# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 1410403'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 N6 Nd2 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1301.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.305(2)
_cell_length_b                   14.497(3)
_cell_length_c                   16.410(3)
_cell_angle_alpha                70.12(3)
_cell_angle_beta                 89.32(4)
_cell_angle_gamma                73.80(3)
_cell_volume                     2418.7(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    69550
_cell_measurement_theta_min      4.740
_cell_measurement_theta_max      60.759
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.327
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5826
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'TWINABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28597
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.657
_diffrn_reflns_theta_max         30.477
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13201
_reflns_number_gt                10717
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0255P)²+1.0266P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13201
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.05688(2) 0.30800(2) 0.56066(2) 0.01808(5) Uani 1 1 d . . . . .
Nd2 Nd 0.54205(2) 0.29966(2) 1.05147(2) 0.01988(5) Uani 1 1 d . . . . .
S3 S 0.27831(8) 0.43660(6) 0.77250(6) 0.03040(19) Uani 1 1 d . . . . .
S1 S -0.44144(7) 0.20710(7) 0.58753(6) 0.02726(17) Uani 1 1 d . . . . .
S2 S 0.04152(8) 0.21101(7) 1.09106(6) 0.0333(2) Uani 1 1 d . . . . .
N2 N 0.1144(2) 0.1077(2) 0.59875(18) 0.0242(6) Uani 1 1 d . . . . .
C31 C 0.5946(3) 0.0401(3) 1.1804(2) 0.0282(7) Uani 1 1 d . . . . .
N5 N 0.6052(2) 0.0984(2) 1.09932(18) 0.0253(6) Uani 1 1 d . . . . .
C43 C 0.3937(3) 0.5170(3) 0.8706(2) 0.0249(7) Uani 1 1 d . . . . .
O3 O 0.2900(2) 0.23012(18) 0.59101(16) 0.0312(5) Uani 1 1 d . . . . .
O4 O 0.2252(2) 0.38411(18) 0.49058(16) 0.0308(5) Uani 1 1 d . . . . .
C9 C 0.1078(4) -0.0554(3) 0.6949(3) 0.0421(10) Uani 1 1 d . . . . .
H9 H 0.1009 -0.0974 0.7508 0.050 Uiso 1 1 calc R U . . .
N1 N 0.1311(3) 0.2367(2) 0.43623(19) 0.0321(7) Uani 1 1 d . . . . .
O1 O -0.1269(2) 0.2653(2) 0.53779(18) 0.0374(6) Uani 1 1 d . . . . .
C34 C 0.5541(4) 0.0885(4) 1.3912(3) 0.0536(12) Uani 1 1 d . . . . .
H34 H 0.5607 0.0528 1.4508 0.064 Uiso 1 1 calc R U . . .
O7 O 0.3581(2) 0.2580(2) 1.0314(2) 0.0470(7) Uani 1 1 d . . . . .
O5 O 0.7116(2) 0.3760(2) 0.97739(18) 0.0404(7) Uani 1 1 d . . . . .
C46 C 0.1657(4) 0.6181(3) 0.6763(2) 0.0429(10) Uani 1 1 d . . . . .
H46 H 0.1150 0.6743 0.6320 0.052 Uiso 1 1 calc R U . . .
O12 O 0.1286(2) 0.38904(18) 0.65258(16) 0.0323(5) Uani 1 1 d . . . . .
C12 C 0.0859(4) 0.0312(3) 0.8340(3) 0.0413(9) Uani 1 1 d . . . . .
H12 H 0.1089 -0.0399 0.8509 0.050 Uiso 1 1 calc R U . . .
C26 C 0.6507(3) 0.1187(3) 0.9511(2) 0.0346(8) Uani 1 1 d . . . . .
OW1 O -0.1405(2) 0.4132(2) 0.60988(17) 0.0393(6) Uani 1 1 d . . . . .
C33 C 0.5780(4) 0.0358(3) 1.3343(2) 0.0421(10) Uani 1 1 d . . . . .
H33 H 0.6003 -0.0355 1.3546 0.050 Uiso 1 1 calc R U . . .
O2 O -0.1712(2) 0.1235(2) 0.61928(19) 0.0390(6) Uani 1 1 d . . . . .
O11 O -0.0411(2) 0.45055(18) 0.43366(15) 0.0314(5) Uani 1 1 d . . . . .
O8 O 0.3114(2) 0.1278(2) 1.1288(2) 0.0450(7) Uani 1 1 d . . . . .
C5 C 0.1549(3) 0.1369(3) 0.4484(2) 0.0338(8) Uani 1 1 d . . . . .
O6 O 0.7741(2) 0.2308(2) 1.08963(18) 0.0394(6) Uani 1 1 d . . . . .
O10 O 0.4421(3) 0.4275(2) 0.91882(17) 0.0440(7) Uani 1 1 d . . . . .
C4 C 0.1979(4) 0.0991(4) 0.3827(3) 0.0518(12) Uani 1 1 d . . . . .
H4 H 0.2146 0.0295 0.3922 0.062 Uiso 1 1 calc R U . . .
N3 N 0.0482(3) 0.1944(2) 0.72062(18) 0.0306(6) Uani 1 1 d . . . . .
C29 C 0.6281(4) -0.1067(3) 1.1398(3) 0.0514(11) Uani 1 1 d . . . . .
H29 H 0.6335 -0.1755 1.1531 0.062 Uiso 1 1 calc R U . . .
N4 N 0.6168(3) 0.2193(2) 0.93344(19) 0.0361(7) Uani 1 1 d . . . . .
C3 C 0.2155(5) 0.1647(4) 0.3043(3) 0.0617(14) Uani 1 1 d . . . . .
H3 H 0.2427 0.1402 0.2597 0.074 Uiso 1 1 calc R U . . .
C13 C 0.0601(4) 0.0781(4) 0.8947(3) 0.0533(12) Uani 1 1 d . . . . .
H13 H 0.0658 0.0387 0.9534 0.064 Uiso 1 1 calc R U . . .
C30 C 0.6078(4) -0.0643(3) 1.2035(3) 0.0425(10) Uani 1 1 d . . . . .
H30 H 0.6030 -0.1042 1.2607 0.051 Uiso 1 1 calc R U . . .
N6 N 0.5379(3) 0.1949(2) 1.21470(18) 0.0305(6) Uani 1 1 d . . . . .
C14 C 0.0264(5) 0.1817(4) 0.8691(3) 0.0531(12) Uani 1 1 d . . . . .
H14 H 0.0063 0.2144 0.9095 0.064 Uiso 1 1 calc R U . . .
O9 O 0.4128(3) 0.5941(2) 0.87781(18) 0.0458(7) Uani 1 1 d . . . . .
C47 C 0.1758(3) 0.5203(2) 0.6855(2) 0.0254(7) Uani 1 1 d . . . . .
C28 C 0.6403(4) -0.0491(3) 1.0577(3) 0.0454(10) Uani 1 1 d . . . . .
H28 H 0.6546 -0.0778 1.0144 0.054 Uiso 1 1 calc R U . . .
C48 C 0.1102(3) 0.4836(2) 0.63062(19) 0.0218(6) Uani 1 1 d . . . . .
C44 C 0.3061(3) 0.5348(2) 0.7962(2) 0.0254(7) Uani 1 1 d . . . . .
C10 C 0.1018(3) 0.0467(3) 0.6778(2) 0.0284(7) Uani 1 1 d . . . . .
C24 C 0.7193(5) 0.1394(5) 0.8083(3) 0.0652(15) Uani 1 1 d . . . . .
H24 H 0.7533 0.1121 0.7667 0.078 Uiso 1 1 calc R U . . .
C17 C -0.3338(3) 0.2674(3) 0.5424(2) 0.0275(7) Uani 1 1 d . . . . .
C20 C 0.4400(3) 0.3116(3) 0.5286(2) 0.0257(7) Uani 1 1 d . . . . .
C6 C 0.1350(3) 0.0691(3) 0.5341(2) 0.0302(7) Uani 1 1 d . . . . .
OW2 O 0.3395(3) 0.4135(2) 1.0923(2) 0.0532(8) Uani 1 1 d . . . . .
C38 C 0.9244(3) 0.3107(3) 1.0252(2) 0.0323(8) Uani 1 1 d . . . . .
C42 C 0.2844(3) 0.2124(3) 1.0707(3) 0.0331(8) Uani 1 1 d . . . . .
C16 C -0.2001(3) 0.2126(3) 0.5699(2) 0.0261(7) Uani 1 1 d . . . . .
C15 C 0.0224(4) 0.2376(3) 0.7818(3) 0.0418(9) Uani 1 1 d . . . . .
H15 H 0.0009 0.3087 0.7645 0.050 Uiso 1 1 calc R U . . .
C8 C 0.1237(5) -0.0931(3) 0.6290(3) 0.0527(12) Uani 1 1 d . . . . .
H8 H 0.1248 -0.1605 0.6391 0.063 Uiso 1 1 calc R U . . .
C25 C 0.7032(5) 0.0761(4) 0.8904(3) 0.0534(12) Uani 1 1 d . . . . .
H25 H 0.7276 0.0053 0.9046 0.064 Uiso 1 1 calc R U . . .
C11 C 0.0770(3) 0.0921(3) 0.7467(2) 0.0300(7) Uani 1 1 d . . . . .
C45 C 0.2393(4) 0.6271(3) 0.7402(3) 0.0454(11) Uani 1 1 d . . . . .
H45 H 0.2417 0.6894 0.7434 0.054 Uiso 1 1 calc R U . . .
C41 C 0.1501(3) 0.2667(3) 1.0423(3) 0.0323(8) Uani 1 1 d . . . . .
C32 C 0.5682(3) 0.0913(3) 1.2458(2) 0.0306(8) Uani 1 1 d . . . . .
C35 C 0.5208(5) 0.1929(4) 1.3605(3) 0.0548(12) Uani 1 1 d . . . . .
H35 H 0.5036 0.2294 1.3982 0.066 Uiso 1 1 calc R U . . .
C27 C 0.6309(3) 0.0544(3) 1.0388(3) 0.0319(8) Uani 1 1 d . . . . .
C21 C 0.3107(3) 0.3083(3) 0.5376(2) 0.0251(7) Uani 1 1 d . . . . .
C7 C 0.1382(4) -0.0319(3) 0.5480(3) 0.0483(11) Uani 1 1 d . . . . .
H7 H 0.1501 -0.0572 0.5025 0.058 Uiso 1 1 calc R U . . .
C39 C -0.0324(4) 0.3847(3) 0.9684(3) 0.0448(10) Uani 1 1 d . . . . .
H39 H -0.0825 0.4449 0.9278 0.054 Uiso 1 1 calc R U . . .
C36 C 0.5134(4) 0.2426(3) 1.2725(3) 0.0432(10) Uani 1 1 d . . . . .
H36 H 0.4899 0.3139 1.2516 0.052 Uiso 1 1 calc R U . . .
C19 C 0.4822(3) 0.3888(3) 0.4769(3) 0.0367(9) Uani 1 1 d . . . . .
H19 H 0.4309 0.4514 0.4404 0.044 Uiso 1 1 calc R U . . .
C18 C -0.3882(3) 0.3635(3) 0.4848(3) 0.0397(9) Uani 1 1 d . . . . .
H18 H -0.3442 0.4077 0.4540 0.048 Uiso 1 1 calc R U . . .
C1 C 0.1494(4) 0.2985(3) 0.3595(3) 0.0442(10) Uani 1 1 d . . . . .
H1 H 0.1319 0.3681 0.3504 0.053 Uiso 1 1 calc R U . . .
C2 C 0.1931(5) 0.2648(4) 0.2920(3) 0.0572(13) Uani 1 1 d . . . . .
H2 H 0.2066 0.3104 0.2396 0.069 Uiso 1 1 calc R U . . .
C37 C 0.7958(3) 0.3057(3) 1.0313(3) 0.0334(8) Uani 1 1 d . . . . .
C40 C 0.0974(4) 0.3587(3) 0.9788(3) 0.0469(11) Uani 1 1 d . . . . .
H40 H 0.1427 0.4003 0.9455 0.056 Uiso 1 1 calc R U . . .
C22 C 0.6326(5) 0.2783(4) 0.8550(3) 0.0564(12) Uani 1 1 d . . . . .
H22 H 0.6077 0.3489 0.8418 0.068 Uiso 1 1 calc R U . . .
C23 C 0.6842(5) 0.2407(4) 0.7912(3) 0.0621(14) Uani 1 1 d . . . . .
H23 H 0.6942 0.2854 0.7372 0.075 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O11 2.385(3) . ?
Nd1 O1 2.395(2) . ?
Nd1 O12 2.466(2) . ?
Nd1 O4 2.533(2) . ?
Nd1 O3 2.541(2) . ?
Nd1 N3 2.600(3) . ?
Nd1 N1 2.618(3) . ?
Nd1 OW1 2.619(3) . ?
Nd1 N2 2.640(3) . ?
Nd1 C21 2.892(3) . ?
Nd2 O10 2.366(3) . ?
Nd2 O9 2.377(2) 2_667 ?
Nd2 O7 2.377(3) . ?
Nd2 O6 2.535(3) . ?
Nd2 O5 2.567(3) . ?
Nd2 N6 2.599(3) . ?
Nd2 N4 2.602(3) . ?
Nd2 N5 2.633(3) . ?
Nd2 OW2 2.650(3) . ?
Nd2 C37 2.906(3) . ?
S3 C44 1.705(3) . ?
S3 C47 1.712(3) . ?
S1 C17 1.710(3) . ?
S1 C20 1.711(3) 1_455 ?
S2 C41 1.700(4) . ?
S2 C38 1.707(4) 1_455 ?
N2 C10 1.331(4) . ?
N2 C6 1.348(4) . ?
C31 N5 1.337(4) . ?
C31 C30 1.394(5) . ?
C31 C32 1.483(5) . ?
N5 C27 1.341(4) . ?
C43 O10 1.236(4) . ?
C43 O9 1.238(4) . ?
C43 C44 1.485(4) . ?
O3 C21 1.256(4) . ?
O4 C21 1.259(4) . ?
C9 C8 1.357(6) . ?
C9 C10 1.392(5) . ?
C9 H9 0.9300 . ?
N1 C1 1.327(5) . ?
N1 C5 1.339(5) . ?
O1 C16 1.271(4) . ?
C34 C35 1.361(7) . ?
C34 C33 1.377(6) . ?
C34 H34 0.9300 . ?
O7 C42 1.245(4) . ?
O5 C37 1.262(4) . ?
C46 C47 1.346(5) . ?
C46 C45 1.409(4) . ?
C46 H46 0.9300 . ?
O12 C48 1.248(4) . ?
C12 C13 1.372(6) . ?
C12 C11 1.392(5) . ?
C12 H12 0.9300 . ?
C26 N4 1.327(5) . ?
C26 C25 1.387(5) . ?
C26 C27 1.480(5) . ?
C33 C32 1.388(5) . ?
C33 H33 0.9300 . ?
O2 C16 1.221(4) . ?
O11 C48 1.246(4) 2_566 ?
O8 C42 1.229(5) . ?
C5 C4 1.392(5) . ?
C5 C6 1.473(5) . ?
O6 C37 1.261(4) . ?
C4 C3 1.367(7) . ?
C4 H4 0.9300 . ?
N3 C11 1.339(4) . ?
N3 C15 1.343(5) . ?
C29 C28 1.352(6) . ?
C29 C30 1.371(6) . ?
C29 H29 0.9300 . ?
N4 C22 1.323(5) . ?
C3 C2 1.345(7) . ?
C3 H3 0.9300 . ?
C13 C14 1.354(7) . ?
C13 H13 0.9300 . ?
C30 H30 0.9300 . ?
N6 C36 1.337(5) . ?
N6 C32 1.352(5) . ?
C14 C15 1.380(6) . ?
C14 H14 0.9300 . ?
O9 Nd2 2.377(2) 2_667 ?
C47 C48 1.486(4) . ?
C28 C27 1.398(5) . ?
C28 H28 0.9300 . ?
C48 O11 1.246(4) 2_566 ?
C44 C45 1.350(5) . ?
C10 C11 1.477(5) . ?
C24 C23 1.338(7) . ?
C24 C25 1.391(7) . ?
C24 H24 0.9300 . ?
C17 C18 1.362(5) . ?
C17 C16 1.490(4) . ?
C20 C19 1.357(5) . ?
C20 C21 1.479(4) . ?
C20 S1 1.711(3) 1_655 ?
C6 C7 1.393(5) . ?
C38 C39 1.363(5) 1_655 ?
C38 C37 1.477(4) . ?
C38 S2 1.707(4) 1_655 ?
C42 C41 1.498(5) . ?
C15 H15 0.9300 . ?
C8 C7 1.362(7) . ?
C8 H8 0.9300 . ?
C25 H25 0.9300 . ?
C45 H45 0.9300 . ?
C41 C40 1.359(6) . ?
C35 C36 1.369(6) . ?
C35 H35 0.9300 . ?
C7 H7 0.9300 . ?
C39 C38 1.363(5) 1_455 ?
C39 C40 1.406(5) . ?
C39 H39 0.9300 . ?
C36 H36 0.9300 . ?
C19 C18 1.404(5) 1_655 ?
C19 H19 0.9300 . ?
C18 C19 1.404(5) 1_455 ?
C18 H18 0.9300 . ?
C1 C2 1.390(6) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C40 H40 0.9300 . ?
C22 C23 1.389(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Nd1 O1 79.62(9) . . ?
O11 Nd1 O12 102.99(8) . . ?
O1 Nd1 O12 136.85(9) . . ?
O11 Nd1 O4 73.63(8) . . ?
O1 Nd1 O4 146.38(9) . . ?
O12 Nd1 O4 70.27(9) . . ?
O11 Nd1 O3 123.49(9) . . ?
O1 Nd1 O3 141.30(9) . . ?
O12 Nd1 O3 72.89(9) . . ?
O4 Nd1 O3 51.46(8) . . ?
O11 Nd1 N3 149.33(9) . . ?
O1 Nd1 N3 82.57(10) . . ?
O12 Nd1 N3 74.00(9) . . ?
O4 Nd1 N3 130.07(9) . . ?
O3 Nd1 N3 85.46(10) . . ?
O11 Nd1 N1 78.02(9) . . ?
O1 Nd1 N1 83.36(10) . . ?
O12 Nd1 N1 139.70(9) . . ?
O4 Nd1 N1 71.59(9) . . ?
O3 Nd1 N1 73.51(10) . . ?
N3 Nd1 N1 124.43(10) . . ?
O11 Nd1 OW1 74.06(9) . . ?
O1 Nd1 OW1 66.35(9) . . ?
O12 Nd1 OW1 73.00(9) . . ?
O4 Nd1 OW1 123.01(8) . . ?
O3 Nd1 OW1 144.50(9) . . ?
N3 Nd1 OW1 75.97(10) . . ?
N1 Nd1 OW1 141.71(9) . . ?
O11 Nd1 N2 132.82(9) . . ?
O1 Nd1 N2 71.53(9) . . ?
O12 Nd1 N2 123.65(9) . . ?
O4 Nd1 N2 113.36(8) . . ?
O3 Nd1 N2 70.34(8) . . ?
N3 Nd1 N2 62.03(9) . . ?
N1 Nd1 N2 62.50(9) . . ?
OW1 Nd1 N2 123.12(9) . . ?
O11 Nd1 C21 98.87(10) . . ?
O1 Nd1 C21 154.44(10) . . ?
O12 Nd1 C21 68.57(9) . . ?
O4 Nd1 C21 25.78(8) . . ?
O3 Nd1 C21 25.71(8) . . ?
N3 Nd1 C21 107.79(11) . . ?
N1 Nd1 C21 71.47(10) . . ?
OW1 Nd1 C21 138.17(9) . . ?
N2 Nd1 C21 92.36(9) . . ?
O10 Nd2 O9 99.29(10) . 2_667 ?
O10 Nd2 O7 76.01(11) . . ?
O9 Nd2 O7 132.19(11) 2_667 . ?
O10 Nd2 O6 125.11(10) . . ?
O9 Nd2 O6 75.71(10) 2_667 . ?
O7 Nd2 O6 145.50(10) . . ?
O10 Nd2 O5 75.16(10) . . ?
O9 Nd2 O5 70.14(10) 2_667 . ?
O7 Nd2 O5 146.22(10) . . ?
O6 Nd2 O5 51.36(8) . . ?
O10 Nd2 N6 150.70(10) . . ?
O9 Nd2 N6 77.60(10) 2_667 . ?
O7 Nd2 N6 84.64(11) . . ?
O6 Nd2 N6 82.82(10) . . ?
O5 Nd2 N6 128.54(9) . . ?
O10 Nd2 N4 75.39(10) . . ?
O9 Nd2 N4 142.24(11) 2_667 . ?
O7 Nd2 N4 83.60(11) . . ?
O6 Nd2 N4 77.43(11) . . ?
O5 Nd2 N4 72.41(10) . . ?
N6 Nd2 N4 124.52(10) . . ?
O10 Nd2 N5 130.07(9) . . ?
O9 Nd2 N5 130.36(9) 2_667 . ?
O7 Nd2 N5 73.93(10) . . ?
O6 Nd2 N5 71.78(9) . . ?
O5 Nd2 N5 113.04(9) . . ?
N6 Nd2 N5 62.14(9) . . ?
N4 Nd2 N5 62.49(10) . . ?
O10 Nd2 OW2 73.94(10) . . ?
O9 Nd2 OW2 67.84(10) 2_667 . ?
O7 Nd2 OW2 65.17(10) . . ?
O6 Nd2 OW2 141.58(10) . . ?
O5 Nd2 OW2 121.78(9) . . ?
N6 Nd2 OW2 78.05(10) . . ?
N4 Nd2 OW2 140.42(10) . . ?
N5 Nd2 OW2 124.70(9) . . ?
O10 Nd2 C37 100.45(11) . . ?
O9 Nd2 C37 70.04(11) 2_667 . ?
O7 Nd2 C37 157.66(11) . . ?
O6 Nd2 C37 25.66(9) . . ?
O5 Nd2 C37 25.73(9) . . ?
N6 Nd2 C37 105.58(11) . . ?
N4 Nd2 C37 74.22(11) . . ?
N5 Nd2 C37 93.04(10) . . ?
OW2 Nd2 C37 135.76(10) . . ?
C44 S3 C47 91.72(16) . . ?
C17 S1 C20 91.46(16) . 1_455 ?
C41 S2 C38 91.75(18) . 1_455 ?
C10 N2 C6 119.1(3) . . ?
C10 N2 Nd1 120.4(2) . . ?
C6 N2 Nd1 119.4(2) . . ?
N5 C31 C30 122.1(3) . . ?
N5 C31 C32 117.1(3) . . ?
C30 C31 C32 120.8(3) . . ?
C31 N5 C27 118.7(3) . . ?
C31 N5 Nd2 121.1(2) . . ?
C27 N5 Nd2 119.5(2) . . ?
O10 C43 O9 125.8(3) . . ?
O10 C43 C44 117.7(3) . . ?
O9 C43 C44 116.5(3) . . ?
C21 O3 Nd1 92.95(19) . . ?
C21 O4 Nd1 93.22(19) . . ?
C8 C9 C10 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C1 N1 C5 118.0(3) . . ?
C1 N1 Nd1 120.6(3) . . ?
C5 N1 Nd1 121.4(2) . . ?
C16 O1 Nd1 147.2(2) . . ?
C35 C34 C33 120.1(4) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C42 O7 Nd2 143.3(3) . . ?
C37 O5 Nd2 92.3(2) . . ?
C47 C46 C45 113.3(3) . . ?
C47 C46 H46 123.3 . . ?
C45 C46 H46 123.3 . . ?
C48 O12 Nd1 123.3(2) . . ?
C13 C12 C11 118.8(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N4 C26 C25 121.5(4) . . ?
N4 C26 C27 116.7(3) . . ?
C25 C26 C27 121.8(4) . . ?
C34 C33 C32 118.6(4) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C48 O11 Nd1 167.9(2) 2_566 . ?
N1 C5 C4 121.0(4) . . ?
N1 C5 C6 117.3(3) . . ?
C4 C5 C6 121.7(4) . . ?
C37 O6 Nd2 93.8(2) . . ?
C43 O10 Nd2 153.7(2) . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C11 N3 C15 117.5(3) . . ?
C11 N3 Nd1 122.5(2) . . ?
C15 N3 Nd1 119.8(2) . . ?
C28 C29 C30 120.4(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C22 N4 C26 117.7(4) . . ?
C22 N4 Nd2 120.0(3) . . ?
C26 N4 Nd2 122.1(2) . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C29 C30 C31 118.2(4) . . ?
C29 C30 H30 120.9 . . ?
C31 C30 H30 120.9 . . ?
C36 N6 C32 117.3(3) . . ?
C36 N6 Nd2 120.0(3) . . ?
C32 N6 Nd2 122.5(2) . . ?
C13 C14 C15 118.4(4) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C43 O9 Nd2 157.9(2) . 2_667 ?
C46 C47 C48 127.4(3) . . ?
C46 C47 S3 111.0(2) . . ?
C48 C47 S3 121.6(2) . . ?
C29 C28 C27 118.9(4) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
O11 C48 O12 125.1(3) 2_566 . ?
O11 C48 C47 117.5(3) 2_566 . ?
O12 C48 C47 117.4(3) . . ?
C45 C44 C43 126.0(3) . . ?
C45 C44 S3 111.7(2) . . ?
C43 C44 S3 122.3(2) . . ?
N2 C10 C9 121.5(4) . . ?
N2 C10 C11 117.6(3) . . ?
C9 C10 C11 120.9(3) . . ?
C23 C24 C25 118.0(4) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C18 C17 C16 129.5(3) . . ?
C18 C17 S1 111.5(2) . . ?
C16 C17 S1 119.0(3) . . ?
C19 C20 C21 128.6(3) . . ?
C19 C20 S1 111.8(3) . 1_655 ?
C21 C20 S1 119.6(3) . 1_655 ?
N2 C6 C7 121.1(4) . . ?
N2 C6 C5 117.9(3) . . ?
C7 C6 C5 121.0(4) . . ?
C39 C38 C37 128.4(3) 1_655 . ?
C39 C38 S2 111.9(3) 1_655 1_655 ?
C37 C38 S2 119.6(3) . 1_655 ?
O8 C42 O7 126.5(4) . . ?
O8 C42 C41 117.7(3) . . ?
O7 C42 C41 115.8(4) . . ?
O2 C16 O1 126.5(3) . . ?
O2 C16 C17 118.5(3) . . ?
O1 C16 C17 115.0(3) . . ?
N3 C15 C14 123.3(4) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C9 C8 C7 119.8(4) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C26 C25 C24 119.9(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N3 C11 C12 122.0(4) . . ?
N3 C11 C10 116.4(3) . . ?
C12 C11 C10 121.6(3) . . ?
C44 C45 C46 112.2(3) . . ?
C44 C45 H45 123.9 . . ?
C46 C45 H45 123.9 . . ?
C40 C41 C42 128.8(3) . . ?
C40 C41 S2 111.5(3) . . ?
C42 C41 S2 119.7(3) . . ?
N6 C32 C33 121.8(4) . . ?
N6 C32 C31 116.3(3) . . ?
C33 C32 C31 121.9(4) . . ?
C34 C35 C36 118.2(4) . . ?
C34 C35 H35 120.9 . . ?
C36 C35 H35 120.9 . . ?
N5 C27 C28 121.5(4) . . ?
N5 C27 C26 117.8(3) . . ?
C28 C27 C26 120.6(4) . . ?
O3 C21 O4 122.2(3) . . ?
O3 C21 C20 119.2(3) . . ?
O4 C21 C20 118.6(3) . . ?
O3 C21 Nd1 61.34(17) . . ?
O4 C21 Nd1 61.00(17) . . ?
C20 C21 Nd1 177.2(2) . . ?
C8 C7 C6 119.1(4) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C38 C39 C40 111.7(4) 1_455 . ?
C38 C39 H39 124.1 1_455 . ?
C40 C39 H39 124.1 . . ?
N6 C36 C35 124.0(4) . . ?
N6 C36 H36 118.0 . . ?
C35 C36 H36 118.0 . . ?
C20 C19 C18 112.5(3) . 1_655 ?
C20 C19 H19 123.7 . . ?
C18 C19 H19 123.7 1_655 . ?
C17 C18 C19 112.7(3) . 1_455 ?
C17 C18 H18 123.6 . . ?
C19 C18 H18 123.6 1_455 . ?
N1 C1 C2 123.4(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.3(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
O6 C37 O5 122.4(3) . . ?
O6 C37 C38 118.9(3) . . ?
O5 C37 C38 118.8(3) . . ?
O6 C37 Nd2 60.51(18) . . ?
O5 C37 Nd2 61.97(18) . . ?
C38 C37 Nd2 176.8(3) . . ?
C41 C40 C39 113.2(4) . . ?
C41 C40 H40 123.4 . . ?
C39 C40 H40 123.4 . . ?
N4 C22 C23 123.7(5) . . ?
N4 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
C24 C23 C22 119.1(5) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?

_refine_diff_density_max         1.200
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.125

