# 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_4
_audit_block_doi                 10.5517/cc14bppv
_database_code_depnum_ccdc_archive 'CCDC 1052967'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H22 F12 N4 O15 Tb2'
_chemical_formula_weight         1440.53

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'
F F 0.0171 0.0103 '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'
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                   13.9969(10)
_cell_length_b                   14.1432(10)
_cell_length_c                   14.9746(11)
_cell_angle_alpha                63.8960(10)
_cell_angle_beta                 81.0240(10)
_cell_angle_gamma                65.4650(10)
_cell_volume                     2420.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6418
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      26.76

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.247
_exptl_absorpt_coefficient_mu    3.020
_shelx_estimated_absorpt_T_min   0.351
_shelx_estimated_absorpt_T_max   0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3513
_exptl_absorpt_correction_T_max  0.5225
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13279
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.515
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             8298
_reflns_number_gt                6308
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.286     0.122     0.996      86.6      14.3
         2     0.716     0.877     0.004      86.8      14.2
_platon_squeeze_details

The unit cell contains 4 water molecules, which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1019P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8298
_refine_ls_number_parameters     730
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1686
_refine_ls_wR_factor_gt          0.1415
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.64870(3) -0.01187(3) 0.55971(3) 0.02187(16) Uani 1 1 d . . . . .
Tb2 Tb 0.60615(3) 0.23992(3) 0.14112(3) 0.02174(15) Uani 1 1 d . . . . .
C1 C 0.8933(8) -0.2244(9) 0.5698(9) 0.042(3) Uani 1 1 d . . . . .
H1 H 0.8509 -0.2519 0.5547 0.051 Uiso 1 1 calc R U . . .
C2 C 1.0028(9) -0.2828(10) 0.5725(12) 0.068(5) Uani 1 1 d . . . . .
H2 H 1.0320 -0.3456 0.5567 0.081 Uiso 1 1 calc R U . . .
C3 C 1.0663(8) -0.2463(9) 0.5988(9) 0.044(3) Uani 1 1 d . . . . .
H3 H 1.1387 -0.2868 0.6055 0.052 Uiso 1 1 calc R U . . .
C4 C 1.0203(7) -0.1474(9) 0.6151(7) 0.034(2) Uani 1 1 d . . . . .
C5 C 1.0809(8) -0.0962(10) 0.6342(8) 0.042(3) Uani 1 1 d . . . . .
H5 H 1.1539 -0.1287 0.6335 0.051 Uiso 1 1 calc R U . . .
C6 C 1.0341(8) -0.0026(10) 0.6532(9) 0.044(3) Uani 1 1 d . . . . .
H6 H 1.0749 0.0282 0.6658 0.052 Uiso 1 1 calc R U . . .
C7 C 0.9242(8) 0.0486(8) 0.6539(8) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.8714(10) 0.1449(9) 0.6783(8) 0.049(3) Uani 1 1 d . . . . .
H8 H 0.9095 0.1776 0.6922 0.059 Uiso 1 1 calc R U . . .
C9 C 0.7654(9) 0.1876(9) 0.6809(8) 0.038(3) Uani 1 1 d . . . . .
H9 H 0.7294 0.2500 0.6966 0.045 Uiso 1 1 calc R U . . .
C10 C 0.7117(8) 0.1372(8) 0.6599(7) 0.032(2) Uani 1 1 d . . . . .
H10 H 0.6389 0.1676 0.6633 0.038 Uiso 1 1 calc R U . . .
C11 C 0.8610(7) 0.0064(7) 0.6318(7) 0.026(2) Uani 1 1 d . . . . .
C12 C 0.9102(7) -0.0930(8) 0.6106(6) 0.024(2) Uani 1 1 d . . . . .
C13 C 0.8489(9) 0.0484(9) 0.1194(9) 0.048(3) Uani 1 1 d . . . . .
H13 H 0.8066 0.0103 0.1242 0.057 Uiso 1 1 calc R U . . .
C14 C 0.9560(9) -0.0070(10) 0.1111(7) 0.045(3) Uani 1 1 d . . . . .
H14 H 0.9843 -0.0790 0.1106 0.054 Uiso 1 1 calc R U . . .
C15 C 1.0172(9) 0.0495(10) 0.1037(8) 0.047(3) Uani 1 1 d . U . . .
H15 H 1.0895 0.0153 0.0989 0.056 Uiso 1 1 calc R U . . .
C16 C 0.9718(8) 0.1609(10) 0.1031(9) 0.046(3) Uani 1 1 d . . . . .
C17 C 1.0335(10) 0.2206(13) 0.0973(11) 0.069(4) Uani 1 1 d . . . . .
H17 H 1.1062 0.1864 0.0954 0.083 Uiso 1 1 calc R U . . .
C18 C 0.9885(10) 0.3264(13) 0.0944(11) 0.065(4) Uani 1 1 d . . . . .
H18 H 1.0307 0.3646 0.0896 0.078 Uiso 1 1 calc R U . . .
C19 C 0.8747(9) 0.3827(11) 0.0986(8) 0.042(3) Uani 1 1 d . . . . .
C20 C 0.8223(10) 0.4923(11) 0.1015(10) 0.056(3) Uani 1 1 d . . . . .
H20 H 0.8605 0.5324 0.1021 0.067 Uiso 1 1 calc R U . . .
C21 C 0.7183(10) 0.5355(10) 0.1033(10) 0.057(4) Uani 1 1 d . . . . .
H21 H 0.6832 0.6093 0.0995 0.069 Uiso 1 1 calc R U . . .
C22 C 0.6603(8) 0.4724(9) 0.1107(8) 0.039(3) Uani 1 1 d . . . . .
H22 H 0.5878 0.5026 0.1165 0.047 Uiso 1 1 calc R U . . .
C23 C 0.8136(8) 0.3218(9) 0.1068(7) 0.032(2) Uani 1 1 d . . . . .
C24 C 0.8625(8) 0.2092(9) 0.1098(8) 0.037(2) Uani 1 1 d . . . . .
C25 C 0.6918(7) -0.0407(7) 0.3349(7) 0.024(2) Uani 1 1 d . . . . .
C26 C 0.7265(8) -0.1548(8) 0.3282(7) 0.026(2) Uani 1 1 d . . . . .
C27 C 0.8284(7) -0.2307(8) 0.3402(7) 0.029(2) Uani 1 1 d . . . . .
C28 C 0.8597(7) -0.3366(8) 0.3403(8) 0.032(2) Uani 1 1 d . . . . .
C29 C 0.7864(8) -0.3687(8) 0.3247(8) 0.035(2) Uani 1 1 d . . . . .
C30 C 0.6816(8) -0.2924(8) 0.3096(8) 0.036(3) Uani 1 1 d . . . . .
C31 C 0.6475(8) -0.1856(8) 0.3127(7) 0.029(2) Uani 1 1 d . . . . .
C32 C 0.5338(7) -0.1057(8) 0.2971(7) 0.026(2) Uani 1 1 d . . . . .
C33 C 0.4028(7) 0.3906(7) 0.1480(6) 0.024(2) Uani 1 1 d . . . . .
C34 C 0.2926(7) 0.4780(7) 0.1532(6) 0.023(2) Uani 1 1 d . . . . .
C35 C 0.2036(7) 0.4559(8) 0.1658(7) 0.030(2) Uani 1 1 d . . . . .
C36 C 0.1076(8) 0.5352(9) 0.1657(8) 0.040(3) Uani 1 1 d . . . . .
C37 C 0.0954(9) 0.6417(9) 0.1546(10) 0.048(3) Uani 1 1 d . . . . .
C38 C 0.1830(8) 0.6658(8) 0.1405(8) 0.036(2) Uani 1 1 d . . . . .
C39 C 0.2822(7) 0.5886(8) 0.1387(6) 0.024(2) Uani 1 1 d . . . . .
C40 C 0.3734(8) 0.6301(8) 0.1182(9) 0.036(3) Uani 1 1 d . . . . .
C41 C 0.6155(7) 0.2285(7) 0.3758(6) 0.0194(19) Uani 1 1 d . U . . .
C42 C 0.5133(7) 0.3186(7) 0.3915(6) 0.0172(18) Uani 1 1 d . . . . .
C43 C 0.5191(7) 0.4134(8) 0.3896(7) 0.029(2) Uani 1 1 d . . . . .
C44 C 0.4339(8) 0.4950(8) 0.4076(8) 0.031(2) Uani 1 1 d . . . . .
C45 C 0.3390(8) 0.4806(8) 0.4288(8) 0.035(2) Uani 1 1 d . . . . .
C46 C 0.3330(7) 0.3875(8) 0.4279(8) 0.030(2) Uani 1 1 d . . . . .
C47 C 0.4186(7) 0.3029(7) 0.4102(7) 0.026(2) Uani 1 1 d . . . . .
C48 C 0.4146(9) 0.1984(9) 0.4118(7) 0.032(2) Uani 1 1 d . . . . .
F1 F 0.9056(4) -0.2038(5) 0.3543(5) 0.0457(16) Uani 1 1 d . . . . .
F2 F 0.9599(5) -0.4101(5) 0.3570(5) 0.0526(18) Uani 1 1 d . . . . .
F3 F 0.8105(5) -0.4698(5) 0.3252(6) 0.061(2) Uani 1 1 d . . . . .
F4 F 0.6079(5) -0.3252(6) 0.2986(6) 0.064(2) Uani 1 1 d . . . . .
F5 F 0.2078(5) 0.3548(5) 0.1762(5) 0.0515(18) Uani 1 1 d . . . . .
F6 F 0.0203(5) 0.5100(6) 0.1820(6) 0.066(2) Uani 1 1 d . . . . .
F7 F -0.0023(5) 0.7215(6) 0.1563(6) 0.065(2) Uani 1 1 d . . . . .
F8 F 0.1700(5) 0.7731(5) 0.1238(5) 0.0479(16) Uani 1 1 d . . . . .
F9 F 0.6099(5) 0.4289(5) 0.3714(5) 0.0480(17) Uani 1 1 d . . . . .
F10 F 0.4390(5) 0.5883(5) 0.4062(6) 0.0543(19) Uani 1 1 d . . . . .
F11 F 0.2533(5) 0.5612(5) 0.4439(5) 0.0530(18) Uani 1 1 d . . . . .
F12 F 0.2363(5) 0.3833(5) 0.4447(5) 0.0463(16) Uani 1 1 d . . . . .
N1 N 0.8474(6) -0.1314(7) 0.5878(6) 0.0277(18) Uani 1 1 d . . . . .
N2 N 0.7532(6) 0.0509(6) 0.6358(6) 0.031(2) Uani 1 1 d . . . . .
N3 N 0.8007(6) 0.1514(7) 0.1213(6) 0.035(2) Uani 1 1 d . . . . .
N4 N 0.7090(6) 0.3668(6) 0.1097(5) 0.0229(17) Uani 1 1 d . . . . .
O1 O 0.7085(5) -0.0447(6) 0.4148(5) 0.0352(17) Uani 1 1 d . . . . .
O2 O 0.6485(6) 0.0451(5) 0.2600(5) 0.0368(17) Uani 1 1 d . . . . .
O3 O 0.4906(5) -0.1005(5) 0.3761(5) 0.0294(15) Uani 1 1 d . . . . .
O4 O 0.4921(5) -0.0550(6) 0.2126(5) 0.0392(18) Uani 1 1 d . . . . .
O5 O 0.4191(5) 0.2874(5) 0.1770(6) 0.047(2) Uani 1 1 d . . . . .
O6 O 0.4737(5) 0.4249(5) 0.1148(5) 0.0342(17) Uani 1 1 d . . . . .
O7 O 0.3905(5) 0.6795(6) 0.0255(5) 0.0365(17) Uani 1 1 d . . . . .
O8 O 0.4099(6) 0.6234(6) 0.1905(5) 0.045(2) Uani 1 1 d . . . . .
O9 O 0.6324(5) 0.2413(5) 0.2884(5) 0.0316(16) Uani 1 1 d . . . . .
O10 O 0.6715(5) 0.1561(5) 0.4499(5) 0.0286(15) Uani 1 1 d . . . . .
O11 O 0.4928(5) 0.1084(5) 0.4335(5) 0.0329(16) Uani 1 1 d . . . . .
O12 O 0.3252(5) 0.2051(6) 0.3968(6) 0.0372(17) Uani 1 1 d . . . . .
O13 O 0.6609(5) -0.1174(5) 0.7377(5) 0.0374(17) Uani 1 1 d D . . . .
H13A H 0.6593 -0.1843 0.7649 0.056 Uiso 1 1 d DR U . . .
H13B H 0.6188 -0.0779 0.7703 0.056 Uiso 1 1 d DR U . . .
O14 O 0.5666(8) 0.1304(7) 0.0771(6) 0.064(3) Uani 1 1 d D . . . .
H14A H 0.5457 0.1586 0.0171 0.096 Uiso 1 1 d DR U . . .
H14B H 0.5561 0.0676 0.1148 0.096 Uiso 1 1 d DR U . . .
O15 O 0.5311(12) 0.1885(11) 0.8908(9) 0.129(5) Uani 1 1 d D U . . .
H15A H 0.4809 0.2062 0.8680 0.193 Uiso 1 1 d DR U . . .
H15B H 0.5416 0.2505 0.8571 0.193 Uiso 1 1 d DR U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O3 2.332(6) 2_656 ?
Tb1 O10 2.340(6) . ?
Tb1 O1 2.371(6) . ?
Tb1 O12 2.388(6) 2_656 ?
Tb1 O13 2.406(7) . ?
Tb1 O11 2.570(7) . ?
Tb1 N1 2.570(8) . ?
Tb1 N2 2.592(7) . ?
Tb1 O11 2.803(7) 2_656 ?
Tb1 C48 2.959(9) 2_656 ?
Tb2 O7 2.243(7) 2_665 ?
Tb2 O9 2.301(6) . ?
Tb2 O6 2.394(6) . ?
Tb2 O2 2.402(6) . ?
Tb2 O14 2.410(7) . ?
Tb2 O5 2.453(7) . ?
Tb2 N3 2.513(8) . ?
Tb2 N4 2.590(7) . ?
Tb2 C33 2.778(9) . ?
C1 N1 1.330(12) . ?
C1 C2 1.405(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.371(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(14) . ?
C3 H3 0.9300 . ?
C4 C12 1.405(13) . ?
C4 C5 1.447(14) . ?
C5 C6 1.346(15) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(14) . ?
C6 H6 0.9300 . ?
C7 C11 1.399(13) . ?
C7 C8 1.433(16) . ?
C8 C9 1.351(16) . ?
C8 H8 0.9300 . ?
C9 C10 1.375(13) . ?
C9 H9 0.9300 . ?
C10 N2 1.300(12) . ?
C10 H10 0.9300 . ?
C11 N2 1.375(12) . ?
C11 C12 1.439(12) . ?
C12 N1 1.356(11) . ?
C13 N3 1.338(13) . ?
C13 C14 1.388(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.359(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.430(16) . ?
C15 H15 0.9300 . ?
C16 C24 1.400(14) . ?
C16 C17 1.409(17) . ?
C17 C18 1.344(18) . ?
C17 H17 0.9300 . ?
C18 C19 1.461(16) . ?
C18 H18 0.9300 . ?
C19 C23 1.405(14) . ?
C19 C20 1.430(16) . ?
C20 C21 1.326(17) . ?
C20 H20 0.9300 . ?
C21 C22 1.397(15) . ?
C21 H21 0.9300 . ?
C22 N4 1.366(12) . ?
C22 H22 0.9300 . ?
C23 N4 1.334(12) . ?
C23 C24 1.432(14) . ?
C24 N3 1.365(13) . ?
C25 O2 1.226(11) . ?
C25 O1 1.226(11) . ?
C25 C26 1.526(12) . ?
C26 C27 1.362(13) . ?
C26 C31 1.427(13) . ?
C27 F1 1.358(10) . ?
C27 C28 1.373(13) . ?
C28 F2 1.334(11) . ?
C28 C29 1.368(14) . ?
C29 F3 1.323(10) . ?
C29 C30 1.393(14) . ?
C30 F4 1.351(11) . ?
C30 C31 1.402(13) . ?
C31 C32 1.502(13) . ?
C32 O4 1.242(11) . ?
C32 O3 1.259(11) . ?
C33 O6 1.225(11) . ?
C33 O5 1.253(11) . ?
C33 C34 1.542(13) . ?
C34 C35 1.372(13) . ?
C34 C39 1.427(12) . ?
C35 F5 1.345(11) . ?
C35 C36 1.346(14) . ?
C36 F6 1.369(12) . ?
C36 C37 1.378(15) . ?
C37 C38 1.366(15) . ?
C37 F7 1.370(12) . ?
C38 F8 1.360(11) . ?
C38 C39 1.370(13) . ?
C39 C40 1.552(13) . ?
C40 O8 1.218(13) . ?
C40 O7 1.287(13) . ?
C41 O10 1.224(10) . ?
C41 O9 1.238(10) . ?
C41 C42 1.540(12) . ?
C42 C43 1.364(12) . ?
C42 C47 1.398(12) . ?
C43 F9 1.344(10) . ?
C43 C44 1.363(13) . ?
C44 F10 1.342(10) . ?
C44 C45 1.394(14) . ?
C45 F11 1.341(11) . ?
C45 C46 1.359(13) . ?
C46 F12 1.359(10) . ?
C46 C47 1.388(13) . ?
C47 C48 1.493(13) . ?
C48 O11 1.230(12) . ?
C48 O12 1.263(11) . ?
C48 Tb1 2.959(9) 2_656 ?
O3 Tb1 2.332(6) 2_656 ?
O7 Tb2 2.243(7) 2_665 ?
O11 Tb1 2.803(6) 2_656 ?
O12 Tb1 2.388(6) 2_656 ?
O13 H13A 0.8578 . ?
O13 H13B 0.8806 . ?
O14 H14A 0.8494 . ?
O14 H14B 0.8784 . ?
O15 H15A 0.7265 . ?
O15 H15B 0.8588 . ?

