -177.6(6) . . . . ?
C25 C26 C27 C28 -176.4(7) . . . . ?
C25 C26 C27 C31 2.7(10) . . . . ?
C26 C27 C28 C29 179.2(6) . . . . ?
C26 C27 C31 C32 -2.2(9) . . . . ?
C26 C27 C31 N2 179.4(6) . . . . ?
C27 C28 C29 C30 0.4(11) . . . . ?
C27 C31 C32 C24 -0.9(9) . . . . ?
C27 C31 C32 N1 -179.7(5) . . . . ?
C27 C31 N2 C30 2.2(8) . . . . ?
C27 C31 N2 Dy2 -163.3(4) . . . . ?
C28 C27 C31 C32 176.9(6) . . . . ?
C28 C27 C31 N2 -1.5(9) . . . . ?
C28 C29 C30 N2 0.3(11) . . . . ?
C29 C30 N2 C31 -1.6(9) . . . . ?
C29 C30 N2 Dy2 162.8(5) . . . . ?
C31 C27 C28 C29 0.2(10) . . . . ?
C31 C32 N1 C21 178.2(6) . . . . ?
C31 C32 N1 Dy2 -16.4(7) . . . . ?
C32 C24 C25 C26 -3.3(10) . . . . ?
C32 C31 N2 C30 -176.3(5) . . . . ?
C32 C31 N2 Dy2 18.2(6) . . . . ?
C33 C34 C35 C36 -1.1(10) . . . . ?
C34 C33 N3 C44 2.8(9) . . . . ?
C34 C33 N3 Dy1 -165.2(5) . . . . ?
C34 C35 C36 C37 -178.7(6) . . . . ?
C34 C35 C36 C44 0.3(9) . . . . ?
C35 C36 C37 C38 179.0(6) . . . . ?
C35 C36 C44 C43 -179.7(5) . . . . ?
C35 C36 C44 N3 2.1(9) . . . . ?
C36 C37 C38 C39 0.2(10) . . . . ?
C36 C44 N3 C33 -3.6(8) . . . . ?
C36 C44 N3 Dy1 165.1(4) . . . . ?
C37 C36 C44 C43 -0.6(9) . . . . ?
C37 C36 C44 N3 -178.8(5) . . . . ?
C37 C38 C39 C40 -179.1(7) . . . . ?
C37 C38 C39 C43 0.3(10) . . . . ?
C38 C39 C40 C41 -179.6(7) . . . . ?
C38 C39 C43 C44 -1.0(9) . . . . ?
C38 C39 C43 N4 178.0(6) . . . . ?
C39 C40 C41 C42 0.8(11) . . . . ?
C39 C43 C44 C36 1.1(9) . . . . ?
C39 C43 C44 N3 179.4(5) . . . . ?
C39 C43 N4 C42 2.2(9) . . . . ?
C39 C43 N4 Dy1 -166.3(4) . . . . ?
C40 C39 C43 C44 178.5(6) . . . . ?
C40 C39 C43 N4 -2.5(9) . . . . ?
C40 C41 C42 N4 -1.2(11) . . . . ?
C41 C42 N4 C43 -0.3(10) . . . . ?
C41 C42 N4 Dy1 167.8(5) . . . . ?
C43 C39 C40 C41 0.9(11) . . . . ?
C43 C44 N3 C33 178.1(5) . . . . ?
C43 C44 N3 Dy1 -13.2(7) . . . . ?
C44 C36 C37 C38 0.0(10) . . . . ?
C44 C43 N4 C42 -178.8(6) . . . . ?
C44 C43 N4 Dy1 12.7(7) . . . . ?
O14 C11 C12 C13 169.3(5) . . . . ?
O14 C11 C20 C19 -169.8(5) . . . . ?
O14 C11 C20 S3 7.5(7) . . . . ?
S1 C1 C2 C3 -174.6(4) . . . . ?
S1 C1 C10 C9 169.5(4) . . . . ?
S1 C1 C10 O7 -13.2(7) . . . . ?
S2 C5 C6 C7 -179.5(5) . . . 4_565 ?
S4 C16 C17 C18 -172.1(4) . . . 4_666 ?
Dy1 O1 S1 C1 61.7(3) . . . . ?
Dy1 O1 S1 O2 -179.8(2) . . . . ?
Dy1 O1 S1 O3 -51.6(3) . . . . ?
Dy1 O8 S3 C20 40.5(3) . . . . ?
Dy1 O8 S3 O9 160.1(2) . . . . ?
Dy1 O8 S3 O10 -71.5(3) . . . . ?
Dy1 O12 S4 C16 -77.1(4) . . . . ?
Dy1 O12 S4 O11 166.8(3) . . . . ?
Dy1 O12 S4 O13 38.6(4) . . . . ?
Dy2 O3 S1 C1 -44.4(3) . . . . ?
Dy2 O3 S1 O1 68.1(3) . . . . ?
Dy2 O3 S1 O2 -164.2(2) . . . . ?
Dy2 O4 S2 C5 -108.4(2) . . . . ?
Dy2 O4 S2 O5 5.5(2) . . . . ?
Dy2 O4 S2 O6 132.4(2) . . . . ?
Dy2 O5 S2 C5 108.3(2) . . . . ?
Dy2 O5 S2 O4 -5.4(2) . . . . ?
Dy2 O5 S2 O6 -131.8(2) . . . . ?
Dy2 O10 S3 C20 -65.7(3) . . . . ?
Dy2 O10 S3 O8 47.3(3) . . . . ?
Dy2 O10 S3 O9 176.7(2) . . . . ?
N1 C21 C22 C23 2.8(11) . . . . ?
N2 C31 C32 C24 177.6(5) . . . . ?
N2 C31 C32 N1 -1.2(8) . . . . ?
N3 C33 C34 C35 -0.5(10) . . . . ?
N4 C43 C44 C36 -177.9(5) . . . . ?
N4 C43 C44 N3 0.4(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Phase3-Tb
_database_code_depnum_ccdc_archive 'CCDC 1477862'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2015-10-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H28 N4 O15 S4 Tb2, 3(H2 O)'
_chemical_formula_sum            'C44 H34 N4 O18 S4 Tb2'
_chemical_formula_weight         1352.83
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2636(6)
_cell_length_b                   17.0354(7)
_cell_length_c                   18.9491(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.088(2)
_cell_angle_gamma                90
_cell_volume                     4546.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.354
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1206 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8208.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2656
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            140387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.493
_diffrn_reflns_theta_min         1.617
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6857
_reflns_number_total             9363
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 20015)'
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0365
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0325P)²+14.2315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0927
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B,O17,H17A,H17B,O18,H18A,H18B)
2.b Rotating group:
 O15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C -0.2375(4) 0.2606(3) 0.2539(3) 0.0231(12) Uani 1 1 d . . . . .
C2 C -0.2089(4) 0.2680(3) 0.3256(3) 0.0260(12) Uani 1 1 d . . . . .
H2 H -0.1936 0.3171 0.3456 0.031 Uiso 1 1 calc R . . . .
C3 C -0.2028(4) 0.2007(3) 0.3693(3) 0.0253(12) Uani 1 1 d . . . . .
C4 C -0.6752(4) 0.2934(4) -0.0554(3) 0.0300(13) Uani 1 1 d . . . . .
H4 H -0.6637 0.2445 -0.0341 0.036 Uiso 1 1 calc R . . . .
C5 C -0.6657(4) 0.3596(4) -0.0144(3) 0.0289(13) Uani 1 1 d . . . . .
C6 C -0.6797(5) 0.4342(4) -0.0464(3) 0.0361(15) Uani 1 1 d . . . . .
H6 H -0.6700 0.4791 -0.0182 0.043 Uiso 1 1 calc R . . . .
C7 C -0.2072(5) 0.0588(4) 0.3818(3) 0.0364(15) Uani 1 1 d . . . . .
H7 H -0.2171 0.0092 0.3615 0.044 Uiso 1 1 calc R . . . .
C8 C -0.2210(4) 0.1263(3) 0.3375(3) 0.0284(13) Uani 1 1 d . . . . .
C9 C -0.2555(4) 0.1199(3) 0.2630(3) 0.0287(13) Uani 1 1 d . . . . .
H9 H -0.2695 0.0709 0.2423 0.034 Uiso 1 1 calc R . . . .
C10 C -0.2680(4) 0.1865(3) 0.2221(3) 0.0224(12) Uani 1 1 d . . . . .
C11 C -0.4111(4) 0.2852(3) -0.0385(3) 0.0237(12) Uani 1 1 d . . . . .
C12 C -0.4125(4) 0.3537(3) -0.0768(3) 0.0297(13) Uani 1 1 d . . . . .
H12 H -0.3954 0.4005 -0.0530 0.036 Uiso 1 1 calc R . . . .
C13 C -0.4392(4) 0.3541(3) -0.1514(3) 0.0276(13) Uani 1 1 d . . . . .
C14 C 0.0690(5) 0.0774(4) 0.3072(3) 0.0369(15) Uani 1 1 d . . . . .
H14 H 0.0843 0.0298 0.3301 0.044 Uiso 1 1 calc R . . . .
C15 C 0.0548(5) 0.0805(4) 0.2340(3) 0.0355(15) Uani 1 1 d . . . . .
H15 H 0.0633 0.0357 0.2076 0.043 Uiso 1 1 calc R . . . .
C16 C 0.0273(4) 0.1512(4) 0.1990(3) 0.0299(13) Uani 1 1 d . . . . .
C17 C 0.0130(4) 0.2176(4) 0.2367(3) 0.0300(13) Uani 1 1 d . . . . .
H17 H -0.0082 0.2634 0.2126 0.036 Uiso 1 1 calc R . . . .
C18 C -0.4697(4) 0.2834(4) -0.1875(3) 0.0271(13) Uani 1 1 d . . . . .
C19 C -0.4787(4) 0.2153(3) -0.1465(3) 0.0255(12) Uani 1 1 d . . . . .
H19 H -0.5042 0.1697 -0.1687 0.031 Uiso 1 1 calc R . . . .
C20 C -0.4501(4) 0.2163(3) -0.0748(3) 0.0234(12) Uani 1 1 d . . . . .
C21 C -0.4681(5) 0.3695(4) 0.2746(3) 0.0427(17) Uani 1 1 d . . . . .
H21 H -0.4716 0.4098 0.2412 0.051 Uiso 1 1 calc R . . . .
C22 C -0.4573(6) 0.3890(5) 0.3472(4) 0.054(2) Uani 1 1 d . . . . .
H22 H -0.4548 0.4412 0.3614 0.065 Uiso 1 1 calc R . . . .
C23 C -0.4505(5) 0.3303(5) 0.3967(4) 0.056(2) Uani 1 1 d . . . . .
H23 H -0.4434 0.3426 0.4450 0.067 Uiso 1 1 calc R . . . .
C24 C -0.4542(5) 0.2517(4) 0.3750(3) 0.0410(16) Uani 1 1 d . . . . .
C25 C -0.4476(5) 0.1874(5) 0.4235(4) 0.053(2) Uani 1 1 d . . . . .
H25 H -0.4382 0.1970 0.4724 0.064 Uiso 1 1 calc R . . . .
C26 C -0.4546(5) 0.1124(5) 0.3996(4) 0.0485(19) Uani 1 1 d . . . . .
H26 H -0.4484 0.0713 0.4323 0.058 Uiso 1 1 calc R . . . .
C27 C -0.4713(5) 0.0954(4) 0.3251(3) 0.0385(15) Uani 1 1 d . . . . .
C28 C -0.4860(5) 0.0190(4) 0.2974(4) 0.0501(19) Uani 1 1 d . . . . .