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1410404'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 N6 O14 S3 Sm2'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1313.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2941(3)
_cell_length_b                   14.5181(4)
_cell_length_c                   16.4145(4)
_cell_angle_alpha                70.151(4)
_cell_angle_beta                 89.570(5)
_cell_angle_gamma                74.061(5)
_cell_volume                     2423.28(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    36145
_cell_measurement_theta_min      4.498
_cell_measurement_theta_max      54.955
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.603
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36143
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.325
_diffrn_reflns_theta_max         29.718
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13231
_reflns_number_gt                10631
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+0.4445P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13231
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.05837(2) 0.30657(2) 0.06071(2) 0.01652(5) Uani 1 1 d . . . . .
Sm2 Sm -0.45823(2) 0.29969(2) -0.44819(2) 0.01782(5) Uani 1 1 d . . . . .
S1 S 0.55923(7) 0.20643(6) 0.08813(6) 0.02594(18) Uani 1 1 d . . . . .
S2 S 0.04109(8) 0.21036(7) -0.40867(6) 0.02989(19) Uani 1 1 d . . . . .
S3 S -0.27729(8) 0.56337(6) -0.27242(5) 0.02861(19) Uani 1 1 d . . . . .
O3 O 0.2249(2) 0.38359(17) -0.00905(15) 0.0279(5) Uani 1 1 d . . . . .
O4 O 0.28899(19) 0.23029(17) 0.09235(15) 0.0286(5) Uani 1 1 d . . . . .
O11 O -0.0390(2) 0.44749(17) -0.06505(14) 0.0294(5) Uani 1 1 d . . . . .
O6 O -0.2282(2) 0.23177(18) -0.40942(16) 0.0341(6) Uani 1 1 d . . . . .
O5 O -0.2901(2) 0.37710(18) -0.52151(16) 0.0351(6) Uani 1 1 d . . . . .
N2 N 0.1147(2) 0.10865(19) 0.09881(17) 0.0208(5) Uani 1 1 d . . . . .
O12 O 0.1265(2) 0.39146(17) 0.14972(14) 0.0294(5) Uani 1 1 d . . . . .
O2 O -0.1699(2) 0.12244(18) 0.11898(17) 0.0357(6) Uani 1 1 d . . . . .
N6 N -0.4629(3) 0.1966(2) -0.28599(18) 0.0280(6) Uani 1 1 d . . . . .
N4 N -0.3839(3) 0.2233(2) -0.56712(18) 0.0326(7) Uani 1 1 d . . . . .
N5 N -0.3950(2) 0.10077(19) -0.40102(17) 0.0214(5) Uani 1 1 d . . . . .
N3 N 0.0481(3) 0.1966(2) 0.21993(17) 0.0285(6) Uani 1 1 d . . . . .
N1 N 0.1306(3) 0.2377(2) -0.06357(18) 0.0292(6) Uani 1 1 d . . . . .
C20 C 0.4400(3) 0.3109(2) 0.0292(2) 0.0236(7) Uani 1 1 d . . . . .
C21 C 0.3107(3) 0.3079(2) 0.0381(2) 0.0232(7) Uani 1 1 d . . . . .
C17 C -0.3326(3) 0.2669(3) 0.0428(2) 0.0250(7) Uani 1 1 d . . . . .
C37 C -0.2057(3) 0.3062(3) -0.4679(2) 0.0294(8) Uani 1 1 d . . . . .
C38 C -0.0771(3) 0.3111(3) -0.4738(2) 0.0277(7) Uani 1 1 d . . . . .
C16 C -0.1982(3) 0.2123(3) 0.0695(2) 0.0245(7) Uani 1 1 d . . . . .
C41 C -0.8500(3) 0.2670(3) -0.4576(2) 0.0290(8) Uani 1 1 d . . . . .
C40 C 0.0971(3) 0.3597(3) -0.5206(3) 0.0405(10) Uani 1 1 d . . . . .
H40 H 0.1422 0.4017 -0.5536 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6121(3) 0.3637(3) -0.0149(3) 0.0368(9) Uani 1 1 d . . . . .
H19 H 0.6557 0.4082 -0.0456 0.044 Uiso 1 1 calc R U . . .
C19 C 0.4823(3) 0.3881(3) -0.0224(2) 0.0349(9) Uani 1 1 d . . . . .
H18 H 0.4309 0.4506 -0.0589 0.042 Uiso 1 1 calc R U . . .
O1 O -0.1246(2) 0.26488(18) 0.03772(17) 0.0337(6) Uani 1 1 d . . . . .
O7 O -0.6410(2) 0.2580(2) -0.46851(18) 0.0414(7) Uani 1 1 d . . . . .
O9 O -0.4148(3) 0.40623(19) -0.37863(16) 0.0408(7) Uani 1 1 d . . . . .
O10 O -0.4404(2) 0.57239(18) -0.42112(16) 0.0389(6) Uani 1 1 d . . . . .
C43 C -0.3938(3) 0.4833(2) -0.37172(19) 0.0211(6) Uani 1 1 d . . . . .
O8 O -0.6887(2) 0.1262(2) -0.37186(17) 0.0392(6) Uani 1 1 d . . . . .
C48 C -0.1091(3) 0.5147(2) -0.12903(19) 0.0194(6) Uani 1 1 d . . . . .
C32 C -0.4328(3) 0.0935(3) -0.2546(2) 0.0257(7) Uani 1 1 d . . . . .
C11 C 0.0769(3) 0.0939(2) 0.2467(2) 0.0258(7) Uani 1 1 d . . . . .
C31 C -0.4064(3) 0.0421(2) -0.3199(2) 0.0262(7) Uani 1 1 d . . . . .
C10 C 0.1025(3) 0.0476(2) 0.1789(2) 0.0264(7) Uani 1 1 d . . . . .
C5 C 0.1548(3) 0.1376(3) -0.0517(2) 0.0298(8) Uani 1 1 d . . . . .
C47 C -0.1750(3) 0.4789(2) -0.18529(19) 0.0231(7) Uani 1 1 d . . . . .
C26 C -0.3499(3) 0.1214(3) -0.5498(2) 0.0301(8) Uani 1 1 d . . . . .
C6 C 0.1354(3) 0.0694(2) 0.0346(2) 0.0271(7) Uani 1 1 d . . . . .
C42 C -0.7151(3) 0.2117(3) -0.4295(2) 0.0280(7) Uani 1 1 d . . . . .
C27 C -0.3689(3) 0.0569(3) -0.4622(2) 0.0276(7) Uani 1 1 d . . . . .
C44 C -0.3065(3) 0.4657(2) -0.2970(2) 0.0240(7) Uani 1 1 d . . . . .
C45 C -0.2400(4) 0.3734(3) -0.2402(2) 0.0414(10) Uani 1 1 d . . . . .
H46 H -0.2434 0.3114 -0.2432 0.050 Uiso 1 1 calc R U . . .
C33 C -0.4241(3) 0.0386(3) -0.1662(2) 0.0367(9) Uani 1 1 d . . . . .
H33 H -0.4029 -0.0324 -0.1460 0.044 Uiso 1 1 calc R U . . .
C15 C 0.0219(4) 0.2412(3) 0.2805(2) 0.0388(9) Uani 1 1 d . . . . .
H15 H 0.0008 0.3122 0.2627 0.047 Uiso 1 1 calc R U . . .
C36 C -0.4872(4) 0.2458(3) -0.2290(2) 0.0396(9) Uani 1 1 d . . . . .
H36 H -0.5092 0.3169 -0.2501 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1086(4) -0.0551(3) 0.1965(3) 0.0382(9) Uani 1 1 d . . . . .
H9 H 0.1018 -0.0968 0.2526 0.046 Uiso 1 1 calc R U . . .
C12 C 0.0844(3) 0.0343(3) 0.3340(2) 0.0360(9) Uani 1 1 d . . . . .
H12 H 0.1059 -0.0366 0.3513 0.043 Uiso 1 1 calc R U . . .
C30 C -0.3929(4) -0.0624(3) -0.2969(3) 0.0392(9) Uani 1 1 d . . . . .
H30 H -0.3981 -0.1018 -0.2397 0.047 Uiso 1 1 calc R U . . .
C46 C -0.1656(4) 0.3815(3) -0.1766(2) 0.0405(10) Uani 1 1 d . . . . .
H45 H -0.1148 0.3252 -0.1327 0.049 Uiso 1 1 calc R U . . .
C25 C -0.2982(4) 0.0798(3) -0.6108(3) 0.0459(10) Uani 1 1 d . . . . .
H25 H -0.2742 0.0093 -0.5974 0.055 Uiso 1 1 calc R U . . .
C1 C 0.1495(4) 0.3000(3) -0.1403(2) 0.0398(9) Uani 1 1 d . . . . .
H1 H 0.1337 0.3691 -0.1489 0.048 Uiso 1 1 calc R U . . .
C4 C 0.1963(4) 0.0990(3) -0.1161(3) 0.0479(11) Uani 1 1 d . . . . .
H4 H 0.2121 0.0296 -0.1063 0.057 Uiso 1 1 calc R U . . .
C39 C -0.0325(3) 0.3851(3) -0.5303(3) 0.0393(9) Uani 1 1 d . . . . .
H39 H -0.0826 0.4454 -0.5706 0.047 Uiso 1 1 calc R U . . .
C34 C -0.4472(4) 0.0903(3) -0.1090(3) 0.0473(11) Uani 1 1 d . . . . .
H34 H -0.4399 0.0545 -0.0494 0.057 Uiso 1 1 calc R U . . .
C7 C 0.1386(4) -0.0320(3) 0.0489(3) 0.0425(10) Uani 1 1 d . . . . .
H7 H 0.1500 -0.0574 0.0036 0.051 Uiso 1 1 calc R U . . .
C13 C 0.0594(4) 0.0817(3) 0.3949(3) 0.0485(11) Uani 1 1 d . . . . .
H13 H 0.0660 0.0429 0.4537 0.058 Uiso 1 1 calc R U . . .
C28 C -0.3597(4) -0.0465(3) -0.4428(3) 0.0414(10) Uani 1 1 d . . . . .
H28 H -0.3453 -0.0749 -0.4862 0.050 Uiso 1 1 calc R U . . .
C35 C -0.4810(4) 0.1952(4) -0.1403(3) 0.0479(11) Uani 1 1 d . . . . .
H35 H -0.4994 0.2316 -0.1026 0.057 Uiso 1 1 calc R U . . .
C22 C -0.3672(4) 0.2834(3) -0.6460(3) 0.0476(11) Uani 1 1 d . . . . .
H22 H -0.3906 0.3538 -0.6586 0.057 Uiso 1 1 calc R U . . .
C8 C 0.1246(4) -0.0931(3) 0.1305(3) 0.0482(11) Uani 1 1 d . . . . .
H8 H 0.1261 -0.1605 0.1409 0.058 Uiso 1 1 calc R U . . .
OW1 O -0.1375(2) 0.41168(18) 0.10862(16) 0.0358(6) Uani 1 1 d . . . . .
OW2 O -0.6601(2) 0.4118(2) -0.40671(18) 0.0464(7) Uani 1 1 d . . . . .
C14 C 0.0249(4) 0.1860(3) 0.3677(3) 0.0478(11) Uani 1 1 d . . . . .
H14 H 0.0039 0.2193 0.4075 0.057 Uiso 1 1 calc R U . . .
C29 C -0.3718(4) -0.1061(3) -0.3600(3) 0.0472(11) Uani 1 1 d . . . . .
H29 H -0.3659 -0.1749 -0.3468 0.057 Uiso 1 1 calc R U . . .
C23 C -0.3171(4) 0.2464(4) -0.7093(3) 0.0540(12) Uani 1 1 d . . . . .
H23 H -0.3072 0.2912 -0.7632 0.065 Uiso 1 1 calc R U . . .
C3 C 0.2143(4) 0.1658(4) -0.1962(3) 0.0590(13) Uani 1 1 d . . . . .
H3 H 0.2415 0.1417 -0.2408 0.071 Uiso 1 1 calc R U . . .
C24 C -0.2824(5) 0.1446(4) -0.6926(3) 0.0604(13) Uani 1 1 d . . . . .
H24 H -0.2486 0.1182 -0.7347 0.072 Uiso 1 1 calc R U . . .
C2 C 0.1913(4) 0.2668(4) -0.2080(3) 0.0507(11) Uani 1 1 d . . . . .
H2 H 0.2036 0.3127 -0.2605 0.061 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O11 2.364(2) . ?
Sm1 O1 2.374(2) . ?
Sm1 O12 2.451(2) . ?
Sm1 O4 2.515(2) . ?
Sm1 O3 2.520(2) . ?
Sm1 N3 2.580(3) . ?
Sm1 N1 2.596(3) . ?
Sm1 OW1 2.603(2) . ?
Sm1 N2 2.614(2) . ?
Sm1 C21 2.876(3) . ?
Sm2 O10 2.350(2) 2_464 ?
Sm2 O9 2.358(2) . ?
Sm2 O7 2.361(2) . ?
Sm2 O6 2.514(2) . ?
Sm2 O5 2.556(2) . ?
Sm2 N6 2.582(3) . ?
Sm2 N4 2.585(3) . ?
Sm2 N5 2.609(3) . ?
Sm2 OW2 2.646(3) . ?
Sm2 C37 2.892(3) . ?
S1 C17 1.717(3) 1_655 ?
S1 C20 1.718(3) . ?
S2 C41 1.710(3) 1_655 ?
S2 C38 1.718(3) . ?
S3 C44 1.712(3) . ?
S3 C47 1.715(3) . ?
O3 C21 1.263(4) . ?
O4 C21 1.261(4) . ?
O11 C48 1.255(3) . ?
O6 C37 1.264(4) . ?
O5 C37 1.265(4) . ?
N2 C10 1.344(4) . ?
N2 C6 1.350(4) . ?
O12 C48 1.246(4) 2_565 ?
O2 C16 1.233(4) . ?
N6 C36 1.342(4) . ?
N6 C32 1.349(4) . ?
N4 C22 1.340(5) . ?
N4 C26 1.349(4) . ?
N5 C31 1.342(4) . ?
N5 C27 1.352(4) . ?
N3 C11 1.347(4) . ?
N3 C15 1.351(4) . ?
N1 C1 1.333(4) . ?
N1 C5 1.348(4) . ?
C20 C19 1.360(4) . ?
C20 C21 1.477(4) . ?
C17 C18 1.372(5) 1_455 ?
C17 C16 1.497(4) . ?
C17 S1 1.717(3) 1_455 ?
C37 C38 1.474(4) . ?
C38 C39 1.372(5) . ?
C16 O1 1.271(4) . ?
C41 C40 1.364(5) 1_455 ?
C41 C42 1.505(5) . ?
C41 S2 1.710(3) 1_455 ?
C40 C41 1.364(5) 1_655 ?
C40 C39 1.404(5) . ?
C40 H40 0.9300 . ?
C18 C17 1.372(5) 1_655 ?
C18 C19 1.406(5) . ?
C18 H19 0.9300 . ?
C19 H18 0.9300 . ?
O7 C42 1.253(4) . ?
O9 C43 1.247(4) . ?
O10 C43 1.236(4) . ?
O10 Sm2 2.350(2) 2_464 ?
C43 C44 1.486(4) . ?
O8 C42 1.237(4) . ?
C48 O12 1.246(4) 2_565 ?
C48 C47 1.492(4) . ?
C32 C33 1.387(5) . ?
C32 C31 1.487(5) . ?
C11 C12 1.390(4) . ?
C11 C10 1.472(5) . ?
C31 C30 1.397(5) . ?
C10 C9 1.401(4) . ?
C5 C4 1.377(5) . ?
C5 C6 1.482(5) . ?
C47 C46 1.346(4) . ?
C26 C25 1.383(5) . ?
C26 C27 1.478(5) . ?
C6 C7 1.400(5) . ?
C27 C28 1.398(5) . ?
C44 C45 1.355(4) . ?
C45 C46 1.400(4) . ?
C45 H46 0.9300 . ?
C33 C34 1.371(5) . ?
C33 H33 0.9300 . ?
C15 C14 1.378(5) . ?
C15 H15 0.9300 . ?
C36 C35 1.383(5) . ?
C36 H36 0.9300 . ?
C9 C8 1.365(6) . ?
C9 H9 0.9300 . ?
C12 C13 1.380(6) . ?
C12 H12 0.9300 . ?
C30 C29 1.377(6) . ?
C30 H30 0.9300 . ?
C46 H45 0.9300 . ?
C25 C24 1.398(6) . ?
C25 H25 0.9300 . ?
C1 C2 1.385(5) . ?
C1 H1 0.9300 . ?
C4 C3 1.396(6) . ?
C4 H4 0.9300 . ?
C39 H39 0.9300 . ?
C34 C35 1.372(6) . ?
C34 H34 0.9300 . ?
C7 C8 1.368(6) . ?
C7 H7 0.9300 . ?
C13 C14 1.366(6) . ?
C13 H13 0.9300 . ?
C28 C29 1.370(6) . ?
C28 H28 0.9300 . ?
C35 H35 0.9300 . ?
C22 C23 1.375(5) . ?
C22 H22 0.9300 . ?
C8 H8 0.9300 . ?
C14 H14 0.9300 . ?
C29 H29 0.9300 . ?
C23 C24 1.350(6) . ?
C23 H23 0.9300 . ?
C3 C2 1.361(6) . ?
C3 H3 0.9300 . ?
C24 H24 0.9300 . ?
C2 H2 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Sm1 O1 79.40(8) . . ?
O11 Sm1 O12 101.48(7) . . ?
O1 Sm1 O12 136.19(9) . . ?
O11 Sm1 O4 123.85(8) . . ?
O1 Sm1 O4 141.83(8) . . ?
O12 Sm1 O4 73.56(8) . . ?
O11 Sm1 O3 73.38(7) . . ?
O1 Sm1 O3 146.26(8) . . ?
O12 Sm1 O3 69.98(8) . . ?
O4 Sm1 O3 51.96(7) . . ?
O11 Sm1 N3 148.55(9) . . ?
O1 Sm1 N3 82.77(9) . . ?
O12 Sm1 N3 74.39(8) . . ?
O4 Sm1 N3 85.55(8) . . ?
O3 Sm1 N3 130.28(8) . . ?
O11 Sm1 N1 77.60(9) . . ?
O1 Sm1 N1 83.50(9) . . ?
O12 Sm1 N1 139.99(9) . . ?
O4 Sm1 N1 74.33(8) . . ?
O3 Sm1 N1 71.60(8) . . ?
N3 Sm1 N1 125.83(9) . . ?
O11 Sm1 OW1 73.65(8) . . ?
O1 Sm1 OW1 66.23(8) . . ?
O12 Sm1 OW1 72.03(8) . . ?
O4 Sm1 OW1 144.05(8) . . ?
O3 Sm1 OW1 122.36(7) . . ?
N3 Sm1 OW1 75.51(8) . . ?
N1 Sm1 OW1 141.25(8) . . ?
O11 Sm1 N2 132.95(8) . . ?
O1 Sm1 N2 71.76(8) . . ?
O12 Sm1 N2 125.10(7) . . ?
O4 Sm1 N2 70.57(7) . . ?
O3 Sm1 N2 113.85(8) . . ?
N3 Sm1 N2 62.80(8) . . ?
N1 Sm1 N2 63.11(8) . . ?
OW1 Sm1 N2 123.31(8) . . ?
O11 Sm1 C21 98.85(9) . . ?
O1 Sm1 C21 154.78(9) . . ?
O12 Sm1 C21 68.99(8) . . ?
O4 Sm1 C21 25.96(8) . . ?
O3 Sm1 C21 26.01(8) . . ?
N3 Sm1 C21 108.10(9) . . ?
N1 Sm1 C21 71.65(9) . . ?
OW1 Sm1 C21 137.84(8) . . ?
N2 Sm1 C21 92.61(8) . . ?
O10 Sm2 O9 98.28(9) 2_464 . ?
O10 Sm2 O7 75.83(9) 2_464 . ?
O9 Sm2 O7 131.87(10) . . ?
O10 Sm2 O6 125.88(9) 2_464 . ?
O9 Sm2 O6 76.12(9) . . ?
O7 Sm2 O6 145.44(9) . . ?
O10 Sm2 O5 75.41(8) 2_464 . ?
O9 Sm2 O5 69.94(9) . . ?
O7 Sm2 O5 146.24(9) . . ?
O6 Sm2 O5 51.76(7) . . ?
O10 Sm2 N6 149.70(9) 2_464 . ?
O9 Sm2 N6 77.64(9) . . ?
O7 Sm2 N6 84.67(9) . . ?
O6 Sm2 N6 82.78(8) . . ?
O5 Sm2 N6 128.60(8) . . ?
O10 Sm2 N4 75.47(9) 2_464 . ?
O9 Sm2 N4 141.68(10) . . ?
O7 Sm2 N4 84.03(9) . . ?
O6 Sm2 N4 77.62(9) . . ?
O5 Sm2 N4 71.93(9) . . ?
N6 Sm2 N4 125.80(9) . . ?
O10 Sm2 N5 130.67(8) 2_464 . ?
O9 Sm2 N5 130.83(8) . . ?
O7 Sm2 N5 74.09(8) . . ?
O6 Sm2 N5 71.53(8) . . ?
O5 Sm2 N5 113.19(8) . . ?
N6 Sm2 N5 62.57(8) . . ?
N4 Sm2 N5 63.34(9) . . ?
O10 Sm2 OW2 73.45(9) 2_464 . ?
O9 Sm2 OW2 67.38(9) . . ?
O7 Sm2 OW2 65.19(9) . . ?
O6 Sm2 OW2 141.28(9) . . ?
O5 Sm2 OW2 121.64(8) . . ?
N6 Sm2 OW2 77.39(9) . . ?
N4 Sm2 OW2 140.49(9) . . ?
N5 Sm2 OW2 124.64(8) . . ?
O10 Sm2 C37 100.89(10) 2_464 . ?
O9 Sm2 C37 70.40(10) . . ?
O7 Sm2 C37 157.59(10) . . ?
O6 Sm2 C37 25.85(8) . . ?
O5 Sm2 C37 25.93(8) . . ?
N6 Sm2 C37 105.72(10) . . ?
N4 Sm2 C37 73.76(10) . . ?
N5 Sm2 C37 92.83(9) . . ?
OW2 Sm2 C37 135.85(9) . . ?
C17 S1 C20 91.61(16) 1_655 . ?
C41 S2 C38 91.73(17) 1_655 . ?
C44 S3 C47 91.63(15) . . ?
C21 O3 Sm1 92.90(18) . . ?
C21 O4 Sm1 93.20(18) . . ?
C48 O11 Sm1 168.2(2) . . ?
C37 O6 Sm2 94.02(19) . . ?
C37 O5 Sm2 92.0(2) . . ?
C10 N2 C6 119.2(3) . . ?
C10 N2 Sm1 120.2(2) . . ?
C6 N2 Sm1 119.6(2) . . ?
C48 O12 Sm1 125.78(19) 2_565 . ?
C36 N6 C32 118.0(3) . . ?
C36 N6 Sm2 119.4(2) . . ?
C32 N6 Sm2 122.4(2) . . ?
C22 N4 C26 117.7(3) . . ?
C22 N4 Sm2 120.5(3) . . ?
C26 N4 Sm2 121.5(2) . . ?
C31 N5 C27 118.7(3) . . ?
C31 N5 Sm2 121.1(2) . . ?
C27 N5 Sm2 119.3(2) . . ?
C11 N3 C15 117.9(3) . . ?
C11 N3 Sm1 122.0(2) . . ?
C15 N3 Sm1 119.9(2) . . ?
C1 N1 C5 117.8(3) . . ?
C1 N1 Sm1 120.9(2) . . ?
C5 N1 Sm1 121.3(2) . . ?
C19 C20 C21 128.4(3) . . ?
C19 C20 S1 111.6(2) . . ?
C21 C20 S1 119.9(2) . . ?
O4 C21 O3 121.9(3) . . ?
O4 C21 C20 119.3(3) . . ?
O3 C21 C20 118.8(3) . . ?
O4 C21 Sm1 60.84(16) . . ?
O3 C21 Sm1 61.09(16) . . ?
C20 C21 Sm1 177.5(2) . . ?
C18 C17 C16 129.4(3) 1_455 . ?
C18 C17 S1 111.3(2) 1_455 1_455 ?
C16 C17 S1 119.3(2) . 1_455 ?
O6 C37 O5 122.1(3) . . ?
O6 C37 C38 119.0(3) . . ?
O5 C37 C38 118.8(3) . . ?
O6 C37 Sm2 60.13(17) . . ?
O5 C37 Sm2 62.07(17) . . ?
C38 C37 Sm2 176.9(3) . . ?
C39 C38 C37 128.8(3) . . ?
C39 C38 S2 111.2(3) . . ?
C37 C38 S2 119.9(3) . . ?
O2 C16 O1 126.8(3) . . ?
O2 C16 C17 117.8(3) . . ?
O1 C16 C17 115.4(3) . . ?
C40 C41 C42 129.0(3) 1_455 . ?
C40 C41 S2 111.7(3) 1_455 1_455 ?
C42 C41 S2 119.3(3) . 1_455 ?
C41 C40 C39 112.8(3) 1_655 . ?
C41 C40 H40 123.6 1_655 . ?
C39 C40 H40 123.6 . . ?
C17 C18 C19 112.6(3) 1_655 . ?
C17 C18 H19 123.7 1_655 . ?
C19 C18 H19 123.7 . . ?
C20 C19 C18 112.9(3) . . ?
C20 C19 H18 123.6 . . ?
C18 C19 H18 123.6 . . ?
C16 O1 Sm1 147.2(2) . . ?
C42 O7 Sm2 143.5(2) . . ?
C43 O9 Sm2 157.9(2) . . ?
C43 O10 Sm2 154.9(2) . 2_464 ?
O10 C43 O9 125.4(3) . . ?
O10 C43 C44 118.0(3) . . ?
O9 C43 C44 116.7(3) . . ?
O12 C48 O11 125.0(3) 2_565 . ?
O12 C48 C47 117.7(3) 2_565 . ?
O11 C48 C47 117.3(3) . . ?
N6 C32 C33 121.8(3) . . ?
N6 C32 C31 116.2(3) . . ?
C33 C32 C31 122.0(3) . . ?
N3 C11 C12 121.7(3) . . ?
N3 C11 C10 116.7(3) . . ?
C12 C11 C10 121.6(3) . . ?
N5 C31 C30 122.2(3) . . ?
N5 C31 C32 116.7(3) . . ?
C30 C31 C32 121.1(3) . . ?
N2 C10 C9 121.3(3) . . ?
N2 C10 C11 117.5(3) . . ?
C9 C10 C11 121.1(3) . . ?
N1 C5 C4 122.2(4) . . ?
N1 C5 C6 116.9(3) . . ?
C4 C5 C6 120.8(3) . . ?
C46 C47 C48 127.2(3) . . ?
C46 C47 S3 111.2(2) . . ?
C48 C47 S3 121.6(2) . . ?
N4 C26 C25 121.5(4) . . ?
N4 C26 C27 116.5(3) . . ?
C25 C26 C27 121.9(3) . . ?
N2 C6 C7 121.2(3) . . ?
N2 C6 C5 117.6(3) . . ?
C7 C6 C5 121.2(3) . . ?
O8 C42 O7 126.9(3) . . ?
O8 C42 C41 117.5(3) . . ?
O7 C42 C41 115.5(3) . . ?
N5 C27 C28 120.9(3) . . ?
N5 C27 C26 117.9(3) . . ?
C28 C27 C26 121.2(3) . . ?
C45 C44 C43 126.1(3) . . ?
C45 C44 S3 111.1(2) . . ?
C43 C44 S3 122.8(2) . . ?
C44 C45 C46 112.8(3) . . ?
C44 C45 H46 123.6 . . ?
C46 C45 H46 123.6 . . ?
C34 C33 C32 119.3(4) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
N3 C15 C14 122.8(4) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
N6 C36 C35 122.8(4) . . ?
N6 C36 H36 118.6 . . ?
C35 C36 H36 118.6 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C13 C12 C11 119.2(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C29 C30 C31 119.0(4) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C47 C46 C45 113.2(3) . . ?
C47 C46 H45 123.4 . . ?
C45 C46 H45 123.4 . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
N1 C1 C2 123.3(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C5 C4 C3 118.9(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C38 C39 C40 112.6(3) . . ?
C38 C39 H39 123.7 . . ?
C40 C39 H39 123.7 . . ?
C33 C34 C35 119.4(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C8 C7 C6 119.1(4) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C14 C13 C12 119.4(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C29 C28 C27 120.2(4) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C34 C35 C36 118.7(4) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
N4 C22 C23 123.4(4) . . ?
N4 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C9 C8 C7 119.9(4) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C28 C29 C30 118.9(4) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C24 C23 C22 119.5(4) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C23 C24 C25 118.6(4) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C3 C2 C1 118.8(4) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?

_refine_diff_density_max         1.208
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.119

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 1410405'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Eu2 N6 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1316.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.990(6)
_cell_length_b                   14.334(7)
_cell_length_c                   18.575(7)
_cell_angle_alpha                110.283(6)
_cell_angle_beta                 99.536(5)
_cell_angle_gamma                99.030(5)
_cell_volume                     2393(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31626
_cell_measurement_theta_min      4.358
_cell_measurement_theta_max      51.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    2.803
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31610
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.203
_diffrn_reflns_theta_max         27.385
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10843
_reflns_number_gt                8423
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+2.2470P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10843
_refine_ls_number_parameters     658
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu2 Eu 0.53750(2) 0.70831(2) 0.05787(2) 0.01981(7) Uani 1 1 d . . . . .
Eu1 Eu 0.04913(2) 0.69557(2) -0.44115(2) 0.01724(7) Uani 1 1 d . . . . .
S2 S 0.35194(13) 0.79510(10) 0.32543(7) 0.0287(3) Uani 1 1 d . . . . .
S1 S 0.84884(15) 0.77951(11) -0.17832(7) 0.0338(3) Uani 1 1 d . . . . .
S3 S 0.25770(15) 0.56416(9) -0.22011(7) 0.0316(3) Uani 1 1 d . . . . .
O11 O 0.0966(4) 0.4437(3) -0.44899(18) 0.0290(8) Uani 1 1 d . . . . .
O3 O -0.0123(4) 0.7645(2) -0.31064(19) 0.0286(8) Uani 1 1 d . . . . .
O5 O 0.4988(4) 0.7713(3) 0.19395(19) 0.0312(8) Uani 1 1 d . . . . .
O4 O -0.1381(4) 0.6128(3) -0.39354(19) 0.0308(8) Uani 1 1 d . . . . .
O7 O 0.0992(4) 0.7393(3) -0.5466(2) 0.0365(9) Uani 1 1 d . . . . .
O9 O 0.3884(4) 0.5807(3) -0.0573(2) 0.0368(9) Uani 1 1 d . . . . .
O12 O 0.1448(4) 0.6044(3) -0.3639(2) 0.0354(9) Uani 1 1 d . . . . .
N2 N 0.0872(4) 0.8920(3) -0.3945(2) 0.0207(8) Uani 1 1 d . . . . .
O10 O 0.6232(4) 0.5841(3) 0.0886(2) 0.0386(9) Uani 1 1 d . . . . .
O6 O 0.3529(4) 0.6296(3) 0.1080(2) 0.0395(9) Uani 1 1 d . . . . .
N3 N -0.1690(4) 0.7644(3) -0.4675(2) 0.0284(9) Uani 1 1 d . . . . .
N5 N 0.5883(4) 0.9064(3) 0.1055(2) 0.0254(9) Uani 1 1 d . . . . .
OW1 O 0.2163(4) 0.5950(3) -0.5133(2) 0.0431(10) Uani 1 1 d . . . . .
O8 O 0.2687(4) 0.8760(3) -0.5244(2) 0.0349(9) Uani 1 1 d . . . . .
N6 N 0.3288(4) 0.7851(3) 0.0305(3) 0.0363(11) Uani 1 1 d . . . . .
N1 N 0.2969(4) 0.8017(3) -0.3662(2) 0.0281(9) Uani 1 1 d . . . . .
C47 C 0.2014(5) 0.4808(4) -0.3156(3) 0.0256(11) Uani 1 1 d . . . . .
N4 N 0.7889(4) 0.8081(3) 0.1330(2) 0.0299(10) Uani 1 1 d . . . . .
C32 C 0.3442(6) 0.8882(4) 0.0538(3) 0.0347(13) Uani 1 1 d . . . . .
C43 C 0.3606(5) 0.4909(4) -0.1064(3) 0.0243(10) Uani 1 1 d . . . . .
C5 C 0.3290(5) 0.9050(4) -0.3392(3) 0.0253(10) Uani 1 1 d . . . . .
C11 C -0.1598(5) 0.8657(4) -0.4477(3) 0.0282(11) Uani 1 1 d . . . . .
C6 C 0.2163(5) 0.9530(3) -0.3608(3) 0.0248(10) Uani 1 1 d . . . . .
C41 C 0.2202(5) 0.7365(4) 0.3546(3) 0.0290(11) Uani 1 1 d . . . . .
C48 C 0.1425(5) 0.5116(3) -0.3814(3) 0.0208(10) Uani 1 1 d . . . . .
C44 C 0.3026(5) 0.4710(4) -0.1890(3) 0.0278(11) Uani 1 1 d . . . . .
O2 O 0.7692(5) 0.8609(4) -0.0285(3) 0.0652(13) Uani 1 1 d . . . . .
C26 C 0.8267(5) 0.9115(4) 0.1606(3) 0.0302(11) Uani 1 1 d . . . . .
C1 C 0.3982(5) 0.7557(4) -0.3486(3) 0.0378(13) Uani 1 1 d . . . . .
H1 H 0.3776 0.6847 -0.3673 0.045 Uiso 1 1 calc R U . . .
C10 C -0.0179(5) 0.9325(4) -0.4147(3) 0.0275(11) Uani 1 1 d . . . . .
C42 C 0.1970(5) 0.7901(4) -0.5651(3) 0.0257(11) Uani 1 1 d . . . . .
C21 C -0.1062(5) 0.6855(4) -0.3269(3) 0.0246(10) Uani 1 1 d . . . . .
C24 C 1.0569(6) 0.9129(6) 0.2210(4) 0.0568(18) Uani 1 1 d . . . . .
H24 H 1.1460 0.9482 0.2517 0.068 Uiso 1 1 calc R U . . .
C27 C 0.7189(5) 0.9642(4) 0.1406(3) 0.0281(11) Uani 1 1 d . . . . .
C3 C 0.5604(6) 0.9130(5) -0.2756(4) 0.0516(17) Uani 1 1 d . . . . .
H3 H 0.6479 0.9505 -0.2437 0.062 Uiso 1 1 calc R U . . .
O1 O 0.6331(6) 0.7161(5) -0.0429(3) 0.118(3) Uani 1 1 d . U . . .
C19 C 0.7202(6) 0.5971(5) -0.2712(3) 0.0464(15) Uani 1 1 d . . . . .
H19 H 0.6897 0.5354 -0.3146 0.056 Uiso 1 1 calc R U . . .
C40 C 0.1533(6) 0.6428(4) 0.2984(3) 0.0408(14) Uani 1 1 d . . . . .
H40 H 0.0805 0.5994 0.3046 0.049 Uiso 1 1 calc R U . . .
OW2 O 0.8676(9) 0.5409(6) -0.0211(5) 0.185(4) Uani 1 1 d . . . . .
C20 C 0.8171(5) 0.6774(4) -0.2670(3) 0.0276(11) Uani 1 1 d . . . . .
C15 C -0.2977(6) 0.7023(5) -0.4958(3) 0.0401(14) Uani 1 1 d . . . . .
H15 H -0.3058 0.6323 -0.5102 0.048 Uiso 1 1 calc R U . . .
C25 C 0.9598(6) 0.9653(5) 0.2054(3) 0.0454(15) Uani 1 1 d . . . . .
H25 H 0.9830 1.0364 0.2245 0.055 Uiso 1 1 calc R U . . .
C36 C 0.2007(6) 0.7245(5) -0.0001(4) 0.0494(16) Uani 1 1 d . . . . .
H36 H 0.1916 0.6542 -0.0166 0.059 Uiso 1 1 calc R U . . .
C31 C 0.4873(6) 0.9520(4) 0.0871(3) 0.0302(11) Uani 1 1 d . . . . .
C38 C 0.3148(5) 0.6943(4) 0.2354(3) 0.0288(11) Uani 1 1 d . . . . .
C29 C 0.6473(7) 1.1135(4) 0.1366(4) 0.0491(16) Uani 1 1 d . . . . .
H29 H 0.6672 1.1829 0.1463 0.059 Uiso 1 1 calc R U . . .
C23 C 1.0226(6) 0.8093(6) 0.1916(4) 0.0553(18) Uani 1 1 d . . . . .
H23 H 1.0881 0.7727 0.2005 0.066 Uiso 1 1 calc R U . . .
C45 C 0.2721(6) 0.3797(4) -0.2523(3) 0.0391(14) Uani 1 1 d . . . . .
H45 H 0.2868 0.3190 -0.2483 0.047 Uiso 1 1 calc R U . . .
C37 C 0.3939(5) 0.6988(4) 0.1759(3) 0.0272(11) Uani 1 1 d . . . . .
C39 C 0.2056(6) 0.6183(4) 0.2297(3) 0.0407(14) Uani 1 1 d . . . . .
H39 H 0.1703 0.5578 0.1855 0.049 Uiso 1 1 calc R U . . .
C17 C 0.7318(6) 0.7145(5) -0.1461(3) 0.0441(15) Uani 1 1 d . . . . .
C22 C 0.8867(6) 0.7588(5) 0.1475(3) 0.0410(14) Uani 1 1 d . . . . .
H22 H 0.8632 0.6877 0.1273 0.049 Uiso 1 1 calc R U . . .
C8 C 0.1367(7) 1.0965(4) -0.3710(3) 0.0460(16) Uani 1 1 d . . . . .
H8 H 0.1528 1.1652 -0.3637 0.055 Uiso 1 1 calc R U . . .
C9 C 0.0057(7) 1.0354(4) -0.4050(3) 0.0429(15) Uani 1 1 d . . . . .
H9 H -0.0672 1.0620 -0.4216 0.052 Uiso 1 1 calc R U . . .
C18 C 0.6705(7) 0.6188(5) -0.2008(4) 0.0560(18) Uani 1 1 d . . . . .
H18 H 0.6036 0.5726 -0.1931 0.067 Uiso 1 1 calc R U . . .
C33 C 0.2276(7) 0.9276(5) 0.0455(4) 0.0519(17) Uani 1 1 d . . . . .
H33 H 0.2374 0.9978 0.0611 0.062 Uiso 1 1 calc R U . . .
C46 C 0.2179(6) 0.3873(4) -0.3218(3) 0.0400(14) Uani 1 1 d . . . . .
H46 H 0.1941 0.3319 -0.3699 0.048 Uiso 1 1 calc R U . . .
C12 C -0.2782(6) 0.9042(5) -0.4566(4) 0.0452(15) Uani 1 1 d . . . . .
H12 H -0.2694 0.9740 -0.4434 0.054 Uiso 1 1 calc R U . . .
C4 C 0.4603(6) 0.9629(4) -0.2938(3) 0.0390(13) Uani 1 1 d . . . . .
H4 H 0.4804 1.0339 -0.2760 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2442(7) 1.0571(4) -0.3477(3) 0.0402(14) Uani 1 1 d . . . . .
H7 H 0.3336 1.0984 -0.3238 0.048 Uiso 1 1 calc R U . . .
C30 C 0.5144(7) 1.0554(4) 0.1006(3) 0.0464(15) Uani 1 1 d . . . . .
H30 H 0.4436 1.0847 0.0856 0.056 Uiso 1 1 calc R U . . .
C13 C -0.4086(6) 0.8388(6) -0.4852(4) 0.0532(17) Uani 1 1 d . . . . .
H13 H -0.4886 0.8637 -0.4911 0.064 Uiso 1 1 calc R U . . .
C16 C 0.7042(7) 0.7677(6) -0.0648(4) 0.0554(18) Uani 1 1 d . . . . .
C2 C 0.5306(6) 0.8085(5) -0.3045(4) 0.0468(15) Uani 1 1 d . . . . .
H2 H 0.5984 0.7740 -0.2946 0.056 Uiso 1 1 calc R U . . .
C35 C 0.0816(7) 0.7603(6) -0.0085(4) 0.0571(18) Uani 1 1 d . . . . .
H35 H -0.0061 0.7158 -0.0289 0.069 Uiso 1 1 calc R U . . .
C28 C 0.7512(7) 1.0694(4) 0.1583(4) 0.0472(15) Uani 1 1 d . . . . .
H28 H 0.8410 1.1087 0.1843 0.057 Uiso 1 1 calc R U . . .
C14 C -0.4177(6) 0.7370(5) -0.5046(4) 0.0521(17) Uani 1 1 d . . . . .
H14 H -0.5044 0.6913 -0.5236 0.063 Uiso 1 1 calc R U . . .
C34 C 0.0963(7) 0.8628(6) 0.0142(4) 0.062(2) Uani 1 1 d . . . . .
H34 H 0.0180 0.8896 0.0086 0.075 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu2 O1 2.265(5) . ?
Eu2 O10 2.291(3) . ?
Eu2 O9 2.350(3) . ?
Eu2 O6 2.487(4) . ?
Eu2 O5 2.491(3) . ?
Eu2 N6 2.565(4) . ?
Eu2 N4 2.575(4) . ?
Eu2 N5 2.600(4) . ?
Eu2 C37 2.841(5) . ?
Eu1 O11 2.356(3) 2_564 ?
Eu1 O7 2.358(3) . ?
Eu1 O12 2.432(3) . ?
Eu1 O3 2.500(3) . ?
Eu1 O4 2.503(3) . ?
Eu1 N1 2.566(4) . ?
Eu1 N3 2.573(4) . ?
Eu1 N2 2.586(4) . ?
Eu1 OW1 2.612(4) . ?
Eu1 C21 2.858(5) . ?
S2 C41 1.714(5) . ?
S2 C38 1.724(5) . ?
S1 C17 1.694(6) . ?
S1 C20 1.722(5) . ?
S3 C47 1.697(5) . ?
S3 C44 1.719(5) . ?
O11 C48 1.247(5) . ?
O11 Eu1 2.356(3) 2_564 ?
O3 C21 1.262(6) . ?
O5 C37 1.262(6) . ?
O4 C21 1.261(6) . ?
O7 C42 1.290(6) . ?
O9 C43 1.247(6) . ?
O12 C48 1.251(5) . ?
N2 C10 1.339(6) . ?
N2 C6 1.349(6) . ?
O10 C43 1.256(5) 2_665 ?
O6 C37 1.256(6) . ?
N3 C15 1.347(7) . ?
N3 C11 1.353(6) . ?
N5 C31 1.345(6) . ?
N5 C27 1.348(6) . ?
O8 C42 1.225(6) . ?
N6 C36 1.335(7) . ?
N6 C32 1.363(7) . ?
N1 C1 1.348(6) . ?
N1 C5 1.353(6) . ?
C47 C46 1.344(7) . ?
C47 C48 1.501(6) . ?
N4 C22 1.338(7) . ?
N4 C26 1.354(6) . ?
C32 C33 1.380(8) . ?
C32 C31 1.472(8) . ?
C43 O10 1.256(5) 2_665 ?
C43 C44 1.455(6) . ?
C5 C4 1.388(7) . ?
C5 C6 1.479(7) . ?
C11 C12 1.391(7) . ?
C11 C10 1.477(7) . ?
C6 C7 1.399(7) . ?
C41 C40 1.362(7) . ?
C41 C42 1.498(6) 1_556 ?
C44 C45 1.370(7) . ?
O2 C16 1.273(8) . ?
C26 C25 1.387(7) . ?
C26 C27 1.479(7) . ?
C1 C2 1.375(7) . ?
C1 H1 0.9300 . ?
C10 C9 1.399(7) . ?
C42 C41 1.498(6) 1_554 ?
C21 C20 1.478(6) 1_455 ?
C24 C23 1.354(9) . ?
C24 C25 1.370(9) . ?
C24 H24 0.9300 . ?
C27 C28 1.398(7) . ?
C3 C2 1.368(9) . ?
C3 C4 1.381(8) . ?
C3 H3 0.9300 . ?
O1 C16 1.165(8) . ?
C19 C20 1.354(7) . ?
C19 C18 1.426(7) . ?
C19 H19 0.9300 . ?
C40 C39 1.411(7) . ?
C40 H40 0.9300 . ?
C20 C21 1.478(6) 1_655 ?
C15 C14 1.375(8) . ?
C15 H15 0.9300 . ?
C25 H25 0.9300 . ?
C36 C35 1.376(8) . ?
C36 H36 0.9300 . ?
C31 C30 1.389(7) . ?
C38 C39 1.377(7) . ?
C38 C37 1.474(7) . ?
C29 C30 1.369(9) . ?
C29 C28 1.372(9) . ?
C29 H29 0.9300 . ?
C23 C22 1.396(8) . ?
C23 H23 0.9300 . ?
C45 C46 1.362(7) . ?
C45 H45 0.9300 . ?
C39 H39 0.9300 . ?
C17 C18 1.362(9) . ?
C17 C16 1.531(8) . ?
C22 H22 0.9300 . ?
C8 C9 1.364(8) . ?
C8 C7 1.366(8) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C18 H18 0.9300 . ?
C33 C34 1.382(9) . ?
C33 H33 0.9300 . ?
C46 H46 0.9300 . ?
C12 C13 1.378(9) . ?
C12 H12 0.9300 . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C30 H30 0.9300 . ?
C13 C14 1.360(9) . ?
C13 H13 0.9300 . ?
C2 H2 0.9300 . ?
C35 C34 1.356(9) . ?
C35 H35 0.9300 . ?
C28 H28 0.9300 . ?
C14 H14 0.9300 . ?
C34 H34 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu2 O10 103.4(2) . . ?
O1 Eu2 O9 74.19(17) . . ?
O10 Eu2 O9 89.18(13) . . ?
O1 Eu2 O6 150.76(16) . . ?
O10 Eu2 O6 75.37(14) . . ?
O9 Eu2 O6 76.59(13) . . ?
O1 Eu2 O5 156.11(17) . . ?
O10 Eu2 O5 86.64(13) . . ?
O9 Eu2 O5 128.29(13) . . ?
O6 Eu2 O5 52.53(11) . . ?
O1 Eu2 N6 98.7(2) . . ?
O10 Eu2 N6 148.86(14) . . ?
O9 Eu2 N6 75.90(13) . . ?
O6 Eu2 N6 74.65(15) . . ?
O5 Eu2 N6 81.81(13) . . ?
O1 Eu2 N4 78.91(17) . . ?
O10 Eu2 N4 79.74(14) . . ?
O9 Eu2 N4 147.61(13) . . ?
O6 Eu2 N4 128.26(13) . . ?
O5 Eu2 N4 81.69(12) . . ?
N6 Eu2 N4 126.46(14) . . ?
O1 Eu2 N5 84.8(2) . . ?
O10 Eu2 N5 139.72(13) . . ?
O9 Eu2 N5 130.54(12) . . ?
O6 Eu2 N5 115.49(12) . . ?
O5 Eu2 N5 74.00(12) . . ?
N6 Eu2 N5 63.54(14) . . ?
N4 Eu2 N5 62.98(13) . . ?
O1 Eu2 C37 174.7(2) . . ?
O10 Eu2 C37 80.37(14) . . ?
O9 Eu2 C37 102.34(14) . . ?
O6 Eu2 C37 26.19(12) . . ?
O5 Eu2 C37 26.34(12) . . ?
N6 Eu2 C37 76.48(15) . . ?
N4 Eu2 C37 105.59(14) . . ?
N5 Eu2 C37 94.78(13) . . ?
O11 Eu1 O7 78.56(12) 2_564 . ?
O11 Eu1 O12 99.77(12) 2_564 . ?
O7 Eu1 O12 136.38(13) . . ?
O11 Eu1 O3 123.37(12) 2_564 . ?
O7 Eu1 O3 143.01(12) . . ?
O12 Eu1 O3 73.82(12) . . ?
O11 Eu1 O4 72.40(11) 2_564 . ?
O7 Eu1 O4 144.63(12) . . ?
O12 Eu1 O4 69.62(12) . . ?
O3 Eu1 O4 52.28(11) . . ?
O11 Eu1 N1 148.35(13) 2_564 . ?
O7 Eu1 N1 85.05(13) . . ?
O12 Eu1 N1 74.02(13) . . ?
O3 Eu1 N1 85.40(13) . . ?
O4 Eu1 N1 129.91(12) . . ?
O11 Eu1 N3 78.12(13) 2_564 . ?
O7 Eu1 N3 83.07(13) . . ?
O12 Eu1 N3 139.87(13) . . ?
O3 Eu1 N3 74.45(12) . . ?
O4 Eu1 N3 71.69(13) . . ?
N1 Eu1 N3 126.75(13) . . ?
O11 Eu1 N2 134.27(12) 2_564 . ?
O7 Eu1 N2 73.07(12) . . ?
O12 Eu1 N2 125.49(12) . . ?
O3 Eu1 N2 70.72(11) . . ?
O4 Eu1 N2 114.47(11) . . ?
N1 Eu1 N2 63.23(12) . . ?
N3 Eu1 N2 63.63(13) . . ?
O11 Eu1 OW1 74.24(12) 2_564 . ?
O7 Eu1 OW1 66.33(12) . . ?
O12 Eu1 OW1 71.27(12) . . ?
O3 Eu1 OW1 143.26(12) . . ?
O4 Eu1 OW1 122.17(12) . . ?
N1 Eu1 OW1 74.41(13) . . ?
N3 Eu1 OW1 141.98(13) . . ?
N2 Eu1 OW1 122.73(12) . . ?
O11 Eu1 C21 98.10(14) 2_564 . ?
O7 Eu1 C21 154.85(13) . . ?
O12 Eu1 C21 68.74(13) . . ?
O3 Eu1 C21 26.16(12) . . ?
O4 Eu1 C21 26.14(12) . . ?
N1 Eu1 C21 107.81(14) . . ?
N3 Eu1 C21 71.90(13) . . ?
N2 Eu1 C21 93.13(13) . . ?
OW1 Eu1 C21 137.24(13) . . ?
C41 S2 C38 91.9(2) . . ?
C17 S1 C20 91.6(3) . . ?
C47 S3 C44 92.2(2) . . ?
C48 O11 Eu1 161.9(3) . 2_564 ?
C21 O3 Eu1 92.9(3) . . ?
C37 O5 Eu2 92.5(3) . . ?
C21 O4 Eu1 92.8(3) . . ?
C42 O7 Eu1 141.5(3) . . ?
C43 O9 Eu2 147.9(3) . . ?
C48 O12 Eu1 131.5(3) . . ?
C10 N2 C6 119.1(4) . . ?
C10 N2 Eu1 119.5(3) . . ?
C6 N2 Eu1 120.6(3) . . ?
C43 O10 Eu2 165.7(3) 2_665 . ?
C37 O6 Eu2 92.9(3) . . ?
C15 N3 C11 117.3(4) . . ?
C15 N3 Eu1 121.5(3) . . ?
C11 N3 Eu1 121.1(3) . . ?
C31 N5 C27 118.6(4) . . ?
C31 N5 Eu2 120.0(3) . . ?
C27 N5 Eu2 120.9(3) . . ?
C36 N6 C32 119.0(5) . . ?
C36 N6 Eu2 119.7(4) . . ?
C32 N6 Eu2 121.0(3) . . ?
C1 N1 C5 117.6(4) . . ?
C1 N1 Eu1 120.4(3) . . ?
C5 N1 Eu1 121.9(3) . . ?
C46 C47 C48 126.9(4) . . ?
C46 C47 S3 110.3(4) . . ?
C48 C47 S3 122.8(4) . . ?
C22 N4 C26 117.6(5) . . ?
C22 N4 Eu2 120.5(4) . . ?
C26 N4 Eu2 121.9(3) . . ?
N6 C32 C33 119.5(6) . . ?
N6 C32 C31 117.0(4) . . ?
C33 C32 C31 123.5(5) . . ?
O9 C43 O10 123.7(4) . 2_665 ?
O9 C43 C44 118.5(4) . . ?
O10 C43 C44 117.8(4) 2_665 . ?
N1 C5 C4 122.0(5) . . ?
N1 C5 C6 116.2(4) . . ?
C4 C5 C6 121.8(5) . . ?
N3 C11 C12 121.4(5) . . ?
N3 C11 C10 116.2(4) . . ?
C12 C11 C10 122.3(5) . . ?
N2 C6 C7 121.9(5) . . ?
N2 C6 C5 117.2(4) . . ?
C7 C6 C5 120.9(5) . . ?
C40 C41 C42 129.8(5) . 1_556 ?
C40 C41 S2 111.5(4) . . ?
C42 C41 S2 118.7(4) 1_556 . ?
O11 C48 O12 125.1(4) . . ?
O11 C48 C47 118.1(4) . . ?
O12 C48 C47 116.8(4) . . ?
C45 C44 C43 127.7(5) . . ?
C45 C44 S3 109.7(4) . . ?
C43 C44 S3 122.6(4) . . ?
N4 C26 C25 121.7(5) . . ?
N4 C26 C27 116.7(4) . . ?
C25 C26 C27 121.5(5) . . ?
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
N2 C10 C9 121.0(5) . . ?
N2 C10 C11 118.3(4) . . ?
C9 C10 C11 120.7(5) . . ?
O8 C42 O7 126.5(4) . . ?
O8 C42 C41 118.7(4) . 1_554 ?
O7 C42 C41 114.8(4) . 1_554 ?
O4 C21 O3 121.8(4) . . ?
O4 C21 C20 118.6(5) . 1_455 ?
O3 C21 C20 119.6(4) . 1_455 ?
O4 C21 Eu1 61.0(2) . . ?
O3 C21 Eu1 60.9(2) . . ?
C20 C21 Eu1 177.5(3) 1_455 . ?
C23 C24 C25 119.8(6) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
N5 C27 C28 121.8(5) . . ?
N5 C27 C26 116.9(4) . . ?
C28 C27 C26 121.3(5) . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C16 O1 Eu2 145.7(6) . . ?
C20 C19 C18 111.6(5) . . ?
C20 C19 H19 124.2 . . ?
C18 C19 H19 124.2 . . ?
C41 C40 C39 113.2(5) . . ?
C41 C40 H40 123.4 . . ?
C39 C40 H40 123.4 . . ?
C19 C20 C21 128.4(5) . 1_655 ?
C19 C20 S1 112.1(4) . . ?
C21 C20 S1 119.5(4) 1_655 . ?
N3 C15 C14 123.3(6) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C24 C25 C26 119.4(6) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
N6 C36 C35 123.5(6) . . ?
N6 C36 H36 118.2 . . ?
C35 C36 H36 118.2 . . ?
N5 C31 C30 122.1(5) . . ?
N5 C31 C32 117.3(5) . . ?
C30 C31 C32 120.6(5) . . ?
C39 C38 C37 128.7(5) . . ?
C39 C38 S2 111.1(4) . . ?
C37 C38 S2 120.2(4) . . ?
C30 C29 C28 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C24 C23 C22 118.6(6) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C46 C45 C44 112.8(5) . . ?
C46 C45 H45 123.6 . . ?
C44 C45 H45 123.6 . . ?
O6 C37 O5 122.0(4) . . ?
O6 C37 C38 118.2(5) . . ?
O5 C37 C38 119.8(4) . . ?
O6 C37 Eu2 60.9(3) . . ?
O5 C37 Eu2 61.1(2) . . ?
C38 C37 Eu2 177.9(4) . . ?
C38 C39 C40 112.3(5) . . ?
C38 C39 H39 123.8 . . ?
C40 C39 H39 123.8 . . ?
C18 C17 C16 128.7(6) . . ?
C18 C17 S1 112.1(4) . . ?
C16 C17 S1 119.2(5) . . ?
N4 C22 C23 122.8(6) . . ?
N4 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C9 C8 C7 120.3(5) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C17 C18 C19 112.6(5) . . ?
C17 C18 H18 123.7 . . ?
C19 C18 H18 123.7 . . ?
C32 C33 C34 120.2(6) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C47 C46 C45 115.0(5) . . ?
C47 C46 H46 122.5 . . ?
C45 C46 H46 122.5 . . ?
C13 C12 C11 120.0(6) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C3 C4 C5 118.6(5) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C8 C7 C6 118.2(5) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
C29 C30 C31 118.8(6) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C14 C13 C12 118.5(6) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
O1 C16 O2 128.9(7) . . ?
O1 C16 C17 115.8(7) . . ?
O2 C16 C17 115.2(6) . . ?
C3 C2 C1 118.4(5) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C34 C35 C36 117.7(6) . . ?
C34 C35 H35 121.1 . . ?
C36 C35 H35 121.1 . . ?
C29 C28 C27 118.5(6) . . ?
C29 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
C13 C14 C15 119.5(6) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C35 C34 C33 120.1(6) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?