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 Tb1 O10 87.3(2) 2_656 . ?
O3 Tb1 O1 143.7(2) 2_656 . ?
O10 Tb1 O1 77.1(2) . . ?
O3 Tb1 O12 120.4(2) 2_656 2_656 ?
O10 Tb1 O12 150.2(2) . 2_656 ?
O1 Tb1 O12 73.8(2) . 2_656 ?
O3 Tb1 O13 73.2(2) 2_656 . ?
O10 Tb1 O13 134.5(2) . . ?
O1 Tb1 O13 139.3(2) . . ?
O12 Tb1 O13 69.7(2) 2_656 . ?
O3 Tb1 O11 70.8(2) 2_656 . ?
O10 Tb1 O11 72.7(2) . . ?
O1 Tb1 O11 73.3(2) . . ?
O12 Tb1 O11 104.2(2) 2_656 . ?
O13 Tb1 O11 132.8(2) . . ?
O3 Tb1 N1 140.6(2) 2_656 . ?
O10 Tb1 N1 93.2(2) . . ?
O1 Tb1 N1 73.6(2) . . ?
O12 Tb1 N1 72.8(2) 2_656 . ?
O13 Tb1 N1 79.0(2) . . ?
O11 Tb1 N1 146.2(2) . . ?
O3 Tb1 N2 81.0(2) 2_656 . ?
O10 Tb1 N2 65.7(2) . . ?
O1 Tb1 N2 119.9(3) . . ?
O12 Tb1 N2 125.3(2) 2_656 . ?
O13 Tb1 N2 70.8(2) . . ?
O11 Tb1 N2 130.4(2) . . ?
N1 Tb1 N2 63.7(2) . . ?
O3 Tb1 O11 83.35(19) 2_656 2_656 ?
O10 Tb1 O11 134.2(2) . 2_656 ?
O1 Tb1 O11 84.6(2) . 2_656 ?
O12 Tb1 O11 48.9(2) 2_656 2_656 ?
O13 Tb1 O11 84.8(2) . 2_656 ?
O11 Tb1 O11 61.8(2) . 2_656 ?
N1 Tb1 O11 121.5(2) . 2_656 ?
N2 Tb1 O11 153.9(2) . 2_656 ?
O3 Tb1 C48 103.2(3) 2_656 2_656 ?
O10 Tb1 C48 148.0(2) . 2_656 ?
O1 Tb1 C48 76.8(3) . 2_656 ?
O12 Tb1 C48 24.5(3) 2_656 2_656 ?
O13 Tb1 C48 77.4(2) . 2_656 ?
O11 Tb1 C48 82.2(3) . 2_656 ?
N1 Tb1 C48 97.0(3) . 2_656 ?
N2 Tb1 C48 145.2(3) . 2_656 ?
O11 Tb1 C48 24.5(2) 2_656 2_656 ?
O7 Tb2 O9 147.1(2) 2_665 . ?
O7 Tb2 O6 82.5(2) 2_665 . ?
O9 Tb2 O6 82.1(2) . . ?
O7 Tb2 O2 132.3(2) 2_665 . ?
O9 Tb2 O2 76.2(2) . . ?
O6 Tb2 O2 138.0(2) . . ?
O7 Tb2 O14 71.3(3) 2_665 . ?
O9 Tb2 O14 141.6(2) . . ?
O6 Tb2 O14 116.6(3) . . ?
O2 Tb2 O14 67.7(2) . . ?
O7 Tb2 O5 104.4(3) 2_665 . ?
O9 Tb2 O5 88.9(3) . . ?
O6 Tb2 O5 52.9(2) . . ?
O2 Tb2 O5 90.8(2) . . ?
O14 Tb2 O5 79.1(3) . . ?
O7 Tb2 N3 81.1(3) 2_665 . ?
O9 Tb2 N3 91.5(3) . . ?
O6 Tb2 N3 138.3(2) . . ?
O2 Tb2 N3 78.3(3) . . ?
O14 Tb2 N3 93.8(3) . . ?
O5 Tb2 N3 168.7(2) . . ?
O7 Tb2 N4 77.7(2) 2_665 . ?
O9 Tb2 N4 70.2(2) . . ?
O6 Tb2 N4 75.1(2) . . ?
O2 Tb2 N4 127.7(2) . . ?
O14 Tb2 N4 144.4(3) . . ?
O5 Tb2 N4 126.4(2) . . ?
N3 Tb2 N4 64.0(2) . . ?
O7 Tb2 C33 94.1(3) 2_665 . ?
O9 Tb2 C33 84.4(2) . . ?
O6 Tb2 C33 26.1(2) . . ?
O2 Tb2 C33 115.1(3) . . ?
O14 Tb2 C33 98.9(3) . . ?
O5 Tb2 C33 26.8(2) . . ?
N3 Tb2 C33 164.3(3) . . ?
N4 Tb2 C33 100.4(2) . . ?
N1 C1 C2 122.9(10) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.3(11) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 118.7(10) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C12 118.8(9) . . ?
C3 C4 C5 122.9(9) . . ?
C12 C4 C5 118.3(9) . . ?
C6 C5 C4 121.5(9) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 120.4(10) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C11 C7 C6 121.0(10) . . ?
C11 C7 C8 116.8(9) . . ?
C6 C7 C8 122.2(10) . . ?
C9 C8 C7 119.1(10) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 118.9(10) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 126.0(10) . . ?
N2 C10 H10 117.0 . . ?
C9 C10 H10 117.0 . . ?
N2 C11 C7 122.9(9) . . ?
N2 C11 C12 118.0(8) . . ?
C7 C11 C12 119.0(8) . . ?
N1 C12 C4 122.3(9) . . ?
N1 C12 C11 118.0(8) . . ?
C4 C12 C11 119.7(8) . . ?
N3 C13 C14 126.3(12) . . ?
N3 C13 H13 116.9 . . ?
C14 C13 H13 116.9 . . ?
C15 C14 C13 116.5(11) . . ?
C15 C14 H14 121.7 . . ?
C13 C14 H14 121.7 . . ?
C14 C15 C16 120.8(10) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C24 C16 C17 120.4(11) . . ?
C24 C16 C15 117.5(11) . . ?
C17 C16 C15 122.0(11) . . ?
C18 C17 C16 120.8(12) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 121.5(12) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C23 C19 C20 118.0(10) . . ?
C23 C19 C18 117.6(11) . . ?
C20 C19 C18 124.3(11) . . ?
C21 C20 C19 118.7(11) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C22 121.3(12) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
N4 C22 C21 120.7(10) . . ?
N4 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
N4 C23 C19 121.9(10) . . ?
N4 C23 C24 117.7(9) . . ?
C19 C23 C24 120.4(9) . . ?
N3 C24 C16 122.1(10) . . ?
N3 C24 C23 118.6(9) . . ?
C16 C24 C23 119.3(10) . . ?
O2 C25 O1 127.2(9) . . ?
O2 C25 C26 116.0(8) . . ?
O1 C25 C26 116.8(8) . . ?
C27 C26 C31 118.4(8) . . ?
C27 C26 C25 123.5(8) . . ?
C31 C26 C25 118.1(8) . . ?
F1 C27 C26 119.9(8) . . ?
F1 C27 C28 116.2(8) . . ?
C26 C27 C28 123.9(9) . . ?
F2 C28 C29 118.8(8) . . ?
F2 C28 C27 121.7(9) . . ?
C29 C28 C27 119.4(9) . . ?
F3 C29 C28 122.8(9) . . ?
F3 C29 C30 118.7(9) . . ?
C28 C29 C30 118.4(8) . . ?
F4 C30 C29 118.9(8) . . ?
F4 C30 C31 117.8(9) . . ?
C29 C30 C31 123.1(9) . . ?
C30 C31 C26 116.7(9) . . ?
C30 C31 C32 121.7(9) . . ?
C26 C31 C32 121.5(8) . . ?
O4 C32 O3 127.2(9) . . ?
O4 C32 C31 119.5(9) . . ?
O3 C32 C31 113.2(8) . . ?
O6 C33 O5 121.1(9) . . ?
O6 C33 C34 118.2(8) . . ?
O5 C33 C34 120.7(8) . . ?
O6 C33 Tb2 59.2(5) . . ?
O5 C33 Tb2 62.0(5) . . ?
C34 C33 Tb2 176.8(6) . . ?
C35 C34 C39 118.8(8) . . ?
C35 C34 C33 122.6(8) . . ?
C39 C34 C33 118.5(8) . . ?
F5 C35 C36 116.7(9) . . ?
F5 C35 C34 121.6(8) . . ?
C36 C35 C34 121.7(9) . . ?
C35 C36 F6 120.7(10) . . ?
C35 C36 C37 120.9(10) . . ?
F6 C36 C37 118.3(10) . . ?
C38 C37 F7 121.1(9) . . ?
C38 C37 C36 118.2(10) . . ?
F7 C37 C36 120.8(10) . . ?
F8 C38 C37 118.0(9) . . ?
F8 C38 C39 118.7(9) . . ?
C37 C38 C39 123.2(9) . . ?
C38 C39 C34 117.2(9) . . ?
C38 C39 C40 117.2(8) . . ?
C34 C39 C40 125.6(8) . . ?
O8 C40 O7 129.0(9) . . ?
O8 C40 C39 115.8(9) . . ?
O7 C40 C39 114.6(9) . . ?
O10 C41 O9 128.1(9) . . ?
O10 C41 C42 116.6(7) . . ?
O9 C41 C42 115.2(7) . . ?
C43 C42 C47 121.0(8) . . ?
C43 C42 C41 117.3(8) . . ?
C47 C42 C41 121.8(8) . . ?
F9 C43 C44 117.4(8) . . ?
F9 C43 C42 121.2(8) . . ?
C44 C43 C42 121.4(8) . . ?
F10 C44 C43 121.9(8) . . ?
F10 C44 C45 119.1(8) . . ?
C43 C44 C45 119.0(8) . . ?
F11 C45 C46 120.6(9) . . ?
F11 C45 C44 120.1(8) . . ?
C46 C45 C44 119.2(9) . . ?
F12 C46 C45 115.1(8) . . ?
F12 C46 C47 121.9(8) . . ?
C45 C46 C47 122.9(9) . . ?
C46 C47 C42 116.4(8) . . ?
C46 C47 C48 123.9(9) . . ?
C42 C47 C48 119.7(9) . . ?
O11 C48 O12 121.9(9) . . ?
O11 C48 C47 121.6(9) . . ?
O12 C48 C47 116.3(9) . . ?
O11 C48 Tb1 70.6(5) . 2_656 ?
O12 C48 Tb1 51.6(5) . 2_656 ?
C47 C48 Tb1 164.4(7) . 2_656 ?
C1 N1 C12 117.8(8) . . ?
C1 N1 Tb1 121.9(6) . . ?
C12 N1 Tb1 119.8(6) . . ?
C10 N2 C11 116.3(8) . . ?
C10 N2 Tb1 124.4(6) . . ?
C11 N2 Tb1 117.9(6) . . ?
C13 N3 C24 116.6(9) . . ?
C13 N3 Tb2 123.1(7) . . ?
C24 N3 Tb2 120.3(6) . . ?
C23 N4 C22 119.1(8) . . ?
C23 N4 Tb2 119.0(6) . . ?
C22 N4 Tb2 121.2(6) . . ?
C25 O1 Tb1 151.3(6) . . ?
C25 O2 Tb2 155.0(6) . . ?
C32 O3 Tb1 144.2(6) . 2_656 ?
C33 O5 Tb2 91.2(6) . . ?
C33 O6 Tb2 94.7(5) . . ?
C40 O7 Tb2 168.9(7) . 2_665 ?
C41 O9 Tb2 155.8(6) . . ?
C41 O10 Tb1 124.4(5) . . ?
C48 O11 Tb1 138.6(6) . . ?
C48 O11 Tb1 84.9(5) . 2_656 ?
Tb1 O11 Tb1 118.2(2) . 2_656 ?
C48 O12 Tb1 104.0(6) . 2_656 ?
Tb1 O13 H13A 121.1 . . ?
Tb1 O13 H13B 114.4 . . ?
H13A O13 H13B 107.9 . . ?
Tb2 O14 H14A 121.5 . . ?
Tb2 O14 H14B 123.9 . . ?
H14A O14 H14B 112.8 . . ?
H15A O15 H15B 98.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 3(2) . . . . ?
C1 C2 C3 C4 -4(2) . . . . ?
C2 C3 C4 C12 4.2(17) . . . . ?
C2 C3 C4 C5 -174.3(12) . . . . ?
C3 C4 C5 C6 -177.7(11) . . . . ?
C12 C4 C5 C6 3.8(16) . . . . ?
C4 C5 C6 C7 -0.6(18) . . . . ?
C5 C6 C7 C11 -2.2(17) . . . . ?
C5 C6 C7 C8 176.9(11) . . . . ?
C11 C7 C8 C9 1.4(15) . . . . ?
C6 C7 C8 C9 -177.7(11) . . . . ?
C7 C8 C9 C10 0.0(16) . . . . ?
C8 C9 C10 N2 -1.0(16) . . . . ?
C6 C7 C11 N2 177.1(10) . . . . ?
C8 C7 C11 N2 -2.0(15) . . . . ?
C6 C7 C11 C12 1.6(15) . . . . ?
C8 C7 C11 C12 -177.6(9) . . . . ?
C3 C4 C12 N1 -2.1(14) . . . . ?
C5 C4 C12 N1 176.4(9) . . . . ?
C3 C4 C12 C11 177.1(9) . . . . ?
C5 C4 C12 C11 -4.3(14) . . . . ?
N2 C11 C12 N1 5.3(13) . . . . ?
C7 C11 C12 N1 -179.0(8) . . . . ?
N2 C11 C12 C4 -174.0(9) . . . . ?
C7 C11 C12 C4 1.7(14) . . . . ?
N3 C13 C14 C15 -0.3(17) . . . . ?
C13 C14 C15 C16 -1.0(16) . . . . ?
C14 C15 C16 C24 -0.4(17) . . . . ?
C14 C15 C16 C17 178.8(12) . . . . ?
C24 C16 C17 C18 -2(2) . . . . ?
C15 C16 C17 C18 178.4(13) . . . . ?
C16 C17 C18 C19 1(2) . . . . ?
C17 C18 C19 C23 0.6(19) . . . . ?
C17 C18 C19 C20 176.3(13) . . . . ?
C23 C19 C20 C21 -5.6(17) . . . . ?
C18 C19 C20 C21 178.7(13) . . . . ?
C19 C20 C21 C22 5(2) . . . . ?
C20 C21 C22 N4 -4.4(19) . . . . ?
C20 C19 C23 N4 5.0(15) . . . . ?
C18 C19 C23 N4 -179.0(10) . . . . ?
C20 C19 C23 C24 -176.6(10) . . . . ?
C18 C19 C23 C24 -0.7(15) . . . . ?
C17 C16 C24 N3 -176.1(11) . . . . ?
C15 C16 C24 N3 3.1(17) . . . . ?
C17 C16 C24 C23 2.4(17) . . . . ?
C15 C16 C24 C23 -178.4(10) . . . . ?
N4 C23 C24 N3 -3.8(14) . . . . ?
C19 C23 C24 N3 177.7(9) . . . . ?
N4 C23 C24 C16 177.6(10) . . . . ?
C19 C23 C24 C16 -0.8(15) . . . . ?
O2 C25 C26 C27 119.5(10) . . . . ?
O1 C25 C26 C27 -61.7(13) . . . . ?
O2 C25 C26 C31 -63.3(12) . . . . ?
O1 C25 C26 C31 115.6(10) . . . . ?
C31 C26 C27 F1 179.4(8) . . . . ?
C25 C26 C27 F1 -3.3(14) . . . . ?
C31 C26 C27 C28 -1.4(15) . . . . ?
C25 C26 C27 C28 175.9(9) . . . . ?
F1 C27 C28 F2 2.4(14) . . . . ?
C26 C27 C28 F2 -176.8(9) . . . . ?
F1 C27 C28 C29 -178.8(9) . . . . ?
C26 C27 C28 C29 2.0(16) . . . . ?
F2 C28 C29 F3 -0.2(16) . . . . ?
C27 C28 C29 F3 -179.1(10) . . . . ?
F2 C28 C29 C30 178.6(9) . . . . ?
C27 C28 C29 C30 -0.3(16) . . . . ?
F3 C29 C30 F4 1.8(16) . . . . ?
C28 C29 C30 F4 -177.0(10) . . . . ?
F3 C29 C30 C31 176.8(10) . . . . ?
C28 C29 C30 C31 -2.0(17) . . . . ?
F4 C30 C31 C26 177.6(9) . . . . ?
C29 C30 C31 C26 2.5(16) . . . . ?
F4 C30 C31 C32 -4.2(15) . . . . ?
C29 C30 C31 C32 -179.3(10) . . . . ?
C27 C26 C31 C30 -0.9(14) . . . . ?
C25 C26 C31 C30 -178.2(9) . . . . ?
C27 C26 C31 C32 -179.0(9) . . . . ?
C25 C26 C31 C32 3.6(13) . . . . ?
C30 C31 C32 O4 -72.3(13) . . . . ?
C26 C31 C32 O4 105.8(11) . . . . ?
C30 C31 C32 O3 106.4(11) . . . . ?
C26 C31 C32 O3 -75.6(11) . . . . ?
O6 C33 C34 C35 163.9(9) . . . . ?
O5 C33 C34 C35 -16.2(14) . . . . ?
O6 C33 C34 C39 -12.5(13) . . . . ?
O5 C33 C34 C39 167.4(9) . . . . ?
C39 C34 C35 F5 177.6(8) . . . . ?
C33 C34 C35 F5 1.3(14) . . . . ?
C39 C34 C35 C36 -0.6(14) . . . . ?
C33 C34 C35 C36 -177.0(9) . . . . ?
F5 C35 C36 F6 4.1(15) . . . . ?
C34 C35 C36 F6 -177.6(9) . . . . ?
F5 C35 C36 C37 -179.5(10) . . . . ?
C34 C35 C36 C37 -1.2(17) . . . . ?
C35 C36 C37 C38 2.1(18) . . . . ?
F6 C36 C37 C38 178.6(10) . . . . ?
C35 C36 C37 F7 -178.8(10) . . . . ?
F6 C36 C37 F7 -2.3(17) . . . . ?
F7 C37 C38 F8 -2.9(17) . . . . ?
C36 C37 C38 F8 176.2(10) . . . . ?
F7 C37 C38 C39 179.7(10) . . . . ?
C36 C37 C38 C39 -1.2(18) . . . . ?
F8 C38 C39 C34 -177.9(8) . . . . ?
C37 C38 C39 C34 -0.5(15) . . . . ?
F8 C38 C39 C40 0.5(14) . . . . ?
C37 C38 C39 C40 177.9(11) . . . . ?
C35 C34 C39 C38 1.4(13) . . . . ?
C33 C34 C39 C38 178.0(8) . . . . ?
C35 C34 C39 C40 -176.8(9) . . . . ?
C33 C34 C39 C40 -0.3(13) . . . . ?
C38 C39 C40 O8 84.9(11) . . . . ?
C34 C39 C40 O8 -96.9(11) . . . . ?
C38 C39 C40 O7 -86.9(11) . . . . ?
C34 C39 C40 O7 91.3(11) . . . . ?
O10 C41 C42 C43 86.5(10) . . . . ?
O9 C41 C42 C43 -91.1(10) . . . . ?
O10 C41 C42 C47 -91.5(10) . . . . ?
O9 C41 C42 C47 90.9(10) . . . . ?
C47 C42 C43 F9 -179.8(8) . . . . ?
C41 C42 C43 F9 2.1(13) . . . . ?
C47 C42 C43 C44 1.3(15) . . . . ?
C41 C42 C43 C44 -176.7(9) . . . . ?
F9 C43 C44 F10 0.9(15) . . . . ?
C42 C43 C44 F10 179.8(9) . . . . ?
F9 C43 C44 C45 -178.7(9) . . . . ?
C42 C43 C44 C45 0.2(16) . . . . ?
F10 C44 C45 F11 2.4(16) . . . . ?
C43 C44 C45 F11 -178.0(9) . . . . ?
F10 C44 C45 C46 178.4(10) . . . . ?
C43 C44 C45 C46 -2.0(16) . . . . ?
F11 C45 C46 F12 -1.0(15) . . . . ?
C44 C45 C46 F12 -177.0(9) . . . . ?
F11 C45 C46 C47 178.4(9) . . . . ?
C44 C45 C46 C47 2.4(16) . . . . ?
F12 C46 C47 C42 178.5(8) . . . . ?
C45 C46 C47 C42 -0.9(15) . . . . ?
F12 C46 C47 C48 -2.5(15) . . . . ?
C45 C46 C47 C48 178.1(10) . . . . ?
C43 C42 C47 C46 -1.0(13) . . . . ?
C41 C42 C47 C46 177.0(8) . . . . ?
C43 C42 C47 C48 180.0(9) . . . . ?
C41 C42 C47 C48 -2.1(13) . . . . ?
C46 C47 C48 O11 -151.9(10) . . . . ?
C42 C47 C48 O11 27.1(14) . . . . ?
C46 C47 C48 O12 23.1(14) . . . . ?
C42 C47 C48 O12 -157.9(8) . . . . ?
C46 C47 C48 Tb1 -13(3) . . . 2_656 ?
C42 C47 C48 Tb1 166(2) . . . 2_656 ?
C2 C1 N1 C12 -0.6(17) . . . . ?
C2 C1 N1 Tb1 171.8(10) . . . . ?
C4 C12 N1 C1 0.3(13) . . . . ?
C11 C12 N1 C1 -179.0(9) . . . . ?
C4 C12 N1 Tb1 -172.2(7) . . . . ?
C11 C12 N1 Tb1 8.5(10) . . . . ?
C9 C10 N2 C11 0.4(15) . . . . ?
C9 C10 N2 Tb1 -165.8(8) . . . . ?
C7 C11 N2 C10 1.2(14) . . . . ?
C12 C11 N2 C10 176.7(8) . . . . ?
C7 C11 N2 Tb1 168.3(7) . . . . ?
C12 C11 N2 Tb1 -16.2(11) . . . . ?
C14 C13 N3 C24 2.9(17) . . . . ?
C14 C13 N3 Tb2 -178.4(8) . . . . ?
C16 C24 N3 C13 -4.2(16) . . . . ?
C23 C24 N3 C13 177.3(10) . . . . ?
C16 C24 N3 Tb2 177.0(8) . . . . ?
C23 C24 N3 Tb2 -1.5(13) . . . . ?
C19 C23 N4 C22 -4.0(14) . . . . ?
C24 C23 N4 C22 177.6(9) . . . . ?
C19 C23 N4 Tb2 -174.5(7) . . . . ?
C24 C23 N4 Tb2 7.1(11) . . . . ?
C21 C22 N4 C23 3.6(15) . . . . ?
C21 C22 N4 Tb2 173.8(9) . . . . ?
O2 C25 O1 Tb1 62.9(19) . . . . ?
C26 C25 O1 Tb1 -115.7(12) . . . . ?
O1 C25 O2 Tb2 37(2) . . . . ?
C26 C25 O2 Tb2 -144.4(12) . . . . ?
O4 C32 O3 Tb1 -24.1(17) . . . 2_656 ?
C31 C32 O3 Tb1 157.4(7) . . . 2_656 ?
O6 C33 O5 Tb2 2.1(10) . . . . ?
C34 C33 O5 Tb2 -177.9(7) . . . . ?
O5 C33 O6 Tb2 -2.1(10) . . . . ?
C34 C33 O6 Tb2 177.9(7) . . . . ?
O8 C40 O7 Tb2 -169(3) . . . 2_665 ?
C39 C40 O7 Tb2 2(4) . . . 2_665 ?
O10 C41 O9 Tb2 111.1(15) . . . . ?
C42 C41 O9 Tb2 -71.6(16) . . . . ?
O9 C41 O10 Tb1 -98.5(10) . . . . ?
C42 C41 O10 Tb1 84.2(8) . . . . ?
O12 C48 O11 Tb1 -133.6(8) . . . . ?
C47 C48 O11 Tb1 41.1(14) . . . . ?
Tb1 C48 O11 Tb1 -128.1(8) 2_656 . . . ?
O12 C48 O11 Tb1 -5.5(9) . . . 2_656 ?
C47 C48 O11 Tb1 169.2(9) . . . 2_656 ?
O11 C48 O12 Tb1 6.7(11) . . . 2_656 ?
C47 C48 O12 Tb1 -168.3(7) . . . 2_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15B O8 0.86 1.97 2.810(14) 165.1 2_666
O15 H15A F4 0.73 2.48 3.057(14) 138.1 2_656
O14 H14B O4 0.88 2.14 3.002(11) 165.1 .
O14 H14A O15 0.85 1.77 2.604(13) 165.6 1_554
O13 H13B O4 0.88 1.97 2.802(10) 156.8 2_656
O13 H13A O5 0.86 2.00 2.783(9) 151.3 2_656
O13 H13A F5 0.86 2.23 2.849(9) 129.1 2_656
C22 H22 O6 0.93 2.29 2.940(12) 126.4 .
C14 H14 F8 0.93 2.54 3.256(12) 134.1 1_645
C14 H14 F7 0.93 2.52 3.394(14) 156.0 1_645
C10 H10 O3 0.93 2.61 3.244(11) 126.3 2_656
C9 H9 F10 0.93 2.59 3.150(13) 119.2 2_666
C1 H1 O12 0.93 2.36 2.937(12) 120.3 2_656
C1 H1 F12 0.93 2.61 3.512(12) 163.4 2_656