H28 H -0.4843 -0.0237 0.3282 0.060 Uiso 1 1 calc R . . . .
C29 C -0.5027(6) 0.0077(4) 0.2256(4) 0.054(2) Uani 1 1 d . . . . .
H29 H -0.5121 -0.0427 0.2069 0.065 Uiso 1 1 calc R . . . .
C30 C -0.5056(5) 0.0720(4) 0.1801(4) 0.0414(16) Uani 1 1 d . . . . .
H30 H -0.5169 0.0631 0.1310 0.050 Uiso 1 1 calc R . . . .
C31 C -0.4772(4) 0.1573(4) 0.2754(3) 0.0280(13) Uani 1 1 d . . . . .
C32 C -0.4686(4) 0.2367(4) 0.3001(3) 0.0289(13) Uani 1 1 d . . . . .
C33 C -0.1745(5) 0.3859(4) -0.0066(3) 0.0370(15) Uani 1 1 d . . . . .
H33 H -0.1656 0.3973 0.0419 0.044 Uiso 1 1 calc R . . . .
C34 C -0.1729(5) 0.4472(4) -0.0547(4) 0.0432(17) Uani 1 1 d . . . . .
H34 H -0.1629 0.4984 -0.0381 0.052 Uiso 1 1 calc R . . . .
C35 C -0.1863(5) 0.4323(4) -0.1267(4) 0.0431(17) Uani 1 1 d . . . . .
H35 H -0.1873 0.4732 -0.1594 0.052 Uiso 1 1 calc R . . . .
C36 C -0.1984(4) 0.3542(4) -0.1501(3) 0.0323(14) Uani 1 1 d . . . . .
C37 C -0.2107(5) 0.3337(4) -0.2243(3) 0.0430(17) Uani 1 1 d . . . . .
H37 H -0.2110 0.3730 -0.2584 0.052 Uiso 1 1 calc R . . . .
C38 C -0.2219(5) 0.2588(5) -0.2452(4) 0.0481(18) Uani 1 1 d . . . . .
H38 H -0.2307 0.2468 -0.2936 0.058 Uiso 1 1 calc R . . . .
C39 C -0.2206(5) 0.1966(4) -0.1937(3) 0.0379(15) Uani 1 1 d . . . . .
C40 C -0.2307(6) 0.1173(4) -0.2131(4) 0.052(2) Uani 1 1 d . . . . .
H40 H -0.2373 0.1028 -0.2609 0.063 Uiso 1 1 calc R . . . .
C41 C -0.2306(6) 0.0619(5) -0.1617(4) 0.053(2) Uani 1 1 d . . . . .
H41 H -0.2358 0.0090 -0.1739 0.064 Uiso 1 1 calc R . . . .
C42 C -0.2226(5) 0.0850(4) -0.0906(3) 0.0422(16) Uani 1 1 d . . . . .
H42 H -0.2244 0.0463 -0.0561 0.051 Uiso 1 1 calc R . . . .
C43 C -0.2108(4) 0.2153(4) -0.1210(3) 0.0305(13) Uani 1 1 d . . . . .
C44 C -0.1984(4) 0.2956(4) -0.0980(3) 0.0311(14) Uani 1 1 d . . . . .
O1 O -0.1866(3) 0.3105(2) 0.1379(2) 0.0308(9) Uani 1 1 d . . . . .
O2 O -0.1906(3) 0.4052(2) 0.2329(2) 0.0364(10) Uani 1 1 d . . . . .
O3 O -0.3380(3) 0.3553(2) 0.16637(19) 0.0279(9) Uani 1 1 d . . . . .
O4 O -0.5309(3) 0.3817(2) 0.0937(2) 0.0375(10) Uani 1 1 d . . . . .
O5 O -0.6279(3) 0.2701(2) 0.0983(2) 0.0298(9) Uani 1 1 d . . . . .
O6 O -0.6954(3) 0.4005(3) 0.1119(2) 0.0465(12) Uani 1 1 d . . . . .
O7 O -0.3111(3) 0.1865(2) 0.15263(18) 0.0250(8) Uani 1 1 d . . . . .
O8 O -0.3602(3) 0.1143(2) 0.0101(2) 0.0296(9) Uani 1 1 d . . . . .
O9 O -0.5062(3) 0.0729(2) -0.0631(2) 0.0313(9) Uani 1 1 d . . . . .
O10 O -0.5096(3) 0.1615(2) 0.03651(19) 0.0299(9) Uani 1 1 d . . . . .
O11 O 0.1048(3) 0.1945(3) 0.0897(2) 0.0464(12) Uani 1 1 d . . . . .
O12 O -0.0634(3) 0.2046(3) 0.0798(2) 0.0347(10) Uani 1 1 d . . . . .
O13 O 0.0086(3) 0.0760(3) 0.0790(2) 0.0422(11) Uani 1 1 d . . . . .
O14 O -0.3718(3) 0.2793(2) 0.03096(18) 0.0257(9) Uani 1 1 d . . . . .
O15 O -0.1853(3) 0.0727(2) 0.0841(2) 0.0418(11) Uani 1 1 d . . . . .
H15A H -0.1826 0.0642 0.1298 0.063 Uiso 1 1 d GR . . . .
H15B H -0.1294 0.0634 0.0728 0.063 Uiso 1 1 d GR . . . .
O16 O 0.0906(3) 0.3706(3) 0.1075(5) 0.147(4) Uani 1 1 d . . . . .
H16A H 0.0948 0.3764 0.1526 0.220 Uiso 1 1 d G . . . .
H16B H 0.1344 0.3968 0.0925 0.220 Uiso 1 1 d G . . . .
O17 O 0.7114(4) 0.9411(2) 0.0635(4) 0.0764(18) Uani 1 1 d G . . . .
H17A H 0.6875 0.9563 0.0998 0.115 Uiso 1 1 d G . . . .
H17B H 0.6910 0.9701 0.0278 0.115 Uiso 1 1 d G . . . .
O18 O 0.2730(4) 0.1149(2) 0.0735(4) 0.087(2) Uani 1 1 d G . . . .
H18A H 0.2180 0.1312 0.0786 0.130 Uiso 1 1 d G . . . .
H18B H 0.3092 0.1539 0.0700 0.130 Uiso 1 1 d G . . . .
S1 S -0.23770(10) 0.34003(8) 0.19510(7) 0.0267(3) Uani 1 1 d . . . . .
S2 S -0.63085(11) 0.35409(9) 0.07874(7) 0.0309(3) Uani 1 1 d . . . . .
S3 S -0.45735(10) 0.13365(8) -0.02012(7) 0.0251(3) Uani 1 1 d . . . . .
S4 S 0.01985(11) 0.15591(10) 0.10514(8) 0.0317(3) Uani 1 1 d . . . . .
Tb1 Tb -0.22952(2) 0.20327(2) 0.05644(2) 0.02546(8) Uani 1 1 d . . . . .
Tb2 Tb -0.45368(2) 0.25787(2) 0.12557(2) 0.02489(8) Uani 1 1 d . . . . .
N1 N -0.4735(3) 0.2953(3) 0.2515(2) 0.0275(11) Uani 1 1 d . . . . .
N2 N -0.4931(3) 0.1455(3) 0.2031(2) 0.0294(11) Uani 1 1 d . . . . .
N3 N -0.1882(3) 0.3113(3) -0.0271(2) 0.0274(11) Uani 1 1 d . . . . .
N4 N -0.2126(4) 0.1595(3) -0.0691(3) 0.0355(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.360(7) . ?
C1 C10 1.438(7) . ?
C1 S1 1.753(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.409(8) . ?
C3 C4 1.424(7) 4_666 ?
C3 C8 1.409(8) . ?
C4 C3 1.424(7) 4_565 ?
C4 H4 0.9300 . ?
C4 C5 1.363(8) . ?
C5 C6 1.410(8) . ?
C5 S2 1.759(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.360(8) 4_565 ?
C7 C6 1.360(8) 4_666 ?
C7 H7 0.9300 . ?
C7 C8 1.419(8) . ?
C8 C9 1.424(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.369(8) . ?
C10 O7 1.362(6) . ?
C11 C12 1.372(8) . ?
C11 C20 1.428(8) . ?
C11 O14 1.350(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.405(7) . ?
C13 C14 1.421(8) 4_565 ?
C13 C18 1.419(8) . ?
C14 C13 1.421(8) 4_666 ?
C14 H14 0.9300 . ?
C14 C15 1.371(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.402(8) . ?
C16 C17 1.371(8) . ?
C16 S4 1.766(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.417(7) 4_666 ?
C18 C17 1.417(7) 4_565 ?
C18 C19 1.415(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.355(7) . ?
C20 S3 1.760(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.399(9) . ?
C21 N1 1.335(8) . ?
C22 H22 0.9300 . ?
C22 C23 1.363(11) . ?
C23 H23 0.9300 . ?
C23 C24 1.399(10) . ?
C24 C25 1.423(10) . ?
C24 C32 1.425(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.354(11) . ?
C26 H26 0.9300 . ?
C26 C27 1.423(9) . ?
C27 C28 1.407(10) . ?
C27 C31 1.408(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.358(10) . ?
C29 H29 0.9300 . ?
C29 C30 1.390(9) . ?
C30 H30 0.9300 . ?
C30 N2 1.329(8) . ?
C31 C32 1.430(8) . ?
C31 N2 1.368(7) . ?
C32 N1 1.353(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.389(9) . ?
C33 N3 1.333(8) . ?
C34 H34 0.9300 . ?
C34 C35 1.370(9) . ?
C35 H35 0.9300 . ?
C35 C36 1.406(9) . ?
C36 C37 1.431(9) . ?
C36 C44 1.405(8) . ?
C37 H37 0.9300 . ?
C37 C38 1.338(10) . ?
C38 H38 0.9300 . ?
C38 C39 1.439(9) . ?
C39 C40 1.401(10) . ?
C39 C43 1.399(8) . ?
C40 H40 0.9300 . ?
C40 C41 1.356(10) . ?
C41 H41 0.9300 . ?
C41 C42 1.391(9) . ?
C42 H42 0.9300 . ?
C42 N4 1.334(8) . ?
C43 C44 1.438(9) . ?
C43 N4 1.370(8) . ?
C44 N3 1.355(7) . ?
O1 S1 1.486(4) . ?
O1 Tb1 2.408(4) . ?
O2 S1 1.430(4) . ?
O3 S1 1.471(4) . ?
O3 Tb2 2.381(4) . ?
O4 S2 1.486(4) . ?
O4 Tb2 2.413(4) . ?
O5 S2 1.477(4) . ?
O5 Tb2 2.466(4) . ?
O6 S2 1.432(4) . ?
O7 Tb1 2.330(4) . ?
O7 Tb2 2.355(4) . ?
O8 S3 1.451(4) . ?
O8 Tb1 2.455(4) . ?
O9 S3 1.430(4) . ?
O10 S3 1.478(4) . ?
O10 Tb2 2.399(4) . ?
O11 S4 1.449(5) . ?
O12 S4 1.466(4) . ?
O12 Tb1 2.340(4) . ?
O13 S4 1.449(5) . ?
O14 Tb1 2.392(4) . ?
O14 Tb2 2.318(4) . ?
O15 H15A 0.8733 . ?
O15 H15B 0.8715 . ?
O15 Tb1 2.349(4) . ?
O16 H16A 0.8530 . ?
O16 H16B 0.8522 . ?
O17 H17A 0.8537 . ?
O17 H17B 0.8515 . ?
O18 H18A 0.8516 . ?
O18 H18B 0.8512 . ?
S2 Tb2 3.0252(15) . ?