_refine_diff_density_max         1.987
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.138

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 1410406'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Gd2 N6 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1327.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.998(6)
_cell_length_b                   14.333(6)
_cell_length_c                   18.542(7)
_cell_angle_alpha                110.286(5)
_cell_angle_beta                 99.753(4)
_cell_angle_gamma                98.966(5)
_cell_volume                     2389(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    32952
_cell_measurement_theta_min      4.352
_cell_measurement_theta_max      55.890
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.958
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32946
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.557
_diffrn_reflns_theta_max         28.030
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11491
_reflns_number_gt                9206
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+2.6668P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11491
_refine_ls_number_parameters     658
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0620
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.64933(10) 0.21918(8) 0.67818(6) 0.0289(2) Uani 1 1 d . . . . .
S2 S 1.14837(10) 0.20429(7) 0.17396(6) 0.0268(2) Uani 1 1 d . . . . .
O3 O 0.5106(3) 0.23582(19) 0.81060(14) 0.0262(6) Uani 1 1 d . . . . .
O6 O 1.0018(3) 0.2282(2) 0.30565(15) 0.0304(6) Uani 1 1 d . . . . .
O4 O 0.6373(3) 0.38753(19) 0.89371(15) 0.0292(6) Uani 1 1 d . . . . .
O5 O 1.1464(3) 0.3713(2) 0.39156(15) 0.0350(7) Uani 1 1 d . . . . .
O7 O 0.4003(3) 0.2609(2) 1.04618(15) 0.0315(6) Uani 1 1 d . . . . .
O8 O 0.2323(3) 0.1236(2) 1.02417(16) 0.0328(6) Uani 1 1 d . . . . .
C37 C 1.1067(4) 0.3024(3) 0.3238(2) 0.0255(8) Uani 1 1 d . . . . .
S3 S 0.24207(11) 0.43578(7) 0.71974(5) 0.0280(2) Uani 1 1 d . . . . .
N4 N 0.7118(3) 0.1930(2) 0.36661(18) 0.0271(7) Uani 1 1 d . . . . .
N2 N 0.4126(3) 0.1089(2) 0.89454(17) 0.0202(6) Uani 1 1 d . . . . .
N1 N 0.2024(3) 0.1995(2) 0.86576(18) 0.0265(7) Uani 1 1 d . . . . .
N5 N 0.9121(3) 0.0944(2) 0.39456(17) 0.0220(6) Uani 1 1 d . . . . .
N3 N 0.6681(3) 0.2363(2) 0.96729(18) 0.0265(7) Uani 1 1 d . . . . .
N6 N 1.1708(3) 0.2161(3) 0.4695(2) 0.0321(8) Uani 1 1 d . . . . .
C20 C 0.6812(4) 0.3219(3) 0.7669(2) 0.0263(8) Uani 1 1 d . . . . .
C38 C 1.1839(4) 0.3054(3) 0.2633(2) 0.0252(8) Uani 1 1 d . . . . .
C42 C 0.3042(4) 0.2099(3) 1.0647(2) 0.0230(8) Uani 1 1 d . . . . .
C41 C 0.2795(4) 0.2637(3) 1.1446(2) 0.0255(8) Uani 1 1 d . . . . .
C21 C 0.6047(4) 0.3143(3) 0.8268(2) 0.0222(7) Uani 1 1 d . . . . .
C17 C 0.7675(4) 0.2848(3) 0.6462(2) 0.0334(9) Uani 1 1 d . . . . .
O2 O 0.7332(4) 0.1386(3) 0.52841(19) 0.0505(8) Uani 1 1 d . . . . .
C16 C 0.7923(5) 0.2309(4) 0.5652(2) 0.0393(10) Uani 1 1 d . . . . .
C19 C 0.7798(5) 0.4017(3) 0.7706(3) 0.0409(11) Uani 1 1 d . . . . .
H19 H 0.8114 0.4634 0.8141 0.049 Uiso 1 1 calc R U . . .
C40 C 0.3464(4) 0.3577(3) 1.2019(2) 0.0355(10) Uani 1 1 d . . . . .
H40 H 0.4199 0.4013 1.1966 0.043 Uiso 1 1 calc R U . . .
O12 O 0.3557(3) 0.39540(19) 0.86371(15) 0.0296(6) Uani 1 1 d . . . . .
C48 C 1.1393(3) 0.5092(3) 0.6054(2) 0.0204(7) Uani 1 1 d . . . . .
C6 C 0.2828(4) 0.0480(3) 0.8607(2) 0.0242(8) Uani 1 1 d . . . . .
C43 C 0.3588(3) 0.4884(3) 0.8813(2) 0.0186(7) Uani 1 1 d . . . . .
C26 C 0.6733(4) 0.0899(3) 0.3396(2) 0.0262(8) Uani 1 1 d . . . . .
C11 C 0.6588(4) 0.1355(3) 0.9476(2) 0.0261(8) Uani 1 1 d . . . . .
C27 C 0.7818(4) 0.0372(3) 0.3593(2) 0.0260(8) Uani 1 1 d . . . . .
C31 C 1.0137(4) 0.0493(3) 0.4130(2) 0.0271(8) Uani 1 1 d . . . . .
C5 C 0.1708(4) 0.0961(3) 0.8393(2) 0.0231(8) Uani 1 1 d . . . . .
C44 C 0.2998(4) 0.5199(3) 0.8159(2) 0.0221(7) Uani 1 1 d . . . . .
C32 C 1.1573(4) 0.1145(3) 0.4470(2) 0.0289(9) Uani 1 1 d . . . . .
C7 C 0.2556(5) -0.0557(3) 0.8479(2) 0.0358(10) Uani 1 1 d . . . . .
H7 H 0.1662 -0.0968 0.8238 0.043 Uiso 1 1 calc R U . . .
C10 C 0.5170(4) 0.0678(3) 0.9146(2) 0.0267(8) Uani 1 1 d . . . . .
C1 C 0.1013(4) 0.2448(3) 0.8479(3) 0.0375(10) Uani 1 1 d . . . . .
H1 H 0.1222 0.3159 0.8667 0.045 Uiso 1 1 calc R U . . .
C28 C 0.7493(5) -0.0677(3) 0.3418(3) 0.0389(10) Uani 1 1 d . . . . .
H28 H 0.6591 -0.1067 0.3162 0.047 Uiso 1 1 calc R U . . .
C46 C 0.2274(4) 0.6213(3) 0.7519(2) 0.0329(9) Uani 1 1 d . . . . .
H46 H 0.2100 0.6813 0.7475 0.040 Uiso 1 1 calc R U . . .
C47 C 0.1981(4) 0.5295(3) 0.6887(2) 0.0242(8) Uani 1 1 d . . . . .
C22 C 0.6138(4) 0.2426(3) 0.3525(3) 0.0390(10) Uani 1 1 d . . . . .
H22 H 0.6378 0.3137 0.3729 0.047 Uiso 1 1 calc R U . . .
C4 C 0.0386(4) 0.0393(3) 0.7937(2) 0.0383(10) Uani 1 1 d . . . . .
H4 H 0.0183 -0.0317 0.7755 0.046 Uiso 1 1 calc R U . . .
C9 C 0.4947(5) -0.0347(3) 0.9051(3) 0.0423(11) Uani 1 1 d . . . . .
H9 H 0.5680 -0.0613 0.9215 0.051 Uiso 1 1 calc R U . . .
C2 C -0.0306(4) 0.1932(4) 0.8038(3) 0.0449(11) Uani 1 1 d . . . . .
H2 H -0.0974 0.2282 0.7932 0.054 Uiso 1 1 calc R U . . .
C25 C 0.5391(4) 0.0339(4) 0.2941(3) 0.0406(11) Uani 1 1 d . . . . .
C15 C 0.7971(4) 0.2987(3) 0.9958(3) 0.0376(10) Uani 1 1 d . . . . .
H15 H 0.8051 0.3686 1.0098 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3621(5) -0.0958(3) 0.8712(3) 0.0442(12) Uani 1 1 d . . . . .
H8 H 0.3452 -0.1644 0.8642 0.053 Uiso 1 1 calc R U . . .
C33 C 1.2737(5) 0.0734(4) 0.4545(3) 0.0455(12) Uani 1 1 d . . . . .
H33 H 1.2633 0.0031 0.4386 0.055 Uiso 1 1 calc R U . . .
C36 C 1.2995(4) 0.2772(4) 0.5003(3) 0.0465(12) Uani 1 1 d . . . . .
H36 H 1.3086 0.3474 0.5165 0.056 Uiso 1 1 calc R U . . .
C30 C 0.9864(5) -0.0544(3) 0.3993(3) 0.0381(10) Uani 1 1 d . . . . .
H30 H 1.0573 -0.0837 0.4144 0.046 Uiso 1 1 calc R U . . .
C3 C -0.0620(4) 0.0883(4) 0.7756(3) 0.0462(12) Uani 1 1 d . . . . .
H3 H -0.1504 0.0508 0.7446 0.055 Uiso 1 1 calc R U . . .
C39 C 1.2922(4) 0.3812(3) 0.2694(2) 0.0352(10) Uani 1 1 d . . . . .
H39 H 1.3263 0.4419 0.3137 0.042 Uiso 1 1 calc R U . . .
C45 C 0.2856(5) 0.6150(3) 0.8228(2) 0.0336(10) Uani 1 1 d . . . . .
H45 H 0.3125 0.6709 0.8709 0.040 Uiso 1 1 calc R U . . .
C35 C 1.4182(5) 0.2412(4) 0.5091(3) 0.0505(13) Uani 1 1 d . . . . .
H35 H 1.5057 0.2859 0.5304 0.061 Uiso 1 1 calc R U . . .
C29 C 0.8537(5) -0.1125(3) 0.3632(3) 0.0433(11) Uani 1 1 d . . . . .
H29 H 0.8338 -0.1821 0.3532 0.052 Uiso 1 1 calc R U . . .
C14 C 0.9174(5) 0.2640(4) 1.0053(3) 0.0471(12) Uani 1 1 d . . . . .
H14 H 1.0041 0.3098 1.0251 0.057 Uiso 1 1 calc R U . . .
C23 C 0.4782(4) 0.1930(4) 0.3088(3) 0.0484(12) Uani 1 1 d . . . . .
H23 H 0.4130 0.2301 0.3000 0.058 Uiso 1 1 calc R U . . .
C12 C 0.7782(5) 0.0962(4) 0.9558(3) 0.0439(11) Uani 1 1 d . . . . .
H12 H 0.7693 0.0262 0.9414 0.053 Uiso 1 1 calc R U . . .
O1 O 0.8662(4) 0.2853(3) 0.5414(2) 0.0771(13) Uani 1 1 d . U . . .
O11 O 0.5956(3) 0.44363(19) 1.05046(14) 0.0277(6) Uani 1 1 d . . . . .
O9 O 1.1120(3) 0.41887(19) 0.55655(14) 0.0301(6) Uani 1 1 d . . . . .
O10 O 0.8763(3) 0.4156(2) 0.41283(16) 0.0323(6) Uani 1 1 d . . . . .
OW1 O 0.2853(3) 0.4043(2) 1.01262(17) 0.0357(7) Uani 1 1 d . . . . .
C34 C 1.4045(5) 0.1383(4) 0.4859(3) 0.0529(13) Uani 1 1 d . . . . .
H34 H 1.4832 0.1118 0.4911 0.064 Uiso 1 1 calc R U . . .
C24 C 0.4423(5) 0.0882(4) 0.2791(3) 0.0534(13) Uani 1 1 d . . . . .
H24 H 0.3526 0.0535 0.2486 0.064 Uiso 1 1 calc R U . . .
C18 C 0.8283(5) 0.3800(4) 0.7009(3) 0.0474(12) Uani 1 1 d . . . . .
H18 H 0.8951 0.4262 0.6933 0.057 Uiso 1 1 calc R U . . .
C13 C 0.9081(5) 0.1616(4) 0.9852(3) 0.0509(13) Uani 1 1 d . . . . .
H13 H 0.9880 0.1367 0.9914 0.061 Uiso 1 1 calc R U . . .
OW2 O 0.6337(7) 0.4586(4) 0.5222(4) 0.177(3) Uani 1 1 d . . . . .
Gd2 Gd 0.96358(2) 0.29145(2) 0.44126(2) 0.01721(5) Uani 1 1 d . . . . .
Gd1 Gd 0.45026(2) 0.30456(2) 0.94079(2) 0.01545(5) 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
S1 C17 1.706(4) . ?
S1 C20 1.723(4) . ?
S2 C38 1.716(4) . ?
S2 C41 1.719(4) 1_654 ?
O3 C21 1.257(4) . ?
O3 Gd1 2.488(3) . ?
O6 C37 1.276(4) . ?
O6 Gd2 2.479(3) . ?
O4 C21 1.265(4) . ?
O4 Gd1 2.500(3) . ?
O5 C37 1.249(4) . ?
O5 Gd2 2.480(3) . ?
O7 C42 1.282(4) . ?
O7 Gd1 2.354(3) . ?
O8 C42 1.227(4) . ?
C37 C38 1.474(5) . ?
C37 Gd2 2.835(4) . ?
S3 C44 1.707(4) . ?
S3 C47 1.721(4) . ?
N4 C22 1.340(5) . ?
N4 C26 1.352(5) . ?
N4 Gd2 2.569(3) . ?
N2 C10 1.336(4) . ?
N2 C6 1.353(5) . ?
N2 Gd1 2.576(3) . ?
N1 C1 1.340(5) . ?
N1 C5 1.353(5) . ?
N1 Gd1 2.562(3) . ?
N5 C27 1.344(5) . ?
N5 C31 1.344(4) . ?
N5 Gd2 2.586(3) . ?
N3 C11 1.345(5) . ?
N3 C15 1.351(5) . ?
N3 Gd1 2.565(3) . ?
N6 C36 1.342(5) . ?
N6 C32 1.345(5) . ?
N6 Gd2 2.541(3) . ?
C20 C19 1.362(5) . ?
C20 C21 1.476(5) . ?
C38 C39 1.368(5) . ?
C42 C41 1.498(5) . ?
C41 C40 1.370(5) . ?
C41 S2 1.719(4) 1_456 ?
C21 Gd1 2.848(4) . ?
C17 C18 1.354(6) . ?
C17 C16 1.514(6) . ?
O2 C16 1.247(5) . ?
C16 O1 1.233(5) . ?
C19 C18 1.407(6) . ?
C40 C39 1.403(5) 1_456 ?
O12 C43 1.252(4) . ?
O12 Gd1 2.418(2) . ?
C48 O9 1.251(4) . ?
C48 O10 1.260(4) 2_766 ?
C48 C47 1.464(5) 1_655 ?
C6 C7 1.395(5) . ?
C6 C5 1.473(5) . ?
C43 O11 1.252(4) 2_667 ?
C43 C44 1.497(5) . ?
C26 C25 1.402(5) . ?
C26 C27 1.481(5) . ?
C11 C12 1.404(5) . ?
C11 C10 1.480(5) . ?
C27 C28 1.395(5) . ?
C31 C30 1.392(5) . ?
C31 C32 1.483(5) . ?
C5 C4 1.391(5) . ?
C44 C45 1.356(5) . ?
C32 C33 1.391(5) . ?
C7 C8 1.363(6) . ?
C10 C9 1.395(5) . ?
C1 C2 1.366(6) . ?
C28 C29 1.380(6) . ?
C46 C47 1.373(5) . ?
C46 C45 1.385(5) . ?
C47 C48 1.464(5) 1_455 ?
C22 C23 1.389(6) . ?
C4 C3 1.373(6) . ?
C9 C8 1.376(6) . ?
C2 C3 1.373(7) . ?
C25 C24 1.384(7) . ?
C15 C14 1.379(6) . ?
C33 C34 1.379(7) . ?
C36 C35 1.374(6) . ?
C30 C29 1.368(6) . ?
C39 C40 1.403(5) 1_654 ?
C35 C34 1.362(7) . ?
C14 C13 1.367(7) . ?
C23 C24 1.371(7) . ?
C12 C13 1.375(7) . ?
O1 Gd2 2.259(3) . ?
O11 C43 1.252(4) 2_667 ?
O11 Gd1 2.346(3) . ?
O9 Gd2 2.341(3) . ?
O10 C48 1.260(4) 2_766 ?
O10 Gd2 2.277(3) . ?
OW1 Gd1 2.587(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
C17 S1 C20 91.2(2) . . ?
C38 S2 C41 91.85(18) . 1_654 ?
C21 O3 Gd1 93.1(2) . . ?
C37 O6 Gd2 92.4(2) . . ?
C21 O4 Gd1 92.4(2) . . ?
C37 O5 Gd2 93.0(2) . . ?
C42 O7 Gd1 141.9(2) . . ?
O5 C37 O6 121.7(3) . . ?
O5 C37 C38 119.4(3) . . ?
O6 C37 C38 118.8(3) . . ?
O5 C37 Gd2 60.88(19) . . ?
O6 C37 Gd2 60.88(18) . . ?
C38 C37 Gd2 177.9(3) . . ?
C44 S3 C47 91.95(17) . . ?
C22 N4 C26 117.5(3) . . ?
C22 N4 Gd2 120.8(3) . . ?
C26 N4 Gd2 121.7(2) . . ?
C10 N2 C6 118.9(3) . . ?
C10 N2 Gd1 120.0(2) . . ?
C6 N2 Gd1 120.2(2) . . ?
C1 N1 C5 117.7(3) . . ?
C1 N1 Gd1 120.9(3) . . ?
C5 N1 Gd1 121.3(2) . . ?
C27 N5 C31 119.1(3) . . ?
C27 N5 Gd2 120.8(2) . . ?
C31 N5 Gd2 119.7(2) . . ?
C11 N3 C15 117.4(3) . . ?
C11 N3 Gd1 120.9(2) . . ?
C15 N3 Gd1 121.5(3) . . ?
C36 N6 C32 118.4(3) . . ?
C36 N6 Gd2 119.7(3) . . ?
C32 N6 Gd2 121.5(3) . . ?
C19 C20 C21 129.0(4) . . ?
C19 C20 S1 111.6(3) . . ?
C21 C20 S1 119.5(3) . . ?
C39 C38 C37 127.5(4) . . ?
C39 C38 S2 111.3(3) . . ?
C37 C38 S2 121.1(3) . . ?
O8 C42 O7 127.0(3) . . ?
O8 C42 C41 118.1(3) . . ?
O7 C42 C41 114.9(3) . . ?
C40 C41 C42 130.0(3) . . ?
C40 C41 S2 111.1(3) . 1_456 ?
C42 C41 S2 118.9(3) . 1_456 ?
O3 C21 O4 121.9(3) . . ?
O3 C21 C20 119.7(3) . . ?
O4 C21 C20 118.4(3) . . ?
O3 C21 Gd1 60.72(18) . . ?
O4 C21 Gd1 61.29(18) . . ?
C20 C21 Gd1 177.7(3) . . ?
C18 C17 C16 129.9(4) . . ?
C18 C17 S1 112.0(3) . . ?
C16 C17 S1 118.1(3) . . ?
O1 C16 O2 126.7(4) . . ?
O1 C16 C17 115.2(4) . . ?
O2 C16 C17 118.0(4) . . ?
C20 C19 C18 112.2(4) . . ?
C41 C40 C39 112.8(4) . 1_456 ?
C43 O12 Gd1 131.4(2) . . ?
O9 C48 O10 124.1(3) . 2_766 ?
O9 C48 C47 118.0(3) . 1_655 ?
O10 C48 C47 117.9(3) 2_766 1_655 ?
N2 C6 C7 121.4(4) . . ?
N2 C6 C5 117.2(3) . . ?
C7 C6 C5 121.3(4) . . ?
O12 C43 O11 125.0(3) . 2_667 ?
O12 C43 C44 117.2(3) . . ?
O11 C43 C44 117.8(3) 2_667 . ?
N4 C26 C25 122.8(4) . . ?
N4 C26 C27 116.4(3) . . ?
C25 C26 C27 120.7(4) . . ?
N3 C11 C12 121.5(4) . . ?
N3 C11 C10 116.8(3) . . ?
C12 C11 C10 121.7(4) . . ?
N5 C27 C28 121.6(4) . . ?
N5 C27 C26 117.3(3) . . ?
C28 C27 C26 121.1(4) . . ?
N5 C31 C30 121.7(4) . . ?
N5 C31 C32 117.0(3) . . ?
C30 C31 C32 121.2(3) . . ?
N1 C5 C4 120.9(4) . . ?
N1 C5 C6 116.8(3) . . ?
C4 C5 C6 122.3(4) . . ?
C45 C44 C43 126.8(3) . . ?
C45 C44 S3 111.0(3) . . ?
C43 C44 S3 122.3(3) . . ?
N6 C32 C33 121.0(4) . . ?
N6 C32 C31 116.9(3) . . ?
C33 C32 C31 122.1(4) . . ?
C8 C7 C6 119.0(4) . . ?
N2 C10 C9 121.9(4) . . ?
N2 C10 C11 117.4(3) . . ?
C9 C10 C11 120.7(4) . . ?
N1 C1 C2 124.1(4) . . ?
C29 C28 C27 118.7(4) . . ?
C47 C46 C45 112.6(3) . . ?
C46 C47 C48 127.1(3) . 1_455 ?
C46 C47 S3 110.5(3) . . ?
C48 C47 S3 122.4(3) 1_455 . ?
N4 C22 C23 123.1(4) . . ?
C3 C4 C5 119.8(4) . . ?
C8 C9 C10 118.7(4) . . ?
C1 C2 C3 118.3(4) . . ?
C24 C25 C26 117.6(4) . . ?
N3 C15 C14 123.2(4) . . ?
C7 C8 C9 120.0(4) . . ?
C34 C33 C32 119.2(4) . . ?
N6 C36 C35 123.3(4) . . ?
C29 C30 C31 119.0(4) . . ?
C2 C3 C4 119.2(4) . . ?
C38 C39 C40 112.9(4) . 1_654 ?
C44 C45 C46 113.9(4) . . ?
C34 C35 C36 118.3(5) . . ?
C30 C29 C28 119.8(4) . . ?
C13 C14 C15 119.4(4) . . ?
C24 C23 C22 118.6(4) . . ?
C13 C12 C11 119.8(4) . . ?
C16 O1 Gd2 145.7(3) . . ?
C43 O11 Gd1 161.4(2) 2_667 . ?
C48 O9 Gd2 147.5(2) . . ?
C48 O10 Gd2 164.4(3) 2_766 . ?
C35 C34 C33 119.8(4) . . ?
C23 C24 C25 120.2(4) . . ?
C17 C18 C19 113.0(4) . . ?
C14 C13 C12 118.6(4) . . ?
O1 Gd2 O10 101.25(14) . . ?
O1 Gd2 O9 74.24(12) . . ?
O10 Gd2 O9 88.62(10) . . ?
O1 Gd2 O6 156.15(12) . . ?
O10 Gd2 O6 88.01(10) . . ?
O9 Gd2 O6 128.42(9) . . ?
O1 Gd2 O5 150.70(11) . . ?
O10 Gd2 O5 75.86(10) . . ?
O9 Gd2 O5 76.53(10) . . ?
O6 Gd2 O5 52.82(9) . . ?
O1 Gd2 N6 99.42(15) . . ?
O10 Gd2 N6 149.51(11) . . ?
O9 Gd2 N6 75.72(10) . . ?
O6 Gd2 N6 81.91(10) . . ?
O5 Gd2 N6 75.13(11) . . ?
O1 Gd2 N4 78.21(13) . . ?
O10 Gd2 N4 79.28(10) . . ?
O9 Gd2 N4 147.04(10) . . ?
O6 Gd2 N4 82.07(10) . . ?
O5 Gd2 N4 128.37(10) . . ?
N6 Gd2 N4 127.09(11) . . ?
O1 Gd2 N5 84.91(13) . . ?
O10 Gd2 N5 140.08(10) . . ?
O9 Gd2 N5 130.44(9) . . ?
O6 Gd2 N5 74.24(9) . . ?
O5 Gd2 N5 116.36(9) . . ?
N6 Gd2 N5 63.87(10) . . ?
N4 Gd2 N5 63.27(10) . . ?
O1 Gd2 C37 175.46(13) . . ?
O10 Gd2 C37 81.26(10) . . ?
O9 Gd2 C37 102.16(11) . . ?
O6 Gd2 C37 26.72(10) . . ?
O5 Gd2 C37 26.10(9) . . ?
N6 Gd2 C37 76.84(11) . . ?
N4 Gd2 C37 106.06(11) . . ?
N5 Gd2 C37 95.60(10) . . ?
O11 Gd1 O7 78.72(10) . . ?
O11 Gd1 O12 99.53(9) . . ?
O7 Gd1 O12 136.45(9) . . ?
O11 Gd1 O3 123.38(9) . . ?
O7 Gd1 O3 143.05(9) . . ?
O12 Gd1 O3 73.69(9) . . ?
O11 Gd1 O4 72.16(9) . . ?
O7 Gd1 O4 144.59(9) . . ?
O12 Gd1 O4 69.48(10) . . ?
O3 Gd1 O4 52.48(8) . . ?
O11 Gd1 N1 148.09(10) . . ?
O7 Gd1 N1 85.01(10) . . ?
O12 Gd1 N1 73.97(10) . . ?
O3 Gd1 N1 85.48(10) . . ?
O4 Gd1 N1 130.04(10) . . ?
O11 Gd1 N3 78.14(10) . . ?
O7 Gd1 N3 83.24(10) . . ?
O12 Gd1 N3 139.60(10) . . ?
O3 Gd1 N3 74.49(9) . . ?
O4 Gd1 N3 71.56(10) . . ?
N1 Gd1 N3 127.17(10) . . ?
O11 Gd1 N2 134.25(9) . . ?
O7 Gd1 N2 72.96(9) . . ?
O12 Gd1 N2 125.73(9) . . ?
O3 Gd1 N2 70.82(9) . . ?
O4 Gd1 N2 114.61(9) . . ?
N1 Gd1 N2 63.65(9) . . ?
N3 Gd1 N2 63.64(10) . . ?
O11 Gd1 OW1 74.11(10) . . ?
O7 Gd1 OW1 66.15(9) . . ?
O12 Gd1 OW1 71.52(9) . . ?
O3 Gd1 OW1 143.34(9) . . ?
O4 Gd1 OW1 122.12(9) . . ?
N1 Gd1 OW1 74.23(10) . . ?
N3 Gd1 OW1 141.85(10) . . ?
N2 Gd1 OW1 122.71(9) . . ?
O11 Gd1 C21 98.07(11) . . ?
O7 Gd1 C21 154.88(10) . . ?
O12 Gd1 C21 68.65(10) . . ?
O3 Gd1 C21 26.15(9) . . ?
O4 Gd1 C21 26.35(9) . . ?
N1 Gd1 C21 107.87(11) . . ?
N3 Gd1 C21 71.76(10) . . ?
N2 Gd1 C21 93.12(10) . . ?
OW1 Gd1 C21 137.41(10) . . ?