_refine_diff_density_max         1.111
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.218



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_audit_block_doi                 10.5517/cc14bpqw
_database_code_depnum_ccdc_archive 'CCDC 1052968'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H22 F12 N4 O15 Sm2'
_chemical_formula_weight         1423.39

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'
F F 0.0171 0.0103 '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'
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                   13.9748(5)
_cell_length_b                   14.1728(5)
_cell_length_c                   15.0597(6)
_cell_angle_alpha                63.6830(10)
_cell_angle_beta                 81.1270(10)
_cell_angle_gamma                65.5600(10)
_cell_volume                     2432.48(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8418
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      26.83

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_F_000             1380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    2.512
_shelx_estimated_absorpt_T_min   0.621
_shelx_estimated_absorpt_T_max   0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6206
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51139
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.891
_diffrn_reflns_theta_max         27.554
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11189
_reflns_number_gt                8868
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.288     0.127     0.995      86.4       7.3
         2     0.716     0.871     1.005      85.9       7.9
_platon_squeeze_details
 
The unit cell contains 4 water molecules, which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0413P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11189
_refine_ls_number_parameters     730
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.64632(2) -0.01400(2) 0.56149(2) 0.02125(6) Uani 1 1 d . . . . .
Sm2 Sm 0.60581(2) 0.23892(2) 0.14070(2) 0.02343(6) Uani 1 1 d . . . . .
C1 C 0.8961(3) -0.2247(3) 0.5717(3) 0.0383(9) Uani 1 1 d . . . . .
H1 H 0.8540 -0.2530 0.5574 0.046 Uiso 1 1 calc R U . . .
C2 C 1.0040(3) -0.2821(3) 0.5740(3) 0.0463(10) Uani 1 1 d . . . . .
H2 H 1.0331 -0.3470 0.5616 0.056 Uiso 1 1 calc R U . . .
C3 C 1.0665(3) -0.2421(4) 0.5947(3) 0.0473(11) Uani 1 1 d . . . . .
H3 H 1.1393 -0.2792 0.5962 0.057 Uiso 1 1 calc R U . . .
C4 C 1.0219(3) -0.1452(3) 0.6139(3) 0.0355(9) Uani 1 1 d . . . . .
C5 C 1.0820(3) -0.0954(4) 0.6336(3) 0.0430(10) Uani 1 1 d . . . . .
H5 H 1.1551 -0.1287 0.6341 0.052 Uiso 1 1 calc R U . . .
C6 C 1.0361(3) -0.0024(4) 0.6511(3) 0.0441(10) Uani 1 1 d . . . . .
H6 H 1.0775 0.0293 0.6614 0.053 Uiso 1 1 calc R U . . .
C7 C 0.9243(3) 0.0495(3) 0.6544(3) 0.0352(9) Uani 1 1 d . . . . .
C8 C 0.8729(3) 0.1426(3) 0.6793(3) 0.0420(10) Uani 1 1 d . . . . .
H8 H 0.9114 0.1754 0.6922 0.050 Uiso 1 1 calc R U . . .
C9 C 0.7663(3) 0.1845(3) 0.6847(3) 0.0411(9) Uani 1 1 d . . . . .
H9 H 0.7315 0.2437 0.7043 0.049 Uiso 1 1 calc R U . . .
C10 C 0.7101(3) 0.1371(3) 0.6602(3) 0.0343(8) Uani 1 1 d . . . . .
H10 H 0.6371 0.1688 0.6609 0.041 Uiso 1 1 calc R U . . .
C11 C 0.8615(3) 0.0048(3) 0.6345(2) 0.0274(7) Uani 1 1 d . . . . .
C12 C 0.9120(2) -0.0933(3) 0.6120(2) 0.0270(7) Uani 1 1 d . . . . .
C13 C 0.8500(3) 0.0509(3) 0.1188(3) 0.0458(10) Uani 1 1 d . . . . .
H13 H 0.8080 0.0118 0.1249 0.055 Uiso 1 1 calc R U . . .
C14 C 0.9578(4) -0.0011(4) 0.1095(3) 0.0565(12) Uani 1 1 d . . . . .
H14 H 0.9867 -0.0734 0.1098 0.068 Uiso 1 1 calc R U . . .
C15 C 1.0205(3) 0.0553(4) 0.0999(3) 0.0568(12) Uani 1 1 d . . . . .
H15 H 1.0926 0.0221 0.0934 0.068 Uiso 1 1 calc R U . . .
C16 C 0.9750(3) 0.1638(4) 0.1000(3) 0.0490(11) Uani 1 1 d . . . . .
C17 C 1.0348(3) 0.2271(5) 0.0942(4) 0.0689(15) Uani 1 1 d . . . . .
H17 H 1.1075 0.1959 0.0896 0.083 Uiso 1 1 calc R U . . .
C18 C 0.9889(4) 0.3298(5) 0.0952(4) 0.0710(15) Uani 1 1 d . . . . .
H18 H 1.0302 0.3682 0.0924 0.085 Uiso 1 1 calc R U . . .
C19 C 0.8775(3) 0.3820(4) 0.1004(3) 0.0501(11) Uani 1 1 d . . . . .
C20 C 0.8252(4) 0.4909(4) 0.0993(4) 0.0653(14) Uani 1 1 d . . . . .
H20 H 0.8633 0.5333 0.0949 0.078 Uiso 1 1 calc R U . . .
C21 C 0.7190(4) 0.5344(4) 0.1047(4) 0.0615(13) Uani 1 1 d . . . . .
H21 H 0.6835 0.6066 0.1039 0.074 Uiso 1 1 calc R U . . .
C22 C 0.6639(3) 0.4690(3) 0.1114(3) 0.0423(10) Uani 1 1 d . . . . .
H22 H 0.5911 0.4995 0.1153 0.051 Uiso 1 1 calc R U . . .
C23 C 0.8148(3) 0.3227(3) 0.1076(3) 0.0342(8) Uani 1 1 d . . . . .
C24 C 0.8656(3) 0.2098(3) 0.1089(3) 0.0360(9) Uani 1 1 d . . . . .
C25 C 0.6926(2) -0.0444(3) 0.3357(3) 0.0250(7) Uani 1 1 d . . . . .
C26 C 0.7272(3) -0.1585(3) 0.3294(2) 0.0254(7) Uani 1 1 d . . . . .
C27 C 0.8296(3) -0.2339(3) 0.3432(3) 0.0325(8) Uani 1 1 d . . . . .
C28 C 0.8598(3) -0.3387(3) 0.3413(3) 0.0379(9) Uani 1 1 d . . . . .
C29 C 0.7853(3) -0.3682(3) 0.3239(3) 0.0413(10) Uani 1 1 d . . . . .
C30 C 0.6829(3) -0.2936(3) 0.3081(3) 0.0365(9) Uani 1 1 d . . . . .
C31 C 0.6514(3) -0.1887(3) 0.3103(2) 0.0263(7) Uani 1 1 d . . . . .
C32 C 0.5362(3) -0.1090(3) 0.2959(3) 0.0274(7) Uani 1 1 d . . . . .
C33 C 0.3982(3) 0.3949(3) 0.1457(2) 0.0288(8) Uani 1 1 d . . . . .
C34 C 0.2922(3) 0.4807(3) 0.1500(2) 0.0281(8) Uani 1 1 d . . . . .
C35 C 0.2024(3) 0.4581(3) 0.1649(3) 0.0367(9) Uani 1 1 d . . . . .
C36 C 0.1053(3) 0.5372(3) 0.1680(3) 0.0423(10) Uani 1 1 d . . . . .
C37 C 0.0942(3) 0.6440(3) 0.1553(3) 0.0434(10) Uani 1 1 d . . . . .
C38 C 0.1835(3) 0.6677(3) 0.1405(3) 0.0355(9) Uani 1 1 d . . . . .
C39 C 0.2811(3) 0.5898(3) 0.1368(2) 0.0291(8) Uani 1 1 d . . . . .
C40 C 0.3711(3) 0.6313(3) 0.1176(3) 0.0280(8) Uani 1 1 d . . . . .
C41 C 0.6121(3) 0.2308(3) 0.3755(3) 0.0249(7) Uani 1 1 d . . . . .
C42 C 0.5127(3) 0.3187(3) 0.3925(2) 0.0239(7) Uani 1 1 d . . . . .
C43 C 0.5189(3) 0.4143(3) 0.3904(3) 0.0316(8) Uani 1 1 d . . . . .
C44 C 0.4325(3) 0.4966(3) 0.4077(3) 0.0328(8) Uani 1 1 d . . . . .
C45 C 0.3393(3) 0.4844(3) 0.4256(3) 0.0333(8) Uani 1 1 d . . . . .
C46 C 0.3305(3) 0.3911(3) 0.4248(3) 0.0301(8) Uani 1 1 d . . . . .
C47 C 0.4165(3) 0.3066(3) 0.4095(2) 0.0242(7) Uani 1 1 d . . . . .
C48 C 0.4079(3) 0.2036(3) 0.4115(2) 0.0233(7) Uani 1 1 d . . . . .
F1 F 0.90612(16) -0.20763(19) 0.35834(19) 0.0493(6) Uani 1 1 d . . . . .
F2 F 0.96125(17) -0.4121(2) 0.3584(2) 0.0589(7) Uani 1 1 d . . . . .
F3 F 0.8133(2) -0.4701(2) 0.3220(2) 0.0686(8) Uani 1 1 d . . . . .
F4 F 0.61052(18) -0.3257(2) 0.2932(2) 0.0582(7) Uani 1 1 d . . . . .
F5 F 0.20432(17) 0.35913(19) 0.1739(2) 0.0542(7) Uani 1 1 d . . . . .
F6 F 0.01863(18) 0.5133(2) 0.1817(2) 0.0690(8) Uani 1 1 d . . . . .
F7 F -0.00089(18) 0.7225(2) 0.1564(2) 0.0658(8) Uani 1 1 d . . . . .
F8 F 0.17047(18) 0.77255(19) 0.12779(18) 0.0509(6) Uani 1 1 d . . . . .
F9 F 0.61070(17) 0.42787(19) 0.37223(18) 0.0482(6) Uani 1 1 d . . . . .
F10 F 0.44080(18) 0.58799(18) 0.40617(18) 0.0487(6) Uani 1 1 d . . . . .
F11 F 0.25405(19) 0.56332(19) 0.4439(2) 0.0581(7) Uani 1 1 d . . . . .
F12 F 0.23505(16) 0.38672(18) 0.44191(18) 0.0484(6) Uani 1 1 d . . . . .
N1 N 0.8492(2) -0.1320(2) 0.5886(2) 0.0288(6) Uani 1 1 d . . . . .
N2 N 0.7553(2) 0.0493(2) 0.6361(2) 0.0261(6) Uani 1 1 d . . . . .
N3 N 0.8043(2) 0.1532(3) 0.1193(2) 0.0358(7) Uani 1 1 d . . . . .
N4 N 0.7090(2) 0.3667(2) 0.1125(2) 0.0306(7) Uani 1 1 d . . . . .
O1 O 0.70627(19) -0.0491(2) 0.41672(18) 0.0355(6) Uani 1 1 d . . . . .
O2 O 0.6510(2) 0.0425(2) 0.25869(18) 0.0403(6) Uani 1 1 d . . . . .
O3 O 0.49280(17) -0.1010(2) 0.37285(17) 0.0309(5) Uani 1 1 d . . . . .
O4 O 0.4946(2) -0.0595(2) 0.21165(19) 0.0415(6) Uani 1 1 d . . . . .
O5 O 0.4145(2) 0.2913(2) 0.1740(2) 0.0484(7) Uani 1 1 d . . . . .
O6 O 0.47215(19) 0.4274(2) 0.1144(2) 0.0427(7) Uani 1 1 d . . . . .
O7 O 0.38995(19) 0.6794(2) 0.02804(17) 0.0331(6) Uani 1 1 d . . . . .
O8 O 0.4107(2) 0.6226(2) 0.18928(19) 0.0459(7) Uani 1 1 d . . . . .
O9 O 0.62994(19) 0.2426(2) 0.28796(17) 0.0345(6) Uani 1 1 d . . . . .
O10 O 0.66934(17) 0.15591(19) 0.44896(17) 0.0271(5) Uani 1 1 d . . . . .
O11 O 0.48704(17) 0.11039(18) 0.43539(17) 0.0279(5) Uani 1 1 d . . . . .
O12 O 0.32058(18) 0.2135(2) 0.39009(19) 0.0357(6) Uani 1 1 d . . . . .
O13 O 0.65899(19) -0.1186(2) 0.74264(17) 0.0363(6) Uani 1 1 d D . . . .
H13A H 0.6593 -0.1839 0.7654 0.054 Uiso 1 1 d DR U . . .
H13B H 0.6187 -0.0775 0.7709 0.054 Uiso 1 1 d DR U . . .
O14 O 0.5643(3) 0.1269(3) 0.0784(2) 0.0714(11) Uani 1 1 d D . . . .
H14A H 0.5557 0.1460 0.0198 0.107 Uiso 1 1 d DR U . . .
H14B H 0.5506 0.0698 0.1132 0.107 Uiso 1 1 d DR U . . .
O15 O 0.5363(5) 0.1863(4) 0.8889(3) 0.133(2) Uani 1 1 d D . . . .
H15A H 0.4776 0.2072 0.8688 0.200 Uiso 1 1 d DR U . . .
H15B H 0.5383 0.2515 0.8580 0.200 Uiso 1 1 d DR 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 O10 2.373(2) . ?
Sm1 O3 2.373(2) 2_656 ?
Sm1 O1 2.399(2) . ?
Sm1 O12 2.436(2) 2_656 ?
Sm1 O13 2.453(2) . ?
Sm1 O11 2.599(2) . ?
Sm1 N1 2.614(3) . ?
Sm1 N2 2.634(3) . ?
Sm1 O11 2.714(2) 2_656 ?
Sm1 C48 2.930(3) 2_656 ?
Sm2 O7 2.281(2) 2_665 ?
Sm2 O9 2.320(2) . ?
Sm2 O2 2.411(2) . ?
Sm2 O6 2.438(2) . ?
Sm2 O14 2.447(3) . ?
Sm2 O5 2.495(2) . ?
Sm2 N3 2.560(3) . ?
Sm2 N4 2.614(3) . ?
Sm2 C33 2.843(3) . ?
C1 N1 1.324(4) . ?
C1 C2 1.383(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.355(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(5) . ?
C3 H3 0.9300 . ?
C4 C12 1.401(5) . ?
C4 C5 1.430(5) . ?
C5 C6 1.332(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.428(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.403(5) . ?
C7 C11 1.404(5) . ?
C8 C9 1.361(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.396(5) . ?
C9 H9 0.9300 . ?
C10 N2 1.326(4) . ?
C10 H10 0.9300 . ?
C11 N2 1.352(4) . ?
C11 C12 1.442(5) . ?
C12 N1 1.364(4) . ?
C13 N3 1.324(5) . ?
C13 C14 1.393(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.368(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.400(6) . ?
C15 H15 0.9300 . ?
C16 C24 1.404(5) . ?
C16 C17 1.429(6) . ?
C17 C18 1.331(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.427(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.402(6) . ?
C19 C23 1.409(5) . ?
C20 C21 1.357(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.395(5) . ?
C21 H21 0.9300 . ?
C22 N4 1.314(5) . ?
C22 H22 0.9300 . ?
C23 N4 1.350(4) . ?
C23 C24 1.450(5) . ?
C24 N3 1.348(5) . ?
C25 O1 1.233(4) . ?
C25 O2 1.244(4) . ?
C25 C26 1.527(4) . ?
C26 C27 1.365(5) . ?
C26 C31 1.403(4) . ?
C27 F1 1.346(4) . ?
C27 C28 1.378(5) . ?
C28 F2 1.347(4) . ?
C28 C29 1.367(5) . ?
C29 F3 1.344(4) . ?
C29 C30 1.361(5) . ?
C30 F4 1.350(4) . ?
C30 C31 1.379(5) . ?
C31 C32 1.517(5) . ?
C32 O4 1.241(4) . ?
C32 O3 1.251(4) . ?
C33 O6 1.247(4) . ?
C33 O5 1.260(4) . ?
C33 C34 1.491(5) . ?
C34 C35 1.382(5) . ?
C34 C39 1.412(5) . ?
C35 F5 1.338(4) . ?
C35 C36 1.367(5) . ?
C36 F6 1.351(4) . ?
C36 C37 1.382(5) . ?
C37 F7 1.338(4) . ?
C37 C38 1.383(5) . ?
C38 F8 1.346(4) . ?
C38 C39 1.367(5) . ?
C39 C40 1.537(5) . ?
C40 O8 1.223(4) . ?
C40 O7 1.256(4) . ?
C41 O10 1.233(4) . ?
C41 O9 1.251(4) . ?
C41 C42 1.513(5) . ?
C42 C43 1.379(4) . ?
C42 C47 1.396(4) . ?
C43 F9 1.345(4) . ?
C43 C44 1.376(5) . ?
C44 F10 1.338(4) . ?
C44 C45 1.354(5) . ?
C45 F11 1.348(4) . ?
C45 C46 1.382(5) . ?
C46 F12 1.341(4) . ?
C46 C47 1.379(5) . ?
C47 C48 1.500(4) . ?
C48 O12 1.247(4) . ?
C48 O11 1.261(4) . ?
C48 Sm1 2.930(3) 2_656 ?
O3 Sm1 2.373(2) 2_656 ?
O7 Sm2 2.281(2) 2_665 ?
O11 Sm1 2.714(2) 2_656 ?
O12 Sm1 2.436(2) 2_656 ?
O13 H13A 0.8304 . ?
O13 H13B 0.8431 . ?
O14 H14A 0.8124 . ?
O14 H14B 0.8303 . ?
O15 H15A 0.8043 . ?
O15 H15B 0.8415 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Sm1 O3 87.02(8) . 2_656 ?
O10 Sm1 O1 77.28(8) . . ?
O3 Sm1 O1 144.65(8) 2_656 . ?
O10 Sm1 O12 149.77(8) . 2_656 ?
O3 Sm1 O12 122.00(8) 2_656 2_656 ?
O1 Sm1 O12 73.70(8) . 2_656 ?
O10 Sm1 O13 133.98(8) . . ?
O3 Sm1 O13 72.20(8) 2_656 . ?
O1 Sm1 O13 139.69(8) . . ?
O12 Sm1 O13 69.55(8) 2_656 . ?
O10 Sm1 O11 72.06(7) . . ?
O3 Sm1 O11 70.74(8) 2_656 . ?
O1 Sm1 O11 74.32(8) . . ?
O12 Sm1 O11 107.40(7) 2_656 . ?
O13 Sm1 O11 132.43(8) . . ?
O10 Sm1 N1 92.15(8) . . ?
O3 Sm1 N1 139.37(8) 2_656 . ?
O1 Sm1 N1 73.50(9) . . ?
O12 Sm1 N1 71.72(8) 2_656 . ?
O13 Sm1 N1 79.71(9) . . ?
O11 Sm1 N1 146.56(8) . . ?
O10 Sm1 N2 65.77(8) . . ?
O3 Sm1 N2 80.61(8) 2_656 . ?
O1 Sm1 N2 119.43(8) . . ?
O12 Sm1 N2 122.93(8) 2_656 . ?
O13 Sm1 N2 70.51(8) . . ?
O11 Sm1 N2 129.63(7) . . ?
N1 Sm1 N2 62.39(8) . . ?
O10 Sm1 O11 133.62(7) . 2_656 ?
O3 Sm1 O11 86.25(7) 2_656 2_656 ?