Tb1 Tb2 3.7587(4) . ?
Tb1 N3 2.556(5) . ?
Tb1 N4 2.541(5) . ?
Tb2 N1 2.529(4) . ?
Tb2 N2 2.530(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 121.6(5) . . ?
C2 C1 S1 122.2(4) . . ?
C10 C1 S1 116.2(4) . . ?
C1 C2 H2 120.3 . . ?
C1 C2 C3 119.5(5) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 C4 120.9(5) . 4_666 ?
C8 C3 C2 119.4(5) . . ?
C8 C3 C4 119.6(5) . 4_666 ?
C3 C4 H4 120.0 4_565 . ?
C5 C4 C3 120.0(5) . 4_565 ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.4(5) . . ?
C4 C5 S2 121.0(5) . . ?
C6 C5 S2 118.6(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(6) 4_565 . ?
C7 C6 H6 119.7 4_565 . ?
C6 C7 H7 119.6 4_666 . ?
C6 C7 C8 120.7(6) 4_666 . ?
C8 C7 H7 119.6 . . ?
C3 C8 C7 118.5(5) . . ?
C3 C8 C9 120.2(5) . . ?
C7 C8 C9 121.2(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.5(5) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C1 119.1(5) . . ?
O7 C10 C1 117.7(5) . . ?
O7 C10 C9 123.2(5) . . ?
C12 C11 C20 118.2(5) . . ?
O14 C11 C12 123.3(5) . . ?
O14 C11 C20 118.5(5) . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 121.1(5) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 121.8(5) . 4_565 ?
C12 C13 C18 119.6(5) . . ?
C18 C13 C14 118.5(5) . 4_565 ?
C13 C14 H14 119.5 4_666 . ?
C15 C14 C13 121.0(6) . 4_666 ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.9(6) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 S4 118.9(4) . . ?
C17 C16 C15 121.0(5) . . ?
C17 C16 S4 119.9(5) . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.1(5) . 4_666 ?
C18 C17 H17 120.0 4_666 . ?
C17 C18 C13 119.4(5) 4_565 . ?
C19 C18 C13 118.6(5) . . ?
C19 C18 C17 122.0(5) . 4_565 ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.2(5) . . ?
C20 C19 H19 119.9 . . ?
C11 C20 S3 115.4(4) . . ?
C19 C20 C11 121.7(5) . . ?
C19 C20 S3 122.9(4) . . ?
C22 C21 H21 118.7 . . ?
N1 C21 H21 118.7 . . ?
N1 C21 C22 122.6(7) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(7) . . ?
C23 C22 H22 120.4 . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C24 120.3(6) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 123.6(6) . . ?
C23 C24 C32 117.2(6) . . ?
C25 C24 C32 119.2(7) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.2(6) . . ?
C26 C25 H25 119.4 . . ?
C25 C26 H26 119.5 . . ?
C25 C26 C27 121.0(6) . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 123.4(6) . . ?
C28 C27 C31 117.0(6) . . ?
C31 C27 C26 119.6(6) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.8(6) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.6(7) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 118.4 . . ?
N2 C30 C29 123.3(6) . . ?
N2 C30 H30 118.4 . . ?
C27 C31 C32 119.8(5) . . ?
N2 C31 C27 122.9(6) . . ?
N2 C31 C32 117.3(5) . . ?
C24 C32 C31 119.2(6) . . ?
N1 C32 C24 122.0(6) . . ?
N1 C32 C31 118.9(5) . . ?
C34 C33 H33 118.5 . . ?
N3 C33 H33 118.5 . . ?
N3 C33 C34 122.9(6) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0(6) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 120.6 . . ?
C34 C35 C36 118.7(6) . . ?
C36 C35 H35 120.6 . . ?
C35 C36 C37 122.1(6) . . ?
C44 C36 C35 117.7(6) . . ?
C44 C36 C37 120.3(6) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 C36 120.9(6) . . ?
C38 C37 H37 119.6 . . ?
C37 C38 H38 119.5 . . ?
C37 C38 C39 120.9(6) . . ?
C39 C38 H38 119.5 . . ?
C40 C39 C38 122.9(6) . . ?
C43 C39 C38 119.2(6) . . ?
C43 C39 C40 117.9(6) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 C39 119.6(6) . . ?
C41 C40 H40 120.2 . . ?
C40 C41 H41 120.3 . . ?
C40 C41 C42 119.3(7) . . ?
C42 C41 H41 120.3 . . ?
C41 C42 H42 118.2 . . ?
N4 C42 C41 123.5(6) . . ?
N4 C42 H42 118.2 . . ?
C39 C43 C44 120.2(6) . . ?
N4 C43 C39 122.6(6) . . ?
N4 C43 C44 117.2(5) . . ?
C36 C44 C43 118.4(5) . . ?
N3 C44 C36 123.0(6) . . ?
N3 C44 C43 118.5(5) . . ?
S1 O1 Tb1 128.3(2) . . ?
S1 O3 Tb2 125.5(2) . . ?
S2 O4 Tb2 99.0(2) . . ?
S2 O5 Tb2 97.0(2) . . ?
C10 O7 Tb1 123.5(3) . . ?
C10 O7 Tb2 117.0(3) . . ?
Tb1 O7 Tb2 106.70(14) . . ?
S3 O8 Tb1 128.6(2) . . ?
S3 O10 Tb2 125.5(2) . . ?
S4 O12 Tb1 143.1(3) . . ?
C11 O14 Tb1 116.5(3) . . ?
C11 O14 Tb2 125.7(3) . . ?
Tb2 O14 Tb1 105.89(14) . . ?
H15A O15 H15B 108.3 . . ?
Tb1 O15 H15A 110.3 . . ?
Tb1 O15 H15B 109.9 . . ?
H16A O16 H16B 109.6 . . ?
H17A O17 H17B 109.5 . . ?
H18A O18 H18B 109.6 . . ?
O1 S1 C1 104.5(2) . . ?
O2 S1 C1 109.1(3) . . ?
O2 S1 O1 112.5(2) . . ?
O2 S1 O3 113.6(3) . . ?
O3 S1 C1 106.0(2) . . ?
O3 S1 O1 110.5(2) . . ?
C5 S2 Tb2 114.4(2) . . ?
O4 S2 C5 106.6(3) . . ?
O4 S2 Tb2 51.97(17) . . ?
O5 S2 C5 107.2(3) . . ?
O5 S2 O4 105.7(2) . . ?
O5 S2 Tb2 54.02(16) . . ?
O6 S2 C5 108.2(3) . . ?
O6 S2 O4 113.9(3) . . ?
O6 S2 O5 114.7(3) . . ?
O6 S2 Tb2 137.34(19) . . ?
O8 S3 C20 105.8(2) . . ?
O8 S3 O10 110.3(2) . . ?
O9 S3 C20 108.2(2) . . ?
O9 S3 O8 114.1(2) . . ?
O9 S3 O10 113.0(2) . . ?
O10 S3 C20 104.7(2) . . ?
O11 S4 C16 107.7(3) . . ?
O11 S4 O12 109.7(3) . . ?
O12 S4 C16 105.8(3) . . ?
O13 S4 C16 106.8(3) . . ?
O13 S4 O11 114.1(3) . . ?
O13 S4 O12 112.3(3) . . ?
O1 Tb1 O8 143.12(13) . . ?
O1 Tb1 Tb2 74.51(9) . . ?
O1 Tb1 N3 77.91(14) . . ?
O1 Tb1 N4 140.44(15) . . ?
O7 Tb1 O1 72.48(13) . . ?
O7 Tb1 O8 76.10(13) . . ?
O7 Tb1 O12 117.95(13) . . ?
O7 Tb1 O14 73.22(12) . . ?
O7 Tb1 O15 81.91(15) . . ?
O7 Tb1 Tb2 36.88(9) . . ?
O7 Tb1 N3 139.92(14) . . ?
O7 Tb1 N4 146.07(15) . . ?
O8 Tb1 Tb2 68.78(9) . . ?
O8 Tb1 N3 117.35(14) . . ?
O8 Tb1 N4 70.28(15) . . ?
O12 Tb1 O1 73.97(14) . . ?
O12 Tb1 O8 139.67(14) . . ?
O12 Tb1 O14 146.55(14) . . ?
O12 Tb1 O15 74.85(15) . . ?
O12 Tb1 Tb2 145.37(10) . . ?
O12 Tb1 N3 77.56(15) . . ?
O12 Tb1 N4 86.41(15) . . ?
O14 Tb1 O1 80.82(13) . . ?
O14 Tb1 O8 71.94(13) . . ?
O14 Tb1 Tb2 36.38(9) . . ?
O14 Tb1 N3 75.92(14) . . ?
O14 Tb1 N4 99.95(15) . . ?
O15 Tb1 O1 122.91(14) . . ?
O15 Tb1 O8 69.94(14) . . ?
O15 Tb1 O14 138.36(14) . . ?
O15 Tb1 Tb2 111.71(11) . . ?
O15 Tb1 N3 137.72(15) . . ?
O15 Tb1 N4 82.49(17) . . ?
N3 Tb1 Tb2 109.26(10) . . ?
N4 Tb1 Tb2 127.64(12) . . ?
N4 Tb1 N3 64.29(16) . . ?
O3 Tb2 O4 74.76(13) . . ?
O3 Tb2 O5 129.25(13) . . ?
O3 Tb2 O10 147.32(13) . . ?
O3 Tb2 S2 102.79(10) . . ?
O3 Tb2 Tb1 72.65(9) . . ?
O3 Tb2 N1 72.12(14) . . ?
O3 Tb2 N2 123.02(14) . . ?
O4 Tb2 O5 57.90(14) . . ?
O4 Tb2 S2 29.02(10) . . ?
O4 Tb2 Tb1 120.60(11) . . ?
O4 Tb2 N1 84.31(15) . . ?
O4 Tb2 N2 132.28(15) . . ?
O5 Tb2 S2 28.99(10) . . ?
O5 Tb2 Tb1 146.37(9) . . ?
O5 Tb2 N1 85.23(14) . . ?
O5 Tb2 N2 82.90(14) . . ?
O7 Tb2 O3 76.04(13) . . ?
O7 Tb2 O4 148.23(14) . . ?
O7 Tb2 O5 153.67(13) . . ?
O7 Tb2 O10 88.85(13) . . ?
O7 Tb2 S2 174.92(9) . . ?
O7 Tb2 Tb1 36.42(8) . . ?
O7 Tb2 N1 98.41(13) . . ?
O7 Tb2 N2 75.32(14) . . ?
O10 Tb2 O4 109.54(13) . . ?
O10 Tb2 O5 72.44(13) . . ?
O10 Tb2 S2 89.70(10) . . ?
O10 Tb2 Tb1 78.00(9) . . ?
O10 Tb2 N1 139.65(14) . . ?
O10 Tb2 N2 79.11(14) . . ?
O14 Tb2 O3 74.55(13) . . ?
O14 Tb2 O4 86.25(14) . . ?
O14 Tb2 O5 116.04(13) . . ?
O14 Tb2 O7 74.12(12) . . ?
O14 Tb2 O10 73.48(13) . . ?
O14 Tb2 S2 100.80(10) . . ?
O14 Tb2 Tb1 37.73(9) . . ?
O14 Tb2 N1 146.66(14) . . ?
O14 Tb2 N2 138.90(14) . . ?
S2 Tb2 Tb1 138.51(3) . . ?
N1 Tb2 S2 85.83(11) . . ?
N1 Tb2 Tb1 128.28(11) . . ?
N1 Tb2 N2 64.82(15) . . ?
N2 Tb2 S2 109.17(11) . . ?
N2 Tb2 Tb1 107.12(11) . . ?