_refine_diff_density_max         1.416
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.115

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 1410407'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 N6 O14 S3 Tb2'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1330.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0115(8)
_cell_length_b                   14.3215(11)
_cell_length_c                   18.4709(15)
_cell_angle_alpha                110.097(10)
_cell_angle_beta                 99.868(11)
_cell_angle_gamma                99.041(10)
_cell_volume                     2382.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    35563
_cell_measurement_theta_min      4.643
_cell_measurement_theta_max      60.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    3.151
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6101
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35551
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.210
_diffrn_reflns_theta_max         30.511
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13171
_reflns_number_gt                10717
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+2.5157P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13171
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0771
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.9915(3) 0.26410(18) 0.18923(14) 0.0255(5) Uani 1 1 d . . . . .
O4 O 0.8641(3) 0.11295(19) 0.10673(15) 0.0286(6) Uani 1 1 d . . . . .
O12 O 1.1432(3) 0.10395(19) 0.13561(16) 0.0308(6) Uani 1 1 d . . . . .
O9 O 0.6099(3) -0.08094(19) -0.44433(15) 0.0302(6) Uani 1 1 d . . . . .
O10 O 0.6241(3) 0.0846(2) -0.41380(16) 0.0338(6) Uani 1 1 d . . . . .
OW1 O 1.2143(3) 0.0961(2) -0.01202(18) 0.0383(7) Uani 1 1 d . . . . .
C43 C 0.6385(3) 0.0087(3) -0.3957(2) 0.0192(7) Uani 1 1 d . . . . .
C21 C 0.8962(4) 0.1857(3) 0.1733(2) 0.0220(7) Uani 1 1 d . . . . .
C19 C 0.7207(5) 0.0997(3) 0.2306(3) 0.0391(10) Uani 1 1 d . . . . .
H19 H 0.6889 0.0379 0.1872 0.047 Uiso 1 1 calc R U . . .
C18 C 0.6721(5) 0.1219(4) 0.3005(3) 0.0432(11) Uani 1 1 d . . . . .
H18 H 0.6056 0.0758 0.3085 0.052 Uiso 1 1 calc R U . . .
OW2 O 0.8637(8) 0.0423(5) 0.4778(4) 0.193(4) Uani 1 1 d . . . . .
C8 C 1.1386(5) 0.5954(3) 0.1295(3) 0.0455(12) Uani 1 1 d . . . . .
H8 H 1.1555 0.6641 0.1367 0.055 Uiso 1 1 calc R U . . .
C9 C 1.0066(5) 0.5347(3) 0.0956(3) 0.0420(11) Uani 1 1 d . . . . .
H9 H 0.9337 0.5616 0.0792 0.050 Uiso 1 1 calc R U . . .
C23 C 2.0221(5) 0.3055(4) -0.3096(3) 0.0492(12) Uani 1 1 d . . . . .
H23 H 2.0876 0.2685 -0.3013 0.059 Uiso 1 1 calc R U . . .
C25 C 1.9602(4) 0.4636(3) -0.2951(3) 0.0391(10) Uani 1 1 d . . . . .
H25 H 1.9837 0.5346 -0.2762 0.047 Uiso 1 1 calc R U . . .
C24 C 2.0573(5) 0.4101(4) -0.2799(3) 0.0508(13) Uani 1 1 d . . . . .
H24 H 2.1469 0.4452 -0.2495 0.061 Uiso 1 1 calc R U . . .
Tb1 Tb 1.04952(2) 0.19602(2) 0.05944(2) 0.01553(5) Uani 1 1 d . . . . .
Tb2 Tb 1.53614(2) 0.20836(2) -0.44069(2) 0.01645(5) Uani 1 1 d . . . . .
C29 C 1.6452(5) 0.6112(3) -0.3645(3) 0.0422(11) Uani 1 1 d . . . . .
H29 H 1.6651 0.6805 -0.3554 0.051 Uiso 1 1 calc R U . . .
S1 S 0.85212(10) 0.28260(7) 0.32221(5) 0.02665(19) Uani 1 1 d . . . . .
S2 S 1.35154(10) 0.29538(7) -0.17378(5) 0.02639(19) Uani 1 1 d . . . . .
S3 S 0.74165(11) -0.06419(7) -0.28041(5) 0.0281(2) Uani 1 1 d . . . . .
O11 O 0.9057(3) 0.05788(19) -0.04978(14) 0.0281(6) Uani 1 1 d . . . . .
N5 N 1.5874(3) 0.4035(2) -0.39511(17) 0.0218(6) Uani 1 1 d . . . . .
N2 N 1.0879(3) 0.3907(2) 0.10559(17) 0.0204(6) Uani 1 1 d . . . . .
O7 O 1.0995(3) 0.2390(2) -0.04574(15) 0.0320(6) Uani 1 1 d . . . . .
N4 N 1.7872(3) 0.3058(2) -0.36640(18) 0.0257(6) Uani 1 1 d . . . . .
C42 C 1.1960(4) 0.2899(3) -0.0643(2) 0.0236(7) Uani 1 1 d . . . . .
N3 N 0.8319(3) 0.2634(2) 0.03250(18) 0.0257(6) Uani 1 1 d . . . . .
N1 N 1.2965(3) 0.2999(2) 0.13442(18) 0.0259(6) Uani 1 1 d . . . . .
N6 N 1.3292(3) 0.2818(2) -0.4699(2) 0.0302(7) Uani 1 1 d . . . . .
C16 C 0.7093(4) 0.2715(3) 0.4357(2) 0.0321(9) Uani 1 1 d . . . . .
O8 O 1.2678(3) 0.3763(2) -0.02386(16) 0.0330(6) Uani 1 1 d . . . . .
O2 O 0.7664(3) 0.3625(2) 0.47208(18) 0.0420(7) Uani 1 1 d . . . . .
C20 C 0.8205(4) 0.1798(3) 0.2340(2) 0.0245(7) Uani 1 1 d . . . . .
C41 C 1.2204(4) 0.2361(3) -0.1443(2) 0.0254(8) Uani 1 1 d . . . . .
C48 C 0.8597(3) -0.0112(2) -0.11789(19) 0.0174(6) Uani 1 1 d . . . . .
C38 C 1.3164(4) 0.1940(3) -0.2632(2) 0.0256(8) Uani 1 1 d . . . . .
C17 C 0.7331(4) 0.2183(3) 0.3552(2) 0.0301(8) Uani 1 1 d . . . . .
C28 C 1.7498(5) 0.5665(3) -0.3421(3) 0.0370(10) Uani 1 1 d . . . . .
H28 H 1.8397 0.6057 -0.3159 0.044 Uiso 1 1 calc R U . . .
C37 C 1.3952(4) 0.1976(3) -0.3230(2) 0.0245(7) Uani 1 1 d . . . . .
C5 C 1.3291(4) 0.4027(3) 0.1603(2) 0.0227(7) Uani 1 1 d . . . . .
C47 C 0.8000(4) 0.0199(3) -0.18363(19) 0.0220(7) Uani 1 1 d . . . . .
C31 C 1.4856(4) 0.4489(3) -0.4131(2) 0.0265(8) Uani 1 1 d . . . . .
C32 C 1.3423(4) 0.3841(3) -0.4471(2) 0.0279(8) Uani 1 1 d . . . . .
C40 C 1.1538(5) 0.1418(3) -0.2011(2) 0.0345(9) Uani 1 1 d . . . . .
H40 H 1.0804 0.0983 -0.1955 0.041 Uiso 1 1 calc R U . . .
C44 C 0.6976(4) 0.0294(3) -0.3118(2) 0.0244(7) Uani 1 1 d . . . . .
C27 C 1.7178(4) 0.4617(3) -0.3597(2) 0.0247(7) Uani 1 1 d . . . . .
C6 C 1.2170(4) 0.4516(3) 0.1394(2) 0.0240(7) Uani 1 1 d . . . . .
C26 C 1.8258(4) 0.4089(3) -0.3395(2) 0.0259(8) Uani 1 1 d . . . . .
C45 C 0.7266(5) 0.1213(3) -0.2487(2) 0.0356(10) Uani 1 1 d . . . . .
H45 H 0.7095 0.1814 -0.2529 0.043 Uiso 1 1 calc R U . . .
C11 C 0.8407(4) 0.3643(3) 0.0524(2) 0.0275(8) Uani 1 1 d . . . . .
C46 C 0.7843(5) 0.1137(3) -0.1781(2) 0.0362(10) Uani 1 1 d . . . . .
H46 H 0.8106 0.1695 -0.1299 0.043 Uiso 1 1 calc R U . . .
C1 C 1.3964(4) 0.2534(3) 0.1518(3) 0.0361(9) Uani 1 1 d . . . . .
H1 H 1.3746 0.1824 0.1333 0.043 Uiso 1 1 calc R U . . .
C36 C 1.2003(4) 0.2205(3) -0.5008(3) 0.0433(11) Uani 1 1 d . . . . .
H36 H 1.1912 0.1503 -0.5173 0.052 Uiso 1 1 calc R U . . .
O1 O 1.6316(4) 0.2163(3) -0.54062(19) 0.0645(11) Uani 1 1 d . . . . .
C30 C 1.5131(5) 0.5529(3) -0.3999(3) 0.0379(10) Uani 1 1 d . . . . .
H30 H 1.4420 0.5821 -0.4151 0.046 Uiso 1 1 calc R U . . .
C12 C 0.7225(5) 0.4029(4) 0.0436(3) 0.0437(11) Uani 1 1 d . . . . .
H12 H 0.7314 0.4729 0.0574 0.052 Uiso 1 1 calc R U . . .
C10 C 0.9831(4) 0.4319(3) 0.0858(2) 0.0257(8) Uani 1 1 d . . . . .
C15 C 0.7042(4) 0.2007(3) 0.0041(3) 0.0366(9) Uani 1 1 d . . . . .
H15 H 0.6971 0.1309 -0.0098 0.044 Uiso 1 1 calc R U . . .
C22 C 1.8857(4) 0.2561(3) -0.3523(3) 0.0381(10) Uani 1 1 d . . . . .
H22 H 1.8613 0.1850 -0.3722 0.046 Uiso 1 1 calc R U . . .
C33 C 1.2257(5) 0.4238(3) -0.4551(3) 0.0423(11) Uani 1 1 d . . . . .
H33 H 1.2357 0.4941 -0.4393 0.051 Uiso 1 1 calc R U . . .
C4 C 1.4617(4) 0.4599(3) 0.2059(2) 0.0368(10) Uani 1 1 d . . . . .
H4 H 1.4823 0.5309 0.2241 0.044 Uiso 1 1 calc R U . . .
C7 C 1.2444(5) 0.5557(3) 0.1528(3) 0.0369(10) Uani 1 1 d . . . . .
H7 H 1.3337 0.5969 0.1772 0.044 Uiso 1 1 calc R U . . .
C39 C 1.2086(4) 0.1178(3) -0.2689(2) 0.0350(9) Uani 1 1 d . . . . .
H39 H 1.1751 0.0567 -0.3129 0.042 Uiso 1 1 calc R U . . .
O5 O 1.3556(3) 0.1275(2) -0.39148(15) 0.0339(6) Uani 1 1 d . . . . .
C3 C 1.5619(5) 0.4098(4) 0.2235(3) 0.0462(12) Uani 1 1 d . . . . .
H3 H 1.6508 0.4468 0.2540 0.055 Uiso 1 1 calc R U . . .
C34 C 1.0946(5) 0.3593(4) -0.4865(3) 0.0513(13) Uani 1 1 d . . . . .
H34 H 1.0160 0.3857 -0.4922 0.062 Uiso 1 1 calc R U . . .
C2 C 1.5296(4) 0.3054(4) 0.1958(3) 0.0452(11) Uani 1 1 d . . . . .
H2 H 1.5962 0.2703 0.2065 0.054 Uiso 1 1 calc R U . . .
C14 C 0.5826(5) 0.2344(4) -0.0057(3) 0.0484(12) Uani 1 1 d . . . . .
H14 H 0.4960 0.1884 -0.0256 0.058 Uiso 1 1 calc R U . . .
C35 C 1.0817(5) 0.2564(4) -0.5092(3) 0.0484(12) Uani 1 1 d . . . . .
H35 H 0.9943 0.2115 -0.5300 0.058 Uiso 1 1 calc R U . . .
O6 O 1.4987(3) 0.27104(19) -0.30575(14) 0.0277(6) Uani 1 1 d . . . . .
C13 C 0.5930(5) 0.3376(4) 0.0147(3) 0.0501(13) Uani 1 1 d . . . . .
H13 H 0.5133 0.3627 0.0088 0.060 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C21 1.264(4) . ?
O3 Tb1 2.467(2) . ?
O4 C21 1.257(4) . ?
O4 Tb1 2.490(2) . ?
O12 C48 1.248(4) 2_755 ?
O12 Tb1 2.410(2) . ?
O9 C43 1.242(4) . ?
O9 Tb2 2.326(2) 2_754 ?
O10 C43 1.264(4) . ?
O10 Tb2 2.260(3) 1_455 ?
OW1 Tb1 2.589(3) . ?
C43 C44 1.468(5) . ?
C21 C20 1.474(5) . ?
C21 Tb1 2.837(3) . ?
C19 C20 1.374(5) . ?
C19 C18 1.409(5) . ?
C19 H19 0.9300 . ?
C18 C17 1.365(6) . ?
C18 H18 0.9300 . ?
C8 C7 1.354(6) . ?
C8 C9 1.369(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.396(5) . ?
C9 H9 0.9300 . ?
C23 C24 1.368(7) . ?
C23 C22 1.390(6) . ?
C23 H23 0.9300 . ?
C25 C24 1.378(7) . ?
C25 C26 1.394(5) . ?
C25 H25 0.9300 . ?
C24 H24 0.9300 . ?
Tb1 O11 2.329(2) . ?
Tb1 O7 2.337(2) . ?
Tb1 N1 2.549(3) . ?
Tb1 N3 2.558(3) . ?
Tb1 N2 2.562(3) . ?
Tb2 O1 2.247(3) . ?
Tb2 O10 2.260(3) 1_655 ?
Tb2 O9 2.326(3) 2_754 ?
Tb2 O6 2.459(2) . ?
Tb2 O5 2.462(3) . ?
Tb2 N6 2.526(3) . ?
Tb2 N4 2.559(3) . ?
Tb2 N5 2.563(3) . ?
Tb2 C37 2.820(3) . ?
C29 C30 1.362(6) . ?
C29 C28 1.387(6) . ?
C29 H29 0.9300 . ?
S1 C17 1.711(4) . ?
S1 C20 1.718(4) . ?
S2 C41 1.718(4) . ?
S2 C38 1.718(4) . ?
S3 C47 1.711(3) . ?
S3 C44 1.720(3) . ?
O11 C48 1.256(4) . ?
N5 C31 1.346(5) . ?
N5 C27 1.348(5) . ?
N2 C10 1.340(4) . ?
N2 C6 1.348(4) . ?
O7 C42 1.282(4) . ?
N4 C22 1.343(5) . ?
N4 C26 1.352(5) . ?
C42 O8 1.228(4) . ?
C42 C41 1.497(5) . ?
N3 C15 1.342(5) . ?
N3 C11 1.346(5) . ?
N1 C1 1.339(5) . ?
N1 C5 1.346(4) . ?
N6 C36 1.345(5) . ?
N6 C32 1.355(5) . ?
C16 O2 1.229(5) . ?
C16 O1 1.258(5) 1_456 ?
C16 C17 1.499(5) . ?
C41 C40 1.368(5) . ?
C48 O12 1.248(4) 2_755 ?
C48 C47 1.496(4) . ?
C38 C39 1.371(5) . ?
C38 C37 1.474(5) . ?
C28 C27 1.392(5) . ?
C28 H28 0.9300 . ?
C37 O6 1.263(4) . ?
C37 O5 1.263(4) . ?
C5 C4 1.394(5) . ?
C5 C6 1.478(5) . ?
C47 C46 1.348(5) . ?
C31 C30 1.398(5) . ?
C31 C32 1.479(5) . ?
C32 C33 1.384(5) . ?
C40 C39 1.410(5) . ?
C40 H40 0.9300 . ?
C44 C45 1.374(5) . ?
C27 C26 1.481(5) . ?
C6 C7 1.398(5) . ?
C45 C46 1.380(5) . ?
C45 H45 0.9300 . ?
C11 C12 1.391(5) . ?
C11 C10 1.485(5) . ?
C46 H46 0.9300 . ?
C1 C2 1.377(6) . ?
C1 H1 0.9300 . ?
C36 C35 1.371(6) . ?
C36 H36 0.9300 . ?
O1 C16 1.257(5) 1_654 ?
C30 H30 0.9300 . ?
C12 C13 1.371(7) . ?
C12 H12 0.9300 . ?
C15 C14 1.385(6) . ?
C15 H15 0.9300 . ?
C22 H22 0.9300 . ?
C33 C34 1.379(7) . ?
C33 H33 0.9300 . ?
C4 C3 1.378(6) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C39 H39 0.9300 . ?
C3 C2 1.367(7) . ?
C3 H3 0.9300 . ?
C34 C35 1.365(7) . ?
C34 H34 0.9300 . ?
C2 H2 0.9300 . ?
C14 C13 1.376(7) . ?
C14 H14 0.9300 . ?
C35 H35 0.9300 . ?
C13 H13 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 O3 Tb1 93.4(2) . . ?
C21 O4 Tb1 92.4(2) . . ?
C48 O12 Tb1 131.8(2) 2_755 . ?
C43 O9 Tb2 148.5(2) . 2_754 ?
C43 O10 Tb2 163.4(3) . 1_455 ?
O9 C43 O10 124.3(3) . . ?
O9 C43 C44 118.4(3) . . ?
O10 C43 C44 117.2(3) . . ?
O4 C21 O3 121.5(3) . . ?
O4 C21 C20 119.3(3) . . ?
O3 C21 C20 119.2(3) . . ?
O4 C21 Tb1 61.29(18) . . ?
O3 C21 Tb1 60.24(17) . . ?
C20 C21 Tb1 178.2(3) . . ?
C20 C19 C18 112.3(4) . . ?
C20 C19 H19 123.8 . . ?
C18 C19 H19 123.8 . . ?
C17 C18 C19 112.9(4) . . ?
C17 C18 H18 123.6 . . ?
C19 C18 H18 123.6 . . ?
C7 C8 C9 120.1(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C9 C10 119.1(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C24 C23 C22 118.2(4) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
C24 C25 C26 118.6(4) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
C23 C24 C25 120.1(4) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
O11 Tb1 O7 78.60(9) . . ?
O11 Tb1 O12 98.95(9) . . ?
O7 Tb1 O12 135.95(10) . . ?
O11 Tb1 O3 123.77(9) . . ?
O7 Tb1 O3 143.32(9) . . ?
O12 Tb1 O3 73.92(9) . . ?
O11 Tb1 O4 72.33(9) . . ?
O7 Tb1 O4 144.83(9) . . ?
O12 Tb1 O4 69.27(9) . . ?
O3 Tb1 O4 52.66(8) . . ?
O11 Tb1 N1 147.78(10) . . ?
O7 Tb1 N1 85.08(10) . . ?
O12 Tb1 N1 74.05(9) . . ?
O3 Tb1 N1 85.22(9) . . ?
O4 Tb1 N1 129.80(9) . . ?
O11 Tb1 N3 78.12(9) . . ?
O7 Tb1 N3 83.54(10) . . ?
O12 Tb1 N3 139.62(10) . . ?
O3 Tb1 N3 74.81(9) . . ?
O4 Tb1 N3 71.60(10) . . ?
N1 Tb1 N3 127.63(10) . . ?
O11 Tb1 N2 134.52(9) . . ?
O7 Tb1 N2 73.19(9) . . ?
O12 Tb1 N2 126.10(9) . . ?
O3 Tb1 N2 70.79(8) . . ?
O4 Tb1 N2 114.79(9) . . ?
N1 Tb1 N2 63.73(9) . . ?
N3 Tb1 N2 64.03(10) . . ?
O11 Tb1 OW1 73.97(9) . . ?
O7 Tb1 OW1 66.15(9) . . ?
O12 Tb1 OW1 70.92(9) . . ?
O3 Tb1 OW1 142.84(9) . . ?
O4 Tb1 OW1 121.81(9) . . ?
N1 Tb1 OW1 74.04(9) . . ?
N3 Tb1 OW1 141.99(10) . . ?
N2 Tb1 OW1 122.75(9) . . ?
O11 Tb1 C21 98.15(10) . . ?
O7 Tb1 C21 155.20(10) . . ?
O12 Tb1 C21 68.79(10) . . ?
O3 Tb1 C21 26.40(9) . . ?
O4 Tb1 C21 26.27(9) . . ?
N1 Tb1 C21 107.85(10) . . ?
N3 Tb1 C21 71.79(10) . . ?
N2 Tb1 C21 93.26(9) . . ?
OW1 Tb1 C21 137.06(9) . . ?
O1 Tb2 O10 101.05(13) . 1_655 ?
O1 Tb2 O9 74.17(11) . 2_754 ?
O10 Tb2 O9 87.81(9) 1_655 2_754 ?
O1 Tb2 O6 155.80(11) . . ?
O10 Tb2 O6 88.88(10) 1_655 . ?
O9 Tb2 O6 128.73(9) 2_754 . ?
O1 Tb2 O5 150.64(11) . . ?
O10 Tb2 O5 76.08(10) 1_655 . ?
O9 Tb2 O5 76.52(9) 2_754 . ?
O6 Tb2 O5 53.14(8) . . ?
O1 Tb2 N6 98.76(14) . . ?
O10 Tb2 N6 149.69(11) 1_655 . ?
O9 Tb2 N6 75.80(10) 2_754 . ?
O6 Tb2 N6 82.17(10) . . ?
O5 Tb2 N6 75.39(11) . . ?
O1 Tb2 N4 78.19(12) . . ?
O10 Tb2 N4 78.98(10) 1_655 . ?
O9 Tb2 N4 146.37(10) 2_754 . ?
O6 Tb2 N4 82.20(9) . . ?
O5 Tb2 N4 128.40(10) . . ?
N6 Tb2 N4 127.77(10) . . ?
O1 Tb2 N5 84.11(12) . . ?
O10 Tb2 N5 140.39(10) 1_655 . ?
O9 Tb2 N5 130.65(9) 2_754 . ?
O6 Tb2 N5 74.46(9) . . ?
O5 Tb2 N5 117.05(9) . . ?
N6 Tb2 N5 64.29(10) . . ?
N4 Tb2 N5 63.53(10) . . ?
O1 Tb2 C37 175.33(13) . . ?
O10 Tb2 C37 82.05(11) 1_655 . ?
O9 Tb2 C37 102.60(10) 2_754 . ?
O6 Tb2 C37 26.57(9) . . ?
O5 Tb2 C37 26.58(9) . . ?
N6 Tb2 C37 77.04(11) . . ?
N4 Tb2 C37 105.94(10) . . ?
N5 Tb2 C37 95.74(10) . . ?
C30 C29 C28 119.5(4) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C17 S1 C20 91.74(18) . . ?
C41 S2 C38 91.94(18) . . ?
C47 S3 C44 92.13(17) . . ?
C48 O11 Tb1 162.0(2) . . ?
C31 N5 C27 118.6(3) . . ?
C31 N5 Tb2 119.8(2) . . ?
C27 N5 Tb2 121.3(2) . . ?
C10 N2 C6 118.8(3) . . ?
C10 N2 Tb1 119.9(2) . . ?
C6 N2 Tb1 120.6(2) . . ?
C42 O7 Tb1 141.8(2) . . ?
C22 N4 C26 117.5(3) . . ?
C22 N4 Tb2 121.1(3) . . ?
C26 N4 Tb2 121.5(2) . . ?
O8 C42 O7 127.0(3) . . ?
O8 C42 C41 118.0(3) . . ?
O7 C42 C41 115.0(3) . . ?
C15 N3 C11 117.6(3) . . ?
C15 N3 Tb1 121.2(3) . . ?
C11 N3 Tb1 120.9(2) . . ?
C1 N1 C5 118.1(3) . . ?
C1 N1 Tb1 120.5(2) . . ?
C5 N1 Tb1 121.4(2) . . ?
C36 N6 C32 118.1(3) . . ?
C36 N6 Tb2 120.1(3) . . ?
C32 N6 Tb2 121.3(2) . . ?
O2 C16 O1 126.4(4) . 1_456 ?
O2 C16 C17 118.4(4) . . ?
O1 C16 C17 115.2(4) 1_456 . ?
C19 C20 C21 128.4(3) . . ?
C19 C20 S1 111.4(3) . . ?
C21 C20 S1 120.2(3) . . ?
C40 C41 C42 129.7(3) . . ?
C40 C41 S2 111.4(3) . . ?
C42 C41 S2 118.9(3) . . ?
O12 C48 O11 126.0(3) 2_755 . ?
O12 C48 C47 116.9(3) 2_755 . ?
O11 C48 C47 117.1(3) . . ?
C39 C38 C37 128.2(3) . . ?
C39 C38 S2 111.1(3) . . ?
C37 C38 S2 120.6(3) . . ?
C18 C17 C16 129.5(4) . . ?
C18 C17 S1 111.7(3) . . ?
C16 C17 S1 118.8(3) . . ?
C29 C28 C27 118.8(4) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
O6 C37 O5 121.3(3) . . ?
O6 C37 C38 119.9(3) . . ?
O5 C37 C38 118.8(3) . . ?
O6 C37 Tb2 60.58(18) . . ?
O5 C37 Tb2 60.73(18) . . ?
C38 C37 Tb2 177.2(3) . . ?
N1 C5 C4 121.3(4) . . ?
N1 C5 C6 116.8(3) . . ?
C4 C5 C6 121.9(3) . . ?
C46 C47 C48 127.5(3) . . ?
C46 C47 S3 109.9(3) . . ?
C48 C47 S3 122.6(3) . . ?
N5 C31 C30 121.8(4) . . ?
N5 C31 C32 117.2(3) . . ?
C30 C31 C32 121.0(4) . . ?
N6 C32 C33 120.6(4) . . ?
N6 C32 C31 116.5(3) . . ?
C33 C32 C31 122.9(4) . . ?
C41 C40 C39 112.6(4) . . ?
C41 C40 H40 123.7 . . ?
C39 C40 H40 123.7 . . ?
C45 C44 C43 127.1(3) . . ?
C45 C44 S3 110.6(3) . . ?
C43 C44 S3 122.2(3) . . ?
N5 C27 C28 121.9(4) . . ?
N5 C27 C26 116.8(3) . . ?
C28 C27 C26 121.3(4) . . ?
N2 C6 C7 121.7(4) . . ?
N2 C6 C5 116.8(3) . . ?
C7 C6 C5 121.5(3) . . ?
N4 C26 C25 122.2(4) . . ?
N4 C26 C27 116.6(3) . . ?
C25 C26 C27 121.2(4) . . ?
C44 C45 C46 111.8(3) . . ?
C44 C45 H45 124.1 . . ?
C46 C45 H45 124.1 . . ?
N3 C11 C12 121.7(4) . . ?
N3 C11 C10 116.3(3) . . ?
C12 C11 C10 121.9(4) . . ?
C47 C46 C45 115.5(4) . . ?
C47 C46 H46 122.2 . . ?
C45 C46 H46 122.2 . . ?
N1 C1 C2 123.4(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
N6 C36 C35 123.4(4) . . ?
N6 C36 H36 118.3 . . ?
C35 C36 H36 118.3 . . ?
C16 O1 Tb2 146.1(3) 1_654 . ?
C29 C30 C31 119.2(4) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
C13 C12 C11 119.8(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
N2 C10 C9 121.3(4) . . ?
N2 C10 C11 117.7(3) . . ?
C9 C10 C11 121.0(4) . . ?
N3 C15 C14 123.5(4) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
N4 C22 C23 123.4(4) . . ?
N4 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C34 C33 C32 120.1(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C38 C39 C40 113.0(4) . . ?
C38 C39 H39 123.5 . . ?
C40 C39 H39 123.5 . . ?
C37 O5 Tb2 92.7(2) . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C35 C34 C33 119.2(4) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C3 C2 C1 118.5(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C13 C14 C15 118.3(4) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C34 C35 C36 118.6(4) . . ?
C34 C35 H35 120.7 . . ?
C36 C35 H35 120.7 . . ?
C37 O6 Tb2 92.8(2) . . ?
C12 C13 C14 119.1(4) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?

_refine_diff_density_max         2.749
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.133