O1 Sm1 O11 82.32(8) . 2_656 ?
O12 Sm1 O11 50.03(7) 2_656 2_656 ?
O13 Sm1 O11 86.55(7) . 2_656 ?
O11 Sm1 O11 62.42(8) . 2_656 ?
N1 Sm1 O11 121.18(8) . 2_656 ?
N2 Sm1 O11 156.12(8) . 2_656 ?
O10 Sm1 C48 147.25(8) . 2_656 ?
O3 Sm1 C48 106.52(8) 2_656 2_656 ?
O1 Sm1 C48 74.69(9) . 2_656 ?
O12 Sm1 C48 24.74(8) 2_656 2_656 ?
O13 Sm1 C48 78.75(8) . 2_656 ?
O11 Sm1 C48 84.25(8) . 2_656 ?
N1 Sm1 C48 95.81(9) . 2_656 ?
N2 Sm1 C48 144.66(9) . 2_656 ?
O11 Sm1 C48 25.45(8) 2_656 2_656 ?
O7 Sm2 O9 146.75(8) 2_665 . ?
O7 Sm2 O2 131.58(8) 2_665 . ?
O9 Sm2 O2 77.11(8) . . ?
O7 Sm2 O6 83.03(9) 2_665 . ?
O9 Sm2 O6 80.63(9) . . ?
O2 Sm2 O6 138.90(9) . . ?
O7 Sm2 O14 72.03(9) 2_665 . ?
O9 Sm2 O14 141.17(9) . . ?
O2 Sm2 O14 67.11(9) . . ?
O6 Sm2 O14 117.20(11) . . ?
O7 Sm2 O5 103.87(9) 2_665 . ?
O9 Sm2 O5 88.51(9) . . ?
O2 Sm2 O5 92.95(9) . . ?
O6 Sm2 O5 52.15(8) . . ?
O14 Sm2 O5 79.06(11) . . ?
O7 Sm2 N3 80.27(9) 2_665 . ?
O9 Sm2 N3 92.14(9) . . ?
O2 Sm2 N3 78.58(10) . . ?
O6 Sm2 N3 136.67(9) . . ?
O14 Sm2 N3 95.01(11) . . ?
O5 Sm2 N3 171.12(9) . . ?
O7 Sm2 N4 78.70(9) 2_665 . ?
O9 Sm2 N4 69.08(8) . . ?
O2 Sm2 N4 126.71(9) . . ?
O6 Sm2 N4 74.35(9) . . ?
O14 Sm2 N4 146.30(10) . . ?
O5 Sm2 N4 124.95(9) . . ?
N3 Sm2 N4 63.31(9) . . ?
O7 Sm2 C33 94.01(9) 2_665 . ?
O9 Sm2 C33 83.60(9) . . ?
O2 Sm2 C33 116.64(9) . . ?
O6 Sm2 C33 25.88(8) . . ?
O14 Sm2 C33 98.93(11) . . ?
O5 Sm2 C33 26.28(9) . . ?
N3 Sm2 C33 162.50(10) . . ?
N4 Sm2 C33 99.44(9) . . ?
N1 C1 C2 124.0(4) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C12 117.7(3) . . ?
C3 C4 C5 123.7(3) . . ?
C12 C4 C5 118.6(3) . . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C11 117.3(3) . . ?
C8 C7 C6 123.2(3) . . ?
C11 C7 C6 119.5(3) . . ?
C9 C8 C7 119.7(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 118.8(4) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 123.5(3) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C7 122.9(3) . . ?
N2 C11 C12 118.2(3) . . ?
C7 C11 C12 118.8(3) . . ?
N1 C12 C4 122.1(3) . . ?
N1 C12 C11 117.8(3) . . ?
C4 C12 C11 120.1(3) . . ?
N3 C13 C14 123.2(4) . . ?
N3 C13 H13 118.4 . . ?
C14 C13 H13 118.4 . . ?
C15 C14 C13 119.2(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.2(4) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C15 C16 C24 117.6(4) . . ?
C15 C16 C17 123.1(4) . . ?
C24 C16 C17 119.3(4) . . ?
C18 C17 C16 121.4(4) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 121.4(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C23 116.9(4) . . ?
C20 C19 C18 123.5(4) . . ?
C23 C19 C18 119.6(4) . . ?
C21 C20 C19 119.8(4) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 118.9(4) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
N4 C22 C21 123.7(4) . . ?
N4 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
N4 C23 C19 122.9(4) . . ?
N4 C23 C24 118.2(3) . . ?
C19 C23 C24 118.8(3) . . ?
N3 C24 C16 122.9(4) . . ?
N3 C24 C23 117.7(3) . . ?
C16 C24 C23 119.4(4) . . ?
O1 C25 O2 127.7(3) . . ?
O1 C25 C26 116.5(3) . . ?
O2 C25 C26 115.8(3) . . ?
C27 C26 C31 118.2(3) . . ?
C27 C26 C25 122.5(3) . . ?
C31 C26 C25 119.3(3) . . ?
F1 C27 C26 120.7(3) . . ?
F1 C27 C28 117.1(3) . . ?
C26 C27 C28 122.2(3) . . ?
F2 C28 C29 120.4(3) . . ?
F2 C28 C27 120.3(3) . . ?
C29 C28 C27 119.3(3) . . ?
F3 C29 C30 120.3(3) . . ?
F3 C29 C28 120.1(3) . . ?
C30 C29 C28 119.6(3) . . ?
F4 C30 C29 118.5(3) . . ?
F4 C30 C31 119.7(3) . . ?
C29 C30 C31 121.8(3) . . ?
C30 C31 C26 118.9(3) . . ?
C30 C31 C32 120.7(3) . . ?
C26 C31 C32 120.5(3) . . ?
O4 C32 O3 126.8(3) . . ?
O4 C32 C31 118.4(3) . . ?
O3 C32 C31 114.8(3) . . ?
O6 C33 O5 119.8(3) . . ?
O6 C33 C34 118.5(3) . . ?
O5 C33 C34 121.7(3) . . ?
O6 C33 Sm2 58.58(17) . . ?
O5 C33 Sm2 61.23(18) . . ?
C34 C33 Sm2 176.4(2) . . ?
C35 C34 C39 117.8(3) . . ?
C35 C34 C33 122.2(3) . . ?
C39 C34 C33 120.0(3) . . ?
F5 C35 C36 115.7(3) . . ?
F5 C35 C34 122.2(3) . . ?
C36 C35 C34 122.1(3) . . ?
F6 C36 C35 120.8(4) . . ?
F6 C36 C37 118.9(3) . . ?
C35 C36 C37 120.2(3) . . ?
F7 C37 C36 120.5(3) . . ?
F7 C37 C38 121.1(4) . . ?
C36 C37 C38 118.3(3) . . ?
F8 C38 C39 120.6(3) . . ?
F8 C38 C37 117.2(3) . . ?
C39 C38 C37 122.2(3) . . ?
C38 C39 C34 119.4(3) . . ?
C38 C39 C40 115.2(3) . . ?
C34 C39 C40 125.4(3) . . ?
O8 C40 O7 126.9(3) . . ?
O8 C40 C39 117.4(3) . . ?
O7 C40 C39 115.4(3) . . ?
O10 C41 O9 126.1(3) . . ?
O10 C41 C42 116.9(3) . . ?
O9 C41 C42 117.1(3) . . ?
C43 C42 C47 119.6(3) . . ?
C43 C42 C41 117.8(3) . . ?
C47 C42 C41 122.7(3) . . ?
F9 C43 C44 118.8(3) . . ?
F9 C43 C42 120.1(3) . . ?
C44 C43 C42 121.2(3) . . ?
F10 C44 C45 120.6(3) . . ?
F10 C44 C43 120.0(3) . . ?
C45 C44 C43 119.4(3) . . ?
F11 C45 C44 120.4(3) . . ?
F11 C45 C46 119.3(3) . . ?
C44 C45 C46 120.4(3) . . ?
F12 C46 C47 122.4(3) . . ?
F12 C46 C45 116.4(3) . . ?
C47 C46 C45 121.1(3) . . ?
C46 C47 C42 118.3(3) . . ?
C46 C47 C48 121.3(3) . . ?
C42 C47 C48 120.4(3) . . ?
O12 C48 O11 121.9(3) . . ?
O12 C48 C47 117.8(3) . . ?
O11 C48 C47 120.3(3) . . ?
O12 C48 Sm1 54.86(16) . 2_656 ?
O11 C48 Sm1 67.66(16) . 2_656 ?
C47 C48 Sm1 168.5(2) . 2_656 ?
C1 N1 C12 117.4(3) . . ?
C1 N1 Sm1 122.1(2) . . ?
C12 N1 Sm1 120.2(2) . . ?
C10 N2 C11 117.6(3) . . ?
C10 N2 Sm1 122.0(2) . . ?
C11 N2 Sm1 119.4(2) . . ?
C13 N3 C24 117.9(3) . . ?
C13 N3 Sm2 120.7(3) . . ?
C24 N3 Sm2 121.4(2) . . ?
C22 N4 C23 117.7(3) . . ?
C22 N4 Sm2 122.9(2) . . ?
C23 N4 Sm2 119.1(2) . . ?
C25 O1 Sm1 153.2(2) . . ?
C25 O2 Sm2 155.8(2) . . ?
C32 O3 Sm1 145.8(2) . 2_656 ?
C33 O5 Sm2 92.5(2) . . ?
C33 O6 Sm2 95.5(2) . . ?
C40 O7 Sm2 167.8(2) . 2_665 ?
C41 O9 Sm2 156.0(2) . . ?
C41 O10 Sm1 125.4(2) . . ?
C48 O11 Sm1 139.8(2) . . ?
C48 O11 Sm1 86.89(18) . 2_656 ?
Sm1 O11 Sm1 117.58(8) . 2_656 ?
C48 O12 Sm1 100.4(2) . 2_656 ?
Sm1 O13 H13A 116.4 . . ?
Sm1 O13 H13B 112.3 . . ?
H13A O13 H13B 114.8 . . ?
Sm2 O14 H14A 123.2 . . ?
Sm2 O14 H14B 125.4 . . ?
H14A O14 H14B 111.1 . . ?
H15A O15 H15B 93.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.0(7) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C3 C4 C12 0.7(6) . . . . ?
C2 C3 C4 C5 -178.1(4) . . . . ?
C3 C4 C5 C6 179.7(4) . . . . ?
C12 C4 C5 C6 0.9(6) . . . . ?
C4 C5 C6 C7 2.1(6) . . . . ?
C5 C6 C7 C8 175.4(4) . . . . ?
C5 C6 C7 C11 -2.8(6) . . . . ?
C11 C7 C8 C9 0.8(6) . . . . ?
C6 C7 C8 C9 -177.4(4) . . . . ?
C7 C8 C9 C10 -3.1(6) . . . . ?
C8 C9 C10 N2 3.2(6) . . . . ?
C8 C7 C11 N2 1.7(5) . . . . ?
C6 C7 C11 N2 -180.0(3) . . . . ?
C8 C7 C11 C12 -177.9(3) . . . . ?
C6 C7 C11 C12 0.4(5) . . . . ?
C3 C4 C12 N1 -2.4(5) . . . . ?
C5 C4 C12 N1 176.4(3) . . . . ?
C3 C4 C12 C11 177.9(3) . . . . ?
C5 C4 C12 C11 -3.2(5) . . . . ?
N2 C11 C12 N1 3.3(5) . . . . ?
C7 C11 C12 N1 -177.1(3) . . . . ?
N2 C11 C12 C4 -177.1(3) . . . . ?
C7 C11 C12 C4 2.5(5) . . . . ?
N3 C13 C14 C15 -0.4(7) . . . . ?
C13 C14 C15 C16 0.2(7) . . . . ?
C14 C15 C16 C24 -0.7(6) . . . . ?
C14 C15 C16 C17 177.6(4) . . . . ?
C15 C16 C17 C18 -179.5(5) . . . . ?
C24 C16 C17 C18 -1.3(8) . . . . ?
C16 C17 C18 C19 -1.1(9) . . . . ?
C17 C18 C19 C20 -178.4(5) . . . . ?
C17 C18 C19 C23 1.9(8) . . . . ?
C23 C19 C20 C21 -0.2(7) . . . . ?
C18 C19 C20 C21 -179.9(5) . . . . ?
C19 C20 C21 C22 0.1(8) . . . . ?
C20 C21 C22 N4 -0.2(8) . . . . ?
C20 C19 C23 N4 0.5(6) . . . . ?
C18 C19 C23 N4 -179.7(4) . . . . ?
C20 C19 C23 C24 179.9(4) . . . . ?
C18 C19 C23 C24 -0.4(6) . . . . ?
C15 C16 C24 N3 1.4(6) . . . . ?
C17 C16 C24 N3 -176.9(4) . . . . ?
C15 C16 C24 C23 -179.0(4) . . . . ?
C17 C16 C24 C23 2.7(6) . . . . ?
N4 C23 C24 N3 -2.9(5) . . . . ?
C19 C23 C24 N3 177.7(4) . . . . ?
N4 C23 C24 C16 177.5(3) . . . . ?
C19 C23 C24 C16 -1.9(5) . . . . ?
O1 C25 C26 C27 -63.4(4) . . . . ?
O2 C25 C26 C27 118.5(4) . . . . ?
O1 C25 C26 C31 115.6(4) . . . . ?
O2 C25 C26 C31 -62.5(4) . . . . ?
C31 C26 C27 F1 177.7(3) . . . . ?
C25 C26 C27 F1 -3.3(5) . . . . ?
C31 C26 C27 C28 -1.6(5) . . . . ?
C25 C26 C27 C28 177.4(3) . . . . ?
F1 C27 C28 F2 2.9(5) . . . . ?
C26 C27 C28 F2 -177.8(3) . . . . ?
F1 C27 C28 C29 -178.5(4) . . . . ?
C26 C27 C28 C29 0.8(6) . . . . ?
F2 C28 C29 F3 -1.2(6) . . . . ?
C27 C28 C29 F3 -179.8(4) . . . . ?
F2 C28 C29 C30 179.1(4) . . . . ?
C27 C28 C29 C30 0.5(6) . . . . ?
F3 C29 C30 F4 1.8(6) . . . . ?
C28 C29 C30 F4 -178.6(4) . . . . ?
F3 C29 C30 C31 179.4(3) . . . . ?
C28 C29 C30 C31 -0.9(6) . . . . ?
F4 C30 C31 C26 177.7(3) . . . . ?
C29 C30 C31 C26 0.1(6) . . . . ?
F4 C30 C31 C32 -0.3(5) . . . . ?
C29 C30 C31 C32 -177.9(4) . . . . ?
C27 C26 C31 C30 1.2(5) . . . . ?
C25 C26 C31 C30 -177.9(3) . . . . ?
C27 C26 C31 C32 179.1(3) . . . . ?
C25 C26 C31 C32 0.1(5) . . . . ?
C30 C31 C32 O4 -72.6(4) . . . . ?
C26 C31 C32 O4 109.5(4) . . . . ?
C30 C31 C32 O3 107.1(4) . . . . ?
C26 C31 C32 O3 -70.9(4) . . . . ?
O6 C33 C34 C35 167.1(3) . . . . ?
O5 C33 C34 C35 -13.9(5) . . . . ?
O6 C33 C34 C39 -11.7(5) . . . . ?
O5 C33 C34 C39 167.2(3) . . . . ?
C39 C34 C35 F5 177.1(3) . . . . ?
C33 C34 C35 F5 -1.7(6) . . . . ?
C39 C34 C35 C36 -0.6(6) . . . . ?
C33 C34 C35 C36 -179.5(4) . . . . ?
F5 C35 C36 F6 1.4(6) . . . . ?
C34 C35 C36 F6 179.3(4) . . . . ?
F5 C35 C36 C37 -177.4(4) . . . . ?
C34 C35 C36 C37 0.5(6) . . . . ?
F6 C36 C37 F7 -0.1(6) . . . . ?
C35 C36 C37 F7 178.7(4) . . . . ?
F6 C36 C37 C38 -179.4(4) . . . . ?
C35 C36 C37 C38 -0.6(6) . . . . ?
F7 C37 C38 F8 0.4(6) . . . . ?
C36 C37 C38 F8 179.7(4) . . . . ?
F7 C37 C38 C39 -178.4(4) . . . . ?
C36 C37 C38 C39 0.8(6) . . . . ?
F8 C38 C39 C34 -179.7(3) . . . . ?
C37 C38 C39 C34 -0.9(6) . . . . ?
F8 C38 C39 C40 0.0(5) . . . . ?
C37 C38 C39 C40 178.8(3) . . . . ?
C35 C34 C39 C38 0.8(5) . . . . ?
C33 C34 C39 C38 179.7(3) . . . . ?
C35 C34 C39 C40 -178.9(3) . . . . ?
C33 C34 C39 C40 0.0(5) . . . . ?
C38 C39 C40 O8 84.8(4) . . . . ?
C34 C39 C40 O8 -95.4(4) . . . . ?
C38 C39 C40 O7 -89.6(4) . . . . ?
C34 C39 C40 O7 90.1(4) . . . . ?
O10 C41 C42 C43 87.8(4) . . . . ?
O9 C41 C42 C43 -90.6(4) . . . . ?
O10 C41 C42 C47 -92.6(4) . . . . ?
O9 C41 C42 C47 89.1(4) . . . . ?
C47 C42 C43 F9 -178.7(3) . . . . ?
C41 C42 C43 F9 0.9(5) . . . . ?
C47 C42 C43 C44 2.0(5) . . . . ?
C41 C42 C43 C44 -178.4(3) . . . . ?
F9 C43 C44 F10 0.1(5) . . . . ?
C42 C43 C44 F10 179.3(3) . . . . ?
F9 C43 C44 C45 179.7(3) . . . . ?
C42 C43 C44 C45 -1.0(6) . . . . ?
F10 C44 C45 F11 -1.1(6) . . . . ?
C43 C44 C45 F11 179.2(3) . . . . ?
F10 C44 C45 C46 178.5(3) . . . . ?
C43 C44 C45 C46 -1.2(6) . . . . ?
F11 C45 C46 F12 0.6(5) . . . . ?
C44 C45 C46 F12 -179.1(3) . . . . ?
F11 C45 C46 C47 -178.0(3) . . . . ?
C44 C45 C46 C47 2.4(6) . . . . ?
F12 C46 C47 C42 -179.8(3) . . . . ?
C45 C46 C47 C42 -1.4(5) . . . . ?
F12 C46 C47 C48 -0.2(5) . . . . ?
C45 C46 C47 C48 178.2(3) . . . . ?
C43 C42 C47 C46 -0.8(5) . . . . ?
C41 C42 C47 C46 179.6(3) . . . . ?
C43 C42 C47 C48 179.6(3) . . . . ?
C41 C42 C47 C48 0.0(5) . . . . ?
C46 C47 C48 O12 26.5(5) . . . . ?
C42 C47 C48 O12 -153.9(3) . . . . ?
C46 C47 C48 O11 -152.7(3) . . . . ?
C42 C47 C48 O11 26.9(5) . . . . ?
C46 C47 C48 Sm1 -21.5(13) . . . 2_656 ?
C42 C47 C48 Sm1 158.1(10) . . . 2_656 ?
C2 C1 N1 C12 -1.7(6) . . . . ?
C2 C1 N1 Sm1 172.3(3) . . . . ?
C4 C12 N1 C1 2.9(5) . . . . ?
C11 C12 N1 C1 -177.5(3) . . . . ?
C4 C12 N1 Sm1 -171.2(3) . . . . ?
C11 C12 N1 Sm1 8.5(4) . . . . ?
C9 C10 N2 C11 -0.7(5) . . . . ?
C9 C10 N2 Sm1 -169.3(3) . . . . ?
C7 C11 N2 C10 -1.8(5) . . . . ?
C12 C11 N2 C10 177.8(3) . . . . ?
C7 C11 N2 Sm1 167.1(3) . . . . ?
C12 C11 N2 Sm1 -13.3(4) . . . . ?
C14 C13 N3 C24 1.0(6) . . . . ?
C14 C13 N3 Sm2 -178.6(3) . . . . ?
C16 C24 N3 C13 -1.6(6) . . . . ?
C23 C24 N3 C13 178.8(3) . . . . ?
C16 C24 N3 Sm2 178.1(3) . . . . ?
C23 C24 N3 Sm2 -1.6(4) . . . . ?
C21 C22 N4 C23 0.5(6) . . . . ?
C21 C22 N4 Sm2 174.5(4) . . . . ?
C19 C23 N4 C22 -0.7(6) . . . . ?
C24 C23 N4 C22 179.9(3) . . . . ?
C19 C23 N4 Sm2 -174.9(3) . . . . ?
C24 C23 N4 Sm2 5.7(4) . . . . ?
O2 C25 O1 Sm1 59.2(7) . . . . ?
C26 C25 O1 Sm1 -118.6(5) . . . . ?
O1 C25 O2 Sm2 33.1(8) . . . . ?
C26 C25 O2 Sm2 -149.1(5) . . . . ?
O4 C32 O3 Sm1 -24.8(6) . . . 2_656 ?
C31 C32 O3 Sm1 155.6(3) . . . 2_656 ?
O6 C33 O5 Sm2 1.4(4) . . . . ?
C34 C33 O5 Sm2 -177.6(3) . . . . ?
O5 C33 O6 Sm2 -1.4(4) . . . . ?
C34 C33 O6 Sm2 177.5(3) . . . . ?
O8 C40 O7 Sm2 -170.5(8) . . . 2_665 ?
C39 C40 O7 Sm2 3.3(13) . . . 2_665 ?
O10 C41 O9 Sm2 109.4(6) . . . . ?
C42 C41 O9 Sm2 -72.5(6) . . . . ?
O9 C41 O10 Sm1 -99.1(3) . . . . ?
C42 C41 O10 Sm1 82.8(3) . . . . ?
O12 C48 O11 Sm1 -139.4(3) . . . . ?
C47 C48 O11 Sm1 39.8(5) . . . . ?
Sm1 C48 O11 Sm1 -130.9(3) 2_656 . . . ?
O12 C48 O11 Sm1 -8.5(3) . . . 2_656 ?
C47 C48 O11 Sm1 170.6(3) . . . 2_656 ?
O11 C48 O12 Sm1 9.6(3) . . . 2_656 ?
C47 C48 O12 Sm1 -169.5(2) . . . 2_656 ?