C21 N1 C32 118.8(5) . . ?
C21 N1 Tb2 122.6(4) . . ?
C32 N1 Tb2 117.0(4) . . ?
C30 N2 C31 117.4(5) . . ?
C30 N2 Tb2 123.6(4) . . ?
C31 N2 Tb2 117.0(4) . . ?
C33 N3 C44 117.6(5) . . ?
C33 N3 Tb1 122.9(4) . . ?
C44 N3 Tb1 118.2(4) . . ?
C42 N4 C43 117.0(5) . . ?
C42 N4 Tb1 122.9(4) . . ?
C43 N4 Tb1 118.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -178.6(5) . . . 4_666 ?
C1 C2 C3 C8 3.7(8) . . . . ?
C1 C10 O7 Tb1 75.0(5) . . . . ?
C1 C10 O7 Tb2 -61.3(5) . . . . ?
C2 C1 C10 C9 -9.3(8) . . . . ?
C2 C1 C10 O7 168.6(5) . . . . ?
C2 C1 S1 O1 129.6(5) . . . . ?
C2 C1 S1 O2 9.1(6) . . . . ?
C2 C1 S1 O3 -113.6(5) . . . . ?
C2 C3 C8 C7 175.1(6) . . . . ?
C2 C3 C8 C9 -7.0(9) . . . . ?
C3 C4 C5 C6 -2.3(9) 4_565 . . . ?
C3 C4 C5 S2 -179.5(4) 4_565 . . . ?
C3 C8 C9 C10 2.0(9) . . . . ?
C4 C3 C8 C7 -2.7(9) 4_666 . . . ?
C4 C3 C8 C9 175.3(5) 4_666 . . . ?
C4 C5 C6 C7 3.1(10) . . . 4_565 ?
C4 C5 S2 O4 106.3(5) . . . . ?
C4 C5 S2 O5 -6.6(6) . . . . ?
C4 C5 S2 O6 -130.8(5) . . . . ?
C4 C5 S2 Tb2 51.1(5) . . . . ?
C6 C5 S2 O4 -71.0(5) . . . . ?
C6 C5 S2 O5 176.1(5) . . . . ?
C6 C5 S2 O6 51.9(6) . . . . ?
C6 C5 S2 Tb2 -126.2(5) . . . . ?
C6 C7 C8 C3 1.9(10) 4_666 . . . ?
C6 C7 C8 C9 -176.0(6) 4_666 . . . ?
C7 C8 C9 C10 180.0(6) . . . . ?
C8 C9 C10 C1 5.9(8) . . . . ?
C8 C9 C10 O7 -171.9(5) . . . . ?
C9 C10 O7 Tb1 -107.2(5) . . . . ?
C9 C10 O7 Tb2 116.5(5) . . . . ?
C10 C1 C2 C3 4.4(8) . . . . ?
C10 C1 S1 O1 -49.6(5) . . . . ?
C10 C1 S1 O2 -170.1(4) . . . . ?
C10 C1 S1 O3 67.2(5) . . . . ?
C11 C12 C13 C14 -172.9(6) . . . 4_565 ?
C11 C12 C13 C18 3.0(9) . . . . ?
C11 C20 S3 O8 -63.0(5) . . . . ?
C11 C20 S3 O9 174.2(4) . . . . ?
C11 C20 S3 O10 53.5(5) . . . . ?
C12 C11 C20 C19 6.9(8) . . . . ?
C12 C11 C20 S3 -173.5(4) . . . . ?
C12 C11 O14 Tb1 -110.6(5) . . . . ?
C12 C11 O14 Tb2 112.2(5) . . . . ?
C12 C13 C18 C17 -173.4(5) . . . 4_565 ?
C12 C13 C18 C19 4.4(8) . . . . ?
C13 C14 C15 C16 -3.0(10) 4_666 . . . ?
C13 C18 C19 C20 -6.1(8) . . . . ?
C14 C13 C18 C17 2.6(8) 4_565 . . 4_565 ?
C14 C13 C18 C19 -179.5(5) 4_565 . . . ?
C14 C15 C16 C17 -1.0(10) . . . . ?
C14 C15 C16 S4 174.4(5) . . . . ?
C15 C16 C17 C18 3.1(9) . . . 4_666 ?
C15 C16 S4 O11 -101.0(5) . . . . ?
C15 C16 S4 O12 141.7(5) . . . . ?
C15 C16 S4 O13 21.9(6) . . . . ?
C17 C16 S4 O11 74.4(6) . . . . ?
C17 C16 S4 O12 -42.9(6) . . . . ?
C17 C16 S4 O13 -162.6(5) . . . . ?
C17 C18 C19 C20 171.7(5) 4_565 . . . ?
C18 C19 C20 C11 0.5(8) . . . . ?
C18 C19 C20 S3 -179.1(4) . . . . ?
C19 C20 S3 O8 116.6(5) . . . . ?
C19 C20 S3 O9 -6.1(6) . . . . ?
C19 C20 S3 O10 -126.9(5) . . . . ?
C20 C11 C12 C13 -8.6(8) . . . . ?
C20 C11 O14 Tb1 67.0(5) . . . . ?
C20 C11 O14 Tb2 -70.3(6) . . . . ?
C21 C22 C23 C24 0.1(12) . . . . ?
C22 C21 N1 C32 0.1(10) . . . . ?
C22 C21 N1 Tb2 -165.0(5) . . . . ?
C22 C23 C24 C25 180.0(7) . . . . ?
C22 C23 C24 C32 -2.2(11) . . . . ?
C23 C24 C25 C26 177.9(7) . . . . ?
C23 C24 C32 C31 -177.2(6) . . . . ?
C23 C24 C32 N1 3.5(10) . . . . ?
C24 C25 C26 C27 -1.6(11) . . . . ?
C24 C32 N1 C21 -2.5(9) . . . . ?
C24 C32 N1 Tb2 163.5(5) . . . . ?
C25 C24 C32 C31 0.7(9) . . . . ?
C25 C24 C32 N1 -178.6(6) . . . . ?
C25 C26 C27 C28 -175.2(7) . . . . ?
C25 C26 C27 C31 2.3(10) . . . . ?
C26 C27 C28 C29 179.2(7) . . . . ?
C26 C27 C31 C32 -1.5(9) . . . . ?
C26 C27 C31 N2 -180.0(6) . . . . ?
C27 C28 C29 C30 -0.4(12) . . . . ?
C27 C31 C32 C24 0.0(9) . . . . ?
C27 C31 C32 N1 179.3(5) . . . . ?
C27 C31 N2 C30 1.7(9) . . . . ?
C27 C31 N2 Tb2 -162.6(4) . . . . ?
C28 C27 C31 C32 176.2(6) . . . . ?
C28 C27 C31 N2 -2.2(9) . . . . ?
C28 C29 C30 N2 -0.2(12) . . . . ?
C29 C30 N2 C31 -0.4(10) . . . . ?
C29 C30 N2 Tb2 162.7(5) . . . . ?
C31 C27 C28 C29 1.5(10) . . . . ?
C31 C32 N1 C21 178.2(6) . . . . ?
C31 C32 N1 Tb2 -15.8(7) . . . . ?
C32 C24 C25 C26 0.1(11) . . . . ?
C32 C31 N2 C30 -176.8(5) . . . . ?
C32 C31 N2 Tb2 18.9(6) . . . . ?
C33 C34 C35 C36 -1.9(10) . . . . ?
C34 C33 N3 C44 1.7(9) . . . . ?
C34 C33 N3 Tb1 -165.3(5) . . . . ?
C34 C35 C36 C37 -178.7(6) . . . . ?
C34 C35 C36 C44 1.5(9) . . . . ?
C35 C36 C37 C38 179.8(6) . . . . ?
C35 C36 C44 C43 180.0(6) . . . . ?
C35 C36 C44 N3 0.6(9) . . . . ?
C36 C37 C38 C39 -0.8(11) . . . . ?
C36 C44 N3 C33 -2.2(9) . . . . ?
C36 C44 N3 Tb1 165.5(4) . . . . ?
C37 C36 C44 C43 0.1(9) . . . . ?
C37 C36 C44 N3 -179.2(6) . . . . ?
C37 C38 C39 C40 -179.0(7) . . . . ?
C37 C38 C39 C43 2.2(10) . . . . ?
C38 C39 C40 C41 -178.7(7) . . . . ?
C38 C39 C43 C44 -2.4(9) . . . . ?
C38 C39 C43 N4 177.4(6) . . . . ?
C39 C40 C41 C42 1.4(12) . . . . ?
C39 C43 C44 C36 1.3(9) . . . . ?
C39 C43 C44 N3 -179.3(5) . . . . ?
C39 C43 N4 C42 1.2(9) . . . . ?
C39 C43 N4 Tb1 -167.0(5) . . . . ?
C40 C39 C43 C44 178.8(6) . . . . ?
C40 C39 C43 N4 -1.4(10) . . . . ?
C40 C41 C42 N4 -1.7(12) . . . . ?
C41 C42 N4 C43 0.3(10) . . . . ?
C41 C42 N4 Tb1 168.0(5) . . . . ?
C43 C39 C40 C41 0.0(11) . . . . ?
C43 C44 N3 C33 178.5(5) . . . . ?
C43 C44 N3 Tb1 -13.9(7) . . . . ?
C44 C36 C37 C38 -0.4(10) . . . . ?
C44 C43 N4 C42 -179.0(6) . . . . ?
C44 C43 N4 Tb1 12.8(7) . . . . ?
O14 C11 C12 C13 169.0(5) . . . . ?
O14 C11 C20 C19 -170.8(5) . . . . ?
O14 C11 C20 S3 8.9(7) . . . . ?
S1 C1 C2 C3 -174.7(4) . . . . ?
S1 C1 C10 C9 169.8(4) . . . . ?
S1 C1 C10 O7 -12.3(6) . . . . ?
S2 C5 C6 C7 -179.6(5) . . . 4_565 ?
S4 C16 C17 C18 -172.2(4) . . . 4_666 ?
Tb1 O1 S1 C1 61.8(3) . . . . ?
Tb1 O1 S1 O2 -180.0(3) . . . . ?
Tb1 O1 S1 O3 -51.8(3) . . . . ?
Tb1 O8 S3 C20 41.2(3) . . . . ?
Tb1 O8 S3 O9 160.1(2) . . . . ?
Tb1 O8 S3 O10 -71.5(3) . . . . ?
Tb1 O12 S4 C16 -77.1(4) . . . . ?
Tb1 O12 S4 O11 166.9(4) . . . . ?
Tb1 O12 S4 O13 39.0(5) . . . . ?
Tb2 O3 S1 C1 -44.3(3) . . . . ?
Tb2 O3 S1 O1 68.4(3) . . . . ?
Tb2 O3 S1 O2 -164.1(2) . . . . ?
Tb2 O4 S2 C5 -108.4(2) . . . . ?
Tb2 O4 S2 O5 5.5(2) . . . . ?
Tb2 O4 S2 O6 132.4(2) . . . . ?
Tb2 O5 S2 C5 108.1(2) . . . . ?
Tb2 O5 S2 O4 -5.3(2) . . . . ?
Tb2 O5 S2 O6 -131.8(2) . . . . ?
Tb2 O10 S3 C20 -65.7(3) . . . . ?
Tb2 O10 S3 O8 47.7(3) . . . . ?
Tb2 O10 S3 O9 176.8(2) . . . . ?
N1 C21 C22 C23 1.1(12) . . . . ?
N2 C31 C32 C24 178.6(5) . . . . ?
N2 C31 C32 N1 -2.1(8) . . . . ?
N3 C33 C34 C35 0.3(10) . . . . ?