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 1410408'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Dy2 N6 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1337.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.007(5)
_cell_length_b                   14.298(6)
_cell_length_c                   18.414(6)
_cell_angle_alpha                109.983(5)
_cell_angle_beta                 99.963(4)
_cell_angle_gamma                99.123(4)
_cell_volume                     2370.3(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    76363
_cell_measurement_theta_min      4.349
_cell_measurement_theta_max      55.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.336
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6295
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'TWINABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23450
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.214
_diffrn_reflns_theta_max         27.759
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             11073
_reflns_number_gt                8725
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0247P)²+2.2588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11073
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0706
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy2 Dy 0.46477(2) 0.79166(2) 0.44024(2) 0.01421(5) Uani 1 1 d . . . . .
Dy1 Dy 0.95066(2) 0.80405(2) 0.94028(2) 0.01357(5) Uani 1 1 d . . . . .
S1 S 0.14733(11) 0.71692(8) 0.67750(6) 0.0234(2) Uani 1 1 d . . . . .
S2 S 0.64877(11) 0.70455(8) 0.17350(6) 0.0240(2) Uani 1 1 d . . . . .
S3 S 0.74184(12) 0.93576(8) 0.71944(6) 0.0252(2) Uani 1 1 d . . . . .
O3 O 1.0075(3) 0.7362(2) 0.81076(16) 0.0230(6) Uani 1 1 d . . . . .
O6 O 0.5001(3) 0.7292(2) 0.30550(16) 0.0257(6) Uani 1 1 d . . . . .
O7 O 0.9011(3) 0.7604(2) 0.04504(17) 0.0280(7) Uani 1 1 d . . . . .
O4 O 1.1356(3) 0.8878(2) 0.89329(16) 0.0258(6) Uani 1 1 d . . . . .
N5 N 0.4136(3) 0.5972(2) 0.39537(18) 0.0182(7) Uani 1 1 d . . . . .
N4 N 0.2135(3) 0.6950(3) 0.3661(2) 0.0236(7) Uani 1 1 d . . . . .
N2 N 0.9126(3) 0.6101(2) 0.89432(18) 0.0179(7) Uani 1 1 d . . . . .
O5 O 0.6435(3) 0.8734(2) 0.39086(17) 0.0321(7) Uani 1 1 d . . . . .
N1 N 0.7044(3) 0.7007(3) 0.86563(19) 0.0230(7) Uani 1 1 d . . . . .
O8 O 0.7333(3) 0.6233(2) 0.02368(17) 0.0310(7) Uani 1 1 d . . . . .
O2 O 0.2340(3) 0.6373(2) 0.52741(18) 0.0361(8) Uani 1 1 d . . . . .
N6 N 0.6715(4) 0.7188(3) 0.4699(2) 0.0281(8) Uani 1 1 d . . . . .
O1 O 0.3688(4) 0.7844(3) 0.53997(19) 0.0521(10) Uani 1 1 d . . . . .
N3 N 1.1686(4) 0.7385(3) 0.9673(2) 0.0249(8) Uani 1 1 d . . . . .
O11 O 0.9056(3) 1.0576(2) 0.95078(15) 0.0241(6) Uani 1 1 d . . . . .
O9 O 0.6104(3) 0.9185(2) 0.55483(16) 0.0260(6) Uani 1 1 d . . . . .
O10 O 0.3768(3) 0.9154(2) 0.41495(17) 0.0291(7) Uani 1 1 d . . . . .
C43 C 0.6379(4) 1.0087(3) 0.6034(2) 0.0182(8) Uani 1 1 d . . . . .
C37 C 0.6046(4) 0.8033(3) 0.3231(2) 0.0210(8) Uani 1 1 d . . . . .
C21 C 0.1027(4) 0.8144(3) 0.8263(2) 0.0203(8) Uani 1 1 d . . . . .
C48 C 0.8604(4) 0.9894(3) 0.8826(2) 0.0159(8) Uani 1 1 d . . . . .
C6 C 0.7838(4) 0.5493(3) 0.8613(2) 0.0221(9) Uani 1 1 d . . . . .
C5 C 0.6710(4) 0.5984(3) 0.8401(2) 0.0220(8) Uani 1 1 d . . . . .
C27 C 0.2834(4) 0.5395(3) 0.3595(2) 0.0222(9) Uani 1 1 d . . . . .
C20 C 0.1788(4) 0.8203(3) 0.7655(2) 0.0215(8) Uani 1 1 d . . . . .
C26 C 0.1747(4) 0.5919(3) 0.3395(2) 0.0227(9) Uani 1 1 d . . . . .
C31 C 0.5150(4) 0.5520(3) 0.4132(2) 0.0234(9) Uani 1 1 d . . . . .
C17 C 0.2670(4) 0.7820(4) 0.6443(2) 0.0273(10) Uani 1 1 d . . . . .
C38 C 0.6838(4) 0.8061(3) 0.2626(2) 0.0229(9) Uani 1 1 d . . . . .
C42 C 0.8056(4) 0.7100(3) 0.0639(2) 0.0203(8) Uani 1 1 d . . . . .
C11 C 1.1595(4) 0.6373(3) 0.9477(2) 0.0239(9) Uani 1 1 d . . . . .
C41 C 0.7801(4) 0.7639(3) 0.1442(2) 0.0220(9) Uani 1 1 d . . . . .
C16 C 0.2904(4) 0.7284(4) 0.5638(2) 0.0263(9) Uani 1 1 d . . . . .
C32 C 0.6583(4) 0.6174(3) 0.4473(2) 0.0240(9) Uani 1 1 d . . . . .
C47 C 0.7991(4) 1.0202(3) 0.8163(2) 0.0207(8) Uani 1 1 d . . . . .
C7 C 0.7558(5) 0.4451(3) 0.8473(3) 0.0344(11) Uani 1 1 d . . . . .
H7 H 0.6664 0.4038 0.8224 0.041 Uiso 1 1 calc R U . . .
C10 C 1.0175(5) 0.5689(3) 0.9145(2) 0.0237(9) Uani 1 1 d . . . . .
C4 C 0.5386(5) 0.5407(4) 0.7941(3) 0.0346(11) Uani 1 1 d . . . . .
H4 H 0.5185 0.4696 0.7759 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6042(5) 0.7473(4) 0.8482(3) 0.0345(11) Uani 1 1 d . . . . .
H1 H 0.6263 0.8184 0.8666 0.041 Uiso 1 1 calc R U . . .
C19 C 0.2781(5) 0.8999(3) 0.7688(3) 0.0343(11) Uani 1 1 d . . . . .
H19 H 0.3096 0.9620 0.8122 0.041 Uiso 1 1 calc R U . . .
C40 C 0.8463(5) 0.8583(3) 0.2011(3) 0.0308(10) Uani 1 1 d . . . . .
H25 H 0.9197 0.9020 0.1956 0.037 Uiso 1 1 calc R U . . .
C28 C 0.2507(5) 0.4342(3) 0.3424(3) 0.0347(11) Uani 1 1 d . . . . .
H28 H 0.1601 0.3954 0.3169 0.042 Uiso 1 1 calc R U . . .
C45 C 0.7261(5) 1.1207(3) 0.7507(2) 0.0317(11) Uani 1 1 d . . . . .
H45 H 0.7084 1.1806 0.7460 0.038 Uiso 1 1 calc R U . . .
C25 C 0.0392(5) 0.5382(4) 0.2957(3) 0.0364(11) Uani 1 1 d . . . . .
H25A H 0.0148 0.4670 0.2770 0.044 Uiso 1 1 calc R U . . .
C22 C 0.1156(5) 0.7448(4) 0.3523(3) 0.0359(11) Uani 1 1 d . . . . .
H22 H 0.1407 0.8160 0.3719 0.043 Uiso 1 1 calc R U . . .
C18 C 0.3274(5) 0.8777(4) 0.6994(3) 0.0375(12) Uani 1 1 d . . . . .
H18 H 0.3947 0.9240 0.6918 0.045 Uiso 1 1 calc R U . . .
C44 C 0.6976(4) 1.0302(3) 0.6885(2) 0.0212(8) Uani 1 1 d . . . . .
C39 C 0.7912(5) 0.8825(3) 0.2693(3) 0.0309(10) Uani 1 1 d . . . . .
H24 H 0.8246 0.9435 0.3135 0.037 Uiso 1 1 calc R U . . .
C12 C 1.2796(5) 0.5988(4) 0.9568(3) 0.0399(12) Uani 1 1 d . . . . .
H12 H 1.2713 0.5289 0.9432 0.048 Uiso 1 1 calc R U . . .
C8 C 0.8630(6) 0.4050(3) 0.8710(3) 0.0397(12) Uani 1 1 d . . . . .
H8 H 0.8465 0.3363 0.8644 0.048 Uiso 1 1 calc R U . . .
C30 C 0.4880(5) 0.4477(3) 0.4002(3) 0.0334(11) Uani 1 1 d . . . . .
H30 H 0.5592 0.4188 0.4157 0.040 Uiso 1 1 calc R U . . .
C46 C 0.7853(5) 1.1147(3) 0.8231(3) 0.0302(10) Uani 1 1 d . . . . .
H46 H 0.8125 1.1707 0.8714 0.036 Uiso 1 1 calc R U . . .
C36 C 0.8007(5) 0.7806(4) 0.5007(3) 0.0369(11) Uani 1 1 d . . . . .
H36 H 0.8097 0.8509 0.5168 0.044 Uiso 1 1 calc R U . . .
C15 C 1.2961(5) 0.8013(4) 0.9957(3) 0.0336(11) Uani 1 1 d . . . . .
H15 H 1.3035 0.8712 1.0096 0.040 Uiso 1 1 calc R U . . .
C9 C 0.9949(5) 0.4669(3) 0.9047(3) 0.0382(12) Uani 1 1 d . . . . .
H9 H 1.0687 0.4405 0.9208 0.046 Uiso 1 1 calc R U . . .
C33 C 0.7754(5) 0.5769(4) 0.4548(3) 0.0391(12) Uani 1 1 d . . . . .
H33 H 0.7654 0.5065 0.4387 0.047 Uiso 1 1 calc R U . . .
C29 C 0.3539(5) 0.3887(3) 0.3640(3) 0.0382(12) Uani 1 1 d . . . . .
H29 H 0.3336 0.3191 0.3542 0.046 Uiso 1 1 calc R U . . .
C35 C 0.9190(5) 0.7452(4) 0.5095(3) 0.0441(13) Uani 1 1 d . . . . .
H35 H 1.0065 0.7902 0.5308 0.053 Uiso 1 1 calc R U . . .
C3 C 0.4376(5) 0.5899(4) 0.7759(3) 0.0420(12) Uani 1 1 d . . . . .
H3 H 0.3489 0.5526 0.7450 0.050 Uiso 1 1 calc R U . . .
C2 C 0.4702(5) 0.6952(4) 0.8043(3) 0.0409(12) Uani 1 1 d . . . . .
H2 H 0.4033 0.7305 0.7941 0.049 Uiso 1 1 calc R U . . .
C23 C -0.0208(5) 0.6962(4) 0.3103(3) 0.0443(13) Uani 1 1 d . . . . .
H23 H -0.0859 0.7337 0.3024 0.053 Uiso 1 1 calc R U . . .
O12 O 0.8581(3) 0.8968(2) 0.86506(17) 0.0277(7) Uani 1 1 d . . . . .
OW1 O 0.7872(3) 0.9038(2) 1.01177(18) 0.0332(7) Uani 1 1 d . . . . .
C13 C 1.4087(5) 0.6645(4) 0.9856(3) 0.0478(14) Uani 1 1 d . . . . .
H13 H 1.4889 0.6400 0.9918 0.057 Uiso 1 1 calc R U . . .
C34 C 0.9056(5) 0.6419(4) 0.4863(3) 0.0467(14) Uani 1 1 d . . . . .
H34 H 0.9845 0.6158 0.4918 0.056 Uiso 1 1 calc R U . . .
C14 C 1.4175(5) 0.7672(4) 1.0052(3) 0.0423(12) Uani 1 1 d . . . . .
H14 H 1.5041 0.8135 1.0248 0.051 Uiso 1 1 calc R U . . .
C24 C -0.0577(5) 0.5913(5) 0.2806(3) 0.0484(14) Uani 1 1 d . . . . .
H24A H -0.1478 0.5565 0.2504 0.058 Uiso 1 1 calc R U . . .
OW2 O 0.8659(9) 1.0429(5) 0.4783(5) 0.199(4) 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
Dy2 O1 2.239(3) . ?
Dy2 O10 2.244(3) . ?
Dy2 O9 2.313(3) . ?
Dy2 O6 2.443(3) . ?
Dy2 O5 2.453(3) . ?
Dy2 N6 2.519(3) . ?
Dy2 N5 2.551(3) . ?
Dy2 N4 2.553(3) . ?
Dy2 C37 2.803(4) . ?
Dy1 O11 2.322(3) 2_777 ?
Dy1 O7 2.326(3) 1_556 ?
Dy1 O12 2.394(3) . ?
Dy1 O3 2.453(3) . ?
Dy1 O4 2.483(3) . ?
Dy1 N1 2.536(3) . ?
Dy1 N3 2.545(3) . ?
Dy1 N2 2.550(3) . ?
Dy1 OW1 2.578(3) . ?
Dy1 C21 2.825(4) 1_655 ?
S1 C20 1.717(4) . ?
S1 C17 1.722(4) . ?
S2 C38 1.713(4) . ?
S2 C41 1.716(4) . ?
S3 C47 1.710(4) . ?
S3 C44 1.724(4) . ?
O3 C21 1.260(5) 1_655 ?
O6 C37 1.272(5) . ?
O7 C42 1.273(5) . ?
O7 Dy1 2.326(3) 1_554 ?
O4 C21 1.263(5) 1_655 ?
N5 C31 1.339(5) . ?
N5 C27 1.342(5) . ?
N4 C22 1.338(5) . ?
N4 C26 1.350(5) . ?
N2 C10 1.340(5) . ?
N2 C6 1.341(5) . ?
O5 C37 1.252(5) . ?
N1 C5 1.339(5) . ?
N1 C1 1.342(5) . ?
O8 C42 1.229(5) . ?
O2 C16 1.226(5) . ?
N6 C32 1.342(5) . ?
N6 C36 1.347(6) . ?
O1 C16 1.269(5) . ?
N3 C15 1.339(6) . ?
N3 C11 1.350(5) . ?
O11 C48 1.249(4) . ?
O11 Dy1 2.322(3) 2_777 ?
O9 C43 1.246(4) . ?
O10 C43 1.265(4) 2_676 ?
C43 O10 1.265(4) 2_676 ?
C43 C44 1.481(5) . ?
C37 C38 1.482(5) . ?
C21 O3 1.260(5) 1_455 ?
C21 O4 1.263(5) 1_455 ?
C21 C20 1.477(5) . ?
C21 Dy1 2.826(4) 1_455 ?
C48 O12 1.247(4) . ?
C48 C47 1.500(5) . ?
C6 C7 1.395(6) . ?
C6 C5 1.486(6) . ?
C5 C4 1.393(6) . ?
C27 C28 1.399(6) . ?
C27 C26 1.480(6) . ?
C20 C19 1.364(6) . ?
C26 C25 1.396(6) . ?
C31 C30 1.399(6) . ?
C31 C32 1.479(6) . ?
C17 C18 1.358(6) . ?
C17 C16 1.496(6) . ?
C38 C39 1.362(6) . ?
C42 C41 1.503(5) . ?
C11 C12 1.407(6) . ?
C11 C10 1.483(6) . ?
C41 C40 1.367(6) . ?
C32 C33 1.393(6) . ?
C47 C46 1.345(5) . ?
C7 C8 1.369(7) . ?
C7 H7 0.9300 . ?
C10 C9 1.383(6) . ?
C4 C3 1.377(7) . ?
C4 H4 0.9300 . ?
C1 C2 1.380(6) . ?
C1 H1 0.9300 . ?
C19 C18 1.404(6) . ?
C19 H19 0.9300 . ?
C40 C39 1.415(6) . ?
C40 H25 0.9300 . ?
C28 C29 1.377(6) . ?
C28 H28 0.9300 . ?
C45 C44 1.351(5) . ?
C45 C46 1.399(6) . ?
C45 H45 0.9300 . ?
C25 C24 1.371(7) . ?
C25 H25A 0.9300 . ?
C22 C23 1.382(6) . ?
C22 H22 0.9300 . ?
C18 H18 0.9300 . ?
C39 H24 0.9300 . ?
C12 C13 1.368(7) . ?
C12 H12 0.9300 . ?
C8 C9 1.372(7) . ?
C8 H8 0.9300 . ?
C30 C29 1.380(7) . ?
C30 H30 0.9300 . ?
C46 H46 0.9300 . ?
C36 C35 1.365(6) . ?
C36 H36 0.9300 . ?
C15 C14 1.384(6) . ?
C15 H15 0.9300 . ?
C9 H9 0.9300 . ?
C33 C34 1.373(7) . ?
C33 H33 0.9300 . ?
C29 H29 0.9300 . ?
C35 C34 1.366(7) . ?
C35 H35 0.9300 . ?
C3 C2 1.376(7) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C23 C24 1.370(7) . ?
C23 H23 0.9300 . ?
C13 C14 1.371(7) . ?
C13 H13 0.9300 . ?
C34 H34 0.9300 . ?
C14 H14 0.9300 . ?
C24 H24A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy2 O10 99.90(13) . . ?
O1 Dy2 O9 74.19(12) . . ?
O10 Dy2 O9 87.36(10) . . ?
O1 Dy2 O6 155.69(11) . . ?
O10 Dy2 O6 89.49(10) . . ?
O9 Dy2 O6 129.01(10) . . ?
O1 Dy2 O5 150.62(12) . . ?
O10 Dy2 O5 76.15(11) . . ?
O9 Dy2 O5 76.53(10) . . ?
O6 Dy2 O5 53.44(9) . . ?
O1 Dy2 N6 99.09(14) . . ?
O10 Dy2 N6 149.90(12) . . ?
O9 Dy2 N6 75.64(11) . . ?
O6 Dy2 N6 82.58(11) . . ?
O5 Dy2 N6 75.82(12) . . ?
O1 Dy2 N5 84.24(12) . . ?
O10 Dy2 N5 140.82(11) . . ?
O9 Dy2 N5 130.49(10) . . ?
O6 Dy2 N5 74.59(10) . . ?
O5 Dy2 N5 117.49(10) . . ?
N6 Dy2 N5 64.35(11) . . ?
O1 Dy2 N4 78.00(12) . . ?
O10 Dy2 N4 78.80(11) . . ?
O9 Dy2 N4 146.19(11) . . ?
O6 Dy2 N4 81.97(10) . . ?
O5 Dy2 N4 128.16(11) . . ?
N6 Dy2 N4 128.15(11) . . ?
N5 Dy2 N4 63.86(10) . . ?
O1 Dy2 C37 175.67(13) . . ?
O10 Dy2 C37 82.58(11) . . ?
O9 Dy2 C37 102.48(12) . . ?
O6 Dy2 C37 26.96(10) . . ?
O5 Dy2 C37 26.50(10) . . ?
N6 Dy2 C37 77.24(12) . . ?
N5 Dy2 C37 96.10(11) . . ?
N4 Dy2 C37 106.04(12) . . ?
O11 Dy1 O7 78.93(10) 2_777 1_556 ?
O11 Dy1 O12 98.34(10) 2_777 . ?
O7 Dy1 O12 135.99(10) 1_556 . ?
O11 Dy1 O3 123.81(10) 2_777 . ?
O7 Dy1 O3 143.07(10) 1_556 . ?
O12 Dy1 O3 74.15(10) . . ?
O11 Dy1 O4 72.05(10) 2_777 . ?
O7 Dy1 O4 144.83(10) 1_556 . ?
O12 Dy1 O4 69.08(10) . . ?
O3 Dy1 O4 52.95(9) . . ?
O11 Dy1 N1 147.66(10) 2_777 . ?
O7 Dy1 N1 84.97(11) 1_556 . ?
O12 Dy1 N1 74.34(11) . . ?
O3 Dy1 N1 85.18(10) . . ?
O4 Dy1 N1 129.93(10) . . ?
O11 Dy1 N3 77.93(11) 2_777 . ?
O7 Dy1 N3 83.77(11) 1_556 . ?
O12 Dy1 N3 139.21(11) . . ?
O3 Dy1 N3 74.79(10) . . ?
O4 Dy1 N3 71.24(11) . . ?
N1 Dy1 N3 128.15(11) . . ?
O11 Dy1 N2 134.67(10) 2_777 . ?
O7 Dy1 N2 73.01(10) 1_556 . ?
O12 Dy1 N2 126.53(10) . . ?
O3 Dy1 N2 70.68(9) . . ?
O4 Dy1 N2 114.92(10) . . ?
N1 Dy1 N2 63.87(10) . . ?
N3 Dy1 N2 64.42(11) . . ?
O11 Dy1 OW1 73.80(10) 2_777 . ?
O7 Dy1 OW1 66.31(10) 1_556 . ?
O12 Dy1 OW1 70.76(10) . . ?
O3 Dy1 OW1 142.85(10) . . ?
O4 Dy1 OW1 121.54(10) . . ?
N1 Dy1 OW1 74.07(11) . . ?
N3 Dy1 OW1 141.94(10) . . ?
N2 Dy1 OW1 122.92(10) . . ?
O11 Dy1 C21 98.14(12) 2_777 1_655 ?
O7 Dy1 C21 155.15(11) 1_556 1_655 ?
O12 Dy1 C21 68.81(10) . 1_655 ?
O3 Dy1 C21 26.43(10) . 1_655 ?
O4 Dy1 C21 26.53(10) . 1_655 ?
N1 Dy1 C21 107.81(12) . 1_655 ?
N3 Dy1 C21 71.55(11) . 1_655 ?
N2 Dy1 C21 93.17(11) . 1_655 ?
OW1 Dy1 C21 137.01(10) . 1_655 ?
C20 S1 C17 91.5(2) . . ?
C38 S2 C41 91.8(2) . . ?
C47 S3 C44 91.41(19) . . ?
C21 O3 Dy1 93.5(2) 1_655 . ?
C37 O6 Dy2 92.5(2) . . ?
C42 O7 Dy1 142.2(3) . 1_554 ?
C21 O4 Dy1 92.0(2) 1_655 . ?
C31 N5 C27 118.9(3) . . ?
C31 N5 Dy2 119.9(3) . . ?
C27 N5 Dy2 120.9(2) . . ?
C22 N4 C26 117.7(4) . . ?
C22 N4 Dy2 121.1(3) . . ?
C26 N4 Dy2 121.2(3) . . ?
C10 N2 C6 118.6(3) . . ?
C10 N2 Dy1 119.9(3) . . ?
C6 N2 Dy1 120.6(2) . . ?
C37 O5 Dy2 92.5(2) . . ?
C5 N1 C1 117.9(4) . . ?
C5 N1 Dy1 121.6(3) . . ?
C1 N1 Dy1 120.5(3) . . ?
C32 N6 C36 118.3(4) . . ?
C32 N6 Dy2 121.1(3) . . ?
C36 N6 Dy2 120.1(3) . . ?
C16 O1 Dy2 145.8(3) . . ?
C15 N3 C11 117.7(4) . . ?
C15 N3 Dy1 121.7(3) . . ?
C11 N3 Dy1 120.4(3) . . ?
C48 O11 Dy1 161.4(3) . 2_777 ?
C43 O9 Dy2 147.9(3) . . ?
C43 O10 Dy2 163.0(3) 2_676 . ?
O9 C43 O10 124.6(4) . 2_676 ?
O9 C43 C44 118.3(3) . . ?
O10 C43 C44 117.0(3) 2_676 . ?
O5 C37 O6 121.5(4) . . ?
O5 C37 C38 119.1(4) . . ?
O6 C37 C38 119.5(4) . . ?
O5 C37 Dy2 61.0(2) . . ?
O6 C37 Dy2 60.5(2) . . ?
C38 C37 Dy2 176.8(3) . . ?
O3 C21 O4 121.5(4) 1_455 1_455 ?
O3 C21 C20 119.5(4) 1_455 . ?
O4 C21 C20 119.0(4) 1_455 . ?
O3 C21 Dy1 60.06(19) 1_455 1_455 ?
O4 C21 Dy1 61.4(2) 1_455 1_455 ?
C20 C21 Dy1 178.5(3) . 1_455 ?
O12 C48 O11 125.4(3) . . ?
O12 C48 C47 116.9(3) . . ?
O11 C48 C47 117.7(3) . . ?
N2 C6 C7 122.2(4) . . ?
N2 C6 C5 116.7(3) . . ?
C7 C6 C5 121.1(4) . . ?
N1 C5 C4 121.9(4) . . ?
N1 C5 C6 116.5(4) . . ?
C4 C5 C6 121.7(4) . . ?
N5 C27 C28 121.7(4) . . ?
N5 C27 C26 117.3(3) . . ?
C28 C27 C26 121.0(4) . . ?
C19 C20 C21 128.4(4) . . ?
C19 C20 S1 111.6(3) . . ?
C21 C20 S1 120.0(3) . . ?
N4 C26 C25 121.6(4) . . ?
N4 C26 C27 116.4(4) . . ?
C25 C26 C27 122.1(4) . . ?
N5 C31 C30 122.1(4) . . ?
N5 C31 C32 116.9(4) . . ?
C30 C31 C32 121.0(4) . . ?
C18 C17 C16 130.4(4) . . ?
C18 C17 S1 111.2(3) . . ?
C16 C17 S1 118.4(3) . . ?
C39 C38 C37 127.2(4) . . ?
C39 C38 S2 111.9(3) . . ?
C37 C38 S2 120.9(3) . . ?
O8 C42 O7 127.1(4) . . ?
O8 C42 C41 117.5(3) . . ?
O7 C42 C41 115.4(4) . . ?
N3 C11 C12 121.3(4) . . ?
N3 C11 C10 116.8(3) . . ?
C12 C11 C10 121.9(4) . . ?
C40 C41 C42 129.7(4) . . ?
C40 C41 S2 111.2(3) . . ?
C42 C41 S2 119.1(3) . . ?
O2 C16 O1 126.3(4) . . ?
O2 C16 C17 118.9(4) . . ?
O1 C16 C17 114.8(4) . . ?
N6 C32 C33 120.8(4) . . ?
N6 C32 C31 116.8(3) . . ?
C33 C32 C31 122.4(4) . . ?
C46 C47 C48 126.3(4) . . ?
C46 C47 S3 111.3(3) . . ?
C48 C47 S3 122.4(3) . . ?
C8 C7 C6 118.5(4) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
N2 C10 C9 121.6(4) . . ?
N2 C10 C11 117.3(3) . . ?
C9 C10 C11 121.1(4) . . ?
C3 C4 C5 119.4(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C1 C2 123.4(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C20 C19 C18 112.5(4) . . ?
C20 C19 H19 123.8 . . ?
C18 C19 H19 123.8 . . ?
C41 C40 C39 112.9(4) . . ?
C41 C40 H25 123.5 . . ?
C39 C40 H25 123.5 . . ?
C29 C28 C27 119.3(4) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C44 C45 C46 112.6(4) . . ?
C44 C45 H45 123.7 . . ?
C46 C45 H45 123.7 . . ?
C24 C25 C26 119.3(5) . . ?
C24 C25 H25A 120.4 . . ?
C26 C25 H25A 120.4 . . ?
N4 C22 C23 123.5(4) . . ?
N4 C22 H22 118.2 . . ?
C23 C22 H22 118.2 . . ?
C17 C18 C19 113.3(4) . . ?
C17 C18 H18 123.3 . . ?
C19 C18 H18 123.3 . . ?
C45 C44 C43 127.5(4) . . ?
C45 C44 S3 111.1(3) . . ?
C43 C44 S3 121.4(3) . . ?
C38 C39 C40 112.2(4) . . ?
C38 C39 H24 123.9 . . ?
C40 C39 H24 123.9 . . ?
C13 C12 C11 119.8(5) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C7 C8 C9 119.4(4) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C29 C30 C31 118.8(4) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C47 C46 C45 113.6(4) . . ?
C47 C46 H46 123.2 . . ?
C45 C46 H46 123.2 . . ?
N6 C36 C35 123.3(4) . . ?
N6 C36 H36 118.3 . . ?
C35 C36 H36 118.3 . . ?
N3 C15 C14 123.2(5) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C8 C9 C10 119.5(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C34 C33 C32 119.4(4) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C28 C29 C30 119.1(4) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C36 C35 C34 118.3(5) . . ?
C36 C35 H35 120.8 . . ?
C34 C35 H35 120.8 . . ?
C2 C3 C4 118.9(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C2 C1 118.5(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C24 C23 C22 118.3(5) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C48 O12 Dy1 132.5(3) . . ?
C12 C13 C14 118.7(4) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C35 C34 C33 119.7(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C13 C14 C15 119.2(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C23 C24 C25 119.5(5) . . ?
C23 C24 H24A 120.2 . . ?
C25 C24 H24A 120.2 . . ?

_refine_diff_density_max         1.723
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.137

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_7
_database_code_depnum_ccdc_archive 'CCDC 1410409'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Ho2 N6 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            'Light Pink'

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1342.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0126(14)
_cell_length_b                   14.278(2)
_cell_length_c                   18.369(3)
_cell_angle_alpha                109.892(4)
_cell_angle_beta                 99.969(4)
_cell_angle_gamma                99.169(3)
_cell_volume                     2363.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    33604
_cell_measurement_theta_min      4.349
_cell_measurement_theta_max      50.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    3.532
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33598
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.216
_diffrn_reflns_theta_max         28.448
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11833
_reflns_number_gt                8016
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0217P)²+5.4025P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11833
_refine_ls_number_parameters     658
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.0916
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ho2 Ho 0.46405(3) 0.29239(2) 0.94017(2) 0.01584(7) Uani 1 1 d . . . . .
Ho1 Ho 0.95145(3) 0.30321(2) 1.44015(2) 0.01548(7) Uani 1 1 d . . . . .
S2 S 0.64867(17) 0.20496(12) 0.67397(9) 0.0262(4) Uani 1 1 d . . . . .
S1 S 0.14691(17) 0.21564(12) 1.17696(9) 0.0249(3) Uani 1 1 d . . . . .
S3 S 0.74162(19) 0.43611(12) 1.21972(10) 0.0301(4) Uani 1 1 d . . . . .
O3 O 1.1356(4) 0.3868(3) 1.3930(2) 0.0262(10) Uani 1 1 d . . . . .
O6 O 0.5009(4) 0.2297(3) 0.8060(2) 0.0279(10) Uani 1 1 d . . . . .
O4 O 1.0061(4) 0.2359(3) 1.3102(2) 0.0236(9) Uani 1 1 d . . . . .
O11 O 0.9061(4) 0.5594(3) 1.4509(2) 0.0265(10) Uani 1 1 d . . . . .
O12 O 0.8594(5) 0.3973(3) 1.3668(3) 0.0336(11) Uani 1 1 d . . . . .
O7 O 0.9001(5) 0.2611(3) 1.5448(3) 0.0321(11) Uani 1 1 d . . . . .
N2 N 0.9125(5) 0.1099(4) 1.3947(3) 0.0201(11) Uani 1 1 d . . . . .
OW1 O 0.7879(5) 0.4038(4) 1.5118(3) 0.0433(13) Uani 1 1 d . . . . .
O9 O 0.6084(5) 0.4188(3) 1.0544(2) 0.0294(10) Uani 1 1 d . . . . .
O5 O 0.6437(5) 0.3741(3) 0.8916(3) 0.0349(11) Uani 1 1 d . . . . .
N6 N 0.6707(5) 0.2208(4) 0.9696(3) 0.0303(13) Uani 1 1 d . . . . .
O8 O 0.7334(5) 0.1237(3) 1.5238(3) 0.0337(11) Uani 1 1 d . . . . .
O10 O 0.3763(5) 0.4144(3) 0.9140(3) 0.0357(11) Uani 1 1 d . . . . .
N3 N 1.1671(5) 0.2381(4) 1.4683(3) 0.0249(12) Uani 1 1 d . . . . .
N5 N 0.4129(5) 0.0989(4) 0.8952(3) 0.0216(11) Uani 1 1 d . . . . .
C43 C 0.6368(6) 0.5088(4) 1.1046(4) 0.0193(13) Uani 1 1 d . . . . .
N1 N 0.7059(5) 0.2018(4) 1.3659(3) 0.0232(11) Uani 1 1 d . . . . .
N4 N 0.2139(5) 0.1969(4) 0.8668(3) 0.0249(12) Uani 1 1 d . . . . .
C12 C 1.2773(8) 0.0978(6) 1.4568(4) 0.045(2) Uani 1 1 d . . . . .
H12 H 1.2686 0.0277 1.4432 0.054 Uiso 1 1 calc R U . . .
O2 O 0.2341(5) 0.1354(4) 1.0270(3) 0.0364(12) Uani 1 1 d . . . . .
O1 O 0.3705(6) 0.2825(4) 1.0402(3) 0.0548(16) Uani 1 1 d . . . . .
C42 C 0.8039(7) 0.2097(5) 1.5636(4) 0.0245(14) Uani 1 1 d . . . . .
C47 C 0.8003(6) 0.5203(5) 1.3158(3) 0.0237(13) Uani 1 1 d . . . . .
C44 C 0.6964(6) 0.5293(5) 1.1879(4) 0.0250(14) Uani 1 1 d . . . . .
C7 C 0.7561(8) -0.0552(5) 1.3470(4) 0.0388(18) Uani 1 1 d . . . . .
H7 H 0.6665 -0.0964 1.3227 0.047 Uiso 1 1 calc R U . . .
C6 C 0.7838(6) 0.0494(5) 1.3608(4) 0.0235(14) Uani 1 1 d . . . . .
C32 C 0.6589(7) 0.1194(5) 0.9480(4) 0.0257(14) Uani 1 1 d . . . . .
C27 C 0.2836(6) 0.0405(4) 0.8604(3) 0.0220(13) Uani 1 1 d . . . . .
C21 C 0.1022(6) 0.3138(5) 1.3261(3) 0.0205(13) Uani 1 1 d . . . . .
C48 C 0.8615(6) 0.4904(4) 1.3839(4) 0.0181(12) Uani 1 1 d . . . . .
C10 C 1.0175(7) 0.0692(5) 1.4150(4) 0.0265(14) Uani 1 1 d . . . . .
C20 C 0.1796(6) 0.3189(5) 1.2656(3) 0.0231(14) Uani 1 1 d . . . . .
C38 C 0.6824(7) 0.3070(5) 0.7625(4) 0.0246(14) Uani 1 1 d . . . . .
C11 C 1.1595(7) 0.1369(5) 1.4478(4) 0.0257(14) Uani 1 1 d . . . . .
C41 C 0.7785(6) 0.2652(5) 0.6442(4) 0.0249(14) Uani 1 1 d . . . . .
C26 C 0.1747(6) 0.0929(5) 0.8403(4) 0.0256(14) Uani 1 1 d . . . . .
C5 C 0.6711(7) 0.0980(5) 1.3395(4) 0.0235(14) Uani 1 1 d . . . . .
C16 C 0.2910(7) 0.2268(5) 1.0637(4) 0.0279(15) Uani 1 1 d . . . . .
C31 C 0.5145(7) 0.0528(5) 0.9134(4) 0.0244(14) Uani 1 1 d . . . . .
C13 C 1.4097(8) 0.1657(7) 1.4868(5) 0.050(2) Uani 1 1 d . . . . .
H13 H 1.4901 0.1415 1.4930 0.059 Uiso 1 1 calc R U . . .
C19 C 0.2792(7) 0.3990(5) 1.2695(4) 0.0338(16) Uani 1 1 d . . . . .
H19 H 0.3108 0.4609 1.3132 0.041 Uiso 1 1 calc R U . . .
C34 C 0.9061(8) 0.1442(6) 0.9868(5) 0.045(2) Uani 1 1 d . . . . .
H34 H 0.9848 0.1179 0.9922 0.054 Uiso 1 1 calc R U . . .
C1 C 0.6058(7) 0.2485(5) 1.3488(4) 0.0362(17) Uani 1 1 d . . . . .
H1 H 0.6276 0.3197 1.3673 0.043 Uiso 1 1 calc R U . . .
C15 C 1.2965(7) 0.3005(6) 1.4965(4) 0.0350(17) Uani 1 1 d . . . . .
H15 H 1.3043 0.3705 1.5100 0.042 Uiso 1 1 calc R U . . .
C17 C 0.2666(7) 0.2799(5) 1.1439(4) 0.0281(15) Uani 1 1 d . . . . .
C18 C 0.3284(7) 0.3772(5) 1.1997(4) 0.0366(17) Uani 1 1 d . . . . .
H18 H 0.3956 0.4236 1.1920 0.044 Uiso 1 1 calc R U . . .
C4 C 0.5392(7) 0.0417(6) 1.2946(4) 0.0379(17) Uani 1 1 d . . . . .
H4 H 0.5181 -0.0295 1.2765 0.046 Uiso 1 1 calc R U . . .
C29 C 0.3555(8) -0.1090(5) 0.8652(4) 0.0380(18) Uani 1 1 d . . . . .
H29 H 0.3350 -0.1784 0.8563 0.046 Uiso 1 1 calc R U . . .
C8 C 0.8634(9) -0.0956(5) 1.3699(4) 0.044(2) Uani 1 1 d . . . . .
H8 H 0.8470 -0.1645 1.3625 0.053 Uiso 1 1 calc R U . . .
C25 C 0.0407(7) 0.0397(6) 0.7972(4) 0.0368(17) Uani 1 1 d . . . . .
H25 H 0.0169 -0.0315 0.7788 0.044 Uiso 1 1 calc R U . . .
C33 C 0.7756(7) 0.0793(6) 0.9554(4) 0.0386(18) Uani 1 1 d . . . . .
H33 H 0.7655 0.0088 0.9391 0.046 Uiso 1 1 calc R U . . .
C14 C 1.4175(7) 0.2672(6) 1.5065(5) 0.046(2) Uani 1 1 d . . . . .
H14 H 1.5037 0.3139 1.5266 0.055 Uiso 1 1 calc R U . . .
C35 C 0.9196(8) 0.2479(6) 1.0101(5) 0.048(2) Uani 1 1 d . . . . .
H35 H 1.0069 0.2931 1.0315 0.057 Uiso 1 1 calc R U . . .
C37 C 0.6036(6) 0.3034(5) 0.8232(4) 0.0243(14) Uani 1 1 d . . . . .
C46 C 0.7826(7) 0.6102(6) 1.3185(5) 0.0402(18) Uani 1 1 d . U . . .
H46 H 0.8092 0.6662 1.3668 0.048 Uiso 1 1 calc R U . . .
C30 C 0.4871(8) -0.0512(5) 0.9004(4) 0.0379(18) Uani 1 1 d . . . . .
H30 H 0.5582 -0.0805 0.9156 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4719(7) 0.1960(6) 1.3049(4) 0.0411(19) Uani 1 1 d . . . . .
H2 H 0.4051 0.2313 1.2947 0.049 Uiso 1 1 calc R U . . .
C36 C 0.8001(7) 0.2827(6) 1.0007(4) 0.0413(19) Uani 1 1 d . . . . .
H36 H 0.8089 0.3531 1.0168 0.050 Uiso 1 1 calc R U . . .
C9 C 0.9958(8) -0.0334(5) 1.4040(4) 0.0394(18) Uani 1 1 d . . . . .
H9 H 1.0698 -0.0600 1.4195 0.047 Uiso 1 1 calc R U . . .
C40 C 0.8454(7) 0.3598(5) 0.7007(4) 0.0342(16) Uani 1 1 d . . . . .
H40 H 0.9193 0.4033 0.6952 0.041 Uiso 1 1 calc R U . . .
C28 C 0.2519(8) -0.0641(5) 0.8427(4) 0.0348(17) Uani 1 1 d . . . . .
H28 H 0.1621 -0.1035 0.8159 0.042 Uiso 1 1 calc R U . . .
C39 C 0.7889(7) 0.3837(5) 0.7684(4) 0.0347(17) Uani 1 1 d . . . . .
H39 H 0.8211 0.4453 0.8123 0.042 Uiso 1 1 calc R U . . .
C22 C 0.1150(7) 0.2450(5) 0.8521(4) 0.0352(17) Uani 1 1 d . . . . .
H22 H 0.1395 0.3162 0.8712 0.042 Uiso 1 1 calc R U . . .
C45 C 0.7265(8) 0.6204(5) 1.2515(4) 0.0369(17) Uani 1 1 d . . . . .
H45 H 0.7098 0.6813 1.2483 0.044 Uiso 1 1 calc R U . . .
C24 C -0.0570(7) 0.0918(7) 0.7815(5) 0.049(2) Uani 1 1 d . . . . .
H24 H -0.1471 0.0566 0.7515 0.058 Uiso 1 1 calc R U . . .
C3 C 0.4389(7) 0.0920(6) 1.2769(4) 0.0424(19) Uani 1 1 d . . . . .
H3 H 0.3499 0.0551 1.2462 0.051 Uiso 1 1 calc R U . . .
C23 C -0.0201(7) 0.1967(6) 0.8108(5) 0.047(2) Uani 1 1 d . . . . .
H23 H -0.0852 0.2342 0.8028 0.057 Uiso 1 1 calc R U . . .
OW2 O 0.1394(15) 0.4564(9) 1.0208(7) 0.245(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho2 O10 2.224(4) . ?
Ho2 O1 2.237(5) . ?
Ho2 O9 2.300(4) . ?
Ho2 O6 2.435(4) . ?
Ho2 O5 2.446(4) . ?
Ho2 N6 2.506(5) . ?
Ho2 N5 2.535(5) . ?
Ho2 N4 2.538(5) . ?
Ho2 C37 2.792(6) . ?
Ho1 O11 2.310(4) 2_768 ?
Ho1 O7 2.314(4) . ?
Ho1 O12 2.380(4) . ?
Ho1 O4 2.445(4) . ?
Ho1 O3 2.476(4) . ?
Ho1 N1 2.522(5) . ?
Ho1 N3 2.524(5) . ?
Ho1 N2 2.538(5) . ?
Ho1 OW1 2.586(5) . ?
Ho1 C21 2.815(6) 1_655 ?
S2 C38 1.710(6) . ?
S2 C41 1.714(6) . ?
S1 C17 1.711(6) . ?
S1 C20 1.721(6) . ?
S3 C47 1.697(6) . ?
S3 C44 1.716(6) . ?
O3 C21 1.257(7) 1_655 ?
O6 C37 1.257(7) . ?
O4 C21 1.260(7) 1_655 ?
O11 C48 1.236(7) . ?
O11 Ho1 2.310(4) 2_768 ?
O12 C48 1.253(7) . ?
O7 C42 1.282(7) . ?
N2 C10 1.337(7) . ?
N2 C6 1.341(7) . ?
O9 C43 1.252(7) . ?
O5 C37 1.263(7) . ?
N6 C32 1.344(8) . ?
N6 C36 1.350(8) . ?
O8 C42 1.214(8) . ?
O10 C43 1.273(7) 2_667 ?
N3 C11 1.349(8) . ?
N3 C15 1.351(8) . ?
N5 C27 1.337(7) . ?
N5 C31 1.350(7) . ?
C43 O10 1.273(7) 2_667 ?
C43 C44 1.453(8) . ?
N1 C1 1.340(7) . ?
N1 C5 1.357(7) . ?
N4 C22 1.332(7) . ?
N4 C26 1.360(8) . ?
C12 C11 1.392(9) . ?
C12 C13 1.405(11) . ?
O2 C16 1.231(8) . ?
O1 C16 1.265(8) . ?
C42 C41 1.511(8) 1_556 ?
C47 C46 1.308(9) . ?
C47 C48 1.518(8) . ?
C44 C45 1.366(8) . ?
C7 C8 1.367(10) . ?
C7 C6 1.399(8) . ?
C6 C5 1.479(8) . ?
C32 C33 1.387(8) . ?
C32 C31 1.493(9) . ?
C27 C28 1.385(8) . ?
C27 C26 1.482(8) . ?
C21 O3 1.257(7) 1_455 ?
C21 O4 1.260(7) 1_455 ?
C21 C20 1.475(8) . ?
C21 Ho1 2.815(6) 1_455 ?
C10 C9 1.385(9) . ?
C10 C11 1.479(9) . ?
C20 C19 1.365(9) . ?
C38 C39 1.362(9) . ?
C38 C37 1.482(8) . ?
C41 C40 1.366(9) . ?
C41 C42 1.511(8) 1_554 ?
C26 C25 1.379(9) . ?
C5 C4 1.380(9) . ?
C16 C17 1.492(8) . ?
C31 C30 1.395(8) . ?
C13 C14 1.355(11) . ?
C19 C18 1.407(8) . ?
C34 C35 1.370(10) . ?
C34 C33 1.374(10) . ?
C1 C2 1.379(9) . ?
C15 C14 1.376(9) . ?
C17 C18 1.379(9) . ?
C4 C3 1.381(10) . ?
C29 C30 1.352(10) . ?
C29 C28 1.379(9) . ?
C8 C9 1.377(10) . ?
C25 C24 1.370(10) . ?
C35 C36 1.373(9) . ?
C46 C45 1.327(9) . ?
C2 C3 1.357(10) . ?
C40 C39 1.414(9) . ?
C22 C23 1.368(9) . ?
C24 C23 1.370(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Ho2 O1 101.3(2) . . ?
O10 Ho2 O9 87.66(16) . . ?
O1 Ho2 O9 74.21(18) . . ?
O10 Ho2 O6 89.54(16) . . ?
O1 Ho2 O6 155.29(18) . . ?
O9 Ho2 O6 128.91(15) . . ?
O10 Ho2 O5 76.44(17) . . ?
O1 Ho2 O5 150.48(18) . . ?
O9 Ho2 O5 76.28(16) . . ?
O6 Ho2 O5 53.60(15) . . ?
O10 Ho2 N6 149.60(18) . . ?
O1 Ho2 N6 98.3(2) . . ?
O9 Ho2 N6 75.63(16) . . ?
O6 Ho2 N6 81.92(16) . . ?
O5 Ho2 N6 75.02(17) . . ?
O10 Ho2 N5 140.33(17) . . ?
O1 Ho2 N5 83.47(18) . . ?
O9 Ho2 N5 130.72(15) . . ?
O6 Ho2 N5 74.26(15) . . ?
O5 Ho2 N5 117.38(15) . . ?
N6 Ho2 N5 64.75(17) . . ?
O10 Ho2 N4 78.35(17) . . ?
O1 Ho2 N4 78.13(18) . . ?
O9 Ho2 N4 145.78(16) . . ?
O6 Ho2 N4 82.51(15) . . ?
O5 Ho2 N4 128.72(16) . . ?
N6 Ho2 N4 128.69(17) . . ?
N5 Ho2 N4 63.99(16) . . ?
O10 Ho2 C37 82.59(18) . . ?
O1 Ho2 C37 174.8(2) . . ?
O9 Ho2 C37 102.65(18) . . ?
O6 Ho2 C37 26.73(16) . . ?
O5 Ho2 C37 26.88(16) . . ?
N6 Ho2 C37 76.71(18) . . ?
N5 Ho2 C37 95.78(17) . . ?
N4 Ho2 C37 106.23(18) . . ?
O11 Ho1 O7 78.53(15) 2_768 . ?
O11 Ho1 O12 97.91(15) 2_768 . ?
O7 Ho1 O12 134.64(15) . . ?
O11 Ho1 O4 124.36(15) 2_768 . ?
O7 Ho1 O4 143.94(14) . . ?
O12 Ho1 O4 74.47(14) . . ?
O11 Ho1 O3 72.41(14) 2_768 . ?
O7 Ho1 O3 145.24(16) . . ?
O12 Ho1 O3 69.27(15) . . ?
O4 Ho1 O3 53.05(14) . . ?
O11 Ho1 N1 147.14(15) 2_768 . ?
O7 Ho1 N1 84.84(16) . . ?
O12 Ho1 N1 74.16(16) . . ?
O4 Ho1 N1 84.95(15) . . ?
O3 Ho1 N1 129.75(15) . . ?
O11 Ho1 N3 77.70(16) 2_768 . ?
O7 Ho1 N3 83.95(16) . . ?
O12 Ho1 N3 140.12(16) . . ?
O4 Ho1 N3 75.87(15) . . ?
O3 Ho1 N3 71.71(15) . . ?
N1 Ho1 N3 128.70(16) . . ?
O11 Ho1 N2 134.54(15) 2_768 . ?
O7 Ho1 N2 73.36(15) . . ?
O12 Ho1 N2 127.23(15) . . ?
O4 Ho1 N2 71.04(14) . . ?
O3 Ho1 N2 115.13(14) . . ?
N1 Ho1 N2 64.24(16) . . ?
N3 Ho1 N2 64.57(17) . . ?
O11 Ho1 OW1 73.59(15) 2_768 . ?
O7 Ho1 OW1 65.69(15) . . ?
O12 Ho1 OW1 69.94(15) . . ?
O4 Ho1 OW1 142.25(15) . . ?
O3 Ho1 OW1 121.39(15) . . ?
N1 Ho1 OW1 73.76(16) . . ?
N3 Ho1 OW1 141.47(16) . . ?
N2 Ho1 OW1 122.84(16) . . ?
O11 Ho1 C21 98.50(17) 2_768 1_655 ?
O7 Ho1 C21 156.08(16) . 1_655 ?
O12 Ho1 C21 69.21(16) . 1_655 ?
O4 Ho1 C21 26.55(15) . 1_655 ?
O3 Ho1 C21 26.51(15) . 1_655 ?
N1 Ho1 C21 107.73(17) . 1_655 ?
N3 Ho1 C21 72.29(16) . 1_655 ?
N2 Ho1 C21 93.46(16) . 1_655 ?
OW1 Ho1 C21 136.71(16) . 1_655 ?
C38 S2 C41 91.6(3) . . ?
C17 S1 C20 91.6(3) . . ?
C47 S3 C44 91.9(3) . . ?
C21 O3 Ho1 92.0(4) 1_655 . ?
C37 O6 Ho2 92.7(4) . . ?
C21 O4 Ho1 93.3(3) 1_655 . ?
C48 O11 Ho1 162.1(4) . 2_768 ?
C48 O12 Ho1 133.6(4) . . ?
C42 O7 Ho1 142.3(4) . . ?
C10 N2 C6 119.3(5) . . ?
C10 N2 Ho1 119.5(4) . . ?
C6 N2 Ho1 120.5(4) . . ?
C43 O9 Ho2 149.0(4) . . ?
C37 O5 Ho2 92.0(4) . . ?
C32 N6 C36 117.7(6) . . ?
C32 N6 Ho2 121.5(4) . . ?
C36 N6 Ho2 120.5(4) . . ?
C43 O10 Ho2 162.3(4) 2_667 . ?
C11 N3 C15 116.4(5) . . ?
C11 N3 Ho1 121.0(4) . . ?
C15 N3 Ho1 122.3(4) . . ?
C27 N5 C31 117.9(5) . . ?
C27 N5 Ho2 121.7(4) . . ?
C31 N5 Ho2 120.1(4) . . ?
O9 C43 O10 123.4(6) . 2_667 ?
O9 C43 C44 119.3(5) . . ?
O10 C43 C44 117.2(5) 2_667 . ?
C1 N1 C5 117.5(5) . . ?
C1 N1 Ho1 121.0(4) . . ?
C5 N1 Ho1 121.5(4) . . ?
C22 N4 C26 116.8(5) . . ?
C22 N4 Ho2 122.3(4) . . ?
C26 N4 Ho2 121.0(4) . . ?
C11 C12 C13 119.0(7) . . ?
C16 O1 Ho2 146.3(5) . . ?
O8 C42 O7 127.1(6) . . ?
O8 C42 C41 118.4(6) . 1_556 ?
O7 C42 C41 114.5(6) . 1_556 ?
C46 C47 C48 128.5(6) . . ?
C46 C47 S3 108.4(5) . . ?
C48 C47 S3 123.1(4) . . ?
C45 C44 C43 127.8(6) . . ?
C45 C44 S3 109.8(5) . . ?
C43 C44 S3 122.4(4) . . ?
C8 C7 C6 118.7(7) . . ?
N2 C6 C7 121.6(6) . . ?
N2 C6 C5 117.3(5) . . ?
C7 C6 C5 121.1(6) . . ?
N6 C32 C33 121.3(6) . . ?
N6 C32 C31 116.5(5) . . ?
C33 C32 C31 122.2(6) . . ?
N5 C27 C28 122.2(6) . . ?
N5 C27 C26 116.6(5) . . ?
C28 C27 C26 121.1(6) . . ?
O3 C21 O4 121.6(5) 1_455 1_455 ?
O3 C21 C20 119.0(6) 1_455 . ?
O4 C21 C20 119.4(5) 1_455 . ?
O3 C21 Ho1 61.5(3) 1_455 1_455 ?
O4 C21 Ho1 60.1(3) 1_455 1_455 ?
C20 C21 Ho1 179.3(4) . 1_455 ?
O11 C48 O12 126.3(5) . . ?
O11 C48 C47 117.2(5) . . ?
O12 C48 C47 116.5(5) . . ?
N2 C10 C9 121.6(7) . . ?
N2 C10 C11 117.8(5) . . ?
C9 C10 C11 120.6(6) . . ?
C19 C20 C21 127.9(6) . . ?
C19 C20 S1 112.0(5) . . ?
C21 C20 S1 120.1(5) . . ?
C39 C38 C37 127.8(6) . . ?
C39 C38 S2 111.6(5) . . ?
C37 C38 S2 120.6(5) . . ?
N3 C11 C12 122.5(7) . . ?
N3 C11 C10 115.9(5) . . ?
C12 C11 C10 121.6(6) . . ?
C40 C41 C42 129.8(6) . 1_554 ?
C40 C41 S2 111.8(5) . . ?
C42 C41 S2 118.4(5) 1_554 . ?
N4 C26 C25 121.6(6) . . ?
N4 C26 C27 116.3(5) . . ?
C25 C26 C27 122.1(6) . . ?
N1 C5 C4 121.8(6) . . ?
N1 C5 C6 115.9(5) . . ?
C4 C5 C6 122.4(6) . . ?
O2 C16 O1 126.3(6) . . ?
O2 C16 C17 118.6(6) . . ?
O1 C16 C17 115.1(6) . . ?
N5 C31 C30 122.2(6) . . ?
N5 C31 C32 116.3(5) . . ?
C30 C31 C32 121.5(6) . . ?
C14 C13 C12 118.5(6) . . ?
C20 C19 C18 112.2(6) . . ?
C35 C34 C33 119.6(7) . . ?
N1 C1 C2 123.1(7) . . ?
N3 C15 C14 124.2(7) . . ?
C18 C17 C16 129.7(6) . . ?
C18 C17 S1 111.3(5) . . ?
C16 C17 S1 118.9(5) . . ?
C17 C18 C19 112.9(6) . . ?
C5 C4 C3 119.4(7) . . ?
C30 C29 C28 119.5(6) . . ?
C7 C8 C9 119.5(6) . . ?
C24 C25 C26 119.9(7) . . ?
C34 C33 C32 119.7(7) . . ?
C13 C14 C15 119.3(7) . . ?
C34 C35 C36 117.9(7) . . ?
O6 C37 O5 121.7(6) . . ?
O6 C37 C38 119.7(6) . . ?
O5 C37 C38 118.6(6) . . ?
O6 C37 Ho2 60.6(3) . . ?
O5 C37 Ho2 61.1(3) . . ?
C38 C37 Ho2 177.4(4) . . ?
C47 C46 C45 119.2(7) . . ?
C29 C30 C31 119.0(6) . . ?
C3 C2 C1 119.1(7) . . ?
N6 C36 C35 123.8(7) . . ?
C8 C9 C10 119.3(6) . . ?
C41 C40 C39 112.0(6) . . ?
C29 C28 C27 119.1(6) . . ?
C38 C39 C40 112.9(6) . . ?
N4 C22 C23 124.4(7) . . ?
C46 C45 C44 110.8(6) . . ?
C23 C24 C25 118.9(7) . . ?
C2 C3 C4 119.2(7) . . ?
C22 C23 C24 118.4(7) . . ?