_refine_diff_density_max         1.031
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.142



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_audit_block_doi                 10.5517/cc14bprx
_database_code_depnum_ccdc_archive 'CCDC 1052969'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H22 Dy2 F12 N4 O15'
_chemical_formula_weight         1447.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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                   14.0352(6)
_cell_length_b                   14.0913(6)
_cell_length_c                   14.8999(6)
_cell_angle_alpha                64.1260(10)
_cell_angle_beta                 80.6990(10)
_cell_angle_gamma                65.5260(10)
_cell_volume                     2412.52(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9099
_cell_measurement_theta_min      3.0399
_cell_measurement_theta_max      27.5664

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_F_000             1396
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    3.196
_shelx_estimated_absorpt_T_min   0.553
_shelx_estimated_absorpt_T_max   0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5534
_exptl_absorpt_correction_T_max  0.5819
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  bruker-CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49488
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.985
_diffrn_reflns_theta_max         27.601
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11134
_reflns_number_gt                10158
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.220     0.876     1.004      85.0       3.8
         2     0.780     0.124     0.996      85.0       3.3
_platon_squeeze_details

The unit cell contains 4 water molecules, which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0301P)²+3.0368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11134
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy2 Dy 0.10612(2) 0.24123(2) 0.14175(2) 0.02312(5) Uani 1 1 d . . . . .
Dy1 Dy 0.15216(2) -0.00789(2) 0.55665(2) 0.02466(5) Uani 1 1 d . . . . .
F8 F -0.33078(19) 0.77333(17) 0.12375(18) 0.0489(6) Uani 1 1 d . . . . .
F7 F -0.49941(18) 0.7200(2) 0.1538(2) 0.0610(7) Uani 1 1 d . . . . .
F6 F -0.47730(18) 0.5082(2) 0.1830(2) 0.0657(8) Uani 1 1 d . . . . .
F5 F -0.29041(18) 0.35258(19) 0.1798(2) 0.0568(7) Uani 1 1 d . . . . .
F4 F 0.10659(19) -0.3231(2) 0.2994(2) 0.0562(6) Uani 1 1 d . . . . .
F3 F 0.3092(2) -0.46827(19) 0.3246(2) 0.0658(8) Uani 1 1 d . . . . .
F2 F 0.45654(18) -0.4075(2) 0.3564(2) 0.0567(6) Uani 1 1 d . . . . .
F1 F 0.40385(16) -0.20071(19) 0.35230(19) 0.0469(5) Uani 1 1 d . . . . .
F9 F 0.10794(18) 0.43307(19) 0.36985(19) 0.0485(6) Uani 1 1 d . . . . .
F10 F -0.0652(2) 0.59083(17) 0.40570(19) 0.0504(6) Uani 1 1 d . . . . .
F11 F -0.2492(2) 0.56082(19) 0.4421(2) 0.0612(7) Uani 1 1 d . . . . .
F12 F -0.26068(16) 0.37868(18) 0.44271(19) 0.0488(6) Uani 1 1 d . . . . .
O6 O -0.02614(19) 0.42494(19) 0.1156(2) 0.0409(6) Uani 1 1 d . . . . .
O5 O -0.0804(2) 0.28668(19) 0.1844(2) 0.0473(7) Uani 1 1 d . . . . .
O8 O -0.0900(2) 0.6245(2) 0.18746(18) 0.0446(6) Uani 1 1 d . . . . .
O7 O -0.1094(2) 0.6780(2) 0.02514(16) 0.0342(5) Uani 1 1 d . . . . .
O4 O -0.0059(2) -0.0535(2) 0.21303(18) 0.0429(6) Uani 1 1 d . . . . .
O3 O -0.01132(18) -0.10120(19) 0.37646(16) 0.0310(5) Uani 1 1 d . . . . .
O2 O 0.1456(2) 0.04907(19) 0.25691(18) 0.0370(6) Uani 1 1 d . . . . .
O1 O 0.2146(2) -0.0393(2) 0.41061(19) 0.0424(6) Uani 1 1 d . . . . .
O10 O 0.17410(18) 0.16030(19) 0.44898(17) 0.0322(5) Uani 1 1 d . . . . .
O9 O 0.1354(2) 0.24209(19) 0.28663(16) 0.0337(5) Uani 1 1 d . . . . .
O12 O -0.1661(2) 0.1923(2) 0.4084(2) 0.0510(7) Uani 1 1 d . . . . .
O11 O 0.0038(2) 0.10664(18) 0.43434(17) 0.0371(6) Uani 1 1 d . . . . .
O13 O 0.1597(2) -0.11622(19) 0.73462(18) 0.0359(5) Uani 1 1 d . . . . .
H13C H 0.1277 -0.0648 0.7668 0.054 Uiso 1 1 d R U . . .
H13D H 0.2315 -0.1612 0.7568 0.054 Uiso 1 1 d R U . . .
O14 O 0.0649(3) 0.1324(3) 0.0790(2) 0.0683(10) Uani 1 1 d . . . . .
H14C H 0.0287 0.1819 0.0157 0.102 Uiso 1 1 d R U . . .
H14D H 0.0211 0.0969 0.1254 0.102 Uiso 1 1 d R U . . .
N1 N 0.3468(2) -0.1307(2) 0.5865(2) 0.0285(6) Uani 1 1 d . . . . .
N2 N 0.2558(2) 0.0514(2) 0.63518(19) 0.0280(5) Uani 1 1 d . . . . .
N4 N 0.2063(2) 0.3685(2) 0.1115(2) 0.0309(6) Uani 1 1 d . . . . .
N3 N 0.2989(2) 0.1531(2) 0.1199(2) 0.0319(6) Uani 1 1 d . . . . .
C1 C 0.3912(3) -0.2243(3) 0.5692(3) 0.0389(8) Uani 1 1 d . . . . .
H1A H 0.3482 -0.2505 0.5532 0.047 Uiso 1 1 calc R U . . .
C2 C 0.4992(3) -0.2853(3) 0.5737(3) 0.0486(10) Uani 1 1 d . . . . .
H2A H 0.5271 -0.3516 0.5626 0.058 Uiso 1 1 calc R U . . .
C3 C 0.5630(3) -0.2466(3) 0.5946(3) 0.0460(9) Uani 1 1 d . . . . .
H3A H 0.6353 -0.2853 0.5962 0.055 Uiso 1 1 calc R U . . .
C4 C 0.5200(3) -0.1484(3) 0.6137(3) 0.0344(7) Uani 1 1 d . . . . .
C5 C 0.5814(3) -0.1002(4) 0.6340(3) 0.0430(9) Uani 1 1 d . . . . .
H5A H 0.6541 -0.1352 0.6349 0.052 Uiso 1 1 calc R U . . .
C6 C 0.5368(3) -0.0059(4) 0.6518(3) 0.0440(9) Uani 1 1 d . . . . .
H6A H 0.5788 0.0252 0.6621 0.053 Uiso 1 1 calc R U . . .
C7 C 0.4253(3) 0.0478(3) 0.6551(3) 0.0346(7) Uani 1 1 d . . . . .
C8 C 0.3742(3) 0.1417(3) 0.6806(3) 0.0433(9) Uani 1 1 d . . . . .
H8A H 0.4132 0.1740 0.6938 0.052 Uiso 1 1 calc R U . . .
C9 C 0.2685(3) 0.1853(3) 0.6860(3) 0.0410(8) Uani 1 1 d . . . . .
H9A H 0.2345 0.2446 0.7065 0.049 Uiso 1 1 calc R U . . .
C10 C 0.2113(3) 0.1393(3) 0.6601(3) 0.0340(7) Uani 1 1 d . . . . .
H10A H 0.1386 0.1723 0.6603 0.041 Uiso 1 1 calc R U . . .
C11 C 0.3616(2) 0.0046(3) 0.6340(2) 0.0273(6) Uani 1 1 d . . . . .
C12 C 0.4103(2) -0.0944(3) 0.6109(2) 0.0282(6) Uani 1 1 d . . . . .
C22 C 0.1609(3) 0.4730(3) 0.1089(3) 0.0429(9) Uani 1 1 d . . . . .
H13A H 0.0883 0.5052 0.1110 0.052 Uiso 1 1 calc R U . . .
C21 C 0.2173(4) 0.5369(4) 0.1031(4) 0.0618(13) Uani 1 1 d . . . . .
H14A H 0.1826 0.6098 0.1019 0.074 Uiso 1 1 calc R U . . .
C20 C 0.3229(4) 0.4920(5) 0.0991(4) 0.0680(14) Uani 1 1 d . . . . .
H15A H 0.3612 0.5338 0.0958 0.082 Uiso 1 1 calc R U . . .
C19 C 0.3749(3) 0.3820(4) 0.1000(3) 0.0500(10) Uani 1 1 d . . . . .
C18 C 0.4855(4) 0.3288(5) 0.0950(4) 0.0663(14) Uani 1 1 d . . . . .
H17A H 0.5270 0.3669 0.0926 0.080 Uiso 1 1 calc R U . . .
C17 C 0.5313(3) 0.2249(5) 0.0937(4) 0.0644(13) Uani 1 1 d . . . . .
H18A H 0.6036 0.1934 0.0881 0.077 Uiso 1 1 calc R U . . .
C16 C 0.4703(3) 0.1618(4) 0.1008(3) 0.0455(9) Uani 1 1 d . . . . .
C15 C 0.5144(3) 0.0521(4) 0.1012(3) 0.0525(11) Uani 1 1 d . . . . .
H20A H 0.5863 0.0173 0.0953 0.063 Uiso 1 1 calc R U . . .
C14 C 0.4511(4) -0.0026(4) 0.1104(3) 0.0538(11) Uani 1 1 d . . . . .
H21A H 0.4792 -0.0749 0.1100 0.065 Uiso 1 1 calc R U . . .
C13 C 0.3440(3) 0.0498(3) 0.1203(3) 0.0413(8) Uani 1 1 d . . . . .
H22A H 0.3020 0.0104 0.1276 0.050 Uiso 1 1 calc R U . . .
C24 C 0.3605(3) 0.2099(3) 0.1089(2) 0.0348(7) Uani 1 1 d . . . . .
C23 C 0.3121(3) 0.3232(3) 0.1072(3) 0.0353(7) Uani 1 1 d . . . . .
C33 C -0.0982(3) 0.3912(3) 0.1508(2) 0.0280(6) Uani 1 1 d . . . . .
C34 C -0.2054(3) 0.4779(3) 0.1519(2) 0.0292(7) Uani 1 1 d . . . . .
C35 C -0.2942(3) 0.4534(3) 0.1685(3) 0.0376(8) Uani 1 1 d . . . . .
C36 C -0.3900(3) 0.5326(3) 0.1682(3) 0.0403(8) Uani 1 1 d . . . . .
C37 C -0.4038(3) 0.6413(3) 0.1550(3) 0.0429(9) Uani 1 1 d . . . . .
C38 C -0.3164(3) 0.6667(3) 0.1387(3) 0.0354(7) Uani 1 1 d . . . . .
C39 C -0.2177(3) 0.5888(3) 0.1358(2) 0.0286(6) Uani 1 1 d . . . . .
C40 C -0.1295(3) 0.6315(2) 0.1163(2) 0.0277(6) Uani 1 1 d . . . . .
C32 C 0.0339(2) -0.1054(3) 0.2980(2) 0.0273(6) Uani 1 1 d . . . . .
C31 C 0.1486(3) -0.1837(3) 0.3113(2) 0.0274(6) Uani 1 1 d . . . . .
C30 C 0.1789(3) -0.2905(3) 0.3114(3) 0.0366(8) Uani 1 1 d . . . . .
C29 C 0.2819(3) -0.3658(3) 0.3256(3) 0.0425(9) Uani 1 1 d . . . . .
C28 C 0.3570(3) -0.3348(3) 0.3404(3) 0.0378(8) Uani 1 1 d . . . . .
C27 C 0.3271(3) -0.2279(3) 0.3402(3) 0.0321(7) Uani 1 1 d . . . . .
C26 C 0.2243(2) -0.1516(3) 0.3273(2) 0.0266(6) Uani 1 1 d . . . . .
C25 C 0.1924(2) -0.0368(3) 0.3330(2) 0.0266(6) Uani 1 1 d . . . . .
C41 C 0.1159(2) 0.2319(2) 0.3741(2) 0.0253(6) Uani 1 1 d . . . . .
C42 C 0.0150(2) 0.3187(2) 0.3918(2) 0.0244(6) Uani 1 1 d . . . . .
C43 C 0.0179(3) 0.4164(3) 0.3895(2) 0.0286(6) Uani 1 1 d . . . . .
C44 C -0.0695(3) 0.4975(3) 0.4067(3) 0.0324(7) Uani 1 1 d . . . . .
C45 C -0.1627(3) 0.4828(3) 0.4247(3) 0.0348(7) Uani 1 1 d . . . . .
C46 C -0.1667(3) 0.3856(3) 0.4252(2) 0.0307(7) Uani 1 1 d . . . . .
C47 C -0.0785(2) 0.3016(2) 0.4112(2) 0.0247(6) Uani 1 1 d . . . . .
C48 C -0.0795(3) 0.1921(3) 0.4183(2) 0.0284(7) Uani 1 1 d . . . . .
O15 O 0.0331(5) 0.1882(4) 0.8894(3) 0.130(2) Uani 1 1 d . . . . .
H15C H -0.0122 0.1570 0.8808 0.195 Uiso 1 1 d R U . . .
H15E H 0.0315 0.2539 0.8296 0.195 Uiso 1 1 d 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
Dy2 O7 2.240(2) 2_565 ?
Dy2 O9 2.268(2) . ?
Dy2 O2 2.365(2) . ?
Dy2 O6 2.382(2) . ?
Dy2 O14 2.391(3) . ?
Dy2 O5 2.468(2) . ?
Dy2 N3 2.500(3) . ?
Dy2 N4 2.565(3) . ?
Dy2 C33 2.794(3) . ?
Dy1 O10 2.326(2) . ?
Dy1 O3 2.334(2) 2_556 ?
Dy1 O12 2.344(3) 2_556 ?
Dy1 O1 2.367(3) . ?
Dy1 O13 2.408(2) . ?
Dy1 O11 2.478(3) . ?
Dy1 N1 2.541(3) . ?
Dy1 N2 2.568(3) . ?
F8 C38 1.349(4) . ?
F7 C37 1.338(4) . ?
F6 C36 1.365(4) . ?
F5 C35 1.335(4) . ?
F4 C30 1.338(4) . ?
F3 C29 1.338(4) . ?
F2 C28 1.329(4) . ?
F1 C27 1.343(4) . ?
F9 C43 1.343(4) . ?
F10 C44 1.335(4) . ?
F11 C45 1.338(4) . ?
F12 C46 1.338(4) . ?
O6 C33 1.238(4) . ?
O5 C33 1.254(4) . ?
O8 C40 1.223(4) . ?
O7 C40 1.267(4) . ?
O7 Dy2 2.240(2) 2_565 ?
O4 C32 1.238(4) . ?
O3 C32 1.250(4) . ?
O3 Dy1 2.334(2) 2_556 ?
O2 C25 1.252(4) . ?
O1 C25 1.227(4) . ?
O10 C41 1.249(4) . ?
O9 C41 1.244(4) . ?
O12 C48 1.246(4) . ?
O12 Dy1 2.344(3) 2_556 ?
O11 C48 1.244(4) . ?
O13 H13C 0.9599 . ?
O13 H13D 0.9599 . ?
O14 H14C 0.9600 . ?
O14 H14D 0.9600 . ?
N1 C1 1.327(4) . ?
N1 C12 1.354(4) . ?
N2 C10 1.322(4) . ?
N2 C11 1.353(4) . ?
N4 C22 1.326(5) . ?
N4 C23 1.355(4) . ?
N3 C13 1.323(5) . ?
N3 C24 1.352(5) . ?
C1 C2 1.395(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.356(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.400(5) . ?
C3 H3A 0.9300 . ?
C4 C12 1.405(4) . ?
C4 C5 1.430(5) . ?
C5 C6 1.338(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.432(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.405(5) . ?
C7 C11 1.405(5) . ?
C8 C9 1.355(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.400(5) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.444(5) . ?
C22 C21 1.394(6) . ?
C22 H13A 0.9300 . ?
C21 C20 1.352(7) . ?
C21 H14A 0.9300 . ?
C20 C19 1.409(7) . ?
C20 H15A 0.9300 . ?
C19 C23 1.404(5) . ?
C19 C18 1.423(6) . ?
C18 C17 1.341(7) . ?
C18 H17A 0.9300 . ?
C17 C16 1.434(7) . ?
C17 H18A 0.9300 . ?
C16 C15 1.404(6) . ?
C16 C24 1.412(5) . ?
C15 C14 1.356(7) . ?
C15 H20A 0.9300 . ?
C14 C13 1.389(6) . ?
C14 H21A 0.9300 . ?
C13 H22A 0.9300 . ?
C24 C23 1.443(5) . ?
C33 C34 1.499(4) . ?
C34 C35 1.384(5) . ?
C34 C39 1.412(4) . ?
C35 C36 1.345(5) . ?
C36 C37 1.387(5) . ?
C37 C38 1.372(5) . ?
C38 C39 1.374(5) . ?
C39 C40 1.525(5) . ?
C32 C31 1.513(4) . ?
C31 C30 1.383(4) . ?
C31 C26 1.402(5) . ?
C30 C29 1.375(5) . ?
C29 C28 1.376(6) . ?
C28 C27 1.384(5) . ?
C27 C26 1.378(4) . ?
C26 C25 1.527(4) . ?
C41 C42 1.516(4) . ?
C42 C43 1.380(4) . ?
C42 C47 1.392(4) . ?
C43 C44 1.367(5) . ?
C44 C45 1.374(5) . ?
C45 C46 1.391(5) . ?
C46 C47 1.377(4) . ?
C47 C48 1.507(4) . ?
O15 H15C 0.9600 . ?
O15 H15E 0.9601 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Dy2 O9 146.40(8) 2_565 . ?
O7 Dy2 O2 131.83(9) 2_565 . ?
O9 Dy2 O2 77.00(8) . . ?
O7 Dy2 O6 82.00(9) 2_565 . ?
O9 Dy2 O6 83.37(9) . . ?
O2 Dy2 O6 137.94(9) . . ?
O7 Dy2 O14 71.78(9) 2_565 . ?
O9 Dy2 O14 141.61(9) . . ?
O2 Dy2 O14 66.71(9) . . ?
O6 Dy2 O14 115.50(12) . . ?
O7 Dy2 O5 105.92(10) 2_565 . ?
O9 Dy2 O5 88.61(10) . . ?
O2 Dy2 O5 89.54(8) . . ?
O6 Dy2 O5 52.81(8) . . ?
O14 Dy2 O5 79.29(12) . . ?
O7 Dy2 N3 81.08(9) 2_565 . ?
O9 Dy2 N3 90.53(9) . . ?
O2 Dy2 N3 78.68(9) . . ?
O6 Dy2 N3 138.84(8) . . ?
O14 Dy2 N3 94.15(12) . . ?
O5 Dy2 N3 168.07(8) . . ?