N4 C43 C44 C36 -178.6(5) . . . . ?
N4 C43 C44 N3 0.8(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Phase3-Yb
_database_code_depnum_ccdc_archive 'CCDC 1477863'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_audit_creation_date             2015-10-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H28 N4 O15 S4 Yb2, 3(H2 O)'
_chemical_formula_sum            'C44 H34 N4 O18 S4 Yb2'
_chemical_formula_weight         1381.07
_chemical_melting_point          ?
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2136(4)
_cell_length_b                   17.0112(5)
_cell_length_c                   18.8325(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.0140(10)
_cell_angle_gamma                90
_cell_volume                     4497.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9216
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      1.6
_cell_measurement_theta_min      26.4
_shelx_estimated_absorpt_T_max   0.879
_shelx_estimated_absorpt_T_min   0.521
_exptl_absorpt_coefficient_mu    4.404
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0942 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.8629.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2696
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         1.622
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7320
_reflns_number_total             9216
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 20015)'
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0276
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0180P)²+5.4786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0576
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B,O17,H17A,H17B,O18,H18A,H18B)
2.b Rotating group:
 O15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15),
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C -0.2363(3) 0.2598(2) 0.2525(2) 0.0182(9) Uani 1 1 d . . . . .
C2 C -0.2074(3) 0.2683(2) 0.3244(2) 0.0197(9) Uani 1 1 d . . . . .
H2 H -0.1921 0.3177 0.3440 0.024 Uiso 1 1 calc R . . . .
C3 C -0.2009(3) 0.2013(2) 0.3687(2) 0.0187(9) Uani 1 1 d . . . . .
C4 C -0.6733(3) 0.2933(2) -0.0556(2) 0.0219(10) Uani 1 1 d . . . . .
H4 H -0.6626 0.2444 -0.0339 0.026 Uiso 1 1 calc R . . . .
C5 C -0.6626(3) 0.3596(2) -0.0148(2) 0.0211(10) Uani 1 1 d . . . . .
C6 C -0.6767(3) 0.4344(3) -0.0467(2) 0.0299(11) Uani 1 1 d . . . . .
H6 H -0.6664 0.4793 -0.0183 0.036 Uiso 1 1 calc R . . . .
C7 C -0.2052(4) 0.0588(2) 0.3814(2) 0.0318(12) Uani 1 1 d . . . . .
H7 H -0.2153 0.0091 0.3611 0.038 Uiso 1 1 calc R . . . .
C8 C -0.2200(3) 0.1260(2) 0.3365(2) 0.0213(10) Uani 1 1 d . . . . .
C9 C -0.2547(3) 0.1201(2) 0.2620(2) 0.0223(10) Uani 1 1 d . . . . .
H9 H -0.2689 0.0710 0.2412 0.027 Uiso 1 1 calc R . . . .
C10 C -0.2675(3) 0.1867(2) 0.2204(2) 0.0190(9) Uani 1 1 d . . . . .
C11 C -0.4096(3) 0.2852(2) -0.0391(2) 0.0185(9) Uani 1 1 d . . . . .
C12 C -0.4113(3) 0.3539(2) -0.0773(2) 0.0225(10) Uani 1 1 d . . . . .
H12 H -0.3941 0.4008 -0.0534 0.027 Uiso 1 1 calc R . . . .
C13 C -0.4393(3) 0.3540(2) -0.1532(2) 0.0201(9) Uani 1 1 d . . . . .
C14 C 0.0701(3) 0.0781(3) 0.3054(2) 0.0307(11) Uani 1 1 d . . . . .
H14 H 0.0872 0.0306 0.3284 0.037 Uiso 1 1 calc R . . . .
C15 C 0.0542(3) 0.0813(3) 0.2321(2) 0.0281(11) Uani 1 1 d . . . . .
H15 H 0.0617 0.0363 0.2055 0.034 Uiso 1 1 calc R . . . .
C16 C 0.0267(3) 0.1521(2) 0.1966(2) 0.0219(10) Uani 1 1 d . . . . .
C17 C 0.0129(3) 0.2186(2) 0.2351(2) 0.0224(10) Uani 1 1 d . . . . .
H17 H -0.0082 0.2647 0.2111 0.027 Uiso 1 1 calc R . . . .
C18 C -0.4694(3) 0.2828(2) -0.1889(2) 0.0194(9) Uani 1 1 d . . . . .
C19 C -0.4780(3) 0.2150(2) -0.1479(2) 0.0214(10) Uani 1 1 d . . . . .
H19 H -0.5035 0.1692 -0.1702 0.026 Uiso 1 1 calc R . . . .
C20 C -0.4486(3) 0.2165(2) -0.0750(2) 0.0183(9) Uani 1 1 d . . . . .
C21 C -0.4641(3) 0.3706(3) 0.2701(2) 0.0332(12) Uani 1 1 d . . . . .
H21 H -0.4673 0.4106 0.2361 0.040 Uiso 1 1 calc R . . . .
C22 C -0.4534(4) 0.3911(3) 0.3431(3) 0.0439(14) Uani 1 1 d . . . . .
H22 H -0.4506 0.4437 0.3570 0.053 Uiso 1 1 calc R . . . .
C23 C -0.4472(4) 0.3336(3) 0.3928(3) 0.0458(14) Uani 1 1 d . . . . .
H23 H -0.4390 0.3466 0.4413 0.055 Uiso 1 1 calc R . . . .
C24 C -0.4531(3) 0.2540(3) 0.3719(2) 0.0327(12) Uani 1 1 d . . . . .
C25 C -0.4465(4) 0.1904(3) 0.4212(3) 0.0428(14) Uani 1 1 d . . . . .
H25 H -0.4366 0.2005 0.4704 0.051 Uiso 1 1 calc R . . . .
C26 C -0.4544(4) 0.1157(3) 0.3976(3) 0.0423(14) Uani 1 1 d . . . . .
H26 H -0.4484 0.0748 0.4308 0.051 Uiso 1 1 calc R . . . .
C27 C -0.4720(3) 0.0980(3) 0.3226(2) 0.0285(11) Uani 1 1 d . . . . .
C28 C -0.4864(4) 0.0210(3) 0.2954(3) 0.0421(14) Uani 1 1 d . . . . .
H28 H -0.4840 -0.0216 0.3266 0.051 Uiso 1 1 calc R . . . .
C29 C -0.5037(4) 0.0099(3) 0.2232(3) 0.0446(14) Uani 1 1 d . . . . .
H29 H -0.5151 -0.0404 0.2046 0.053 Uiso 1 1 calc R . . . .
C30 C -0.5043(3) 0.0733(3) 0.1771(2) 0.0315(11) Uani 1 1 d . . . . .
H30 H -0.5153 0.0639 0.1279 0.038 Uiso 1 1 calc R . . . .
C31 C -0.4762(3) 0.1597(3) 0.2723(2) 0.0219(10) Uani 1 1 d . . . . .
C32 C -0.4657(3) 0.2388(3) 0.2972(2) 0.0236(10) Uani 1 1 d . . . . .
C33 C -0.1756(4) 0.3857(3) -0.0061(2) 0.0343(12) Uani 1 1 d . . . . .
H33 H -0.1673 0.3976 0.0427 0.041 Uiso 1 1 calc R . . . .
C34 C -0.1734(4) 0.4470(3) -0.0546(3) 0.0366(12) Uani 1 1 d . . . . .
H34 H -0.1633 0.4984 -0.0382 0.044 Uiso 1 1 calc R . . . .
C35 C -0.1860(3) 0.4312(3) -0.1266(3) 0.0357(12) Uani 1 1 d . . . . .
H35 H -0.1871 0.4718 -0.1597 0.043 Uiso 1 1 calc R . . . .
C36 C -0.1974(3) 0.3537(3) -0.1497(2) 0.0276(11) Uani 1 1 d . . . . .
C37 C -0.2091(3) 0.3313(3) -0.2241(2) 0.0371(13) Uani 1 1 d . . . . .
H37 H -0.2096 0.3701 -0.2589 0.045 Uiso 1 1 calc R . . . .
C38 C -0.2193(4) 0.2562(3) -0.2448(2) 0.0399(13) Uani 1 1 d . . . . .
H38 H -0.2267 0.2437 -0.2934 0.048 Uiso 1 1 calc R . . . .
C39 C -0.2190(3) 0.1947(3) -0.1928(2) 0.0323(11) Uani 1 1 d . . . . .
C40 C -0.2276(4) 0.1145(3) -0.2113(3) 0.0481(15) Uani 1 1 d . . . . .
H40 H -0.2331 0.0992 -0.2592 0.058 Uiso 1 1 calc R . . . .
C41 C -0.2278(4) 0.0597(3) -0.1588(3) 0.0505(15) Uani 1 1 d . . . . .
H41 H -0.2327 0.0065 -0.1703 0.061 Uiso 1 1 calc R . . . .
C42 C -0.2207(4) 0.0840(3) -0.0877(3) 0.0378(13) Uani 1 1 d . . . . .
H42 H -0.2224 0.0459 -0.0526 0.045 Uiso 1 1 calc R . . . .
C43 C -0.2101(3) 0.2140(3) -0.1193(2) 0.0233(10) Uani 1 1 d . . . . .
C44 C -0.1982(3) 0.2942(3) -0.0975(2) 0.0250(10) Uani 1 1 d . . . . .
O1 O -0.1854(2) 0.30802(16) 0.13511(14) 0.0237(7) Uani 1 1 d . . . . .
O2 O -0.1883(2) 0.40469(16) 0.22967(15) 0.0292(7) Uani 1 1 d . . . . .
O3 O -0.3363(2) 0.35441(15) 0.16359(14) 0.0225(7) Uani 1 1 d . . . . .
O4 O -0.5234(2) 0.37953(17) 0.09156(15) 0.0291(7) Uani 1 1 d . . . . .
O5 O -0.6219(2) 0.26993(16) 0.09938(14) 0.0262(7) Uani 1 1 d . . . . .
O6 O -0.6861(2) 0.40215(19) 0.11327(15) 0.0378(9) Uani 1 1 d . . . . .
O7 O -0.31035(19) 0.18690(15) 0.15058(13) 0.0189(6) Uani 1 1 d . . . . .
O8 O -0.3572(2) 0.11481(15) 0.01098(14) 0.0221(7) Uani 1 1 d . . . . .
O9 O -0.5062(2) 0.07281(16) -0.06145(14) 0.0264(7) Uani 1 1 d . . . . .
O10 O -0.5077(2) 0.16399(16) 0.03771(13) 0.0224(7) Uani 1 1 d . . . . .
O11 O 0.1021(2) 0.1956(2) 0.08597(16) 0.0382(8) Uani 1 1 d . . . . .
O12 O -0.0670(2) 0.20521(17) 0.07715(14) 0.0274(7) Uani 1 1 d . . . . .
O13 O 0.0064(2) 0.07675(18) 0.07597(15) 0.0356(8) Uani 1 1 d . . . . .
O14 O -0.3693(2) 0.27890(15) 0.03077(13) 0.0199(6) Uani 1 1 d . . . . .
O15 O -0.1858(2) 0.07670(17) 0.08567(16) 0.0343(8) Uani 1 1 d . . . . .
H15A H -0.1898 0.0666 0.1303 0.051 Uiso 1 1 d GR . . . .
H15B H -0.1273 0.0689 0.0793 0.051 Uiso 1 1 d GR . . . .
O16 O 0.0915(2) 0.37184(17) 0.1069(3) 0.156(3) Uani 1 1 d . . . . .
H16A H 0.0957 0.3774 0.1520 0.233 Uiso 1 1 d G . . . .