_refine_diff_density_max         2.903
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.184

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_8
_database_code_depnum_ccdc_archive 'CCDC 1410410'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Er2 N6 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            'Light Pink'

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1347.49

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2143(6)
_cell_length_b                   14.1588(7)
_cell_length_c                   16.1350(8)
_cell_angle_alpha                109.045(9)
_cell_angle_beta                 94.266(8)
_cell_angle_gamma                99.948(9)
_cell_volume                     2361.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    51617
_cell_measurement_theta_min      4.799
_cell_measurement_theta_max      60.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_F_000             1316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.738
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'TWINABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25678
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.348
_diffrn_reflns_theta_max         30.394
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13324
_reflns_number_gt                10390
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0260P)²+18.7071P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13324
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.93220(2) 0.79345(2) 0.95547(2) 0.01489(6) Uani 1 1 d . . . . .
Er2 Er 1.40944(2) 0.79593(2) 1.44660(2) 0.01490(6) Uani 1 1 d . . . . .
S2 S 0.92227(12) 0.70856(11) 1.41349(10) 0.0250(3) Uani 1 1 d . . . . .
S1 S 1.44484(12) 0.71296(12) 0.91063(10) 0.0258(3) Uani 1 1 d . . . . .
S3 S 1.22035(13) 0.93993(11) 1.23795(10) 0.0246(3) Uani 1 1 d . . . . .
O5 O 1.2495(3) 0.8799(3) 1.5104(3) 0.0306(10) Uani 1 1 d . . . . .
O2 O 0.7151(3) 0.7350(3) 0.9062(3) 0.0277(9) Uani 1 1 d . . . . .
O12 O 1.3880(4) 0.9068(3) 1.3751(3) 0.0294(9) Uani 1 1 d . . . . .
N5 N 1.3775(4) 0.6058(3) 1.4039(3) 0.0208(9) Uani 1 1 d . . . . .
O11 O 1.4933(4) 1.0674(3) 1.4332(3) 0.0253(8) Uani 1 1 d . . . . .
O9 O 1.0352(4) 0.9166(3) 1.0851(3) 0.0250(8) Uani 1 1 d . . . . .
N2 N 0.8915(4) 0.6015(3) 0.9062(3) 0.0199(9) Uani 1 1 d . . . . .
O7 O 1.6050(4) 0.7803(4) 1.4539(3) 0.0433(13) Uani 1 1 d . . . . .
O10 O 0.9335(4) 0.9183(3) 0.8994(3) 0.0279(9) Uani 1 1 d . . . . .
O1 O 0.7718(4) 0.8774(3) 1.0204(3) 0.0326(10) Uani 1 1 d . . . . .
O4 O 1.1781(4) 0.6356(4) 0.8769(3) 0.0347(10) Uani 1 1 d . . . . .
N4 N 1.3574(4) 0.7295(4) 1.5672(3) 0.0244(10) Uani 1 1 d . . . . .
O3 O 1.1269(4) 0.7787(4) 0.9576(3) 0.0403(12) Uani 1 1 d . . . . .
N6 N 1.4255(4) 0.7005(4) 1.2865(3) 0.0262(10) Uani 1 1 d . . . . .
O6 O 1.1926(3) 0.7299(3) 1.4043(3) 0.0274(9) Uani 1 1 d . . . . .
O8 O 1.6553(4) 0.6323(3) 1.3799(3) 0.0365(11) Uani 1 1 d . . . . .
N3 N 0.9446(4) 0.7008(4) 0.7931(3) 0.0244(10) Uani 1 1 d . . . . .
C48 C 1.4120(5) 0.9990(4) 1.3797(3) 0.0179(10) Uani 1 1 d . . . . .
N1 N 0.8777(5) 0.7207(4) 1.0723(3) 0.0284(11) Uani 1 1 d . . . . .
C47 C 1.3377(5) 1.0262(4) 1.3142(4) 0.0207(11) Uani 1 1 d . . . . .
C43 C 1.0903(4) 1.0073(4) 1.1200(3) 0.0171(10) Uani 1 1 d . . . . .
C20 C 1.3347(5) 0.7774(5) 0.9548(4) 0.0271(12) Uani 1 1 d . . . . .
C10 C 0.9039(5) 0.5432(4) 0.8238(4) 0.0219(11) Uani 1 1 d . . . . .
C44 C 1.1915(5) 1.0312(4) 1.1943(4) 0.0218(11) Uani 1 1 d . . . . .
C37 C 1.1659(5) 0.8064(4) 1.4616(4) 0.0226(11) Uani 1 1 d . . . . .
C32 C 1.4139(5) 0.5980(4) 1.2570(4) 0.0250(12) Uani 1 1 d . . . . .
C31 C 1.3906(5) 0.5463(4) 1.3232(4) 0.0243(12) Uani 1 1 d . . . . .
C6 C 0.8634(5) 0.5542(4) 0.9645(4) 0.0245(12) Uani 1 1 d . . . . .
C41 C 1.8127(5) 0.7743(5) 1.4571(4) 0.0256(12) Uani 1 1 d . . . . .
C5 C 0.8439(5) 0.6201(5) 1.0534(4) 0.0260(12) Uani 1 1 d . . . . .
C26 C 1.3370(5) 0.6284(5) 1.5533(4) 0.0256(12) Uani 1 1 d . . . . .
C42 C 1.6818(5) 0.7231(5) 1.4272(4) 0.0247(12) Uani 1 1 d . . . . .
C9 C 0.8933(6) 0.4379(5) 0.7986(5) 0.0337(14) Uani 1 1 d . . . . .
H9 H 0.9004 0.3993 0.7409 0.040 Uiso 1 1 calc R U . . .
C11 C 0.9297(5) 0.5989(5) 0.7614(4) 0.0250(12) Uani 1 1 d . . . . .
C28 C 1.3532(7) 0.4579(5) 1.4480(5) 0.0381(16) Uani 1 1 d . . . . .
H28 H 1.3422 0.4293 1.4919 0.046 Uiso 1 1 calc R U . . .
C27 C 1.3561(5) 0.5620(4) 1.4661(4) 0.0257(12) Uani 1 1 d . . . . .
C38 C 1.0380(5) 0.8107(4) 1.4721(4) 0.0232(11) Uani 1 1 d . . . . .
C17 C 0.5600(5) 0.8144(5) 0.9734(4) 0.0241(11) Uani 1 1 d . . . . .
C29 C 1.3668(7) 0.3989(5) 1.3642(5) 0.047(2) Uani 1 1 d . . . . .
H29 H 1.3647 0.3295 1.3510 0.057 Uiso 1 1 calc R U . . .
C21 C 1.2029(5) 0.7246(5) 0.9266(4) 0.0259(12) Uani 1 1 d . . . . .
C15 C 0.9697(6) 0.7525(6) 0.7381(4) 0.0353(15) Uani 1 1 d . . . . .
H15 H 0.9813 0.8233 0.7602 0.042 Uiso 1 1 calc R U . . .
C16 C 0.6887(5) 0.8089(5) 0.9664(4) 0.0232(11) Uani 1 1 d . . . . .
C36 C 1.4517(7) 0.7497(6) 1.2293(5) 0.0418(17) Uani 1 1 d . . . . .
H36 H 1.4604 0.8204 1.2488 0.050 Uiso 1 1 calc R U . . .
C39 C 0.9931(6) 0.8905(5) 1.5229(5) 0.0352(15) Uani 1 1 d . . . . .
H39 H 1.0425 0.9520 1.5596 0.042 Uiso 1 1 calc R U . . .
C45 C 1.2694(6) 1.1223(5) 1.2363(4) 0.0314(14) Uani 1 1 d . . . . .
H45 H 1.2679 1.1802 1.2211 0.038 Uiso 1 1 calc R U . . .
C22 C 1.3386(6) 0.7922(6) 1.6461(4) 0.0349(14) Uani 1 1 d . . . . .
H22 H 1.3527 0.8620 1.6562 0.042 Uiso 1 1 calc R U . . .
C30 C 1.3834(6) 0.4420(5) 1.3002(5) 0.0383(16) Uani 1 1 d . . . . .
H30 H 1.3897 0.4022 1.2427 0.046 Uiso 1 1 calc R U . . .
C35 C 1.4663(8) 0.6993(7) 1.1425(5) 0.0489(19) Uani 1 1 d . . . . .
H35 H 1.4857 0.7357 1.1049 0.059 Uiso 1 1 calc R U . . .
C13 C 0.9591(8) 0.6005(7) 0.6165(5) 0.052(2) Uani 1 1 d . . . . .
H13 H 0.9622 0.5670 0.5569 0.062 Uiso 1 1 calc R U . . .
C33 C 1.4254(7) 0.5430(6) 1.1702(5) 0.0420(17) Uani 1 1 d . . . . .
H33 H 1.4154 0.4723 1.1510 0.050 Uiso 1 1 calc R U . . .
C1 C 0.8628(7) 0.7825(6) 1.1523(4) 0.0385(16) Uani 1 1 d . . . . .
H1 H 0.8880 0.8527 1.1665 0.046 Uiso 1 1 calc R U . . .
C40 C 0.8646(5) 0.8706(5) 1.5144(5) 0.0383(16) Uani 1 1 d . . . . .
H40 H 0.8200 0.9175 1.5442 0.046 Uiso 1 1 calc R U . . .
C8 C 0.8720(7) 0.3917(5) 0.8613(5) 0.0400(16) Uani 1 1 d . . . . .
H8 H 0.8688 0.3221 0.8470 0.048 Uiso 1 1 calc R U . . .
C24 C 1.2793(7) 0.6553(7) 1.6978(5) 0.0460(18) Uani 1 1 d . . . . .
H24 H 1.2536 0.6301 1.7415 0.055 Uiso 1 1 calc R U . . .
C19 C 1.3850(6) 0.8713(5) 1.0152(5) 0.0380(16) Uani 1 1 d . . . . .
H19 H 1.3392 0.9165 1.0460 0.046 Uiso 1 1 calc R U . . .
C25 C 1.2977(7) 0.5894(6) 1.6175(5) 0.0416(17) Uani 1 1 d . . . . .
H25 H 1.2840 0.5195 1.6065 0.050 Uiso 1 1 calc R U . . .
C14 C 0.9793(7) 0.7054(6) 0.6502(4) 0.0430(17) Uani 1 1 d . . . . .
H14 H 0.9991 0.7438 0.6143 0.052 Uiso 1 1 calc R U . . .
C46 C 1.3525(6) 1.1203(5) 1.3050(4) 0.0342(15) Uani 1 1 d . . . . .
H46 H 1.4113 1.1768 1.3405 0.041 Uiso 1 1 calc R U . . .
C18 C 0.5134(5) 0.8928(5) 1.0262(5) 0.0349(15) Uani 1 1 d . . . . .
H18 H 0.5617 0.9536 1.0651 0.042 Uiso 1 1 calc R U . . .
C12 C 0.9338(6) 0.5451(6) 0.6726(4) 0.0393(16) Uani 1 1 d . . . . .
H12 H 0.9200 0.4741 0.6513 0.047 Uiso 1 1 calc R U . . .
C4 C 0.7912(6) 0.5785(6) 1.1124(5) 0.0382(15) Uani 1 1 d . . . . .
H4 H 0.7680 0.5080 1.0974 0.046 Uiso 1 1 calc R U . . .
C23 C 1.2994(7) 0.7580(6) 1.7125(5) 0.0442(17) Uani 1 1 d . . . . .
H23 H 1.2870 0.8036 1.7659 0.053 Uiso 1 1 calc R U . . .
C2 C 0.8117(8) 0.7465(6) 1.2147(5) 0.0472(19) Uani 1 1 d . . . . .
H2 H 0.8031 0.7913 1.2697 0.057 Uiso 1 1 calc R U . . .
C7 C 0.8557(6) 0.4491(5) 0.9438(5) 0.0363(15) Uani 1 1 d . . . . .
H7 H 0.8397 0.4188 0.9861 0.044 Uiso 1 1 calc R U . . .
C34 C 1.4519(8) 0.5955(7) 1.1129(5) 0.052(2) Uani 1 1 d . . . . .
H34 H 1.4599 0.5603 1.0546 0.063 Uiso 1 1 calc R U . . .
C3 C 0.7740(8) 0.6424(7) 1.1929(5) 0.0483(19) Uani 1 1 d . . . . .
H3 H 0.7372 0.6158 1.2326 0.058 Uiso 1 1 calc R U . . .
OW1 O 0.2919(10) 0.0565(7) 0.6574(7) 0.136(4) Uani 1 1 d . . . . .
OW2 O 0.2114(13) 0.9701(10) 0.8082(11) 0.233(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
Er1 O3 2.228(4) . ?
Er1 O10 2.231(4) . ?
Er1 O9 2.305(4) . ?
Er1 O2 2.414(4) . ?
Er1 O1 2.440(4) . ?
Er1 N1 2.492(5) . ?
Er1 N2 2.517(4) . ?
Er1 N3 2.545(5) . ?
Er1 C16 2.791(5) . ?
Er2 O7 2.240(4) . ?
Er2 O12 2.264(4) . ?
Er2 O11 2.281(4) 2_878 ?
Er2 O6 2.409(4) . ?
Er2 O5 2.430(4) . ?
Er2 N4 2.488(5) . ?
Er2 N5 2.504(5) . ?
Er2 N6 2.531(5) . ?
Er2 C37 2.784(5) . ?
S2 C38 1.717(6) . ?
S2 C41 1.722(5) 1_455 ?
S1 C20 1.721(6) . ?
S1 C17 1.723(6) 1_655 ?
S3 C47 1.720(5) . ?
S3 C44 1.725(5) . ?
O5 C37 1.264(7) . ?
O2 C16 1.270(7) . ?
O12 C48 1.262(6) . ?
N5 C31 1.336(7) . ?
N5 C27 1.355(7) . ?
O11 C48 1.244(6) . ?
O11 Er2 2.281(4) 2_878 ?
O9 C43 1.246(6) . ?
N2 C6 1.348(7) . ?
N2 C10 1.349(7) . ?
O7 C42 1.285(7) . ?
O10 C43 1.257(6) 2_777 ?
O1 C16 1.258(7) . ?
O4 C21 1.223(8) . ?
N4 C22 1.348(8) . ?
N4 C26 1.350(7) . ?
O3 C21 1.266(7) . ?
N6 C36 1.347(8) . ?
N6 C32 1.350(8) . ?
O6 C37 1.272(7) . ?
O8 C42 1.231(7) . ?
N3 C15 1.338(8) . ?
N3 C11 1.340(8) . ?
C48 C47 1.485(7) . ?
N1 C5 1.333(8) . ?
N1 C1 1.343(8) . ?
C47 C46 1.373(8) . ?
C43 O10 1.257(6) 2_777 ?
C43 C44 1.496(7) . ?
C20 C19 1.360(9) . ?
C20 C21 1.498(8) . ?
C10 C9 1.393(8) . ?
C10 C11 1.483(8) . ?
C44 C45 1.356(8) . ?
C37 C38 1.467(7) . ?
C32 C33 1.391(9) . ?
C32 C31 1.494(9) . ?
C31 C30 1.387(8) . ?
C6 C7 1.401(8) . ?
C6 C5 1.490(9) . ?
C41 C40 1.369(9) 1_655 ?
C41 C42 1.488(7) . ?
C41 S2 1.722(5) 1_655 ?
C5 C4 1.390(8) . ?
C26 C25 1.388(9) . ?
C26 C27 1.470(9) . ?
C9 C8 1.385(10) . ?
C9 H9 0.9300 . ?
C11 C12 1.395(8) . ?
C28 C29 1.373(11) . ?
C28 C27 1.400(8) . ?
C28 H28 0.9300 . ?
C38 C39 1.361(8) . ?
C17 C18 1.371(8) . ?
C17 C16 1.470(7) . ?
C17 S1 1.723(6) 1_455 ?
C29 C30 1.369(11) . ?
C29 H29 0.9300 . ?
C15 C14 1.378(9) . ?
C15 H15 0.9300 . ?
C36 C35 1.386(10) . ?
C36 H36 0.9300 . ?
C39 C40 1.407(8) . ?
C39 H39 0.9300 . ?
C45 C46 1.405(7) . ?
C45 H45 0.9300 . ?
C22 C23 1.383(9) . ?
C22 H22 0.9300 . ?
C30 H30 0.9300 . ?
C35 C34 1.365(12) . ?
C35 H35 0.9300 . ?
C13 C14 1.374(11) . ?
C13 C12 1.393(11) . ?
C13 H13 0.9300 . ?
C33 C34 1.380(11) . ?
C33 H33 0.9300 . ?
C1 C2 1.387(10) . ?
C1 H1 0.9300 . ?
C40 C41 1.369(9) 1_455 ?
C40 H40 0.9300 . ?
C8 C7 1.358(10) . ?
C8 H8 0.9300 . ?
C24 C23 1.369(11) . ?
C24 C25 1.382(11) . ?
C24 H24 0.9300 . ?
C19 C18 1.406(8) 1_655 ?
C19 H19 0.9300 . ?
C25 H25 0.9300 . ?
C14 H14 0.9300 . ?
C46 H46 0.9300 . ?
C18 C19 1.406(8) 1_455 ?
C18 H18 0.9300 . ?
C12 H12 0.9300 . ?
C4 C3 1.369(11) . ?
C4 H4 0.9300 . ?
C23 H23 0.9300 . ?
C2 C3 1.378(11) . ?
C2 H2 0.9300 . ?
C7 H7 0.9300 . ?
C34 H34 0.9300 . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Er1 O10 101.24(18) . . ?
O3 Er1 O9 74.23(16) . . ?
O10 Er1 O9 87.40(14) . . ?
O3 Er1 O2 154.50(16) . . ?
O10 Er1 O2 89.83(15) . . ?
O9 Er1 O2 129.71(14) . . ?
O3 Er1 O1 151.15(16) . . ?
O10 Er1 O1 76.21(16) . . ?
O9 Er1 O1 76.94(14) . . ?
O2 Er1 O1 53.78(14) . . ?
O3 Er1 N1 98.83(18) . . ?
O10 Er1 N1 149.29(17) . . ?
O9 Er1 N1 75.97(16) . . ?
O2 Er1 N1 81.69(16) . . ?
O1 Er1 N1 74.98(17) . . ?
O3 Er1 N2 83.25(16) . . ?
O10 Er1 N2 140.25(15) . . ?
O9 Er1 N2 130.96(14) . . ?
O2 Er1 N2 73.81(14) . . ?
O1 Er1 N2 117.41(15) . . ?
N1 Er1 N2 65.07(16) . . ?
O3 Er1 N3 77.29(16) . . ?
O10 Er1 N3 78.30(16) . . ?
O9 Er1 N3 144.83(15) . . ?
O2 Er1 N3 82.68(15) . . ?
O1 Er1 N3 128.74(15) . . ?
N1 Er1 N3 129.09(17) . . ?
N2 Er1 N3 64.06(16) . . ?
O3 Er1 C16 175.13(18) . . ?
O10 Er1 C16 82.63(16) . . ?
O9 Er1 C16 103.18(16) . . ?
O2 Er1 C16 27.02(15) . . ?
O1 Er1 C16 26.77(15) . . ?
N1 Er1 C16 76.45(17) . . ?
N2 Er1 C16 95.68(16) . . ?
N3 Er1 C16 106.55(16) . . ?
O7 Er2 O12 108.01(19) . . ?
O7 Er2 O11 75.94(16) . 2_878 ?
O12 Er2 O11 87.94(15) . 2_878 ?
O7 Er2 O6 153.39(16) . . ?
O12 Er2 O6 86.85(15) . . ?
O11 Er2 O6 127.80(14) 2_878 . ?
O7 Er2 O5 150.09(16) . . ?
O12 Er2 O5 74.97(16) . . ?
O11 Er2 O5 74.43(14) 2_878 . ?
O6 Er2 O5 54.10(14) . . ?
O7 Er2 N4 96.62(18) . . ?
O12 Er2 N4 149.07(16) . . ?
O11 Er2 N4 80.04(15) 2_878 . ?
O6 Er2 N4 78.55(15) . . ?
O5 Er2 N4 74.37(16) . . ?
O7 Er2 N5 80.70(16) . . ?
O12 Er2 N5 135.79(15) . . ?
O11 Er2 N5 135.34(14) 2_878 . ?
O6 Er2 N5 73.47(14) . . ?
O5 Er2 N5 118.68(15) . . ?
N4 Er2 N5 65.41(16) . . ?
O7 Er2 N6 77.86(17) . . ?
O12 Er2 N6 74.87(16) . . ?
O11 Er2 N6 142.23(16) 2_878 . ?
O6 Er2 N6 85.27(15) . . ?
O5 Er2 N6 129.93(15) . . ?
N4 Er2 N6 129.92(16) . . ?
N5 Er2 N6 64.58(16) . . ?
O7 Er2 C37 170.78(19) . . ?
O12 Er2 C37 80.36(17) . . ?
O11 Er2 C37 100.99(16) 2_878 . ?
O6 Er2 C37 27.13(15) . . ?
O5 Er2 C37 26.98(15) . . ?
N4 Er2 C37 74.22(16) . . ?
N5 Er2 C37 96.06(16) . . ?
N6 Er2 C37 108.67(16) . . ?
C38 S2 C41 91.6(3) . 1_455 ?
C20 S1 C17 91.4(3) . 1_655 ?
C47 S3 C44 91.5(3) . . ?
C37 O5 Er2 92.3(3) . . ?
C16 O2 Er1 93.2(3) . . ?
C48 O12 Er2 145.6(4) . . ?
C31 N5 C27 118.4(5) . . ?
C31 N5 Er2 121.9(4) . . ?
C27 N5 Er2 119.5(4) . . ?
C48 O11 Er2 161.9(4) . 2_878 ?
C43 O9 Er1 144.9(3) . . ?
C6 N2 C10 117.9(5) . . ?
C6 N2 Er1 119.8(4) . . ?
C10 N2 Er1 122.1(4) . . ?
C42 O7 Er2 147.2(4) . . ?
C43 O10 Er1 163.9(4) 2_777 . ?
C16 O1 Er1 92.4(3) . . ?
C22 N4 C26 117.8(5) . . ?
C22 N4 Er2 121.0(4) . . ?
C26 N4 Er2 120.9(4) . . ?
C21 O3 Er1 147.5(4) . . ?
C36 N6 C32 117.8(6) . . ?
C36 N6 Er2 121.7(4) . . ?
C32 N6 Er2 120.5(4) . . ?
C37 O6 Er2 93.1(3) . . ?
C15 N3 C11 118.4(5) . . ?
C15 N3 Er1 121.1(4) . . ?
C11 N3 Er1 120.4(4) . . ?
O11 C48 O12 125.4(5) . . ?
O11 C48 C47 118.1(5) . . ?
O12 C48 C47 116.5(5) . . ?
C5 N1 C1 118.0(5) . . ?
C5 N1 Er1 121.2(4) . . ?
C1 N1 Er1 120.0(4) . . ?
C46 C47 C48 125.9(5) . . ?
C46 C47 S3 111.1(4) . . ?
C48 C47 S3 123.0(4) . . ?
O9 C43 O10 126.1(5) . 2_777 ?
O9 C43 C44 117.3(5) . . ?
O10 C43 C44 116.6(5) 2_777 . ?
C19 C20 C21 129.5(5) . . ?
C19 C20 S1 111.7(4) . . ?
C21 C20 S1 118.7(5) . . ?
N2 C10 C9 122.5(6) . . ?
N2 C10 C11 115.5(5) . . ?
C9 C10 C11 122.1(5) . . ?
C45 C44 C43 127.0(5) . . ?
C45 C44 S3 111.5(4) . . ?
C43 C44 S3 121.5(4) . . ?
O5 C37 O6 120.4(5) . . ?
O5 C37 C38 119.0(5) . . ?
O6 C37 C38 120.6(5) . . ?
O5 C37 Er2 60.7(3) . . ?
O6 C37 Er2 59.8(3) . . ?
C38 C37 Er2 178.0(4) . . ?
N6 C32 C33 122.3(6) . . ?
N6 C32 C31 116.4(5) . . ?
C33 C32 C31 121.3(6) . . ?
N5 C31 C30 123.0(6) . . ?
N5 C31 C32 116.4(5) . . ?
C30 C31 C32 120.6(6) . . ?
N2 C6 C7 122.0(6) . . ?
N2 C6 C5 116.5(5) . . ?
C7 C6 C5 121.5(6) . . ?
C40 C41 C42 130.2(5) 1_655 . ?
C40 C41 S2 111.4(4) 1_655 1_655 ?
C42 C41 S2 118.4(4) . 1_655 ?
N1 C5 C4 122.2(6) . . ?
N1 C5 C6 116.3(5) . . ?
C4 C5 C6 121.5(6) . . ?
N4 C26 C25 121.5(6) . . ?
N4 C26 C27 116.4(5) . . ?
C25 C26 C27 122.1(6) . . ?
O8 C42 O7 125.5(5) . . ?
O8 C42 C41 119.3(5) . . ?
O7 C42 C41 115.1(5) . . ?
C8 C9 C10 118.6(6) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
N3 C11 C12 122.2(6) . . ?
N3 C11 C10 117.6(5) . . ?
C12 C11 C10 120.2(6) . . ?
C29 C28 C27 118.8(6) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
N5 C27 C28 121.3(6) . . ?
N5 C27 C26 117.3(5) . . ?
C28 C27 C26 121.4(6) . . ?
C39 C38 C37 128.1(5) . . ?
C39 C38 S2 111.3(4) . . ?
C37 C38 S2 120.6(4) . . ?
C18 C17 C16 128.4(6) . . ?
C18 C17 S1 111.2(4) . 1_455 ?
C16 C17 S1 120.3(4) . 1_455 ?
C30 C29 C28 120.1(6) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
O4 C21 O3 126.1(6) . . ?
O4 C21 C20 118.7(5) . . ?
O3 C21 C20 115.2(6) . . ?
N3 C15 C14 122.9(7) . . ?
N3 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
O1 C16 O2 120.6(5) . . ?
O1 C16 C17 119.6(5) . . ?
O2 C16 C17 119.8(5) . . ?
O1 C16 Er1 60.9(3) . . ?
O2 C16 Er1 59.7(3) . . ?
C17 C16 Er1 178.1(4) . . ?
N6 C36 C35 122.6(7) . . ?
N6 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?
C38 C39 C40 113.4(6) . . ?
C38 C39 H39 123.3 . . ?
C40 C39 H39 123.3 . . ?
C44 C45 C46 113.0(5) . . ?
C44 C45 H45 123.5 . . ?
C46 C45 H45 123.5 . . ?
N4 C22 C23 123.3(7) . . ?
N4 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C29 C30 C31 118.4(6) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
C34 C35 C36 119.0(7) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C14 C13 C12 119.3(7) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C34 C33 C32 118.7(7) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
N1 C1 C2 123.0(7) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C41 C40 C39 112.3(6) 1_455 . ?
C41 C40 H40 123.9 1_455 . ?
C39 C40 H40 123.9 . . ?
C7 C8 C9 119.5(6) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C23 C24 C25 119.3(6) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C20 C19 C18 112.9(6) . 1_655 ?
C20 C19 H19 123.5 . . ?
C18 C19 H19 123.5 1_655 . ?
C24 C25 C26 119.6(7) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C13 C14 C15 118.8(7) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C47 C46 C45 112.9(5) . . ?
C47 C46 H46 123.6 . . ?
C45 C46 H46 123.6 . . ?
C17 C18 C19 112.7(6) . 1_455 ?
C17 C18 H18 123.6 . . ?
C19 C18 H18 123.6 1_455 . ?
C13 C12 C11 118.2(7) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C3 C4 C5 119.2(7) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C24 C23 C22 118.4(7) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C3 C2 C1 118.0(7) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C8 C7 C6 119.4(6) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C35 C34 C33 119.7(7) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?

_refine_diff_density_max         1.121
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.208

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_9
_database_code_depnum_ccdc_archive 'CCDC 1410411'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 N6 O14 S3 Tm2'
_chemical_melting_point          ?
_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1350.83