O7 Dy2 N4 78.07(9) 2_565 . ?
O9 Dy2 N4 68.99(8) . . ?
O2 Dy2 N4 128.68(9) . . ?
O6 Dy2 N4 75.11(9) . . ?
O14 Dy2 N4 145.67(10) . . ?
O5 Dy2 N4 125.59(9) . . ?
N3 Dy2 N4 64.80(9) . . ?
O7 Dy2 C33 94.10(9) 2_565 . ?
O9 Dy2 C33 85.62(9) . . ?
O2 Dy2 C33 114.49(9) . . ?
O6 Dy2 C33 26.15(8) . . ?
O14 Dy2 C33 97.95(12) . . ?
O5 Dy2 C33 26.67(8) . . ?
N3 Dy2 C33 164.88(9) . . ?
N4 Dy2 C33 100.24(9) . . ?
O10 Dy1 O3 87.81(8) . 2_556 ?
O10 Dy1 O12 150.37(9) . 2_556 ?
O3 Dy1 O12 117.51(9) 2_556 2_556 ?
O10 Dy1 O1 76.98(9) . . ?
O3 Dy1 O1 144.14(8) 2_556 . ?
O12 Dy1 O1 73.43(10) 2_556 . ?
O10 Dy1 O13 135.78(8) . . ?
O3 Dy1 O13 72.51(8) 2_556 . ?
O12 Dy1 O13 70.67(10) 2_556 . ?
O1 Dy1 O13 138.98(8) . . ?
O10 Dy1 O11 72.82(8) . . ?
O3 Dy1 O11 71.24(8) 2_556 . ?
O12 Dy1 O11 99.68(10) 2_556 . ?
O1 Dy1 O11 73.27(9) . . ?
O13 Dy1 O11 131.75(9) . . ?
O10 Dy1 N1 95.12(8) . . ?
O3 Dy1 N1 141.10(9) 2_556 . ?
O12 Dy1 N1 75.13(9) 2_556 . ?
O1 Dy1 N1 73.37(9) . . ?
O13 Dy1 N1 78.80(9) . . ?
O11 Dy1 N1 146.30(9) . . ?
O10 Dy1 N2 66.39(8) . . ?
O3 Dy1 N2 82.08(8) 2_556 . ?
O12 Dy1 N2 128.60(10) 2_556 . ?
O1 Dy1 N2 119.25(9) . . ?
O13 Dy1 N2 71.82(8) . . ?
O11 Dy1 N2 131.61(8) . . ?
N1 Dy1 N2 64.10(9) . . ?
C33 O6 Dy2 95.87(19) . . ?
C33 O5 Dy2 91.31(19) . . ?
C40 O7 Dy2 167.6(2) . 2_565 ?
C32 O3 Dy1 145.1(2) . 2_556 ?
C25 O2 Dy2 151.9(2) . . ?
C25 O1 Dy1 146.9(2) . . ?
C41 O10 Dy1 122.3(2) . . ?
C41 O9 Dy2 154.0(2) . . ?
C48 O12 Dy1 111.0(2) . 2_556 ?
C48 O11 Dy1 138.0(2) . . ?
Dy1 O13 H13C 109.4 . . ?
Dy1 O13 H13D 109.4 . . ?
H13C O13 H13D 109.5 . . ?
Dy2 O14 H14C 109.7 . . ?
Dy2 O14 H14D 109.3 . . ?
H14C O14 H14D 109.5 . . ?
C1 N1 C12 117.8(3) . . ?
C1 N1 Dy1 122.3(2) . . ?
C12 N1 Dy1 119.6(2) . . ?
C10 N2 C11 118.1(3) . . ?
C10 N2 Dy1 122.6(2) . . ?
C11 N2 Dy1 118.1(2) . . ?
C22 N4 C23 118.0(3) . . ?
C22 N4 Dy2 123.3(2) . . ?
C23 N4 Dy2 118.4(2) . . ?
C13 N3 C24 118.0(3) . . ?
C13 N3 Dy2 121.6(3) . . ?
C24 N3 Dy2 120.4(2) . . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C12 117.2(3) . . ?
C3 C4 C5 123.6(3) . . ?
C12 C4 C5 119.2(3) . . ?
C6 C5 C4 121.5(3) . . ?
C6 C5 H5A 119.2 . . ?
C4 C5 H5A 119.2 . . ?
C5 C6 C7 120.9(3) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C11 116.9(3) . . ?
C8 C7 C6 123.5(3) . . ?
C11 C7 C6 119.6(3) . . ?
C9 C8 C7 120.3(3) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 118.7(3) . . ?
C8 C9 H9A 120.6 . . ?
C10 C9 H9A 120.6 . . ?
N2 C10 C9 123.1(3) . . ?
N2 C10 H10A 118.4 . . ?
C9 C10 H10A 118.4 . . ?
N2 C11 C7 122.7(3) . . ?
N2 C11 C12 118.1(3) . . ?
C7 C11 C12 119.2(3) . . ?
N1 C12 C4 122.7(3) . . ?
N1 C12 C11 117.7(3) . . ?
C4 C12 C11 119.6(3) . . ?
N4 C22 C21 122.9(4) . . ?
N4 C22 H13A 118.6 . . ?
C21 C22 H13A 118.6 . . ?
C20 C21 C22 119.4(4) . . ?
C20 C21 H14A 120.3 . . ?
C22 C21 H14A 120.3 . . ?
C21 C20 C19 120.0(4) . . ?
C21 C20 H15A 120.0 . . ?
C19 C20 H15A 120.0 . . ?
C23 C19 C20 116.8(4) . . ?
C23 C19 C18 119.5(4) . . ?
C20 C19 C18 123.7(4) . . ?
C17 C18 C19 121.5(4) . . ?
C17 C18 H17A 119.3 . . ?
C19 C18 H17A 119.3 . . ?
C18 C17 C16 120.9(4) . . ?
C18 C17 H18A 119.6 . . ?
C16 C17 H18A 119.6 . . ?
C15 C16 C24 117.3(4) . . ?
C15 C16 C17 123.2(4) . . ?
C24 C16 C17 119.5(4) . . ?
C14 C15 C16 119.3(4) . . ?
C14 C15 H20A 120.4 . . ?
C16 C15 H20A 120.4 . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 H21A 120.1 . . ?
C13 C14 H21A 120.1 . . ?
N3 C13 C14 123.1(4) . . ?
N3 C13 H22A 118.5 . . ?
C14 C13 H22A 118.5 . . ?
N3 C24 C16 122.5(3) . . ?
N3 C24 C23 118.5(3) . . ?
C16 C24 C23 119.0(3) . . ?
N4 C23 C19 122.9(3) . . ?
N4 C23 C24 117.5(3) . . ?
C19 C23 C24 119.6(3) . . ?
O6 C33 O5 120.0(3) . . ?
O6 C33 C34 118.3(3) . . ?
O5 C33 C34 121.7(3) . . ?
O6 C33 Dy2 57.98(16) . . ?
O5 C33 Dy2 62.03(17) . . ?
C34 C33 Dy2 176.3(2) . . ?
C35 C34 C39 118.1(3) . . ?
C35 C34 C33 122.3(3) . . ?
C39 C34 C33 119.6(3) . . ?
F5 C35 C36 116.3(3) . . ?
F5 C35 C34 122.1(3) . . ?
C36 C35 C34 121.6(3) . . ?
C35 C36 F6 121.1(3) . . ?
C35 C36 C37 121.4(3) . . ?
F6 C36 C37 117.5(3) . . ?
F7 C37 C38 121.2(3) . . ?
F7 C37 C36 121.0(3) . . ?
C38 C37 C36 117.7(3) . . ?
F8 C38 C37 117.3(3) . . ?
F8 C38 C39 120.3(3) . . ?
C37 C38 C39 122.4(3) . . ?
C38 C39 C34 118.8(3) . . ?
C38 C39 C40 115.6(3) . . ?
C34 C39 C40 125.6(3) . . ?
O8 C40 O7 126.5(3) . . ?
O8 C40 C39 118.3(3) . . ?
O7 C40 C39 115.1(3) . . ?
O4 C32 O3 126.6(3) . . ?
O4 C32 C31 118.3(3) . . ?
O3 C32 C31 115.0(3) . . ?
C30 C31 C26 119.4(3) . . ?
C30 C31 C32 119.5(3) . . ?
C26 C31 C32 121.0(3) . . ?
F4 C30 C29 118.6(3) . . ?
F4 C30 C31 119.7(3) . . ?
C29 C30 C31 121.7(3) . . ?
F3 C29 C30 120.5(4) . . ?
F3 C29 C28 120.1(3) . . ?
C30 C29 C28 119.5(3) . . ?
F2 C28 C29 120.2(3) . . ?
F2 C28 C27 120.7(3) . . ?
C29 C28 C27 119.1(3) . . ?
F1 C27 C26 120.8(3) . . ?
F1 C27 C28 116.7(3) . . ?
C26 C27 C28 122.5(3) . . ?
C27 C26 C31 117.9(3) . . ?
C27 C26 C25 121.6(3) . . ?
C31 C26 C25 120.5(3) . . ?
O1 C25 O2 127.9(3) . . ?
O1 C25 C26 117.1(3) . . ?
O2 C25 C26 115.0(3) . . ?
O9 C41 O10 126.4(3) . . ?
O9 C41 C42 117.5(3) . . ?
O10 C41 C42 116.0(3) . . ?
C43 C42 C47 120.0(3) . . ?
C43 C42 C41 117.9(3) . . ?
C47 C42 C41 122.1(3) . . ?
F9 C43 C44 118.9(3) . . ?
F9 C43 C42 119.9(3) . . ?
C44 C43 C42 121.2(3) . . ?
F10 C44 C43 120.7(3) . . ?
F10 C44 C45 119.7(3) . . ?
C43 C44 C45 119.6(3) . . ?
F11 C45 C44 120.7(3) . . ?
F11 C45 C46 119.8(3) . . ?
C44 C45 C46 119.5(3) . . ?
F12 C46 C47 123.1(3) . . ?
F12 C46 C45 115.5(3) . . ?
C47 C46 C45 121.4(3) . . ?
C46 C47 C42 118.2(3) . . ?
C46 C47 C48 122.3(3) . . ?
C42 C47 C48 119.5(3) . . ?
O11 C48 O12 123.2(3) . . ?
O11 C48 C47 119.7(3) . . ?
O12 C48 C47 117.0(3) . . ?
H15C O15 H15E 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 C2 -0.8(5) . . . . ?
Dy1 N1 C1 C2 172.2(3) . . . . ?
N1 C1 C2 C3 -1.5(6) . . . . ?
C1 C2 C3 C4 1.6(7) . . . . ?
C2 C3 C4 C12 0.4(6) . . . . ?
C2 C3 C4 C5 -178.5(4) . . . . ?
C3 C4 C5 C6 179.9(4) . . . . ?
C12 C4 C5 C6 1.0(5) . . . . ?
C4 C5 C6 C7 2.6(6) . . . . ?
C5 C6 C7 C8 175.2(4) . . . . ?
C5 C6 C7 C11 -3.5(5) . . . . ?
C11 C7 C8 C9 1.3(5) . . . . ?
C6 C7 C8 C9 -177.4(4) . . . . ?
C7 C8 C9 C10 -3.7(6) . . . . ?
C11 N2 C10 C9 -0.6(5) . . . . ?
Dy1 N2 C10 C9 -168.2(3) . . . . ?
C8 C9 C10 N2 3.5(6) . . . . ?
C10 N2 C11 C7 -2.0(4) . . . . ?
Dy1 N2 C11 C7 166.2(2) . . . . ?
C10 N2 C11 C12 177.5(3) . . . . ?
Dy1 N2 C11 C12 -14.3(3) . . . . ?
C8 C7 C11 N2 1.7(5) . . . . ?
C6 C7 C11 N2 -179.6(3) . . . . ?
C8 C7 C11 C12 -177.8(3) . . . . ?
C6 C7 C11 C12 0.9(5) . . . . ?
C1 N1 C12 C4 3.1(5) . . . . ?
Dy1 N1 C12 C4 -170.1(2) . . . . ?
C1 N1 C12 C11 -177.3(3) . . . . ?
Dy1 N1 C12 C11 9.5(4) . . . . ?
C3 C4 C12 N1 -2.9(5) . . . . ?
C5 C4 C12 N1 176.1(3) . . . . ?
C3 C4 C12 C11 177.5(3) . . . . ?
C5 C4 C12 C11 -3.5(5) . . . . ?
N2 C11 C12 N1 3.4(4) . . . . ?
C7 C11 C12 N1 -177.1(3) . . . . ?
N2 C11 C12 C4 -177.0(3) . . . . ?
C7 C11 C12 C4 2.5(4) . . . . ?
C23 N4 C22 C21 -0.7(6) . . . . ?
Dy2 N4 C22 C21 172.9(4) . . . . ?
N4 C22 C21 C20 0.5(8) . . . . ?
C22 C21 C20 C19 0.5(8) . . . . ?
C21 C20 C19 C23 -1.2(8) . . . . ?
C21 C20 C19 C18 179.3(5) . . . . ?
C23 C19 C18 C17 2.2(8) . . . . ?
C20 C19 C18 C17 -178.3(5) . . . . ?
C19 C18 C17 C16 -2.2(8) . . . . ?
C18 C17 C16 C15 -179.0(5) . . . . ?
C18 C17 C16 C24 0.3(7) . . . . ?
C24 C16 C15 C14 -0.7(6) . . . . ?
C17 C16 C15 C14 178.6(4) . . . . ?
C16 C15 C14 C13 -0.7(6) . . . . ?
C24 N3 C13 C14 0.3(5) . . . . ?
Dy2 N3 C13 C14 -178.7(3) . . . . ?
C15 C14 C13 N3 1.0(6) . . . . ?
C13 N3 C24 C16 -1.9(5) . . . . ?
Dy2 N3 C24 C16 177.1(3) . . . . ?
C13 N3 C24 C23 179.3(3) . . . . ?
Dy2 N3 C24 C23 -1.7(4) . . . . ?
C15 C16 C24 N3 2.1(5) . . . . ?
C17 C16 C24 N3 -177.2(4) . . . . ?
C15 C16 C24 C23 -179.1(3) . . . . ?
C17 C16 C24 C23 1.6(6) . . . . ?
C22 N4 C23 C19 -0.1(5) . . . . ?
Dy2 N4 C23 C19 -174.0(3) . . . . ?
C22 N4 C23 C24 -179.3(3) . . . . ?
Dy2 N4 C23 C24 6.8(4) . . . . ?
C20 C19 C23 N4 1.1(6) . . . . ?
C18 C19 C23 N4 -179.5(4) . . . . ?
C20 C19 C23 C24 -179.8(4) . . . . ?
C18 C19 C23 C24 -0.3(6) . . . . ?
N3 C24 C23 N4 -3.5(5) . . . . ?
C16 C24 C23 N4 177.7(3) . . . . ?
N3 C24 C23 C19 177.3(3) . . . . ?
C16 C24 C23 C19 -1.6(5) . . . . ?
Dy2 O6 C33 O5 0.5(4) . . . . ?
Dy2 O6 C33 C34 -179.6(3) . . . . ?
Dy2 O5 C33 O6 -0.5(4) . . . . ?
Dy2 O5 C33 C34 179.6(3) . . . . ?
O6 C33 C34 C35 165.3(3) . . . . ?
O5 C33 C34 C35 -14.8(5) . . . . ?
O6 C33 C34 C39 -14.8(5) . . . . ?
O5 C33 C34 C39 165.1(3) . . . . ?
C39 C34 C35 F5 176.9(3) . . . . ?
C33 C34 C35 F5 -3.2(6) . . . . ?
C39 C34 C35 C36 0.8(5) . . . . ?
C33 C34 C35 C36 -179.3(3) . . . . ?
F5 C35 C36 F6 2.6(6) . . . . ?
C34 C35 C36 F6 178.9(4) . . . . ?
F5 C35 C36 C37 -178.8(4) . . . . ?
C34 C35 C36 C37 -2.4(6) . . . . ?
C35 C36 C37 F7 179.3(4) . . . . ?
F6 C36 C37 F7 -2.0(6) . . . . ?
C35 C36 C37 C38 2.2(6) . . . . ?
F6 C36 C37 C38 -179.1(4) . . . . ?
F7 C37 C38 F8 1.4(6) . . . . ?
C36 C37 C38 F8 178.6(3) . . . . ?
F7 C37 C38 C39 -177.5(3) . . . . ?
C36 C37 C38 C39 -0.4(6) . . . . ?
F8 C38 C39 C34 179.9(3) . . . . ?
C37 C38 C39 C34 -1.1(5) . . . . ?
F8 C38 C39 C40 0.7(5) . . . . ?
C37 C38 C39 C40 179.6(3) . . . . ?
C35 C34 C39 C38 0.9(5) . . . . ?
C33 C34 C39 C38 -179.0(3) . . . . ?
C35 C34 C39 C40 -179.9(3) . . . . ?
C33 C34 C39 C40 0.2(5) . . . . ?
Dy2 O7 C40 O8 -164.3(8) 2_565 . . . ?
Dy2 O7 C40 C39 10.8(12) 2_565 . . . ?
C38 C39 C40 O8 85.9(4) . . . . ?
C34 C39 C40 O8 -93.3(4) . . . . ?
C38 C39 C40 O7 -89.6(4) . . . . ?
C34 C39 C40 O7 91.2(4) . . . . ?
Dy1 O3 C32 O4 -24.4(6) 2_556 . . . ?
Dy1 O3 C32 C31 156.5(3) 2_556 . . . ?
O4 C32 C31 C30 -77.5(4) . . . . ?
O3 C32 C31 C30 101.7(4) . . . . ?
O4 C32 C31 C26 105.0(4) . . . . ?
O3 C32 C31 C26 -75.8(4) . . . . ?
C26 C31 C30 F4 177.7(3) . . . . ?
C32 C31 C30 F4 0.2(5) . . . . ?
C26 C31 C30 C29 -0.9(5) . . . . ?
C32 C31 C30 C29 -178.4(3) . . . . ?
F4 C30 C29 F3 1.9(6) . . . . ?
C31 C30 C29 F3 -179.5(4) . . . . ?
F4 C30 C29 C28 -178.4(4) . . . . ?
C31 C30 C29 C28 0.2(6) . . . . ?
F3 C29 C28 F2 -1.8(6) . . . . ?
C30 C29 C28 F2 178.5(4) . . . . ?
F3 C29 C28 C27 179.4(4) . . . . ?
C30 C29 C28 C27 -0.3(6) . . . . ?
F2 C28 C27 F1 2.9(5) . . . . ?
C29 C28 C27 F1 -178.3(3) . . . . ?
F2 C28 C27 C26 -177.6(3) . . . . ?
C29 C28 C27 C26 1.2(6) . . . . ?
F1 C27 C26 C31 177.6(3) . . . . ?
C28 C27 C26 C31 -1.8(5) . . . . ?
F1 C27 C26 C25 -4.0(5) . . . . ?
C28 C27 C26 C25 176.6(3) . . . . ?
C30 C31 C26 C27 1.6(5) . . . . ?
C32 C31 C26 C27 179.1(3) . . . . ?
C30 C31 C26 C25 -176.8(3) . . . . ?
C32 C31 C26 C25 0.7(4) . . . . ?
Dy1 O1 C25 O2 68.6(6) . . . . ?
Dy1 O1 C25 C26 -111.0(4) . . . . ?
Dy2 O2 C25 O1 35.2(7) . . . . ?
Dy2 O2 C25 C26 -145.3(4) . . . . ?
C27 C26 C25 O1 -57.7(4) . . . . ?
C31 C26 C25 O1 120.6(4) . . . . ?
C27 C26 C25 O2 122.7(3) . . . . ?
C31 C26 C25 O2 -59.0(4) . . . . ?
Dy2 O9 C41 O10 118.1(5) . . . . ?
Dy2 O9 C41 C42 -65.9(6) . . . . ?
Dy1 O10 C41 O9 -98.8(3) . . . . ?
Dy1 O10 C41 C42 85.2(3) . . . . ?
O9 C41 C42 C43 -90.5(4) . . . . ?
O10 C41 C42 C43 85.9(3) . . . . ?
O9 C41 C42 C47 90.3(4) . . . . ?
O10 C41 C42 C47 -93.3(4) . . . . ?
C47 C42 C43 F9 -179.4(3) . . . . ?
C41 C42 C43 F9 1.4(4) . . . . ?
C47 C42 C43 C44 0.5(5) . . . . ?
C41 C42 C43 C44 -178.7(3) . . . . ?
F9 C43 C44 F10 -1.1(5) . . . . ?
C42 C43 C44 F10 179.0(3) . . . . ?
F9 C43 C44 C45 178.5(3) . . . . ?
C42 C43 C44 C45 -1.3(5) . . . . ?
F10 C44 C45 F11 -0.6(5) . . . . ?
C43 C44 C45 F11 179.7(3) . . . . ?
F10 C44 C45 C46 179.7(3) . . . . ?
C43 C44 C45 C46 0.0(5) . . . . ?
F11 C45 C46 F12 0.7(5) . . . . ?
C44 C45 C46 F12 -179.6(3) . . . . ?
F11 C45 C46 C47 -177.6(3) . . . . ?
C44 C45 C46 C47 2.1(5) . . . . ?
F12 C46 C47 C42 178.9(3) . . . . ?
C45 C46 C47 C42 -2.9(5) . . . . ?
F12 C46 C47 C48 -2.4(5) . . . . ?
C45 C46 C47 C48 175.8(3) . . . . ?
C43 C42 C47 C46 1.6(5) . . . . ?
C41 C42 C47 C46 -179.2(3) . . . . ?
C43 C42 C47 C48 -177.1(3) . . . . ?
C41 C42 C47 C48 2.1(4) . . . . ?
Dy1 O11 C48 O12 -126.8(3) . . . . ?
Dy1 O11 C48 C47 52.6(4) . . . . ?
Dy1 O12 C48 O11 7.0(4) 2_556 . . . ?
Dy1 O12 C48 C47 -172.4(2) 2_556 . . . ?
C46 C47 C48 O11 -159.0(3) . . . . ?
C42 C47 C48 O11 19.7(4) . . . . ?
C46 C47 C48 O12 20.4(5) . . . . ?
C42 C47 C48 O12 -160.9(3) . . . . ?