H16B H 0.1352 0.3982 0.0920 0.233 Uiso 1 1 d G . . . .
O17 O 0.7118(3) 0.94333(17) 0.0655(2) 0.0710(13) Uani 1 1 d G . . . .
H17A H 0.6880 0.9582 0.1018 0.106 Uiso 1 1 d G . . . .
H17B H 0.6914 0.9725 0.0299 0.106 Uiso 1 1 d G . . . .
O18 O 0.2738(2) 0.11659(14) 0.0714(2) 0.0746(13) Uani 1 1 d G . . . .
H18A H 0.2189 0.1328 0.0766 0.112 Uiso 1 1 d G . . . .
H18B H 0.3100 0.1557 0.0680 0.112 Uiso 1 1 d G . . . .
S1 S -0.23615(8) 0.33905(6) 0.19230(5) 0.0200(2) Uani 1 1 d . . . . .
S2 S -0.62384(8) 0.35400(6) 0.07877(5) 0.0238(3) Uani 1 1 d . . . . .
S3 S -0.45591(8) 0.13435(6) -0.01940(5) 0.0192(2) Uani 1 1 d . . . . .
S4 S 0.01754(8) 0.15684(7) 0.10205(5) 0.0254(3) Uani 1 1 d . . . . .
Yb1 Yb -0.22995(2) 0.20395(2) 0.05569(2) 0.01895(5) Uani 1 1 d . . . . .
Yb2 Yb -0.44979(2) 0.25758(2) 0.12421(2) 0.01803(5) Uani 1 1 d . . . . .
N1 N -0.4698(3) 0.2965(2) 0.24709(17) 0.0235(8) Uani 1 1 d . . . . .
N2 N -0.4902(3) 0.14682(19) 0.19944(17) 0.0224(8) Uani 1 1 d . . . . .
N3 N -0.1892(3) 0.3108(2) -0.02587(17) 0.0230(8) Uani 1 1 d . . . . .
N4 N -0.2116(3) 0.1590(2) -0.06712(18) 0.0263(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.360(5) . ?
C1 C10 1.423(5) . ?
C1 S1 1.761(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.408(5) . ?
C3 C4 1.421(5) 4_666 ?
C3 C8 1.424(5) . ?
C4 C3 1.421(5) 4_565 ?
C4 H4 0.9300 . ?
C4 C5 1.359(5) . ?
C5 C6 1.408(6) . ?
C5 S2 1.764(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.357(6) 4_565 ?
C7 C6 1.357(6) 4_666 ?
C7 H7 0.9300 . ?
C7 C8 1.418(6) . ?
C8 C9 1.416(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.373(5) . ?
C10 O7 1.360(4) . ?
C10 Yb2 3.159(4) . ?
C11 C12 1.371(5) . ?
C11 C20 1.418(5) . ?
C11 O14 1.355(4) . ?
C11 Yb1 3.192(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.421(5) . ?
C13 C14 1.412(6) 4_565 ?
C13 C18 1.418(6) . ?
C14 C13 1.412(6) 4_666 ?
C14 H14 0.9300 . ?
C14 C15 1.366(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.403(6) . ?
C16 C17 1.374(6) . ?
C16 S4 1.767(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.414(5) 4_666 ?
C18 C17 1.414(5) 4_565 ?
C18 C19 1.403(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.371(5) . ?
C20 S3 1.760(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.405(6) . ?
C21 N1 1.332(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.346(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.410(7) . ?
C24 C25 1.420(6) . ?
C24 C32 1.412(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.346(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.428(6) . ?
C27 C28 1.408(7) . ?
C27 C31 1.410(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.357(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.384(6) . ?
C30 H30 0.9300 . ?
C30 N2 1.324(5) . ?
C31 C32 1.426(6) . ?
C31 N2 1.373(5) . ?
C32 N1 1.356(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.390(6) . ?
C33 N3 1.334(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.366(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.390(6) . ?
C36 C37 1.437(6) . ?
C36 C44 1.412(6) . ?
C37 H37 0.9300 . ?
C37 C38 1.337(7) . ?
C38 H38 0.9300 . ?
C38 C39 1.433(6) . ?
C39 C40 1.408(7) . ?
C39 C43 1.409(6) . ?
C40 H40 0.9300 . ?
C40 C41 1.361(7) . ?
C41 H41 0.9300 . ?
C41 C42 1.389(6) . ?
C42 H42 0.9300 . ?
C42 N4 1.334(5) . ?
C43 C44 1.427(6) . ?
C43 N4 1.358(5) . ?
C44 N3 1.365(5) . ?
O1 S1 1.484(3) . ?
O1 Yb1 2.340(3) . ?
O2 S1 1.433(3) . ?
O3 S1 1.465(3) . ?
O3 Yb2 2.343(3) . ?
O4 S2 1.475(3) . ?
O4 Yb2 2.361(3) . ?
O5 S2 1.481(3) . ?
O5 Yb2 2.426(3) . ?
O6 S2 1.434(3) . ?
O7 Yb1 2.285(3) . ?
O7 Yb2 2.305(3) . ?
O8 S3 1.468(3) . ?
O8 Yb1 2.409(3) . ?
O9 S3 1.434(3) . ?
O10 S3 1.483(3) . ?
O10 Yb2 2.334(3) . ?
O11 S4 1.445(3) . ?
O12 S4 1.471(3) . ?
O12 Yb1 2.287(3) . ?
O13 S4 1.449(3) . ?
O14 Yb1 2.340(3) . ?
O14 Yb2 2.273(3) . ?
O15 H15A 0.8680 . ?
O15 H15B 0.8685 . ?
O15 Yb1 2.299(3) . ?
O16 H16A 0.8476 . ?
O16 H16B 0.8490 . ?
O17 H17A 0.8482 . ?
O17 H17B 0.8484 . ?
O18 H18A 0.8486 . ?
O18 H18B 0.8493 . ?
S1 Yb1 3.4611(10) . ?
S1 Yb2 3.4009(11) . ?
S2 Yb2 2.9797(11) . ?
S3 Yb2 3.4121(10) . ?
Yb1 H15A 2.7393 . ?
Yb1 H15B 2.7197 . ?
Yb1 Yb2 3.6776(3) . ?
Yb1 N3 2.506(3) . ?
Yb1 N4 2.488(3) . ?
Yb2 N1 2.466(3) . ?
Yb2 N2 2.478(3) . ?

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
C2 C1 C10 122.7(4) . . ?
C2 C1 S1 121.9(3) . . ?
C10 C1 S1 115.3(3) . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.1(4) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 121.7(4) . 4_666 ?
C2 C3 C8 119.0(3) . . ?
C4 C3 C8 119.3(4) 4_666 . ?
C3 C4 H4 119.9 4_565 . ?
C5 C4 C3 120.2(4) . 4_565 ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 S2 120.6(3) . . ?
C6 C5 S2 118.4(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(4) 4_565 . ?
C7 C6 H6 119.9 4_565 . ?
C6 C7 H7 119.3 4_666 . ?
C6 C7 C8 121.3(4) 4_666 . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 118.0(4) . . ?
C9 C8 C3 120.0(4) . . ?
C9 C8 C7 122.0(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9 120.0 . . ?
C1 C10 Yb2 94.7(2) . . ?
C9 C10 C1 118.3(4) . . ?
C9 C10 Yb2 131.7(3) . . ?
O7 C10 C1 118.1(3) . . ?
O7 C10 C9 123.6(4) . . ?
O7 C10 Yb2 40.66(17) . . ?
C12 C11 C20 118.6(3) . . ?
C12 C11 Yb1 127.6(3) . . ?
C20 C11 Yb1 97.4(2) . . ?
O14 C11 C12 123.2(4) . . ?
O14 C11 C20 118.2(3) . . ?
O14 C11 Yb1 40.80(17) . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 121.3(4) 4_565 . ?
C14 C13 C18 119.0(4) 4_565 . ?
C18 C13 C12 119.4(4) . . ?
C13 C14 H14 119.6 4_666 . ?
C15 C14 C13 120.7(4) . 4_666 ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.3(4) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 S4 119.3(3) . . ?
C17 C16 C15 120.6(4) . . ?
C17 C16 S4 120.0(3) . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.1(4) . 4_666 ?
C18 C17 H17 119.9 4_666 . ?
C17 C18 C13 119.2(4) 4_565 . ?
C19 C18 C13 119.2(3) . . ?
C19 C18 C17 121.6(4) . 4_565 ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.7(4) . . ?
C20 C19 H19 120.2 . . ?
C11 C20 S3 115.2(3) . . ?
C19 C20 C11 121.9(4) . . ?
C19 C20 S3 123.0(3) . . ?
C22 C21 H21 118.5 . . ?
N1 C21 H21 118.5 . . ?
N1 C21 C22 123.1(4) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 C21 119.0(5) . . ?
C23 C22 H22 120.5 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.6(4) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 123.6(4) . . ?
C23 C24 C32 116.5(4) . . ?
C32 C24 C25 119.8(4) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.7(5) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.2(4) . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 123.3(4) . . ?
C28 C27 C31 117.4(4) . . ?
C31 C27 C26 119.4(4) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 C27 119.1(4) . . ?
C29 C28 H28 120.4 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 118.3 . . ?
N2 C30 C29 123.4(4) . . ?
N2 C30 H30 118.3 . . ?
C27 C31 C32 119.4(4) . . ?
N2 C31 C27 122.5(4) . . ?
N2 C31 C32 118.1(4) . . ?
C24 C32 C31 119.4(4) . . ?
N1 C32 C24 123.1(4) . . ?
N1 C32 C31 117.5(4) . . ?
C34 C33 H33 118.3 . . ?
N3 C33 H33 118.3 . . ?
N3 C33 C34 123.4(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 C33 119.4(5) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 120.4 . . ?
C34 C35 C36 119.2(4) . . ?
C36 C35 H35 120.4 . . ?
C35 C36 C37 123.1(4) . . ?
C35 C36 C44 118.4(4) . . ?
C44 C36 C37 118.5(4) . . ?
C36 C37 H37 119.1 . . ?
C38 C37 C36 121.9(4) . . ?
C38 C37 H37 119.1 . . ?
C37 C38 H38 119.7 . . ?
C37 C38 C39 120.6(4) . . ?
C39 C38 H38 119.7 . . ?
C40 C39 C38 123.1(4) . . ?
C40 C39 C43 117.4(4) . . ?
C43 C39 C38 119.5(4) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 C39 119.6(5) . . ?
C41 C40 H40 120.2 . . ?
C40 C41 H41 120.4 . . ?
C40 C41 C42 119.2(5) . . ?
C42 C41 H41 120.4 . . ?
C41 C42 H42 118.1 . . ?
N4 C42 C41 123.7(5) . . ?
N4 C42 H42 118.1 . . ?
C39 C43 C44 119.6(4) . . ?
N4 C43 C39 122.7(4) . . ?
N4 C43 C44 117.7(4) . . ?
C36 C44 C43 119.9(4) . . ?
N3 C44 C36 122.0(4) . . ?
N3 C44 C43 118.1(4) . . ?
S1 O1 Yb1 128.27(17) . . ?
S1 O3 Yb2 124.92(16) . . ?
S2 O4 Yb2 99.31(15) . . ?
S2 O5 Yb2 96.37(15) . . ?
C10 O7 Yb1 123.6(2) . . ?
C10 O7 Yb2 116.7(2) . . ?
Yb1 O7 Yb2 106.49(10) . . ?
S3 O8 Yb1 127.81(16) . . ?
S3 O10 Yb2 125.28(16) . . ?
S4 O12 Yb1 143.60(18) . . ?
C11 O14 Yb1 117.0(2) . . ?