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1911(7)
_cell_length_b                   14.1360(9)
_cell_length_c                   16.1242(10)
_cell_angle_alpha                108.997(11)
_cell_angle_beta                 94.492(10)
_cell_angle_gamma                99.700(12)
_cell_volume                     2353.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    34546
_cell_measurement_theta_min      4.340
_cell_measurement_theta_max      58.471
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.956
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6423
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34531
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.349
_diffrn_reflns_theta_max         29.235
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12575
_reflns_number_gt                11562
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0163P)²+1.1538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12575
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0165
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.56685(2) 0.20652(2) 0.54449(2) 0.01370(2) Uani 1 1 d . . . . .
Tm2 Tm -0.09124(2) -0.20428(2) -0.05342(2) 0.01348(2) Uani 1 1 d . . . . .
S1 S 1.05397(4) 0.28715(4) 0.58887(3) 0.02461(10) Uani 1 1 d . . . . .
S2 S -0.57827(4) -0.29195(4) -0.08663(3) 0.02364(9) Uani 1 1 d . . . . .
S3 S 0.27867(4) 0.06017(3) 0.26211(3) 0.02283(9) Uani 1 1 d . . . . .
O3 O 0.37298(13) 0.22175(13) 0.54195(11) 0.0391(4) Uani 1 1 d . . . . .
O7 O 0.10419(13) -0.21931(12) -0.04620(12) 0.0384(4) Uani 1 1 d . . . . .
O2 O 0.78329(12) 0.26512(11) 0.59412(9) 0.0264(3) Uani 1 1 d . . . . .
N6 N -0.07568(15) -0.29946(13) -0.21334(11) 0.0249(3) Uani 1 1 d . . . . .
O6 O -0.30751(12) -0.27043(11) -0.09605(9) 0.0268(3) Uani 1 1 d . . . . .
N3 N 0.55408(15) 0.29803(13) 0.70589(11) 0.0236(3) Uani 1 1 d . . . . .
C40 C 0.36371(19) -0.12971(17) 0.01399(16) 0.0351(5) Uani 1 1 d . . . . .
H40 H 0.3185 -0.0829 0.0434 0.042 Uiso 1 1 calc R U . . .
O9 O 0.46382(12) 0.08383(10) 0.41601(9) 0.0244(3) Uani 1 1 d . . . . .
C23 C -0.1991(2) -0.2407(2) 0.21266(16) 0.0429(6) Uani 1 1 d . . . . .
H23 H -0.2113 -0.1949 0.2661 0.051 Uiso 1 1 calc R U . . .
C19 C 1.11457(19) 0.12836(17) 0.48524(16) 0.0349(5) Uani 1 1 d . . . . .
H19 H 1.1607 0.0827 0.4553 0.042 Uiso 1 1 calc R U . . .
O11 O 0.00645(12) -0.06764(10) 0.06544(9) 0.0241(3) Uani 1 1 d . . . . .
N2 N 0.60808(13) 0.39807(11) 0.59320(10) 0.0192(3) Uani 1 1 d . . . . .
O5 O -0.25046(12) -0.12026(11) 0.00964(10) 0.0287(3) Uani 1 1 d . . . . .
O10 O 0.56595(13) 0.08125(10) 0.59981(9) 0.0251(3) Uani 1 1 d . . . . .
O12 O 0.11044(13) 0.09321(10) 0.12422(9) 0.0269(3) Uani 1 1 d . . . . .
C2 C 0.6866(3) 0.2520(2) 0.28538(16) 0.0456(6) Uani 1 1 d . . . . .
H2 H 0.6955 0.2067 0.2307 0.055 Uiso 1 1 calc R U . . .
C29 C -0.1355(3) -0.60096(17) -0.13509(18) 0.0453(6) Uani 1 1 d . . . . .
H29 H -0.1392 -0.6706 -0.1484 0.054 Uiso 1 1 calc R U . . .
N5 N -0.12223(13) -0.39372(11) -0.09537(10) 0.0190(3) Uani 1 1 d . . . . .
C35 C -0.0345(3) -0.3004(2) -0.35763(16) 0.0470(6) Uani 1 1 d . . . . .
H35 H -0.0152 -0.2638 -0.3951 0.056 Uiso 1 1 calc R U . . .
C25 C -0.2007(2) -0.40948(19) 0.11854(17) 0.0398(5) Uani 1 1 d . . . . .
H25 H -0.2136 -0.4794 0.1079 0.048 Uiso 1 1 calc R U . . .
C24 C -0.2193(3) -0.3434(2) 0.19814(17) 0.0464(6) Uani 1 1 d . . . . .
H24 H -0.2456 -0.3683 0.2418 0.056 Uiso 1 1 calc R U . . .
C13 C 0.5408(3) 0.3985(2) 0.88338(16) 0.0484(7) Uani 1 1 d . . . . .
H13 H 0.5386 0.4324 0.9431 0.058 Uiso 1 1 calc R U . . .
C15 C 0.5276(2) 0.24700(18) 0.76154(15) 0.0349(5) Uani 1 1 d . . . . .
H15 H 0.5135 0.1760 0.7392 0.042 Uiso 1 1 calc R U . . .
C8 C 0.6290(2) 0.60766(16) 0.63909(17) 0.0371(5) Uani 1 1 d . . . . .
H8 H 0.6342 0.6777 0.6540 0.044 Uiso 1 1 calc R U . . .
C4 C 0.7086(2) 0.42016(18) 0.38701(16) 0.0368(5) Uani 1 1 d . . . . .
H4 H 0.7329 0.4905 0.4018 0.044 Uiso 1 1 calc R U . . .
O1 O 0.72689(12) 0.12214(11) 0.47946(10) 0.0316(3) Uani 1 1 d . . . . .
C3 C 0.7248(2) 0.3552(2) 0.30599(16) 0.0437(6) Uani 1 1 d . . . . .
H3 H 0.7612 0.3811 0.2658 0.052 Uiso 1 1 calc R U . . .
N4 N -0.14149(15) -0.26923(12) 0.06787(11) 0.0243(3) Uani 1 1 d . . . . .
C34 C -0.0489(3) -0.4046(2) -0.38682(16) 0.0509(7) Uani 1 1 d . . . . .
H34 H -0.0411 -0.4401 -0.4452 0.061 Uiso 1 1 calc R U . . .
C30 C -0.1184(2) -0.55818(16) -0.19950(16) 0.0364(5) Uani 1 1 d . . . . .
H30 H -0.1126 -0.5985 -0.2569 0.044 Uiso 1 1 calc R U . . .
C47 C 0.30872(16) -0.03067(13) 0.30607(12) 0.0189(3) Uani 1 1 d . . . . .
O4 O 0.32028(13) 0.36530(12) 0.62305(11) 0.0336(3) Uani 1 1 d . . . . .
N1 N 0.61999(16) 0.27796(13) 0.42734(11) 0.0263(3) Uani 1 1 d . . . . .
C45 C 0.1480(2) -0.11997(15) 0.19445(14) 0.0326(5) Uani 1 1 d . . . . .
H45 H 0.0895 -0.1765 0.1586 0.039 Uiso 1 1 calc R U . . .
OW1 O 0.2068(3) 0.9439(2) 0.8431(2) 0.1197(12) Uani 1 1 d . . . . .
C37 C -0.33356(16) -0.19389(15) -0.03916(13) 0.0212(4) Uani 1 1 d . . . . .
C16 C 0.80952(16) 0.19102(15) 0.53380(13) 0.0224(4) Uani 1 1 d . . . . .
C20 C 0.16456(17) 0.22313(16) 0.54467(14) 0.0246(4) Uani 1 1 d . . . . .
C14 C 0.5202(3) 0.2944(2) 0.85039(16) 0.0453(6) Uani 1 1 d . . . . .
H14 H 0.5017 0.2561 0.8867 0.054 Uiso 1 1 calc R U . . .
O8 O 0.15547(13) -0.36724(11) -0.11989(11) 0.0343(3) Uani 1 1 d . . . . .
C5 C 0.65555(18) 0.37956(15) 0.44683(13) 0.0244(4) Uani 1 1 d . . . . .
C7 C 0.6443(2) 0.55005(16) 0.55555(16) 0.0333(5) Uani 1 1 d . . . . .
H7 H 0.6603 0.5804 0.5132 0.040 Uiso 1 1 calc R U . . .
C43 C 0.08770(16) 0.00122(13) 0.11921(11) 0.0171(3) Uani 1 1 d . . . . .
C41 C 0.31230(16) -0.22606(15) -0.04298(13) 0.0235(4) Uani 1 1 d . . . . .
C44 C 0.16174(16) -0.02658(13) 0.18527(12) 0.0196(3) Uani 1 1 d . . . . .
C6 C 0.63566(17) 0.44523(14) 0.53498(13) 0.0228(4) Uani 1 1 d . . . . .
C10 C 0.59511(16) 0.45533(14) 0.67573(13) 0.0219(4) Uani 1 1 d . . . . .
C42 C 0.18036(16) -0.27662(15) -0.07274(13) 0.0227(4) Uani 1 1 d . . . . .
C36 C -0.0494(2) -0.25130(19) -0.27100(15) 0.0379(5) Uani 1 1 d . . . . .
H36 H -0.0408 -0.1806 -0.2514 0.045 Uiso 1 1 calc R U . . .
C9 C 0.6057(2) 0.56121(16) 0.70104(15) 0.0324(5) Uani 1 1 d . . . . .
H9 H 0.5973 0.5996 0.7585 0.039 Uiso 1 1 calc R U . . .
C31 C -0.10987(17) -0.45304(14) -0.17707(13) 0.0226(4) Uani 1 1 d . . . . .
C48 C 0.40955(15) -0.00732(13) 0.38044(11) 0.0170(3) Uani 1 1 d . . . . .
C33 C -0.0748(2) -0.45647(19) -0.32955(15) 0.0404(6) Uani 1 1 d . . . . .
H33 H -0.0848 -0.5273 -0.3487 0.048 Uiso 1 1 calc R U . . .
C32 C -0.08595(17) -0.40155(15) -0.24231(13) 0.0236(4) Uani 1 1 d . . . . .
C27 C -0.14316(17) -0.43748(14) -0.03385(13) 0.0237(4) Uani 1 1 d . . . . .
C22 C -0.1601(2) -0.20646(18) 0.14630(14) 0.0334(5) Uani 1 1 d . . . . .
H22 H -0.1462 -0.1366 0.1564 0.040 Uiso 1 1 calc R U . . .
C28 C -0.1471(2) -0.54142(17) -0.05138(17) 0.0394(5) Uani 1 1 d . . . . .
H28 H -0.1574 -0.5696 -0.0071 0.047 Uiso 1 1 calc R U . . .
C11 C 0.56995(17) 0.40086(15) 0.73883(12) 0.0231(4) Uani 1 1 d . . . . .
C21 C 0.29655(16) 0.27584(16) 0.57327(13) 0.0233(4) Uani 1 1 d . . . . .
C1 C 0.6345(2) 0.21646(18) 0.34729(15) 0.0385(5) Uani 1 1 d . . . . .
H1 H 0.6083 0.1463 0.3327 0.046 Uiso 1 1 calc R U . . .
C26 C -0.16213(18) -0.37019(15) 0.05401(13) 0.0249(4) Uani 1 1 d . . . . .
C39 C -0.50674(18) -0.10899(17) 0.02330(16) 0.0334(5) Uani 1 1 d . . . . .
H39 H -0.4572 -0.0477 0.0604 0.040 Uiso 1 1 calc R U . . .
C17 C 0.93923(16) 0.18600(15) 0.52673(13) 0.0237(4) Uani 1 1 d . . . . .
C38 C -0.46266(16) -0.18968(15) -0.02866(13) 0.0224(4) Uani 1 1 d . . . . .
C46 C 0.23088(19) -0.12264(15) 0.26354(14) 0.0316(5) Uani 1 1 d . . . . .
H46 H 0.2325 -0.1806 0.2786 0.038 Uiso 1 1 calc R U . . .
C18 C 0.98487(18) 0.10677(17) 0.47387(16) 0.0337(5) Uani 1 1 d . . . . .
H18 H 0.9363 0.0460 0.4351 0.040 Uiso 1 1 calc R U . . .
C12 C 0.5647(2) 0.45320(19) 0.82752(15) 0.0384(5) Uani 1 1 d . . . . .
H12 H 0.5772 0.5242 0.8489 0.046 Uiso 1 1 calc R U . . .
OW2 O 0.7112(4) 0.9709(3) 0.3085(3) 0.210(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O3 2.2146(14) . ?
Tm1 O10 2.2260(13) . ?
Tm1 O9 2.2894(13) . ?
Tm1 O2 2.4046(13) . ?
Tm1 O1 2.4351(14) . ?
Tm1 N1 2.4814(16) . ?
Tm1 N2 2.5099(15) . ?
Tm1 N3 2.5289(16) . ?
Tm1 C16 2.7752(18) . ?
Tm2 O7 2.2305(14) . ?
Tm2 O12 2.2488(13) 2 ?
Tm2 O11 2.2692(13) . ?
Tm2 O6 2.4006(13) . ?
Tm2 O5 2.4145(13) . ?
Tm2 N4 2.4801(16) . ?
Tm2 N5 2.4941(15) . ?
Tm2 N6 2.5260(16) . ?
Tm2 C37 2.7637(17) . ?
S1 C17 1.716(2) . ?
S1 C20 1.7189(19) 1_655 ?
S2 C38 1.714(2) . ?
S2 C41 1.7192(19) 1_455 ?
S3 C47 1.7219(18) . ?
S3 C44 1.7226(18) . ?
O3 C21 1.268(2) . ?
O7 C42 1.277(2) . ?
O2 C16 1.271(2) . ?
N6 C32 1.346(2) . ?
N6 C36 1.342(3) . ?
O6 C37 1.265(2) . ?
N3 C11 1.350(2) . ?
N3 C15 1.343(3) . ?
C40 C41 1.367(3) . ?
C40 C39 1.416(3) 1_655 ?
O9 C48 1.249(2) . ?
C23 C24 1.369(4) . ?
C23 C22 1.381(3) . ?
C19 C20 1.362(3) 1_655 ?
C19 C18 1.416(3) . ?
O11 C43 1.247(2) . ?
N2 C6 1.343(2) . ?
N2 C10 1.347(2) . ?
O5 C37 1.262(2) . ?
O10 C48 1.252(2) 2_656 ?
O12 C43 1.257(2) . ?
O12 Tm2 2.2488(13) 2 ?
C2 C3 1.369(4) . ?
C2 C1 1.381(3) . ?
C29 C28 1.368(4) . ?
C29 C30 1.372(4) . ?
N5 C31 1.344(2) . ?
N5 C27 1.345(2) . ?
C35 C34 1.368(4) . ?
C35 C36 1.380(3) . ?
C25 C24 1.375(4) . ?
C25 C26 1.394(3) . ?
C13 C14 1.364(4) . ?
C13 C12 1.379(4) . ?
C15 C14 1.386(3) . ?
C8 C7 1.370(3) . ?
C8 C9 1.381(3) . ?
C4 C3 1.377(3) . ?
C4 C5 1.396(3) . ?
O1 C16 1.259(2) . ?
N4 C26 1.347(2) . ?
N4 C22 1.343(3) . ?
C34 C33 1.373(4) . ?
C30 C31 1.395(3) . ?
C47 C46 1.365(3) . ?
C47 C48 1.492(2) . ?
O4 C21 1.227(3) . ?
N1 C5 1.347(3) . ?
N1 C1 1.341(3) . ?
C45 C44 1.360(3) . ?
C45 C46 1.407(3) . ?
C37 C38 1.477(2) . ?
C16 C17 1.477(2) . ?
C20 C19 1.362(3) 1_455 ?
C20 C21 1.500(3) . ?
C20 S1 1.7189(19) 1_455 ?
O8 C42 1.228(2) . ?
C5 C6 1.481(3) . ?
C7 C6 1.393(3) . ?
C43 C44 1.490(2) . ?
C41 C42 1.494(2) . ?
C41 S2 1.7192(19) 1_655 ?
C10 C9 1.398(3) . ?
C10 C11 1.480(3) . ?
C31 C32 1.478(3) . ?
C48 O10 1.252(2) 2_656 ?
C33 C32 1.395(3) . ?
C27 C28 1.395(3) . ?
C27 C26 1.481(3) . ?
C11 C12 1.391(3) . ?
C39 C38 1.371(3) . ?
C39 C40 1.416(3) 1_455 ?
C17 C18 1.372(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
O3 Tm1 O10 101.44(6) . . ?
O3 Tm1 O9 74.12(6) . . ?
O10 Tm1 O9 86.89(5) . . ?
O3 Tm1 O2 154.23(5) . . ?
O10 Tm1 O2 90.01(5) . . ?
O9 Tm1 O2 130.06(5) . . ?
O3 Tm1 O1 150.98(5) . . ?
O10 Tm1 O1 76.04(5) . . ?
O9 Tm1 O1 76.86(5) . . ?
O2 Tm1 O1 54.17(5) . . ?
O3 Tm1 N1 98.59(6) . . ?
O10 Tm1 N1 148.81(5) . . ?
O9 Tm1 N1 75.88(5) . . ?
O2 Tm1 N1 81.93(6) . . ?
O1 Tm1 N1 74.84(6) . . ?
O3 Tm1 N2 83.40(6) . . ?
O10 Tm1 N2 140.67(5) . . ?
O9 Tm1 N2 131.12(5) . . ?
O2 Tm1 N2 73.39(5) . . ?
O1 Tm1 N2 117.21(5) . . ?
N1 Tm1 N2 65.18(5) . . ?
O3 Tm1 N3 77.24(6) . . ?
O10 Tm1 N3 78.44(5) . . ?
O9 Tm1 N3 144.39(5) . . ?
O2 Tm1 N3 82.66(5) . . ?
O1 Tm1 N3 128.95(5) . . ?
N1 Tm1 N3 129.63(5) . . ?
N2 Tm1 N3 64.47(5) . . ?
O3 Tm1 C16 174.95(6) . . ?
O10 Tm1 C16 82.64(5) . . ?
O9 Tm1 C16 103.32(6) . . ?
O2 Tm1 C16 27.21(5) . . ?
O1 Tm1 C16 26.97(5) . . ?
N1 Tm1 C16 76.47(6) . . ?
N2 Tm1 C16 95.36(5) . . ?
N3 Tm1 C16 106.68(6) . . ?
O7 Tm2 O12 106.96(6) . 2 ?
O7 Tm2 O11 75.68(5) . . ?
O12 Tm2 O11 87.09(5) 2 . ?
O7 Tm2 O6 153.44(5) . . ?
O12 Tm2 O6 87.68(5) 2 . ?
O11 Tm2 O6 128.24(5) . . ?
O7 Tm2 O5 150.02(5) . . ?
O12 Tm2 O5 75.27(5) 2 . ?
O11 Tm2 O5 74.59(5) . . ?
O6 Tm2 O5 54.34(5) . . ?
O7 Tm2 N4 96.74(6) . . ?
O12 Tm2 N4 149.31(5) 2 . ?
O11 Tm2 N4 80.05(5) . . ?
O6 Tm2 N4 78.94(5) . . ?
O5 Tm2 N4 74.48(5) . . ?
O7 Tm2 N5 80.90(6) . . ?
O12 Tm2 N5 136.30(5) 2 . ?
O11 Tm2 N5 135.49(5) . . ?
O6 Tm2 N5 73.41(5) . . ?
O5 Tm2 N5 118.83(5) . . ?
N4 Tm2 N5 65.66(5) . . ?
O7 Tm2 N6 77.90(6) . . ?
O12 Tm2 N6 74.80(5) 2 . ?
O11 Tm2 N6 141.79(5) . . ?
O6 Tm2 N6 85.06(5) . . ?
O5 Tm2 N6 129.75(5) . . ?
N4 Tm2 N6 130.40(5) . . ?
N5 Tm2 N6 64.80(5) . . ?
O7 Tm2 C37 171.15(6) . . ?
O12 Tm2 C37 81.00(6) 2 . ?
O11 Tm2 C37 101.34(5) . . ?
O6 Tm2 C37 27.20(5) . . ?
O5 Tm2 C37 27.16(5) . . ?
N4 Tm2 C37 74.48(6) . . ?
N5 Tm2 C37 96.06(5) . . ?
N6 Tm2 C37 108.44(6) . . ?
C17 S1 C20 91.56(10) . 1_655 ?
C38 S2 C41 91.58(9) . 1_455 ?
C47 S3 C44 91.68(9) . . ?
C21 O3 Tm1 147.49(14) . . ?
C42 O7 Tm2 146.77(14) . . ?
C16 O2 Tm1 92.86(11) . . ?
C32 N6 C36 117.29(18) . . ?
C32 N6 Tm2 120.19(13) . . ?
C36 N6 Tm2 122.38(14) . . ?
C37 O6 Tm2 92.61(11) . . ?
C11 N3 C15 117.26(17) . . ?
C11 N3 Tm1 120.80(13) . . ?
C15 N3 Tm1 121.90(14) . . ?
C41 C40 C39 112.63(18) . 1_655 ?
C48 O9 Tm1 145.39(12) . . ?
C24 C23 C22 118.6(2) . . ?
C20 C19 C18 112.82(18) 1_655 . ?
C43 O11 Tm2 162.43(13) . . ?
C6 N2 C10 118.53(16) . . ?
C6 N2 Tm1 120.08(12) . . ?
C10 N2 Tm1 121.24(12) . . ?
C37 O5 Tm2 92.02(11) . . ?
C48 O10 Tm1 164.02(13) 2_656 . ?
C43 O12 Tm2 145.92(12) . 2 ?
C3 C2 C1 118.7(2) . . ?
C28 C29 C30 120.2(2) . . ?
C31 N5 C27 118.72(16) . . ?
C31 N5 Tm2 121.29(12) . . ?
C27 N5 Tm2 119.82(12) . . ?
C34 C35 C36 118.1(2) . . ?
C24 C25 C26 119.1(2) . . ?
C23 C24 C25 119.5(2) . . ?
C14 C13 C12 119.5(2) . . ?
N3 C15 C14 123.6(2) . . ?
C7 C8 C9 119.7(2) . . ?
C3 C4 C5 119.5(2) . . ?
C16 O1 Tm1 91.75(11) . . ?
C2 C3 C4 119.1(2) . . ?
C26 N4 C22 117.85(18) . . ?
C26 N4 Tm2 120.60(13) . . ?
C22 N4 Tm2 121.26(14) . . ?
C35 C34 C33 119.7(2) . . ?
C29 C30 C31 118.6(2) . . ?
C46 C47 C48 126.63(16) . . ?
C46 C47 S3 111.34(13) . . ?
C48 C47 S3 122.02(13) . . ?
C5 N1 C1 117.78(18) . . ?
C5 N1 Tm1 120.70(13) . . ?
C1 N1 Tm1 120.53(14) . . ?
C44 C45 C46 113.40(17) . . ?
O6 C37 O5 120.98(16) . . ?
O6 C37 C38 120.14(17) . . ?
O5 C37 C38 118.89(17) . . ?
O6 C37 Tm2 60.19(9) . . ?
O5 C37 Tm2 60.82(9) . . ?
C38 C37 Tm2 177.84(14) . . ?
O1 C16 O2 121.19(17) . . ?
O1 C16 C17 119.35(18) . . ?
O2 C16 C17 119.46(17) . . ?
O1 C16 Tm1 61.29(10) . . ?
O2 C16 Tm1 59.93(9) . . ?
C17 C16 Tm1 177.80(14) . . ?
C19 C20 C21 129.48(18) 1_455 . ?
C19 C20 S1 111.71(14) 1_455 1_455 ?
C21 C20 S1 118.79(15) . 1_455 ?
C13 C14 C15 118.4(2) . . ?
N1 C5 C4 121.5(2) . . ?
N1 C5 C6 116.34(17) . . ?
C4 C5 C6 122.12(19) . . ?
C8 C7 C6 118.9(2) . . ?
O11 C43 O12 125.53(16) . . ?
O11 C43 C44 117.58(16) . . ?
O12 C43 C44 116.85(15) . . ?
C40 C41 C42 129.59(18) . . ?
C40 C41 S2 111.65(14) . 1_655 ?
C42 C41 S2 118.71(15) . 1_655 ?
C45 C44 C43 126.39(16) . . ?
C45 C44 S3 111.04(13) . . ?
C43 C44 S3 122.57(13) . . ?
N2 C6 C7 122.24(19) . . ?
N2 C6 C5 116.35(16) . . ?
C7 C6 C5 121.40(18) . . ?
N2 C10 C9 121.85(19) . . ?
N2 C10 C11 116.76(16) . . ?
C9 C10 C11 121.40(18) . . ?
O8 C42 O7 126.55(18) . . ?
O8 C42 C41 118.09(17) . . ?
O7 C42 C41 115.35(17) . . ?
N6 C36 C35 123.9(2) . . ?
C8 C9 C10 118.7(2) . . ?
N5 C31 C30 121.83(19) . . ?
N5 C31 C32 116.85(16) . . ?
C30 C31 C32 121.32(19) . . ?
O9 C48 O10 125.86(16) . 2_656 ?
O9 C48 C47 117.07(15) . . ?
O10 C48 C47 117.06(15) 2_656 . ?
C34 C33 C32 119.1(2) . . ?
N6 C32 C33 121.9(2) . . ?
N6 C32 C31 116.71(16) . . ?
C33 C32 C31 121.42(19) . . ?
N5 C27 C28 121.9(2) . . ?
N5 C27 C26 116.94(16) . . ?
C28 C27 C26 121.15(19) . . ?
N4 C22 C23 123.1(2) . . ?
C29 C28 C27 118.6(2) . . ?
N3 C11 C12 122.0(2) . . ?
N3 C11 C10 116.38(16) . . ?
C12 C11 C10 121.62(19) . . ?
O4 C21 O3 126.63(18) . . ?
O4 C21 C20 118.20(17) . . ?
O3 C21 C20 115.17(18) . . ?
N1 C1 C2 123.4(2) . . ?
N4 C26 C25 121.8(2) . . ?
N4 C26 C27 116.49(17) . . ?
C25 C26 C27 121.72(19) . . ?
C38 C39 C40 112.25(19) . 1_455 ?
C18 C17 C16 127.69(19) . . ?
C18 C17 S1 111.77(14) . . ?
C16 C17 S1 120.54(15) . . ?
C39 C38 C37 127.33(18) . . ?
C39 C38 S2 111.87(14) . . ?
C37 C38 S2 120.78(14) . . ?
C47 C46 C45 112.54(17) . . ?
C17 C18 C19 112.14(19) . . ?
C13 C12 C11 119.2(2) . . ?

_refine_diff_density_max         0.803
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_10
_database_code_depnum_ccdc_archive 'CCDC 1410412'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 N6 O14 S3 Yb2'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1359.05

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.165(5)
_cell_length_b                   14.113(7)
_cell_length_c                   16.117(8)
_cell_angle_alpha                108.934(7)
_cell_angle_beta                 94.613(6)
_cell_angle_gamma                99.554(6)
_cell_volume                     2344(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    61085
_cell_measurement_theta_min      4.833
_cell_measurement_theta_max      49.798
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_F_000             1324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    4.175
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5913
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'TWINABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27783
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.350
_diffrn_reflns_theta_max         28.850
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12232
_reflns_number_gt                9389
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0266P)²+24.1250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12232
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.43378(2) 0.79351(2) 0.95549(2) 0.01580(7) Uani 1 1 d . . . . .
Yb2 Yb 0.09123(2) 1.20448(2) 0.55356(2) 0.01542(7) Uani 1 1 d . . . . .
S2 S 0.57794(14) 1.29200(13) 0.58678(12) 0.0249(3) Uani 1 1 d . . . . .
S1 S -0.05293(15) 0.71289(13) 0.91122(12) 0.0258(4) Uani 1 1 d . . . . .
S3 S 0.27806(16) 1.06037(12) 0.76214(12) 0.0250(4) Uani 1 1 d . . . . .
O2 O 0.2186(4) 0.7354(4) 0.9064(3) 0.0273(11) Uani 1 1 d . . . . .
O1 O 0.2743(4) 0.8781(4) 1.0206(3) 0.0323(12) Uani 1 1 d . . . . .
O5 O 0.2500(4) 1.1202(4) 0.4907(3) 0.0309(12) Uani 1 1 d . . . . .
O6 O 0.3068(4) 1.2701(4) 0.5962(3) 0.0269(11) Uani 1 1 d . . . . .
O12 O 0.1088(5) 1.0931(3) 0.6233(3) 0.0282(11) Uani 1 1 d . . . . .
O10 O 0.4344(5) 0.9179(4) 0.9002(3) 0.0271(11) Uani 1 1 d . . . . .
N3 N 0.4465(5) 0.7028(4) 0.7945(4) 0.0249(12) Uani 1 1 d . . . . .
C18 C 0.0151(7) 0.8928(6) 1.0253(6) 0.0373(19) Uani 1 1 d . . . . .
H18 H 0.0637 0.9542 1.0632 0.045 Uiso 1 1 calc R U . . .
N2 N 0.3936(5) 0.6024(4) 0.9061(4) 0.0218(11) Uani 1 1 d . . . . .
O9 O 0.5370(4) 0.9161(3) 1.0831(3) 0.0242(10) Uani 1 1 d . . . . .
O4 O 0.6804(5) 0.6345(4) 0.8771(4) 0.0352(12) Uani 1 1 d . . . . .
N6 N 0.1405(5) 1.2685(4) 0.4328(4) 0.0247(12) Uani 1 1 d . . . . .
O11 O 0.0063(4) 0.9316(3) 0.5644(3) 0.0243(10) Uani 1 1 d . . . . .
C48 C 0.0873(6) 1.0006(5) 0.6178(4) 0.0201(13) Uani 1 1 d . . . . .
N4 N 0.0760(5) 1.2983(4) 0.7131(4) 0.0272(13) Uani 1 1 d . . . . .
O3 O 0.6268(4) 0.7779(4) 0.9585(4) 0.0400(14) Uani 1 1 d . . . . .
C3 C 0.2767(8) 0.6462(7) 1.1944(6) 0.042(2) Uani 1 1 d . . . . .
H3 H 0.2412 0.6207 1.2351 0.050 Uiso 1 1 calc R U . . .
C37 C 0.3326(6) 1.1939(5) 0.5398(5) 0.0239(14) Uani 1 1 d . . . . .
N1 N 0.3810(6) 0.7222(5) 1.0719(4) 0.0289(13) Uani 1 1 d . . . . .
C39 C 0.5066(6) 1.1082(6) 0.4768(5) 0.0325(17) Uani 1 1 d . . . . .
H39 H 0.4573 1.0468 0.4395 0.039 Uiso 1 1 calc R U . . .
C34 C 0.2181(8) 1.3429(7) 0.3012(6) 0.047(2) Uani 1 1 d . . . . .
H34 H 0.2431 1.3678 0.2573 0.056 Uiso 1 1 calc R U . . .
C20 C 0.8343(6) 0.7767(5) 0.9548(5) 0.0251(14) Uani 1 1 d . . . . .
C43 C 0.4095(6) 0.9932(5) 0.8808(4) 0.0183(12) Uani 1 1 d . . . . .
C24 C 0.0469(9) 1.4035(8) 0.8856(6) 0.051(2) Uani 1 1 d . . . . .
H24 H 0.0381 1.4387 0.9438 0.062 Uiso 1 1 calc R U . . .
C8 C 0.3717(7) 0.3922(6) 0.8587(6) 0.0347(18) Uani 1 1 d . . . . .
H8 H 0.3675 0.3221 0.8433 0.042 Uiso 1 1 calc R U . . .
C47 C 0.1621(6) 0.9729(5) 0.6851(4) 0.0207(13) Uani 1 1 d . . . . .
C44 C 0.3097(6) 0.9691(5) 0.8055(4) 0.0210(13) Uani 1 1 d . . . . .
C6 C 0.3637(6) 0.5548(5) 0.9653(5) 0.0249(14) Uani 1 1 d . . . . .
C10 C 0.4049(6) 0.5443(5) 0.8241(5) 0.0227(14) Uani 1 1 d . . . . .
C9 C 0.3942(7) 0.4388(6) 0.7989(5) 0.0343(17) Uani 1 1 d . . . . .
H9 H 0.4025 0.4007 0.7413 0.041 Uiso 1 1 calc R U . . .
C21 C 0.7037(6) 0.7238(5) 0.9268(5) 0.0245(14) Uani 1 1 d . . . . .
C46 C 0.1483(7) 0.8791(5) 0.6939(5) 0.0346(18) Uani 1 1 d . . . . .
H46 H 0.0901 0.8224 0.6579 0.042 Uiso 1 1 calc R U . . .
C26 C 0.0863(6) 1.4014(5) 0.7423(5) 0.0258(14) Uani 1 1 d . . . . .
C22 C 0.0486(8) 1.2500(7) 0.7702(5) 0.0379(18) Uani 1 1 d . . . . .
H22 H 0.0390 1.1792 0.7507 0.046 Uiso 1 1 calc R U . . .
C5 C 0.3448(6) 0.6211(5) 1.0531(5) 0.0251(14) Uani 1 1 d . . . . .
C16 C 0.1914(6) 0.8095(5) 0.9665(5) 0.0249(14) Uani 1 1 d . . . . .
C38 C 0.4628(6) 1.1897(5) 0.5298(4) 0.0218(13) Uani 1 1 d . . . . .
C35 C 0.1981(8) 1.2395(7) 0.2875(6) 0.045(2) Uani 1 1 d . . . . .
H35 H 0.2108 1.1933 0.2344 0.054 Uiso 1 1 calc R U . . .
C36 C 0.1591(8) 1.2058(6) 0.3539(5) 0.0354(17) Uani 1 1 d . . . . .
H36 H 0.1446 1.1359 0.3436 0.042 Uiso 1 1 calc R U . . .
C32 C 0.1624(6) 1.3694(5) 0.4458(5) 0.0252(14) Uani 1 1 d . . . . .
C11 C 0.4315(6) 0.6000(5) 0.7615(5) 0.0255(14) Uani 1 1 d . . . . .
C12 C 0.4371(8) 0.5482(6) 0.6731(5) 0.0394(19) Uani 1 1 d . . . . .
H12 H 0.4245 0.4771 0.6515 0.047 Uiso 1 1 calc R U . . .
C1 C 0.3674(8) 0.7847(6) 1.1528(5) 0.0395(19) Uani 1 1 d . . . . .
H1 H 0.3944 0.8548 1.1675 0.047 Uiso 1 1 calc R U . . .
C45 C 0.2313(7) 0.8772(6) 0.7632(5) 0.0353(18) Uani 1 1 d . . . . .
H45 H 0.2327 0.8194 0.7787 0.042 Uiso 1 1 calc R U . . .
C25 C 0.0736(8) 1.4565(7) 0.8281(5) 0.042(2) Uani 1 1 d . . . . .
H25 H 0.0827 1.5273 0.8468 0.050 Uiso 1 1 calc R U . . .
C17 C 0.0610(6) 0.8150(5) 0.9736(5) 0.0251(14) Uani 1 1 d . . . . .
C13 C 0.4615(9) 0.6030(8) 0.6177(6) 0.050(2) Uani 1 1 d . . . . .
H13 H 0.4645 0.5693 0.5580 0.060 Uiso 1 1 calc R U . . .
C33 C 0.2003(8) 1.4084(6) 0.3816(5) 0.0387(19) Uani 1 1 d . . . . .
H33 H 0.2136 1.4785 0.3927 0.046 Uiso 1 1 calc R U . . .
C15 C 0.4741(8) 0.7534(7) 0.7393(5) 0.0370(18) Uani 1 1 d . . . . .
H15 H 0.4894 0.8245 0.7619 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2910(8) 0.5808(6) 1.1131(5) 0.0381(19) Uani 1 1 d . . . . .
H4 H 0.2652 0.5105 1.0982 0.046 Uiso 1 1 calc R U . . .
C23 C 0.0337(9) 1.3001(8) 0.8566(6) 0.048(2) Uani 1 1 d . . . . .
H23 H 0.0150 1.2636 0.8944 0.057 Uiso 1 1 calc R U . . .
C2 C 0.3154(9) 0.7489(7) 1.2143(6) 0.047(2) Uani 1 1 d . . . . .
H2 H 0.3067 0.7943 1.2690 0.056 Uiso 1 1 calc R U . . .
C19 C -0.1135(7) 0.8712(6) 1.0158(6) 0.0365(18) Uani 1 1 d . . . . .
H19 H -0.1589 0.9165 1.0476 0.044 Uiso 1 1 calc R U . . .
C14 C 0.4813(9) 0.7068(7) 0.6507(5) 0.046(2) Uani 1 1 d . . . . .
H14 H 0.4991 0.7454 0.6145 0.056 Uiso 1 1 calc R U . . .
C7 C 0.3545(8) 0.4503(6) 0.9446(6) 0.0383(19) Uani 1 1 d . . . . .
H7 H 0.3375 0.4193 0.9864 0.046 Uiso 1 1 calc R U . . .
OW1 O 0.2068(9) 0.9438(8) 0.3441(8) 0.115(4) Uani 1 1 d . . . . .
C31 C 0.1434(6) 1.4368(5) 0.5329(5) 0.0263(15) Uani 1 1 d . . . . .
C27 C 0.1103(6) 1.4527(5) 0.6770(5) 0.0244(14) Uani 1 1 d . . . . .
C28 C 0.1190(8) 1.5577(5) 0.6990(6) 0.0371(19) Uani 1 1 d . . . . .
H28 H 0.1142 1.5978 0.7568 0.044 Uiso 1 1 calc R U . . .
C29 C 0.1342(8) 1.6008(6) 0.6371(6) 0.044(2) Uani 1 1 d . . . . .
H29 H 0.1347 1.6701 0.6505 0.053 Uiso 1 1 calc R U . . .
C30 C 0.1494(8) 1.5404(6) 0.5510(6) 0.043(2) Uani 1 1 d . . . . .
H30 H 0.1632 1.5696 0.5076 0.052 Uiso 1 1 calc R U . . .
O8 O -0.1559(5) 1.3673(4) 0.6199(4) 0.0362(13) Uani 1 1 d . . . . .
N5 N 0.1212(5) 1.3934(4) 0.5963(4) 0.0235(12) Uani 1 1 d . . . . .
C42 C -0.1806(6) 1.2767(5) 0.5728(5) 0.0246(14) Uani 1 1 d . . . . .
C41 C 0.6877(6) 1.2260(5) 0.5434(5) 0.0240(14) Uani 1 1 d . . . . .
C40 C 0.6366(7) 1.1303(6) 0.4867(6) 0.0368(19) Uani 1 1 d . . . . .
H40 H 0.6825 1.0838 0.4572 0.044 Uiso 1 1 calc R U . . .
O7 O -0.1036(4) 1.2196(4) 0.5469(4) 0.0377(13) Uani 1 1 d . . . . .
OW2 O 0.2898(13) 1.0265(10) 0.1944(11) 0.194(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O3 2.201(5) . ?
Yb1 O10 2.211(5) . ?
Yb1 O9 2.280(4) . ?
Yb1 O2 2.385(5) . ?
Yb1 O1 2.427(5) . ?
Yb1 N1 2.467(6) . ?
Yb1 N2 2.501(5) . ?
Yb1 N3 2.521(6) . ?
Yb1 C16 2.768(6) . ?
Yb2 O7 2.218(5) . ?
Yb2 O12 2.234(5) . ?
Yb2 O11 2.256(4) 2_576 ?
Yb2 O6 2.388(5) . ?
Yb2 O5 2.406(5) . ?
Yb2 N6 2.460(6) . ?
Yb2 N5 2.483(5) . ?
Yb2 N4 2.516(6) . ?
Yb2 C37 2.746(6) . ?
S2 C38 1.707(7) . ?
S2 C41 1.718(7) . ?
S1 C17 1.718(7) . ?
S1 C20 1.731(7) 1_455 ?
S3 C47 1.720(6) . ?
S3 C44 1.724(6) . ?
O2 C16 1.272(8) . ?
O1 C16 1.256(8) . ?
O5 C37 1.261(8) . ?
O6 C37 1.255(8) . ?
O12 C48 1.259(8) . ?
O10 C43 1.266(7) . ?
N3 C15 1.335(10) . ?
N3 C11 1.348(9) . ?
C18 C17 1.351(10) . ?
C18 C19 1.403(10) . ?
C18 H18 0.9300 . ?
N2 C10 1.338(9) . ?
N2 C6 1.366(9) . ?
O9 C43 1.242(7) 2_677 ?
O4 C21 1.225(9) . ?
N6 C32 1.346(9) . ?
N6 C36 1.349(9) . ?
O11 C48 1.244(7) . ?
O11 Yb2 2.256(4) 2_576 ?
C48 C47 1.504(9) . ?
N4 C22 1.337(9) . ?
N4 C26 1.357(9) . ?
O3 C21 1.271(8) . ?
C3 C2 1.363(12) . ?
C3 C4 1.374(12) . ?
C3 H3 0.9300 . ?
C37 C38 1.485(9) . ?
N1 C5 1.341(9) . ?
N1 C1 1.352(10) . ?
C39 C38 1.381(9) . ?
C39 C40 1.418(10) . ?
C39 H39 0.9300 . ?
C34 C33 1.378(12) . ?
C34 C35 1.380(13) . ?
C34 H34 0.9300 . ?
C20 C19 1.372(10) 1_655 ?
C20 C21 1.484(9) . ?
C20 S1 1.731(7) 1_655 ?
C43 O9 1.242(7) 2_677 ?
C43 C44 1.489(8) . ?
C24 C23 1.359(13) . ?
C24 C25 1.388(13) . ?
C24 H24 0.9300 . ?
C8 C9 1.349(12) . ?
C8 C7 1.409(12) . ?
C8 H8 0.9300 . ?
C47 C46 1.362(9) . ?
C44 C45 1.366(9) . ?
C6 C7 1.387(10) . ?
C6 C5 1.475(10) . ?
C10 C9 1.392(10) . ?
C10 C11 1.487(10) . ?
C9 H9 0.9300 . ?
C46 C45 1.403(10) . ?
C46 H46 0.9300 . ?
C26 C25 1.381(10) . ?
C26 C27 1.476(10) . ?
C22 C23 1.380(11) . ?
C22 H22 0.9300 . ?
C5 C4 1.399(10) . ?
C16 C17 1.482(9) . ?
C35 C36 1.377(11) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C32 C33 1.385(10) . ?
C32 C31 1.473(10) . ?
C11 C12 1.387(10) . ?
C12 C13 1.374(12) . ?
C12 H12 0.9300 . ?
C1 C2 1.377(12) . ?
C1 H1 0.9300 . ?
C45 H45 0.9300 . ?
C25 H25 0.9300 . ?
C13 C14 1.359(13) . ?
C13 H13 0.9300 . ?
C33 H33 0.9300 . ?
C15 C14 1.380(11) . ?
C15 H15 0.9300 . ?
C4 H4 0.9300 . ?
C23 H23 0.9300 . ?
C2 H2 0.9300 . ?
C19 C20 1.373(10) 1_455 ?
C19 H19 0.9300 . ?
C14 H14 0.9300 . ?
C7 H7 0.9300 . ?
C31 N5 1.370(9) . ?
C31 C30 1.384(10) . ?
C27 N5 1.328(9) . ?
C27 C28 1.392(9) . ?
C28 C29 1.335(12) . ?
C28 H28 0.9300 . ?
C29 C30 1.413(13) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
O8 C42 1.227(9) . ?
C42 O7 1.277(8) . ?
C42 C41 1.490(9) 1_455 ?
C41 C40 1.358(10) . ?
C41 C42 1.490(9) 1_655 ?
C40 H40 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Yb1 O10 101.6(2) . . ?
O3 Yb1 O9 74.00(19) . . ?
O10 Yb1 O9 86.78(17) . . ?
O3 Yb1 O2 154.21(18) . . ?
O10 Yb1 O2 90.12(18) . . ?
O9 Yb1 O2 130.13(17) . . ?
O3 Yb1 O1 150.78(19) . . ?
O10 Yb1 O1 76.16(19) . . ?
O9 Yb1 O1 76.79(17) . . ?
O2 Yb1 O1 54.30(16) . . ?
O3 Yb1 N1 98.4(2) . . ?
O10 Yb1 N1 148.9(2) . . ?
O9 Yb1 N1 76.17(19) . . ?
O2 Yb1 N1 81.76(19) . . ?
O1 Yb1 N1 74.8(2) . . ?
O3 Yb1 N2 83.08(19) . . ?
O10 Yb1 N2 140.24(18) . . ?
O9 Yb1 N2 131.52(17) . . ?
O2 Yb1 N2 73.47(16) . . ?
O1 Yb1 N2 117.61(18) . . ?
N1 Yb1 N2 65.5(2) . . ?
O3 Yb1 N3 77.4(2) . . ?
O10 Yb1 N3 78.16(18) . . ?
O9 Yb1 N3 144.10(19) . . ?
O2 Yb1 N3 82.77(18) . . ?
O1 Yb1 N3 129.05(18) . . ?
N1 Yb1 N3 129.8(2) . . ?
N2 Yb1 N3 64.24(19) . . ?
O3 Yb1 C16 174.6(2) . . ?
O10 Yb1 C16 82.7(2) . . ?
O9 Yb1 C16 103.3(2) . . ?
O2 Yb1 C16 27.32(18) . . ?
O1 Yb1 C16 26.98(18) . . ?
N1 Yb1 C16 76.4(2) . . ?
N2 Yb1 C16 95.66(19) . . ?
N3 Yb1 C16 106.8(2) . . ?
O7 Yb2 O12 106.3(2) . . ?
O7 Yb2 O11 75.75(18) . 2_576 ?
O12 Yb2 O11 86.52(17) . 2_576 ?
O7 Yb2 O6 153.41(18) . . ?
O12 Yb2 O6 88.17(18) . . ?
O11 Yb2 O6 128.35(16) 2_576 . ?
O7 Yb2 O5 150.07(18) . . ?
O12 Yb2 O5 75.42(19) . . ?
O11 Yb2 O5 74.54(17) 2_576 . ?
O6 Yb2 O5 54.47(16) . . ?
O7 Yb2 N6 96.9(2) . . ?
O12 Yb2 N6 149.35(19) . . ?
O11 Yb2 N6 80.03(18) 2_576 . ?
O6 Yb2 N6 79.12(18) . . ?
O5 Yb2 N6 74.49(19) . . ?
O7 Yb2 N5 80.73(19) . . ?
O12 Yb2 N5 136.35(18) . . ?
O11 Yb2 N5 135.81(18) 2_576 . ?
O6 Yb2 N5 73.58(17) . . ?
O5 Yb2 N5 119.28(18) . . ?
N6 Yb2 N5 66.22(19) . . ?
O7 Yb2 N4 77.8(2) . . ?
O12 Yb2 N4 74.61(18) . . ?
O11 Yb2 N4 141.49(19) 2_576 . ?
O6 Yb2 N4 85.01(18) . . ?
O5 Yb2 N4 129.60(18) . . ?
N6 Yb2 N4 130.91(19) . . ?
N5 Yb2 N4 64.75(19) . . ?
O7 Yb2 C37 171.5(2) . . ?
O12 Yb2 C37 81.3(2) . . ?
O11 Yb2 C37 101.48(19) 2_576 . ?
O6 Yb2 C37 27.16(18) . . ?
O5 Yb2 C37 27.32(18) . . ?
N6 Yb2 C37 74.6(2) . . ?
N5 Yb2 C37 96.33(19) . . ?
N4 Yb2 C37 108.2(2) . . ?
C38 S2 C41 91.5(3) . . ?
C17 S1 C20 91.5(3) . 1_455 ?
C47 S3 C44 91.4(3) . . ?
C16 O2 Yb1 93.3(4) . . ?
C16 O1 Yb1 91.8(4) . . ?
C37 O5 Yb2 91.5(4) . . ?
C37 O6 Yb2 92.5(4) . . ?
C48 O12 Yb2 146.2(4) . . ?
C43 O10 Yb1 163.7(5) . . ?
C15 N3 C11 116.9(6) . . ?
C15 N3 Yb1 122.2(5) . . ?
C11 N3 Yb1 120.9(5) . . ?
C17 C18 C19 112.9(7) . . ?
C17 C18 H18 123.6 . . ?
C19 C18 H18 123.6 . . ?
C10 N2 C6 118.2(6) . . ?
C10 N2 Yb1 122.4(4) . . ?
C6 N2 Yb1 119.4(4) . . ?
C43 O9 Yb1 146.1(4) 2_677 . ?
C32 N6 C36 116.8(6) . . ?
C32 N6 Yb2 121.1(4) . . ?
C36 N6 Yb2 121.7(5) . . ?
C48 O11 Yb2 162.6(5) . 2_576 ?
O11 C48 O12 125.7(6) . . ?
O11 C48 C47 117.4(6) . . ?
O12 C48 C47 116.8(5) . . ?
C22 N4 C26 117.3(6) . . ?
C22 N4 Yb2 122.6(5) . . ?
C26 N4 Yb2 119.9(5) . . ?
C21 O3 Yb1 147.5(5) . . ?
C2 C3 C4 119.0(8) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
O6 C37 O5 121.5(6) . . ?
O6 C37 C38 119.9(6) . . ?
O5 C37 C38 118.7(6) . . ?
O6 C37 Yb2 60.3(3) . . ?
O5 C37 Yb2 61.2(3) . . ?
C38 C37 Yb2 178.0(5) . . ?
C5 N1 C1 117.6(6) . . ?
C5 N1 Yb1 121.1(5) . . ?
C1 N1 Yb1 120.3(5) . . ?
C38 C39 C40 111.2(6) . . ?
C38 C39 H39 124.4 . . ?
C40 C39 H39 124.4 . . ?
C33 C34 C35 118.5(8) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
C19 C20 C21 130.5(6) 1_655 . ?
C19 C20 S1 110.3(5) 1_655 1_655 ?
C21 C20 S1 119.0(5) . 1_655 ?
O9 C43 O10 126.0(6) 2_677 . ?
O9 C43 C44 117.6(5) 2_677 . ?
O10 C43 C44 116.4(5) . . ?
C23 C24 C25 119.8(8) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C9 C8 C7 119.6(7) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C46 C47 C48 126.0(6) . . ?
C46 C47 S3 111.6(5) . . ?
C48 C47 S3 122.4(5) . . ?
C45 C44 C43 127.0(6) . . ?
C45 C44 S3 111.2(5) . . ?
C43 C44 S3 121.9(5) . . ?
N2 C6 C7 121.7(7) . . ?
N2 C6 C5 116.3(6) . . ?
C7 C6 C5 121.9(7) . . ?
N2 C10 C9 122.6(7) . . ?
N2 C10 C11 115.6(6) . . ?
C9 C10 C11 121.8(6) . . ?
C8 C9 C10 119.4(7) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
O4 C21 O3 126.7(6) . . ?
O4 C21 C20 118.3(6) . . ?
O3 C21 C20 114.9(6) . . ?
C47 C46 C45 112.8(6) . . ?
C47 C46 H46 123.6 . . ?
C45 C46 H46 123.6 . . ?
N4 C26 C25 122.5(7) . . ?
N4 C26 C27 116.6(6) . . ?
C25 C26 C27 120.9(7) . . ?
N4 C22 C23 123.3(8) . . ?
N4 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
N1 C5 C4 121.8(7) . . ?
N1 C5 C6 116.4(6) . . ?
C4 C5 C6 121.8(7) . . ?
O1 C16 O2 120.5(6) . . ?
O1 C16 C17 119.4(6) . . ?
O2 C16 C17 120.0(6) . . ?
O1 C16 Yb1 61.2(3) . . ?
O2 C16 Yb1 59.4(3) . . ?
C17 C16 Yb1 178.0(5) . . ?
C39 C38 C37 126.9(6) . . ?
C39 C38 S2 112.2(5) . . ?
C37 C38 S2 120.9(5) . . ?
C36 C35 C34 118.7(8) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
N6 C36 C35 123.7(8) . . ?
N6 C36 H36 118.1 . . ?
C35 C36 H36 118.1 . . ?
N6 C32 C33 122.6(7) . . ?
N6 C32 C31 116.1(6) . . ?
C33 C32 C31 121.4(7) . . ?
N3 C11 C12 122.0(7) . . ?
N3 C11 C10 116.6(6) . . ?
C12 C11 C10 121.3(7) . . ?
C13 C12 C11 119.2(8) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
N1 C1 C2 122.9(8) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C44 C45 C46 113.0(6) . . ?
C44 C45 H45 123.5 . . ?
C46 C45 H45 123.5 . . ?
C26 C25 C24 118.3(8) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
C18 C17 C16 128.2(7) . . ?
C18 C17 S1 112.0(5) . . ?
C16 C17 S1 119.8(5) . . ?
C14 C13 C12 119.5(8) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C34 C33 C32 119.6(8) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
N3 C15 C14 124.1(8) . . ?
N3 C15 H15 118.0 . . ?
C14 C15 H15 118.0 . . ?
C3 C4 C5 119.4(7) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C24 C23 C22 118.8(8) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C3 C2 C1 119.4(8) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C20 C19 C18 113.3(7) 1_455 . ?
C20 C19 H19 123.4 1_455 . ?
C18 C19 H19 123.4 . . ?
C13 C14 C15 118.2(8) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C6 C7 C8 118.3(8) . . ?
C6 C7 H7 120.8 . . ?
C8 C7 H7 120.8 . . ?
N5 C31 C30 120.9(7) . . ?
N5 C31 C32 117.4(6) . . ?
C30 C31 C32 121.7(7) . . ?
N5 C27 C28 122.0(7) . . ?
N5 C27 C26 116.5(6) . . ?
C28 C27 C26 121.5(7) . . ?
C29 C28 C27 119.8(7) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 119.7(7) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 118.3(8) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C27 N5 C31 119.1(6) . . ?
C27 N5 Yb2 122.1(5) . . ?
C31 N5 Yb2 118.6(4) . . ?
O8 C42 O7 126.3(6) . . ?
O8 C42 C41 118.2(6) . 1_455 ?
O7 C42 C41 115.6(6) . 1_455 ?
C40 C41 C42 129.6(6) . 1_655 ?
C40 C41 S2 111.7(5) . . ?
C42 C41 S2 118.7(5) 1_655 . ?
C41 C40 C39 113.3(6) . . ?
C41 C40 H40 123.3 . . ?
C39 C40 H40 123.3 . . ?
C42 O7 Yb2 147.2(5) . . ?