_refine_diff_density_max         1.657
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.123



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_audit_block_doi                 10.5517/cc14bpsy
_database_code_depnum_ccdc_archive 'CCDC 1052970'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H22 F12 Gd2 N4 O15'
_chemical_formula_weight         1437.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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'

_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                   13.9713(6)
_cell_length_b                   14.1629(6)
_cell_length_c                   15.0301(6)
_cell_angle_alpha                63.6820(10)
_cell_angle_beta                 81.1340(10)
_cell_angle_gamma                65.4950(10)
_cell_volume                     2424.06(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8196
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.11

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_F_000             1388
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    2.834
_shelx_estimated_absorpt_T_min   0.574
_shelx_estimated_absorpt_T_max   0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_T_max  0.6295
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50363
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.912
_diffrn_reflns_theta_max         27.589
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11201
_reflns_number_gt                10163
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.288     0.128     0.493      85.7       7.1
         2     0.714     0.871     0.507      85.6       7.9
_platon_squeeze_details

The unit cell contains 4 water molecules, which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+1.3517P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11201
_refine_ls_number_parameters     730
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.64692(2) -0.01347(2) 1.06083(2) 0.02185(5) Uani 1 1 d . . . . .
Gd2 Gd 0.60636(2) 0.23924(2) 0.64101(2) 0.02331(5) Uani 1 1 d . . . . .
C1 C 0.8939(3) -0.2236(3) 1.0703(3) 0.0396(7) Uani 1 1 d . . . . .
H1 H 0.8515 -0.2510 1.0551 0.048 Uiso 1 1 calc R U . . .
C2 C 1.0027(3) -0.2822(3) 1.0736(3) 0.0483(8) Uani 1 1 d . . . . .
H2 H 1.0315 -0.3474 1.0617 0.058 Uiso 1 1 calc R U . . .
C3 C 1.0665(3) -0.2427(3) 1.0948(3) 0.0498(8) Uani 1 1 d . . . . .
H3 H 1.1393 -0.2803 1.0967 0.060 Uiso 1 1 calc R U . . .
C4 C 1.0208(2) -0.1451(3) 1.1134(2) 0.0362(6) Uani 1 1 d . . . . .
C5 C 1.0822(2) -0.0961(3) 1.1336(2) 0.0451(8) Uani 1 1 d . . . . .
H5 H 1.1553 -0.1296 1.1341 0.054 Uiso 1 1 calc R U . . .
C6 C 1.0352(3) -0.0026(3) 1.1518(3) 0.0450(8) Uani 1 1 d . . . . .
H6 H 1.0764 0.0288 1.1628 0.054 Uiso 1 1 calc R U . . .
C7 C 0.9234(2) 0.0496(3) 1.1548(2) 0.0351(6) Uani 1 1 d . . . . .
C8 C 0.8716(3) 0.1430(3) 1.1795(2) 0.0427(7) Uani 1 1 d . . . . .
H8 H 0.9101 0.1760 1.1923 0.051 Uiso 1 1 calc R U . . .
C9 C 0.7650(3) 0.1851(3) 1.1847(2) 0.0406(7) Uani 1 1 d . . . . .
H9 H 0.7302 0.2441 1.2046 0.049 Uiso 1 1 calc R U . . .
C10 C 0.7087(2) 0.1379(2) 1.1596(2) 0.0339(6) Uani 1 1 d . . . . .
H10 H 0.6356 0.1700 1.1598 0.041 Uiso 1 1 calc R U . . .
C11 C 0.8601(2) 0.0051(2) 1.13420(19) 0.0274(5) Uani 1 1 d . . . . .
C12 C 0.9101(2) -0.0929(2) 1.11139(19) 0.0282(5) Uani 1 1 d . . . . .
C13 C 0.8478(3) 0.0491(3) 0.6198(3) 0.0449(8) Uani 1 1 d . . . . .
H13 H 0.8057 0.0100 0.6267 0.054 Uiso 1 1 calc R U . . .
C14 C 0.9557(3) -0.0036(3) 0.6103(3) 0.0573(10) Uani 1 1 d . . . . .
H14 H 0.9843 -0.0759 0.6107 0.069 Uiso 1 1 calc R U . . .
C15 C 1.0185(3) 0.0523(4) 0.6004(3) 0.0574(10) Uani 1 1 d . . . . .
H15 H 1.0906 0.0185 0.5936 0.069 Uiso 1 1 calc R U . . .
C16 C 0.9741(3) 0.1609(3) 0.6005(3) 0.0499(9) Uani 1 1 d . . . . .
C17 C 1.0348(3) 0.2242(5) 0.5944(4) 0.0697(12) Uani 1 1 d . . . . .
H17 H 1.1075 0.1925 0.5900 0.084 Uiso 1 1 calc R U . . .
C18 C 0.9892(3) 0.3271(5) 0.5949(4) 0.0715(13) Uani 1 1 d . . . . .
H18 H 1.0308 0.3657 0.5912 0.086 Uiso 1 1 calc R U . . .
C19 C 0.8775(3) 0.3801(4) 0.6009(3) 0.0529(9) Uani 1 1 d . . . . .
C20 C 0.8259(3) 0.4893(4) 0.5999(4) 0.0659(12) Uani 1 1 d . . . . .
H20 H 0.8643 0.5311 0.5959 0.079 Uiso 1 1 calc R U . . .
C21 C 0.7194(4) 0.5337(4) 0.6047(4) 0.0659(12) Uani 1 1 d . . . . .
H21 H 0.6841 0.6062 0.6036 0.079 Uiso 1 1 calc R U . . .
C22 C 0.6635(3) 0.4687(3) 0.6114(3) 0.0437(7) Uani 1 1 d . . . . .
H22 H 0.5907 0.5000 0.6149 0.052 Uiso 1 1 calc R U . . .
C23 C 0.8150(2) 0.3205(3) 0.6076(2) 0.0354(6) Uani 1 1 d . . . . .
C24 C 0.8644(2) 0.2081(3) 0.6095(2) 0.0353(6) Uani 1 1 d . . . . .
C25 C 0.6915(2) -0.0424(2) 0.8356(2) 0.0266(5) Uani 1 1 d . . . . .
C26 C 0.7265(2) -0.1569(2) 0.82899(19) 0.0261(5) Uani 1 1 d . . . . .
C27 C 0.8295(2) -0.2319(2) 0.8422(2) 0.0330(6) Uani 1 1 d . . . . .
C28 C 0.8600(2) -0.3374(3) 0.8407(3) 0.0394(7) Uani 1 1 d . . . . .
C29 C 0.7847(3) -0.3675(3) 0.8238(3) 0.0428(7) Uani 1 1 d . . . . .
C30 C 0.6824(3) -0.2931(3) 0.8093(2) 0.0375(7) Uani 1 1 d . . . . .
C31 C 0.6505(2) -0.1875(2) 0.8110(2) 0.0277(5) Uani 1 1 d . . . . .
C32 C 0.5356(2) -0.1080(2) 0.7969(2) 0.0273(5) Uani 1 1 d . . . . .
C33 C 0.4000(2) 0.3931(2) 0.64671(19) 0.0280(5) Uani 1 1 d . . . . .
C34 C 0.2936(2) 0.4796(2) 0.6496(2) 0.0290(6) Uani 1 1 d . . . . .
C35 C 0.2033(2) 0.4565(3) 0.6653(2) 0.0382(7) Uani 1 1 d . . . . .
C36 C 0.1064(3) 0.5365(3) 0.6671(3) 0.0438(7) Uani 1 1 d . . . . .
C37 C 0.0949(2) 0.6422(3) 0.6552(3) 0.0436(7) Uani 1 1 d . . . . .
C38 C 0.1839(2) 0.6664(2) 0.6400(2) 0.0363(6) Uani 1 1 d . . . . .
C39 C 0.2823(2) 0.5892(2) 0.63585(19) 0.0291(5) Uani 1 1 d . . . . .
C40 C 0.3714(2) 0.6308(2) 0.6166(2) 0.0289(5) Uani 1 1 d . . . . .
C41 C 0.6126(2) 0.2301(2) 0.87403(19) 0.0247(5) Uani 1 1 d . . . . .
C42 C 0.5136(2) 0.3180(2) 0.89205(19) 0.0251(5) Uani 1 1 d . . . . .
C43 C 0.5196(2) 0.4134(2) 0.8901(2) 0.0310(6) Uani 1 1 d . . . . .
C44 C 0.4334(3) 0.4958(2) 0.9074(2) 0.0333(6) Uani 1 1 d . . . . .
C45 C 0.3391(2) 0.4838(2) 0.9253(2) 0.0355(6) Uani 1 1 d . . . . .
C46 C 0.3315(2) 0.3900(2) 0.9249(2) 0.0309(6) Uani 1 1 d . . . . .
C47 C 0.4175(2) 0.3052(2) 0.90954(19) 0.0255(5) Uani 1 1 d . . . . .
C48 C 0.4092(2) 0.2018(2) 0.91234(19) 0.0263(5) Uani 1 1 d . . . . .
F1 F 0.90593(14) -0.20542(18) 0.85673(17) 0.0499(5) Uani 1 1 d . . . . .
F2 F 0.96111(16) -0.41111(18) 0.85766(19) 0.0607(6) Uani 1 1 d . . . . .
F3 F 0.81303(19) -0.46965(17) 0.8228(2) 0.0675(7) Uani 1 1 d . . . . .
F4 F 0.60930(16) -0.32514(18) 0.79553(19) 0.0577(6) Uani 1 1 d . . . . .
F5 F 0.20618(16) 0.35724(17) 0.67443(18) 0.0549(5) Uani 1 1 d . . . . .
F6 F 0.01983(16) 0.5118(2) 0.6815(2) 0.0682(7) Uani 1 1 d . . . . .
F7 F -0.00048(16) 0.72160(19) 0.6555(2) 0.0663(7) Uani 1 1 d . . . . .
F8 F 0.17060(16) 0.77192(16) 0.62684(16) 0.0518(5) Uani 1 1 d . . . . .
F9 F 0.23582(14) 0.38511(16) 0.94252(17) 0.0489(5) Uani 1 1 d . . . . .
F10 F 0.25406(17) 0.56276(17) 0.94343(19) 0.0597(6) Uani 1 1 d . . . . .
F11 F 0.44109(17) 0.58743(16) 0.90604(17) 0.0501(5) Uani 1 1 d . . . . .
F12 F 0.61125(15) 0.42728(17) 0.87150(17) 0.0487(5) Uani 1 1 d . . . . .
N1 N 0.84760(18) -0.1310(2) 1.08741(18) 0.0302(5) Uani 1 1 d . . . . .
N2 N 0.75379(18) 0.05031(19) 1.13555(16) 0.0272(5) Uani 1 1 d . . . . .
N3 N 0.80248(19) 0.1518(2) 0.61963(18) 0.0346(5) Uani 1 1 d . . . . .
N4 N 0.70831(19) 0.3656(2) 0.61298(18) 0.0324(5) Uani 1 1 d . . . . .
O1 O 0.70611(18) -0.04781(18) 0.91660(16) 0.0372(5) Uani 1 1 d . . . . .
O2 O 0.65009(19) 0.04457(17) 0.75831(16) 0.0400(5) Uani 1 1 d . . . . .
O3 O 0.49235(15) -0.10066(16) 0.87453(14) 0.0304(4) Uani 1 1 d . . . . .
O4 O 0.49345(18) -0.0574(2) 0.71242(16) 0.0423(5) Uani 1 1 d . . . . .
O5 O 0.41675(18) 0.28914(18) 0.6766(2) 0.0495(6) Uani 1 1 d . . . . .
O6 O 0.47321(16) 0.42671(17) 0.61339(18) 0.0412(5) Uani 1 1 d . . . . .
O7 O 0.39030(17) 0.67893(18) 0.52685(14) 0.0343(4) Uani 1 1 d . . . . .
O8 O 0.4117(2) 0.6220(2) 0.68799(16) 0.0472(6) Uani 1 1 d . . . . .
O9 O 0.63112(17) 0.24182(17) 0.78742(14) 0.0351(4) Uani 1 1 d . . . . .
O10 O 0.67036(15) 0.15470(16) 0.94852(14) 0.0298(4) Uani 1 1 d . . . . .
O11 O 0.48905(16) 0.10882(16) 0.93496(14) 0.0306(4) Uani 1 1 d . . . . .
O12 O 0.32155(17) 0.21099(19) 0.89206(18) 0.0396(5) Uani 1 1 d . . . . .
O13 O 0.65958(18) -0.11786(18) 1.24032(15) 0.0368(5) Uani 1 1 d D . . . .
H13A H 0.6621 -0.1836 1.2637 0.055 Uiso 1 1 d DR U . . .
H13B H 0.6222 -0.0763 1.2693 0.055 Uiso 1 1 d DR U . . .
O14 O 0.5650(3) 0.1287(2) 0.57922(18) 0.0672(9) Uani 1 1 d D . . . .
H14A H 0.5635 0.0644 0.6162 0.101 Uiso 1 1 d DR U . . .
H14B H 0.5473 0.1546 0.5192 0.101 Uiso 1 1 d DR U . . .