C11 O14 Yb2 125.2(2) . . ?
Yb2 O14 Yb1 105.70(10) . . ?
H15A O15 H15B 108.3 . . ?
Yb1 O15 H15A 111.5 . . ?
Yb1 O15 H15B 109.8 . . ?
H16A O16 H16B 109.5 . . ?
H17A O17 H17B 109.4 . . ?
H18A O18 H18B 109.5 . . ?
C1 S1 Yb1 88.45(13) . . ?
C1 S1 Yb2 80.76(14) . . ?
O1 S1 C1 104.16(18) . . ?
O1 S1 Yb1 32.05(11) . . ?
O1 S1 Yb2 95.06(11) . . ?
O2 S1 C1 109.20(18) . . ?
O2 S1 O1 112.74(18) . . ?
O2 S1 O3 113.63(18) . . ?
O2 S1 Yb1 144.78(14) . . ?
O2 S1 Yb2 146.03(14) . . ?
O3 S1 C1 105.94(18) . . ?
O3 S1 O1 110.50(16) . . ?
O3 S1 Yb1 88.88(11) . . ?
O3 S1 Yb2 34.40(11) . . ?
Yb2 S1 Yb1 64.807(18) . . ?
C5 S2 Yb2 115.60(14) . . ?
O4 S2 C5 106.88(19) . . ?
O4 S2 O5 105.28(17) . . ?
O4 S2 Yb2 51.44(11) . . ?
O5 S2 C5 107.69(18) . . ?
O5 S2 Yb2 54.03(12) . . ?
O6 S2 C5 107.63(19) . . ?
O6 S2 O4 114.08(19) . . ?
O6 S2 O5 114.85(19) . . ?
O6 S2 Yb2 136.71(13) . . ?
C20 S3 Yb2 89.27(13) . . ?
O8 S3 C20 105.67(18) . . ?
O8 S3 O10 110.29(16) . . ?
O8 S3 Yb2 85.77(11) . . ?
O9 S3 C20 108.78(17) . . ?
O9 S3 O8 114.38(17) . . ?
O9 S3 O10 112.83(18) . . ?
O9 S3 Yb2 146.61(13) . . ?
O10 S3 C20 104.10(18) . . ?
O10 S3 Yb2 33.94(11) . . ?
O11 S4 C16 107.42(19) . . ?
O11 S4 O12 110.07(19) . . ?
O11 S4 O13 114.1(2) . . ?
O12 S4 C16 105.93(18) . . ?
O13 S4 C16 106.61(19) . . ?
O13 S4 O12 112.16(18) . . ?
C11 Yb1 H15A 137.7 . . ?
C11 Yb1 H15B 144.9 . . ?
C11 Yb1 S1 90.98(7) . . ?
C11 Yb1 Yb2 55.93(7) . . ?
O1 Yb1 C11 98.21(10) . . ?
O1 Yb1 O8 144.39(10) . . ?
O1 Yb1 O14 81.48(9) . . ?
O1 Yb1 H15A 107.7 . . ?
O1 Yb1 H15B 116.7 . . ?
O1 Yb1 S1 19.67(7) . . ?
O1 Yb1 Yb2 75.39(7) . . ?
O1 Yb1 N3 77.15(10) . . ?
O1 Yb1 N4 140.28(11) . . ?
O7 Yb1 C11 92.19(10) . . ?
O7 Yb1 O1 73.42(9) . . ?
O7 Yb1 O8 75.73(9) . . ?
O7 Yb1 O12 118.65(9) . . ?
O7 Yb1 O14 73.43(9) . . ?
O7 Yb1 O15 80.75(11) . . ?
O7 Yb1 H15A 65.2 . . ?
O7 Yb1 H15B 95.0 . . ?
O7 Yb1 S1 55.18(7) . . ?
O7 Yb1 Yb2 36.94(7) . . ?
O7 Yb1 N3 139.76(10) . . ?
O7 Yb1 N4 145.69(11) . . ?
O8 Yb1 C11 65.54(10) . . ?
O8 Yb1 H15A 74.2 . . ?
O8 Yb1 H15B 83.1 . . ?
O8 Yb1 S1 124.95(7) . . ?
O8 Yb1 Yb2 69.29(7) . . ?
O8 Yb1 N3 118.39(10) . . ?
O8 Yb1 N4 70.37(11) . . ?
O12 Yb1 C11 142.53(10) . . ?
O12 Yb1 O1 73.44(10) . . ?
O12 Yb1 O8 138.71(10) . . ?
O12 Yb1 O14 146.28(10) . . ?
O12 Yb1 O15 74.67(11) . . ?
O12 Yb1 H15A 78.1 . . ?
O12 Yb1 H15B 58.5 . . ?
O12 Yb1 S1 90.31(7) . . ?
O12 Yb1 Yb2 145.89(7) . . ?
O12 Yb1 N3 77.09(11) . . ?
O12 Yb1 N4 85.20(11) . . ?
O14 Yb1 C11 22.23(9) . . ?
O14 Yb1 O8 72.99(9) . . ?
O14 Yb1 H15A 132.0 . . ?
O14 Yb1 H15B 155.3 . . ?
O14 Yb1 S1 70.61(6) . . ?
O14 Yb1 Yb2 36.52(6) . . ?
O14 Yb1 N3 75.61(10) . . ?
O14 Yb1 N4 100.93(10) . . ?
O15 Yb1 C11 135.11(10) . . ?
O15 Yb1 O1 121.28(10) . . ?
O15 Yb1 O8 69.77(10) . . ?
O15 Yb1 O14 138.76(11) . . ?
O15 Yb1 H15A 17.1 . . ?
O15 Yb1 H15B 17.5 . . ?
O15 Yb1 S1 118.71(8) . . ?
O15 Yb1 Yb2 111.20(8) . . ?
O15 Yb1 N3 138.85(12) . . ?
O15 Yb1 N4 82.80(11) . . ?
H15A Yb1 H15B 29.9 . . ?
S1 Yb1 H15A 102.3 . . ?
S1 Yb1 H15B 121.0 . . ?
S1 Yb1 Yb2 56.805(19) . . ?
Yb2 Yb1 H15A 98.7 . . ?
Yb2 Yb1 H15B 128.0 . . ?
N3 Yb1 C11 65.45(11) . . ?
N3 Yb1 H15A 152.0 . . ?
N3 Yb1 H15B 122.9 . . ?
N3 Yb1 S1 90.53(8) . . ?
N3 Yb1 Yb2 109.02(8) . . ?
N4 Yb1 C11 78.71(11) . . ?
N4 Yb1 H15A 99.8 . . ?
N4 Yb1 H15B 76.1 . . ?
N4 Yb1 S1 155.99(8) . . ?
N4 Yb1 Yb2 128.39(9) . . ?
N4 Yb1 N3 65.47(11) . . ?
C10 Yb2 S1 48.37(8) . . ?
C10 Yb2 S3 97.85(7) . . ?
O3 Yb2 C10 67.96(10) . . ?
O3 Yb2 O4 73.73(9) . . ?
O3 Yb2 O5 128.56(9) . . ?
O3 Yb2 S1 20.68(7) . . ?
O3 Yb2 S2 101.73(7) . . ?
O3 Yb2 S3 127.85(7) . . ?
O3 Yb2 N1 71.90(11) . . ?
O3 Yb2 N2 124.28(10) . . ?
O4 Yb2 C10 140.81(10) . . ?
O4 Yb2 O5 58.77(10) . . ?
O4 Yb2 S1 94.20(7) . . ?
O4 Yb2 S2 29.25(7) . . ?
O4 Yb2 S3 112.22(7) . . ?
O4 Yb2 N1 84.10(10) . . ?
O4 Yb2 N2 133.16(11) . . ?
O5 Yb2 C10 148.77(10) . . ?
O5 Yb2 S1 148.32(7) . . ?
O5 Yb2 S2 29.60(7) . . ?
O5 Yb2 S3 90.04(7) . . ?
O5 Yb2 N1 84.07(10) . . ?
O5 Yb2 N2 81.91(10) . . ?
O7 Yb2 C10 22.60(9) . . ?
O7 Yb2 O3 76.85(9) . . ?
O7 Yb2 O4 147.72(10) . . ?
O7 Yb2 O5 153.33(9) . . ?
O7 Yb2 O10 89.52(9) . . ?
O7 Yb2 S1 56.25(7) . . ?
O7 Yb2 S2 175.03(7) . . ?
O7 Yb2 S3 76.38(6) . . ?
O7 Yb2 N1 99.17(10) . . ?
O7 Yb2 N2 75.44(10) . . ?
O10 Yb2 C10 107.90(10) . . ?
O10 Yb2 O3 148.26(10) . . ?
O10 Yb2 O4 108.93(9) . . ?
O10 Yb2 O5 71.95(10) . . ?
O10 Yb2 S1 137.52(7) . . ?
O10 Yb2 S2 89.38(7) . . ?
O10 Yb2 S3 20.78(7) . . ?
O10 Yb2 N1 139.32(11) . . ?
O10 Yb2 N2 78.02(10) . . ?
O14 Yb2 C10 92.16(10) . . ?
O14 Yb2 O3 74.21(9) . . ?
O14 Yb2 O4 85.09(10) . . ?
O14 Yb2 O5 116.83(9) . . ?
O14 Yb2 O7 74.33(9) . . ?
O14 Yb2 O10 74.54(9) . . ?
O14 Yb2 S1 72.48(7) . . ?
O14 Yb2 S2 100.70(7) . . ?
O14 Yb2 S3 55.80(7) . . ?
O14 Yb2 N1 146.07(11) . . ?
O14 Yb2 N2 138.90(10) . . ?
S1 Yb2 S3 117.36(3) . . ?
S2 Yb2 C10 160.80(7) . . ?
S2 Yb2 S1 122.42(3) . . ?
S2 Yb2 S3 101.16(3) . . ?
N1 Yb2 C10 76.65(11) . . ?
N1 Yb2 S1 76.37(9) . . ?
N1 Yb2 S2 84.80(8) . . ?
N1 Yb2 S3 156.39(8) . . ?
N1 Yb2 N2 66.19(11) . . ?
N2 Yb2 C10 67.95(11) . . ?
N2 Yb2 S1 111.55(8) . . ?
N2 Yb2 S2 109.05(8) . . ?
N2 Yb2 S3 90.38(8) . . ?
C21 N1 C32 117.7(4) . . ?
C21 N1 Yb2 123.3(3) . . ?
C32 N1 Yb2 117.5(3) . . ?
C30 N2 C31 117.3(4) . . ?
C30 N2 Yb2 125.0(3) . . ?
C31 N2 Yb2 116.1(3) . . ?
C33 N3 C44 117.5(4) . . ?
C33 N3 Yb1 124.0(3) . . ?
C44 N3 Yb1 117.4(3) . . ?
C42 N4 C43 117.3(4) . . ?
C42 N4 Yb1 123.0(3) . . ?
C43 N4 Yb1 118.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -178.5(4) . . . 4_666 ?
C1 C2 C3 C8 3.3(6) . . . . ?
C1 C10 O7 Yb1 74.2(4) . . . . ?
C1 C10 O7 Yb2 -61.5(4) . . . . ?
C2 C1 C10 C9 -9.7(7) . . . . ?
C2 C1 C10 O7 168.7(4) . . . . ?
C2 C1 C10 Yb2 133.7(4) . . . . ?
C2 C1 S1 O1 129.7(4) . . . . ?
C2 C1 S1 O2 9.0(4) . . . . ?
C2 C1 S1 O3 -113.7(4) . . . . ?
C2 C1 S1 Yb1 157.9(4) . . . . ?