_refine_diff_density_max         1.539
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.215

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Compound_11
_database_code_depnum_ccdc_archive 'CCDC 1410413'
_audit_update_record             
;
2015-07-02 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Lu2 N6 O14 S3'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1362.91

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1563(4)
_cell_length_b                   14.0857(5)
_cell_length_c                   16.1004(6)
_cell_angle_alpha                108.865(3)
_cell_angle_beta                 94.701(2)
_cell_angle_gamma                99.566(2)
_cell_volume                     2335.79(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31904
_cell_measurement_theta_min      4.841
_cell_measurement_theta_max      49.876
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    4.413
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6728
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31904
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.351
_diffrn_reflns_theta_max         27.837
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11080
_reflns_number_gt                8224
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11080
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0561
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Lu1 Lu 0.06594(2) 0.20645(2) 0.54456(2) 0.01399(6) Uani 1 1 d . . . . .
Lu2 Lu -0.40853(2) 0.20448(2) 0.05377(2) 0.01366(6) Uani 1 1 d . . . . .
S1 S -0.44721(11) 0.28696(10) 0.58875(9) 0.0254(3) Uani 1 1 d . . . . .
S2 S 0.07816(10) 0.29202(10) 0.08685(9) 0.0237(3) Uani 1 1 d . . . . .
S3 S -0.22225(11) 0.06054(9) 0.26238(8) 0.0225(3) Uani 1 1 d . . . . .
O9 O -0.0374(3) 0.0839(3) 0.4177(2) 0.0224(8) Uani 1 1 d . . . . .
O2 O 0.2815(3) 0.2648(3) 0.5942(2) 0.0249(8) Uani 1 1 d . . . . .
O6 O -0.1934(3) 0.2702(3) 0.0962(2) 0.0256(8) Uani 1 1 d . . . . .
C47 C -0.3384(4) -0.0270(4) 0.1846(3) 0.0180(10) Uani 1 1 d . . . . .
O5 O -0.2508(3) 0.1196(3) -0.0093(2) 0.0286(9) Uani 1 1 d . . . . .
C6 C 0.1354(4) 0.4441(4) 0.5349(3) 0.0223(11) Uani 1 1 d . . . . .
O8 O -0.6555(3) 0.3668(3) 0.1196(3) 0.0330(9) Uani 1 1 d . . . . .
O10 O 0.0656(3) 0.0821(3) 0.5994(2) 0.0229(8) Uani 1 1 d . . . . .
N3 N 0.0528(3) 0.2958(3) 0.7052(3) 0.0236(10) Uani 1 1 d . . . . .
O12 O -0.3908(3) 0.0937(2) 0.1236(2) 0.0255(8) Uani 1 1 d . . . . .
C23 C -0.3032(5) 0.2375(5) -0.2137(4) 0.0421(16) Uani 1 1 d . . . . .
H23 H -0.2920 0.1911 -0.2672 0.051 Uiso 1 1 calc R U . . .
C33 C -0.4266(5) 0.4554(5) 0.3285(4) 0.0415(16) Uani 1 1 d . . . . .
H33 H -0.4171 0.5263 0.3477 0.050 Uiso 1 1 calc R U . . .
N2 N 0.1074(3) 0.3972(3) 0.5937(3) 0.0174(9) Uani 1 1 d . . . . .
C2 C 0.1840(5) 0.2504(5) 0.2866(4) 0.0418(15) Uani 1 1 d . . . . .
H2 H 0.1934 0.2049 0.2322 0.050 Uiso 1 1 calc R U . . .
O11 O -0.4935(3) -0.0686(2) 0.0634(2) 0.0206(8) Uani 1 1 d . . . . .
C35 C -0.4667(5) 0.2984(5) 0.3565(4) 0.0436(16) Uani 1 1 d . . . . .
H35 H -0.4856 0.2612 0.3937 0.052 Uiso 1 1 calc R U . . .
N6 N -0.4239(3) 0.2990(3) 0.2126(3) 0.0227(9) Uani 1 1 d . . . . .
O7 O -0.6031(3) 0.2190(3) 0.0473(2) 0.0340(10) Uani 1 1 d . . . . .
N5 N -0.3787(3) 0.3924(3) 0.0950(3) 0.0184(9) Uani 1 1 d . . . . .
C12 C 0.0626(5) 0.4512(5) 0.8269(4) 0.0384(15) Uani 1 1 d . . . . .
H12 H 0.0759 0.5224 0.8487 0.046 Uiso 1 1 calc R U . . .
C24 C -0.2823(5) 0.3404(5) -0.1991(4) 0.0421(16) Uani 1 1 d . . . . .
H24 H -0.2558 0.3653 -0.2429 0.050 Uiso 1 1 calc R U . . .
O1 O 0.2255(3) 0.1216(3) 0.4791(2) 0.0308(9) Uani 1 1 d . . . . .
C3 C 0.2223(5) 0.3533(5) 0.3066(4) 0.0398(15) Uani 1 1 d . . . . .
H3 H 0.2579 0.3786 0.2658 0.048 Uiso 1 1 calc R U . . .
N1 N 0.1183(3) 0.2770(3) 0.4281(3) 0.0231(9) Uani 1 1 d . . . . .
N4 N -0.3599(3) 0.2667(3) -0.0679(3) 0.0239(10) Uani 1 1 d . . . . .
O4 O -0.1806(3) 0.3654(3) 0.6226(3) 0.0324(9) Uani 1 1 d . . . . .
C30 C -0.3806(5) 0.5575(4) 0.1984(4) 0.0343(14) Uani 1 1 d . . . . .
H30 H -0.3859 0.5978 0.2560 0.041 Uiso 1 1 calc R U . . .
C7 C 0.1448(5) 0.5496(4) 0.5561(4) 0.0314(13) Uani 1 1 d . . . . .
H7 H 0.1609 0.5804 0.5140 0.038 Uiso 1 1 calc R U . . .
O3 O -0.1268(3) 0.2223(3) 0.5420(3) 0.0367(10) Uani 1 1 d . . . . .
C28 C -0.3517(5) 0.5405(4) 0.0511(4) 0.0379(15) Uani 1 1 d . . . . .
H28 H -0.3404 0.5686 0.0067 0.046 Uiso 1 1 calc R U . . .
C48 C -0.4124(4) 0.0014(4) 0.1185(3) 0.0154(10) Uani 1 1 d . . . . .
C14 C 0.0172(5) 0.2909(5) 0.8489(4) 0.0413(15) Uani 1 1 d . . . . .
H14 H -0.0007 0.2523 0.8851 0.050 Uiso 1 1 calc R U . . .
C41 C -0.8127(4) 0.2247(4) 0.0429(3) 0.0234(12) Uani 1 1 d . . . . .
C34 C -0.4535(6) 0.4028(5) 0.3862(4) 0.0483(18) Uani 1 1 d . . . . .
H34 H -0.4624 0.4380 0.4444 0.058 Uiso 1 1 calc R U . . .
C9 C 0.1057(5) 0.5609(4) 0.7009(4) 0.0303(13) Uani 1 1 d . . . . .
H9 H 0.0972 0.5995 0.7583 0.036 Uiso 1 1 calc R U . . .
C20 C -0.3366(4) 0.2228(4) 0.5443(3) 0.0250(12) Uani 1 1 d . . . . .
C43 C -0.0905(4) -0.0074(4) 0.3817(3) 0.0159(10) Uani 1 1 d . . . . .
C10 C 0.0936(4) 0.4545(4) 0.6755(3) 0.0213(11) Uani 1 1 d . . . . .
C27 C -0.3569(4) 0.4364(4) 0.0337(3) 0.0227(11) Uani 1 1 d . . . . .
C29 C -0.3634(5) 0.6010(4) 0.1343(4) 0.0429(16) Uani 1 1 d . . . . .
H29 H -0.3597 0.6708 0.1473 0.051 Uiso 1 1 calc R U . . .
C37 C -0.1672(4) 0.1927(4) 0.0397(3) 0.0219(11) Uani 1 1 d . . . . .
C21 C -0.2041(4) 0.2756(4) 0.5730(3) 0.0235(12) Uani 1 1 d . . . . .
C42 C -0.6798(4) 0.2769(4) 0.0737(3) 0.0235(12) Uani 1 1 d . . . . .
C32 C -0.4138(4) 0.4013(4) 0.2417(3) 0.0222(11) Uani 1 1 d . . . . .
C36 C -0.4515(5) 0.2500(5) 0.2704(4) 0.0374(14) Uani 1 1 d . . . . .
H36 H -0.4607 0.1791 0.2505 0.045 Uiso 1 1 calc R U . . .
C5 C 0.1545(4) 0.3785(4) 0.4466(3) 0.0258(12) Uani 1 1 d . . . . .
OW1 O 0.7878(7) 0.0244(6) 0.6954(6) 0.180(4) Uani 1 1 d . . . . .
C44 C -0.1913(4) -0.0308(4) 0.3061(3) 0.0215(11) Uani 1 1 d . . . . .
C15 C 0.0243(5) 0.2442(4) 0.7603(4) 0.0317(13) Uani 1 1 d . . . . .
H15 H 0.0085 0.1730 0.7374 0.038 Uiso 1 1 calc R U . . .
C1 C 0.1315(5) 0.2147(4) 0.3478(4) 0.0358(14) Uani 1 1 d . . . . .
H1 H 0.1039 0.1444 0.3330 0.043 Uiso 1 1 calc R U . . .
C31 C -0.3899(4) 0.4521(4) 0.1759(3) 0.0217(11) Uani 1 1 d . . . . .
C11 C 0.0685(4) 0.3991(4) 0.7380(3) 0.0244(12) Uani 1 1 d . . . . .
C8 C 0.1301(5) 0.6068(4) 0.6395(4) 0.0348(14) Uani 1 1 d . . . . .
H8 H 0.1368 0.6772 0.6547 0.042 Uiso 1 1 calc R U . . .
C26 C -0.3394(4) 0.3685(4) -0.0543(3) 0.0236(12) Uani 1 1 d . . . . .
C25 C -0.3006(5) 0.4069(5) -0.1197(4) 0.0391(15) Uani 1 1 d . . . . .
H25 H -0.2874 0.4770 -0.1095 0.047 Uiso 1 1 calc R U . . .
C22 C -0.3414(5) 0.2048(4) -0.1465(3) 0.0326(13) Uani 1 1 d . . . . .
H22 H -0.3554 0.1348 -0.1564 0.039 Uiso 1 1 calc R U . . .
C17 C 0.4373(4) 0.1845(4) 0.5265(3) 0.0242(12) Uani 1 1 d . . . . .
C16 C 0.3078(4) 0.1904(4) 0.5338(3) 0.0225(12) Uani 1 1 d . . . . .
C38 C -0.0377(4) 0.1894(4) 0.0294(3) 0.0189(11) Uani 1 1 d . . . . .
C4 C 0.2078(5) 0.4188(4) 0.3870(4) 0.0326(13) Uani 1 1 d . . . . .
H4 H 0.2332 0.4892 0.4016 0.039 Uiso 1 1 calc R U . . .
C13 C 0.0370(6) 0.3959(5) 0.8821(4) 0.0490(18) Uani 1 1 d . . . . .
H13 H 0.0331 0.4295 0.9417 0.059 Uiso 1 1 calc R U . . .
C39 C 0.0063(4) 0.1091(4) -0.0221(4) 0.0306(13) Uani 1 1 d . . . . .
H39 H -0.0430 0.0475 -0.0592 0.037 Uiso 1 1 calc R U . . .
C19 C -0.3860(4) 0.1280(4) 0.4846(4) 0.0351(15) Uani 1 1 d . . . . .
H19 H -0.3398 0.0825 0.4541 0.042 Uiso 1 1 calc R U . . .
C45 C -0.2681(4) -0.1227(4) 0.2629(4) 0.0313(13) Uani 1 1 d . . . . .
H45 H -0.2670 -0.1809 0.2780 0.038 Uiso 1 1 calc R U . . .
C40 C 0.1355(5) 0.1304(4) -0.0124(4) 0.0351(14) Uani 1 1 d . . . . .
H40 H 0.1806 0.0832 -0.0418 0.042 Uiso 1 1 calc R U . . .
C18 C 0.4842(4) 0.1069(4) 0.4743(4) 0.0318(13) Uani 1 1 d . . . . .
H18 H 0.4357 0.0459 0.4356 0.038 Uiso 1 1 calc R U . . .
C46 C -0.3494(4) -0.1199(4) 0.1927(4) 0.0332(14) Uani 1 1 d . . . . .
H46 H -0.4058 -0.1772 0.1552 0.040 Uiso 1 1 calc R U . . .
OW2 O -0.2938(5) -0.0565(5) -0.1557(4) 0.109(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O3 2.197(3) . ?
Lu1 O10 2.202(3) . ?
Lu1 O9 2.270(3) . ?
Lu1 O2 2.388(3) . ?
Lu1 O1 2.431(3) . ?
Lu1 N1 2.457(4) . ?
Lu1 N2 2.492(4) . ?
Lu1 N3 2.513(4) . ?
Lu1 C16 2.759(4) . ?
Lu2 O7 2.212(3) . ?
Lu2 O12 2.223(3) . ?
Lu2 O11 2.247(3) 2_455 ?
Lu2 O6 2.380(3) . ?
Lu2 O5 2.400(3) . ?
Lu2 N4 2.454(4) . ?
Lu2 N5 2.468(4) . ?
Lu2 N6 2.507(4) . ?
Lu2 C37 2.748(5) . ?
S1 C20 1.717(5) . ?
S1 C17 1.726(5) 1_455 ?
S2 C38 1.713(5) . ?
S2 C41 1.725(5) 1_655 ?
S3 C44 1.722(5) . ?
S3 C47 1.723(4) . ?
O9 C43 1.244(5) . ?
O2 C16 1.273(6) . ?
O6 C37 1.270(6) . ?
C47 C46 1.343(6) . ?
C47 C48 1.489(6) . ?
O5 C37 1.260(6) . ?
C6 N2 1.347(6) . ?
C6 C7 1.396(7) . ?
C6 C5 1.478(7) . ?
O8 C42 1.213(6) . ?
O10 C43 1.252(5) 2_556 ?
N3 C15 1.342(6) . ?
N3 C11 1.354(6) . ?
O12 C48 1.255(5) . ?
C23 C24 1.367(8) . ?
C23 C22 1.378(7) . ?
C23 H23 0.9300 . ?
C33 C34 1.384(8) . ?
C33 C32 1.391(7) . ?
C33 H33 0.9300 . ?
N2 C10 1.340(6) . ?
C2 C3 1.362(8) . ?
C2 C1 1.372(7) . ?
C2 H2 0.9300 . ?
O11 C48 1.259(5) . ?
O11 Lu2 2.247(3) 2_455 ?
C35 C34 1.370(8) . ?
C35 C36 1.371(8) . ?
C35 H35 0.9300 . ?
N6 C32 1.344(6) . ?
N6 C36 1.353(6) . ?
O7 C42 1.282(6) . ?
N5 C31 1.332(6) . ?
N5 C27 1.342(6) . ?
C12 C13 1.376(8) . ?
C12 C11 1.395(7) . ?
C12 H12 0.9300 . ?
C24 C25 1.374(8) . ?
C24 H24 0.9300 . ?
O1 C16 1.256(6) . ?
C3 C4 1.366(8) . ?
C3 H3 0.9300 . ?
N1 C1 1.344(6) . ?
N1 C5 1.345(6) . ?
N4 C22 1.339(6) . ?
N4 C26 1.355(6) . ?
O4 C21 1.228(6) . ?
C30 C29 1.371(8) . ?
C30 C31 1.394(7) . ?
C30 H30 0.9300 . ?
C7 C8 1.364(8) . ?
C7 H7 0.9300 . ?
O3 C21 1.264(5) . ?
C28 C29 1.365(8) . ?
C28 C27 1.391(7) . ?
C28 H28 0.9300 . ?
C14 C13 1.372(8) . ?
C14 C15 1.380(7) . ?
C14 H14 0.9300 . ?
C41 C40 1.338(7) 1_455 ?
C41 C42 1.505(6) . ?
C41 S2 1.725(5) 1_455 ?
C34 H34 0.9300 . ?
C9 C8 1.367(7) . ?
C9 C10 1.399(7) . ?
C9 H9 0.9300 . ?
C20 C19 1.360(7) . ?
C20 C21 1.501(7) . ?
C43 O10 1.253(5) 2_556 ?
C43 C44 1.499(6) . ?
C10 C11 1.476(7) . ?
C27 C26 1.481(7) . ?
C29 H29 0.9300 . ?
C37 C38 1.474(6) . ?
C32 C31 1.476(7) . ?
C36 H36 0.9300 . ?
C5 C4 1.389(7) . ?
C44 C45 1.359(6) . ?
C15 H15 0.9300 . ?
C1 H1 0.9300 . ?
C8 H8 0.9300 . ?
C26 C25 1.397(7) . ?
C25 H25 0.9300 . ?
C22 H22 0.9300 . ?
C17 C18 1.357(7) . ?
C17 C16 1.474(6) . ?
C17 S1 1.726(5) 1_655 ?
C38 C39 1.361(6) . ?
C4 H4 0.9300 . ?
C13 H13 0.9300 . ?
C39 C40 1.407(6) . ?
C39 H39 0.9300 . ?
C19 C18 1.414(6) 1_455 ?
C19 H19 0.9300 . ?
C45 C46 1.405(6) . ?
C45 H45 0.9300 . ?
C40 C41 1.338(7) 1_655 ?
C40 H40 0.9300 . ?
C18 C19 1.414(6) 1_655 ?
C18 H18 0.9300 . ?
C46 H46 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Lu1 O10 101.66(13) . . ?
O3 Lu1 O9 74.15(12) . . ?
O10 Lu1 O9 86.47(12) . . ?
O3 Lu1 O2 153.97(13) . . ?
O10 Lu1 O2 89.98(11) . . ?
O9 Lu1 O2 130.34(11) . . ?
O3 Lu1 O1 150.86(13) . . ?
O10 Lu1 O1 76.04(12) . . ?
O9 Lu1 O1 76.72(11) . . ?
O2 Lu1 O1 54.50(11) . . ?
O3 Lu1 N1 98.55(14) . . ?
O10 Lu1 N1 148.59(13) . . ?
O9 Lu1 N1 76.20(13) . . ?
O2 Lu1 N1 81.99(12) . . ?
O1 Lu1 N1 74.60(13) . . ?
O3 Lu1 N2 83.32(13) . . ?
O10 Lu1 N2 140.39(12) . . ?
O9 Lu1 N2 131.80(12) . . ?
O2 Lu1 N2 73.15(11) . . ?
O1 Lu1 N2 117.32(12) . . ?
N1 Lu1 N2 65.61(13) . . ?
O3 Lu1 N3 77.12(13) . . ?
O10 Lu1 N3 77.95(13) . . ?
O9 Lu1 N3 143.64(13) . . ?
O2 Lu1 N3 82.78(12) . . ?
O1 Lu1 N3 129.12(12) . . ?
N1 Lu1 N3 130.35(14) . . ?
N2 Lu1 N3 64.76(13) . . ?
O3 Lu1 C16 174.85(14) . . ?
O10 Lu1 C16 82.54(13) . . ?
O9 Lu1 C16 103.34(14) . . ?
O2 Lu1 C16 27.43(13) . . ?
O1 Lu1 C16 27.07(13) . . ?
N1 Lu1 C16 76.41(14) . . ?
N2 Lu1 C16 95.37(14) . . ?
N3 Lu1 C16 106.86(14) . . ?
O7 Lu2 O12 106.08(13) . . ?
O7 Lu2 O11 75.54(12) . 2_455 ?
O12 Lu2 O11 86.50(11) . 2_455 ?
O7 Lu2 O6 153.52(13) . . ?
O12 Lu2 O6 88.18(12) . . ?
O11 Lu2 O6 128.55(11) 2_455 . ?
O7 Lu2 O5 149.80(12) . . ?
O12 Lu2 O5 75.39(12) . . ?
O11 Lu2 O5 74.45(11) 2_455 . ?
O6 Lu2 O5 54.76(11) . . ?
O7 Lu2 N4 97.22(13) . . ?
O12 Lu2 N4 148.98(13) . . ?
O11 Lu2 N4 79.69(13) 2_455 . ?
O6 Lu2 N4 79.26(12) . . ?
O5 Lu2 N4 74.19(13) . . ?
O7 Lu2 N5 80.94(12) . . ?
O12 Lu2 N5 136.65(12) . . ?
O11 Lu2 N5 135.54(11) 2_455 . ?
O6 Lu2 N5 73.57(11) . . ?
O5 Lu2 N5 119.34(12) . . ?
N4 Lu2 N5 66.39(14) . . ?
O7 Lu2 N6 77.58(13) . . ?
O12 Lu2 N6 74.88(13) . . ?
O11 Lu2 N6 141.36(12) 2_455 . ?
O6 Lu2 N6 85.08(12) . . ?
O5 Lu2 N6 130.02(11) . . ?
N4 Lu2 N6 131.17(14) . . ?
N5 Lu2 N6 64.84(13) . . ?
O7 Lu2 C37 171.80(14) . . ?
O12 Lu2 C37 81.10(13) . . ?
O11 Lu2 C37 101.37(13) 2_455 . ?
O6 Lu2 C37 27.49(13) . . ?
O5 Lu2 C37 27.28(12) . . ?
N4 Lu2 C37 74.68(14) . . ?
N5 Lu2 C37 96.61(14) . . ?
N6 Lu2 C37 108.57(13) . . ?
C20 S1 C17 91.3(2) . 1_455 ?
C38 S2 C41 91.1(2) . 1_655 ?
C44 S3 C47 91.5(2) . . ?
C43 O9 Lu1 146.1(3) . . ?
C16 O2 Lu1 92.8(3) . . ?
C37 O6 Lu2 92.6(3) . . ?
C46 C47 C48 126.9(4) . . ?
C46 C47 S3 110.9(3) . . ?
C48 C47 S3 122.2(3) . . ?
C37 O5 Lu2 91.9(3) . . ?
N2 C6 C7 121.5(5) . . ?
N2 C6 C5 116.9(4) . . ?
C7 C6 C5 121.6(5) . . ?
C43 O10 Lu1 163.6(3) 2_556 . ?
C15 N3 C11 117.6(4) . . ?
C15 N3 Lu1 122.2(3) . . ?
C11 N3 Lu1 120.1(3) . . ?
C48 O12 Lu2 146.3(3) . . ?
C24 C23 C22 117.8(6) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
C34 C33 C32 119.5(6) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C10 N2 C6 118.7(4) . . ?
C10 N2 Lu1 121.7(3) . . ?
C6 N2 Lu1 119.4(3) . . ?
C3 C2 C1 119.3(6) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C48 O11 Lu2 163.6(3) . 2_455 ?
C34 C35 C36 118.3(6) . . ?
C34 C35 H35 120.8 . . ?
C36 C35 H35 120.8 . . ?
C32 N6 C36 117.2(5) . . ?
C32 N6 Lu2 120.4(3) . . ?
C36 N6 Lu2 122.2(4) . . ?
C42 O7 Lu2 146.7(3) . . ?
C31 N5 C27 118.2(4) . . ?
C31 N5 Lu2 121.8(3) . . ?
C27 N5 Lu2 119.9(3) . . ?
C13 C12 C11 119.2(6) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C23 C24 C25 119.7(6) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C16 O1 Lu1 91.2(3) . . ?
C2 C3 C4 119.4(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C1 N1 C5 117.5(4) . . ?
C1 N1 Lu1 120.3(3) . . ?
C5 N1 Lu1 121.2(3) . . ?
C22 N4 C26 117.1(5) . . ?
C22 N4 Lu2 122.6(4) . . ?
C26 N4 Lu2 120.0(3) . . ?
C29 C30 C31 118.9(5) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C8 C7 C6 119.0(5) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C21 O3 Lu1 148.2(4) . . ?
C29 C28 C27 119.1(5) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
O12 C48 O11 125.4(4) . . ?
O12 C48 C47 117.4(4) . . ?
O11 C48 C47 117.2(4) . . ?
C13 C14 C15 118.3(6) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C40 C41 C42 131.0(5) 1_455 . ?
C40 C41 S2 111.4(4) 1_455 1_455 ?
C42 C41 S2 117.5(4) . 1_455 ?
C35 C34 C33 119.2(6) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C8 C9 C10 118.5(5) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
C19 C20 C21 129.1(5) . . ?
C19 C20 S1 112.2(4) . . ?
C21 C20 S1 118.7(4) . . ?
O9 C43 O10 126.4(4) . 2_556 ?
O9 C43 C44 116.9(4) . . ?
O10 C43 C44 116.7(4) 2_556 . ?
N2 C10 C9 122.0(5) . . ?
N2 C10 C11 116.0(4) . . ?
C9 C10 C11 121.9(5) . . ?
N5 C27 C28 122.1(5) . . ?
N5 C27 C26 116.7(4) . . ?
C28 C27 C26 121.2(5) . . ?
C28 C29 C30 119.2(5) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
O5 C37 O6 120.7(4) . . ?
O5 C37 C38 119.5(4) . . ?
O6 C37 C38 119.7(4) . . ?
O5 C37 Lu2 60.8(2) . . ?
O6 C37 Lu2 59.9(2) . . ?
C38 C37 Lu2 177.2(4) . . ?
O4 C21 O3 126.3(5) . . ?
O4 C21 C20 118.0(4) . . ?
O3 C21 C20 115.7(5) . . ?
O8 C42 O7 126.9(5) . . ?
O8 C42 C41 118.6(4) . . ?
O7 C42 C41 114.6(5) . . ?
N6 C32 C33 121.7(5) . . ?
N6 C32 C31 116.0(4) . . ?
C33 C32 C31 122.2(5) . . ?
N6 C36 C35 124.1(6) . . ?
N6 C36 H36 118.0 . . ?
C35 C36 H36 118.0 . . ?
N1 C5 C4 122.1(5) . . ?
N1 C5 C6 115.6(4) . . ?
C4 C5 C6 122.3(5) . . ?
C45 C44 C43 126.7(4) . . ?
C45 C44 S3 111.2(3) . . ?
C43 C44 S3 122.1(4) . . ?
N3 C15 C14 123.6(5) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
N1 C1 C2 122.7(5) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
N5 C31 C30 122.3(5) . . ?
N5 C31 C32 116.8(4) . . ?
C30 C31 C32 120.9(5) . . ?
N3 C11 C12 121.6(5) . . ?
N3 C11 C10 117.0(4) . . ?
C12 C11 C10 121.4(5) . . ?
C7 C8 C9 120.2(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
N4 C26 C25 121.3(5) . . ?
N4 C26 C27 116.6(4) . . ?
C25 C26 C27 122.1(5) . . ?
C24 C25 C26 119.5(6) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
N4 C22 C23 124.6(6) . . ?
N4 C22 H22 117.7 . . ?
C23 C22 H22 117.7 . . ?
C18 C17 C16 128.9(5) . . ?
C18 C17 S1 111.1(4) . 1_655 ?
C16 C17 S1 120.0(4) . 1_655 ?
O1 C16 O2 121.5(4) . . ?
O1 C16 C17 118.6(5) . . ?
O2 C16 C17 119.8(4) . . ?
O1 C16 Lu1 61.7(2) . . ?
O2 C16 Lu1 59.8(2) . . ?
C17 C16 Lu1 178.0(4) . . ?
C39 C38 C37 127.0(5) . . ?
C39 C38 S2 111.8(4) . . ?
C37 C38 S2 121.2(4) . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C14 C13 C12 119.6(6) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C38 C39 C40 112.0(5) . . ?
C38 C39 H39 124.0 . . ?
C40 C39 H39 124.0 . . ?
C20 C19 C18 112.0(5) . 1_455 ?
C20 C19 H19 124.0 . . ?
C18 C19 H19 124.0 1_455 . ?
C44 C45 C46 112.4(4) . . ?
C44 C45 H45 123.8 . . ?
C46 C45 H45 123.8 . . ?
C41 C40 C39 113.7(5) 1_655 . ?
C41 C40 H40 123.2 1_655 . ?
C39 C40 H40 123.2 . . ?
C17 C18 C19 113.4(5) . 1_655 ?
C17 C18 H18 123.3 . . ?
C19 C18 H18 123.3 1_655 . ?
C47 C46 C45 113.9(4) . . ?
C47 C46 H46 123.0 . . ?
C45 C46 H46 123.0 . . ?

_refine_diff_density_max         1.040
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.162

_shelxl_version_number           2013-4

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

#===END