C2 C1 S1 Yb2 -137.4(4) . . . . ?
C2 C3 C8 C7 174.8(4) . . . . ?
C2 C3 C8 C9 -6.6(6) . . . . ?
C3 C4 C5 C6 -1.3(7) 4_565 . . . ?
C3 C4 C5 S2 -177.4(3) 4_565 . . . ?
C3 C8 C9 C10 1.8(6) . . . . ?
C4 C3 C8 C7 -3.6(6) 4_666 . . . ?
C4 C3 C8 C9 175.0(4) 4_666 . . . ?
C4 C5 C6 C7 2.8(7) . . . 4_565 ?
C4 C5 S2 O4 104.6(4) . . . . ?
C4 C5 S2 O5 -8.1(4) . . . . ?
C4 C5 S2 O6 -132.4(4) . . . . ?
C4 C5 S2 Yb2 49.9(4) . . . . ?
C6 C5 S2 O4 -71.6(4) . . . . ?
C6 C5 S2 O5 175.7(4) . . . . ?
C6 C5 S2 O6 51.4(4) . . . . ?
C6 C5 S2 Yb2 -126.4(3) . . . . ?
C6 C7 C8 C3 2.1(7) 4_666 . . . ?
C6 C7 C8 C9 -176.5(5) 4_666 . . . ?
C7 C8 C9 C10 -179.6(4) . . . . ?
C8 C9 C10 C1 6.1(6) . . . . ?
C8 C9 C10 O7 -172.3(4) . . . . ?
C8 C9 C10 Yb2 -121.2(4) . . . . ?
C9 C10 O7 Yb1 -107.4(4) . . . . ?
C9 C10 O7 Yb2 116.9(4) . . . . ?
C10 C1 C2 C3 4.9(7) . . . . ?
C10 C1 S1 O1 -49.5(4) . . . . ?
C10 C1 S1 O2 -170.1(3) . . . . ?
C10 C1 S1 O3 67.1(4) . . . . ?
C10 C1 S1 Yb1 -21.3(3) . . . . ?
C10 C1 S1 Yb2 43.5(3) . . . . ?
C11 C12 C13 C14 -171.8(4) . . . 4_565 ?
C11 C12 C13 C18 2.7(6) . . . . ?
C11 C20 S3 O8 -63.2(3) . . . . ?
C11 C20 S3 O9 173.5(3) . . . . ?
C11 C20 S3 O10 53.0(4) . . . . ?
C11 C20 S3 Yb2 22.2(3) . . . . ?
C12 C11 C20 C19 7.4(6) . . . . ?
C12 C11 C20 S3 -172.8(3) . . . . ?
C12 C11 O14 Yb1 -110.9(4) . . . . ?
C12 C11 O14 Yb2 112.1(4) . . . . ?
C12 C13 C18 C17 -173.1(4) . . . 4_565 ?
C12 C13 C18 C19 4.8(6) . . . . ?
C13 C14 C15 C16 -1.1(7) 4_666 . . . ?
C13 C18 C19 C20 -6.2(6) . . . . ?
C14 C13 C18 C17 1.5(6) 4_565 . . 4_565 ?
C14 C13 C18 C19 179.5(4) 4_565 . . . ?
C14 C15 C16 C17 -1.8(7) . . . . ?
C14 C15 C16 S4 174.2(4) . . . . ?
C15 C16 C17 C18 3.0(7) . . . 4_666 ?
C15 C16 S4 O11 -101.5(4) . . . . ?
C15 C16 S4 O12 140.8(4) . . . . ?
C15 C16 S4 O13 21.2(4) . . . . ?
C17 C16 S4 O11 74.4(4) . . . . ?
C17 C16 S4 O12 -43.2(4) . . . . ?
C17 C16 S4 O13 -162.8(4) . . . . ?
C17 C18 C19 C20 171.7(4) 4_565 . . . ?
C18 C19 C20 C11 0.1(6) . . . . ?
C18 C19 C20 S3 -179.6(3) . . . . ?
C19 C20 S3 O8 116.6(4) . . . . ?
C19 C20 S3 O9 -6.7(4) . . . . ?
C19 C20 S3 O10 -127.2(4) . . . . ?
C19 C20 S3 Yb2 -158.0(4) . . . . ?
C20 C11 C12 C13 -8.7(6) . . . . ?
C20 C11 O14 Yb1 66.6(4) . . . . ?
C20 C11 O14 Yb2 -70.4(4) . . . . ?
C21 C22 C23 C24 -1.1(8) . . . . ?
C22 C21 N1 C32 0.5(7) . . . . ?
C22 C21 N1 Yb2 -164.8(4) . . . . ?
C22 C23 C24 C25 179.6(5) . . . . ?
C22 C23 C24 C32 -0.1(8) . . . . ?
C23 C24 C25 C26 178.8(5) . . . . ?
C23 C24 C32 C31 -177.3(4) . . . . ?
C23 C24 C32 N1 1.6(7) . . . . ?
C24 C25 C26 C27 -1.6(8) . . . . ?
C24 C32 N1 C21 -1.8(7) . . . . ?
C24 C32 N1 Yb2 164.4(3) . . . . ?
C25 C24 C32 C31 3.0(7) . . . . ?
C25 C24 C32 N1 -178.1(4) . . . . ?
C25 C26 C27 C28 -176.1(5) . . . . ?
C25 C26 C27 C31 3.3(7) . . . . ?
C26 C27 C28 C29 179.3(5) . . . . ?
C26 C27 C31 C32 -1.8(6) . . . . ?
C26 C27 C31 N2 178.1(4) . . . . ?
C27 C28 C29 C30 1.9(8) . . . . ?
C27 C31 C32 C24 -1.3(6) . . . . ?
C27 C31 C32 N1 179.7(4) . . . . ?
C27 C31 N2 C30 3.2(6) . . . . ?
C27 C31 N2 Yb2 -163.2(3) . . . . ?
C28 C27 C31 C32 177.7(4) . . . . ?
C28 C27 C31 N2 -2.4(7) . . . . ?
C28 C29 C30 N2 -1.1(8) . . . . ?
C29 C30 N2 C31 -1.4(7) . . . . ?
C29 C30 N2 Yb2 163.6(4) . . . . ?
C31 C27 C28 C29 -0.2(7) . . . . ?
C31 C32 N1 C21 177.2(4) . . . . ?
C31 C32 N1 Yb2 -16.7(5) . . . . ?
C32 C24 C25 C26 -1.6(8) . . . . ?
C32 C31 N2 C30 -176.9(4) . . . . ?
C32 C31 N2 Yb2 16.7(5) . . . . ?
C33 C34 C35 C36 -2.4(7) . . . . ?
C34 C33 N3 C44 2.1(7) . . . . ?
C34 C33 N3 Yb1 -165.7(4) . . . . ?
C34 C35 C36 C37 -178.6(5) . . . . ?
C34 C35 C36 C44 1.9(7) . . . . ?
C35 C36 C37 C38 179.6(5) . . . . ?
C35 C36 C44 C43 179.7(4) . . . . ?
C35 C36 C44 N3 0.6(7) . . . . ?
C36 C37 C38 C39 0.1(8) . . . . ?
C36 C44 N3 C33 -2.6(6) . . . . ?
C36 C44 N3 Yb1 166.0(3) . . . . ?
C37 C36 C44 C43 0.2(6) . . . . ?
C37 C36 C44 N3 -178.8(4) . . . . ?
C37 C38 C39 C40 -178.8(5) . . . . ?
C37 C38 C39 C43 1.5(7) . . . . ?
C38 C39 C40 C41 -179.2(5) . . . . ?
C38 C39 C43 C44 -2.2(7) . . . . ?
C38 C39 C43 N4 178.4(4) . . . . ?
C39 C40 C41 C42 0.8(9) . . . . ?
C39 C43 C44 C36 1.3(6) . . . . ?
C39 C43 C44 N3 -179.6(4) . . . . ?
C39 C43 N4 C42 0.8(7) . . . . ?
C39 C43 N4 Yb1 -167.1(3) . . . . ?
C40 C39 C43 C44 178.1(4) . . . . ?
C40 C39 C43 N4 -1.3(7) . . . . ?
C40 C41 C42 N4 -1.4(9) . . . . ?
C41 C42 N4 C43 0.6(7) . . . . ?
C41 C42 N4 Yb1 167.9(4) . . . . ?
C43 C39 C40 C41 0.5(8) . . . . ?
C43 C44 N3 C33 178.3(4) . . . . ?
C43 C44 N3 Yb1 -13.1(5) . . . . ?
C44 C36 C37 C38 -1.0(7) . . . . ?
C44 C43 N4 C42 -178.6(4) . . . . ?
C44 C43 N4 Yb1 13.5(5) . . . . ?
O14 C11 C12 C13 168.9(4) . . . . ?
O14 C11 C20 C19 -170.3(4) . . . . ?
O14 C11 C20 S3 9.5(5) . . . . ?
S1 C1 C2 C3 -174.2(3) . . . . ?
S1 C1 C10 C9 169.4(3) . . . . ?
S1 C1 C10 O7 -12.1(5) . . . . ?
S1 C1 C10 Yb2 -47.2(3) . . . . ?
S2 C5 C6 C7 179.1(4) . . . 4_565 ?
S4 C16 C17 C18 -172.9(3) . . . 4_666 ?
Yb1 C11 C12 C13 118.5(4) . . . . ?
Yb1 C11 C20 C19 -133.1(4) . . . . ?
Yb1 C11 C20 S3 46.7(3) . . . . ?
Yb1 C11 O14 Yb2 -137.0(3) . . . . ?
Yb1 O1 S1 C1 62.9(2) . . . . ?
Yb1 O1 S1 O2 -178.85(18) . . . . ?
Yb1 O1 S1 O3 -50.5(2) . . . . ?
Yb1 O1 S1 Yb2 -18.84(18) . . . . ?
Yb1 O8 S3 C20 41.6(2) . . . . ?
Yb1 O8 S3 O9 161.25(17) . . . . ?
Yb1 O8 S3 O10 -70.3(2) . . . . ?
Yb1 O8 S3 Yb2 -46.41(16) . . . . ?
Yb1 O12 S4 C16 -76.8(3) . . . . ?
Yb1 O12 S4 O11 167.4(3) . . . . ?
Yb1 O12 S4 O13 39.1(3) . . . . ?
Yb2 C10 O7 Yb1 135.7(3) . . . . ?
Yb2 O3 S1 C1 -44.5(2) . . . . ?
Yb2 O3 S1 O1 67.7(2) . . . . ?
Yb2 O3 S1 O2 -164.43(17) . . . . ?
Yb2 O3 S1 Yb1 43.52(16) . . . . ?
Yb2 O4 S2 C5 -109.61(17) . . . . ?
Yb2 O4 S2 O5 4.73(17) . . . . ?
Yb2 O4 S2 O6 131.56(16) . . . . ?
Yb2 O5 S2 C5 109.21(17) . . . . ?
Yb2 O5 S2 O4 -4.57(16) . . . . ?
Yb2 O5 S2 O6 -130.92(16) . . . . ?
Yb2 O10 S3 C20 -66.6(2) . . . . ?
Yb2 O10 S3 O8 46.3(2) . . . . ?
Yb2 O10 S3 O9 175.62(17) . . . . ?
N1 C21 C22 C23 1.0(8) . . . . ?
N2 C31 C32 C24 178.8(4) . . . . ?
N2 C31 C32 N1 -0.2(6) . . . . ?
N3 C33 C34 C35 0.4(8) . . . . ?
N4 C43 C44 C36 -179.2(4) . . . . ?
N4 C43 C44 N3 -0.1(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