O15 O 0.5342(5) 0.1889(4) 0.3888(2) 0.134(2) Uani 1 1 d D . . . .
H15A H 0.4983 0.1795 0.3569 0.202 Uiso 1 1 d DR U . . .
H15B H 0.5286 0.2562 0.3647 0.202 Uiso 1 1 d DR 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
Gd1 O10 2.3540(19) . ?
Gd1 O3 2.3544(19) 2_657 ?
Gd1 O1 2.381(2) . ?
Gd1 O12 2.416(2) 2_657 ?
Gd1 O13 2.427(2) . ?
Gd1 O11 2.580(2) . ?
Gd1 N1 2.584(2) . ?
Gd1 N2 2.616(2) . ?
Gd1 O11 2.7298(19) 2_657 ?
Gd1 C48 2.929(3) 2_657 ?
Gd2 O7 2.2642(19) 2_666 ?
Gd2 O9 2.2980(19) . ?
Gd2 O2 2.389(2) . ?
Gd2 O6 2.418(2) . ?
Gd2 O14 2.420(2) . ?
Gd2 O5 2.480(2) . ?
Gd2 N3 2.532(2) . ?
Gd2 N4 2.583(2) . ?
Gd2 C33 2.819(3) . ?
C1 N1 1.322(4) . ?
C1 C2 1.393(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.366(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(5) . ?
C3 H3 0.9300 . ?
C4 C12 1.409(4) . ?
C4 C5 1.438(4) . ?
C5 C6 1.343(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.428(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.403(5) . ?
C7 C11 1.413(4) . ?
C8 C9 1.360(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.400(4) . ?
C9 H9 0.9300 . ?
C10 N2 1.321(4) . ?
C10 H10 0.9300 . ?
C11 N2 1.353(3) . ?
C11 C12 1.441(4) . ?
C12 N1 1.359(3) . ?
C13 N3 1.323(4) . ?
C13 C14 1.394(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.360(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.400(6) . ?
C15 H15 0.9300 . ?
C16 C24 1.407(4) . ?
C16 C17 1.438(6) . ?
C17 C18 1.330(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.432(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.404(6) . ?
C19 C23 1.412(4) . ?
C20 C21 1.359(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.398(5) . ?
C21 H21 0.9300 . ?
C22 N4 1.319(4) . ?
C22 H22 0.9300 . ?
C23 N4 1.363(4) . ?
C23 C24 1.438(4) . ?
C24 N3 1.353(4) . ?
C25 O1 1.229(3) . ?
C25 O2 1.244(3) . ?
C25 C26 1.532(4) . ?
C26 C27 1.367(4) . ?
C26 C31 1.401(4) . ?
C27 F1 1.344(3) . ?
C27 C28 1.385(4) . ?
C28 F2 1.342(4) . ?
C28 C29 1.380(5) . ?
C29 F3 1.338(3) . ?
C29 C30 1.359(5) . ?
C30 F4 1.351(3) . ?
C30 C31 1.383(4) . ?
C31 C32 1.512(4) . ?
C32 O4 1.243(3) . ?
C32 O3 1.255(3) . ?
C33 O6 1.249(3) . ?
C33 O5 1.259(3) . ?
C33 C34 1.492(4) . ?
C34 C35 1.391(4) . ?
C34 C39 1.414(4) . ?
C35 F5 1.335(4) . ?
C35 C36 1.364(5) . ?
C36 F6 1.355(4) . ?
C36 C37 1.369(5) . ?
C37 F7 1.341(4) . ?
C37 C38 1.383(4) . ?
C38 F8 1.351(3) . ?
C38 C39 1.370(4) . ?
C39 C40 1.526(4) . ?
C40 O8 1.222(3) . ?
C40 O7 1.256(3) . ?
C41 O9 1.236(3) . ?
C41 O10 1.244(3) . ?
C41 C42 1.515(4) . ?
C42 C43 1.374(4) . ?
C42 C47 1.399(4) . ?
C43 F12 1.344(3) . ?
C43 C44 1.373(4) . ?
C44 F11 1.337(3) . ?
C44 C45 1.369(4) . ?
C45 F10 1.343(3) . ?
C45 C46 1.379(4) . ?
C46 F9 1.347(3) . ?
C46 C47 1.378(4) . ?
C47 C48 1.498(3) . ?
C48 O12 1.248(3) . ?
C48 O11 1.264(3) . ?
C48 Gd1 2.929(2) 2_657 ?
O3 Gd1 2.3545(19) 2_657 ?
O7 Gd2 2.2642(19) 2_666 ?
O11 Gd1 2.7298(19) 2_657 ?
O12 Gd1 2.416(2) 2_657 ?
O13 H13A 0.8237 . ?
O13 H13B 0.8434 . ?
O14 H14A 0.8377 . ?
O14 H14B 0.8418 . ?
O15 H15A 0.8284 . ?
O15 H15B 0.8294 . ?

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 Gd1 O3 87.50(7) . 2_657 ?
O10 Gd1 O1 76.87(7) . . ?
O3 Gd1 O1 144.14(7) 2_657 . ?
O10 Gd1 O12 149.41(7) . 2_657 ?
O3 Gd1 O12 121.61(7) 2_657 2_657 ?
O1 Gd1 O12 73.64(8) . 2_657 ?
O10 Gd1 O13 134.43(7) . . ?
O3 Gd1 O13 72.56(7) 2_657 . ?
O1 Gd1 O13 139.63(7) . . ?
O12 Gd1 O13 69.63(8) 2_657 . ?
O10 Gd1 O11 72.39(6) . . ?
O3 Gd1 O11 70.73(6) 2_657 . ?
O1 Gd1 O11 73.80(7) . . ?
O12 Gd1 O11 106.39(7) 2_657 . ?
O13 Gd1 O11 132.53(7) . . ?
O10 Gd1 N1 92.06(7) . . ?
O3 Gd1 N1 140.08(7) 2_657 . ?
O1 Gd1 N1 73.44(8) . . ?
O12 Gd1 N1 71.98(7) 2_657 . ?
O13 Gd1 N1 79.74(8) . . ?
O11 Gd1 N1 146.16(7) . . ?
O10 Gd1 N2 65.84(7) . . ?
O3 Gd1 N2 80.67(7) 2_657 . ?
O1 Gd1 N2 119.82(8) . . ?
O12 Gd1 N2 123.75(7) 2_657 . ?
O13 Gd1 N2 70.64(7) . . ?
O11 Gd1 N2 129.80(6) . . ?
N1 Gd1 N2 63.08(7) . . ?
O10 Gd1 O11 133.58(6) . 2_657 ?
O3 Gd1 O11 85.08(6) 2_657 2_657 ?
O1 Gd1 O11 82.97(7) . 2_657 ?
O12 Gd1 O11 50.02(6) 2_657 2_657 ?
O13 Gd1 O11 86.08(7) . 2_657 ?
O11 Gd1 O11 61.91(7) . 2_657 ?
N1 Gd1 O11 121.53(7) . 2_657 ?
N2 Gd1 O11 155.45(6) . 2_657 ?
O10 Gd1 C48 146.99(7) . 2_657 ?
O3 Gd1 C48 105.71(7) 2_657 2_657 ?
O1 Gd1 C48 74.97(7) . 2_657 ?
O12 Gd1 C48 24.69(7) 2_657 2_657 ?
O13 Gd1 C48 78.57(7) . 2_657 ?
O11 Gd1 C48 83.45(7) . 2_657 ?
N1 Gd1 C48 96.08(8) . 2_657 ?
N2 Gd1 C48 145.10(7) . 2_657 ?
O11 Gd1 C48 25.50(7) 2_657 2_657 ?
O7 Gd2 O9 146.83(7) 2_666 . ?
O7 Gd2 O2 131.86(8) 2_666 . ?
O9 Gd2 O2 76.91(7) . . ?
O7 Gd2 O6 82.32(8) 2_666 . ?
O9 Gd2 O6 81.47(8) . . ?
O2 Gd2 O6 138.86(8) . . ?
O7 Gd2 O14 72.09(8) 2_666 . ?
O9 Gd2 O14 141.03(7) . . ?
O2 Gd2 O14 67.01(8) . . ?
O6 Gd2 O14 116.68(10) . . ?
O7 Gd2 O5 104.39(9) 2_666 . ?
O9 Gd2 O5 88.23(9) . . ?
O2 Gd2 O5 91.80(8) . . ?
O6 Gd2 O5 52.67(7) . . ?
O14 Gd2 O5 78.97(10) . . ?
O7 Gd2 N3 80.47(8) 2_666 . ?
O9 Gd2 N3 92.38(8) . . ?
O2 Gd2 N3 78.43(8) . . ?
O6 Gd2 N3 137.48(8) . . ?
O14 Gd2 N3 94.30(10) . . ?
O5 Gd2 N3 169.79(8) . . ?
O7 Gd2 N4 78.68(7) 2_666 . ?
O9 Gd2 N4 69.18(7) . . ?
O2 Gd2 N4 127.09(8) . . ?
O6 Gd2 N4 74.50(7) . . ?
O14 Gd2 N4 146.31(9) . . ?
O5 Gd2 N4 125.29(8) . . ?
N3 Gd2 N4 64.15(8) . . ?
O7 Gd2 C33 93.96(8) 2_666 . ?
O9 Gd2 C33 83.85(8) . . ?
O2 Gd2 C33 115.94(8) . . ?
O6 Gd2 C33 26.17(7) . . ?
O14 Gd2 C33 98.66(10) . . ?
O5 Gd2 C33 26.50(7) . . ?
N3 Gd2 C33 163.60(8) . . ?
N4 Gd2 C33 99.71(8) . . ?
N1 C1 C2 123.6(3) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C12 118.1(3) . . ?
C3 C4 C5 122.7(3) . . ?
C12 C4 C5 119.3(3) . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.6(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C11 117.2(3) . . ?
C8 C7 C6 123.3(3) . . ?
C11 C7 C6 119.4(3) . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 118.8(3) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 123.5(3) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C7 122.7(3) . . ?
N2 C11 C12 118.3(2) . . ?
C7 C11 C12 119.1(3) . . ?
N1 C12 C4 122.2(3) . . ?
N1 C12 C11 118.0(2) . . ?
C4 C12 C11 119.8(2) . . ?
N3 C13 C14 123.3(4) . . ?
N3 C13 H13 118.4 . . ?
C14 C13 H13 118.4 . . ?
C15 C14 C13 119.1(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.6(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C24 117.5(4) . . ?
C15 C16 C17 123.5(4) . . ?
C24 C16 C17 119.0(4) . . ?
C18 C17 C16 121.4(4) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 121.6(4) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C20 C19 C23 117.6(3) . . ?
C20 C19 C18 123.5(4) . . ?
C23 C19 C18 118.8(4) . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 119.0(4) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
N4 C22 C21 123.7(3) . . ?
N4 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
N4 C23 C19 122.2(3) . . ?
N4 C23 C24 118.1(3) . . ?
C19 C23 C24 119.7(3) . . ?
N3 C24 C16 122.5(3) . . ?
N3 C24 C23 118.1(3) . . ?
C16 C24 C23 119.4(3) . . ?
O1 C25 O2 128.2(3) . . ?
O1 C25 C26 116.2(2) . . ?
O2 C25 C26 115.6(2) . . ?
C27 C26 C31 118.5(2) . . ?
C27 C26 C25 122.3(2) . . ?
C31 C26 C25 119.2(2) . . ?
F1 C27 C26 121.0(3) . . ?
F1 C27 C28 116.9(3) . . ?
C26 C27 C28 122.0(3) . . ?
F2 C28 C29 120.1(3) . . ?
F2 C28 C27 120.8(3) . . ?
C29 C28 C27 119.1(3) . . ?
F3 C29 C30 120.9(3) . . ?
F3 C29 C28 119.8(3) . . ?
C30 C29 C28 119.3(3) . . ?
F4 C30 C29 118.5(3) . . ?
F4 C30 C31 119.2(3) . . ?
C29 C30 C31 122.2(3) . . ?
C30 C31 C26 118.7(3) . . ?
C30 C31 C32 120.7(2) . . ?
C26 C31 C32 120.5(2) . . ?
O4 C32 O3 126.7(3) . . ?
O4 C32 C31 118.7(2) . . ?
O3 C32 C31 114.7(2) . . ?
O6 C33 O5 120.2(3) . . ?
O6 C33 C34 118.0(2) . . ?
O5 C33 C34 121.9(3) . . ?
O6 C33 Gd2 58.66(14) . . ?
O5 C33 Gd2 61.52(15) . . ?
C34 C33 Gd2 176.4(2) . . ?
C35 C34 C39 117.9(3) . . ?
C35 C34 C33 122.1(3) . . ?
C39 C34 C33 120.0(2) . . ?
F5 C35 C36 116.4(3) . . ?
F5 C35 C34 121.8(3) . . ?
C36 C35 C34 121.6(3) . . ?
F6 C36 C35 120.2(3) . . ?
F6 C36 C37 118.9(3) . . ?
C35 C36 C37 120.9(3) . . ?
F7 C37 C36 121.0(3) . . ?
F7 C37 C38 120.7(3) . . ?
C36 C37 C38 118.2(3) . . ?
F8 C38 C39 120.0(3) . . ?
F8 C38 C37 117.3(3) . . ?
C39 C38 C37 122.6(3) . . ?
C38 C39 C34 118.7(3) . . ?
C38 C39 C40 115.7(2) . . ?
C34 C39 C40 125.5(2) . . ?
O8 C40 O7 126.5(3) . . ?
O8 C40 C39 117.7(2) . . ?
O7 C40 C39 115.6(2) . . ?
O9 C41 O10 126.0(3) . . ?
O9 C41 C42 117.9(2) . . ?
O10 C41 C42 116.1(2) . . ?
C43 C42 C47 119.8(3) . . ?
C43 C42 C41 118.2(2) . . ?
C47 C42 C41 122.0(2) . . ?
F12 C43 C44 118.5(2) . . ?
F12 C43 C42 120.1(3) . . ?
C44 C43 C42 121.4(3) . . ?
F11 C44 C45 120.1(3) . . ?
F11 C44 C43 120.5(3) . . ?
C45 C44 C43 119.4(2) . . ?
F10 C45 C44 120.4(3) . . ?
F10 C45 C46 119.9(3) . . ?
C44 C45 C46 119.7(3) . . ?
F9 C46 C47 122.3(2) . . ?
F9 C46 C45 115.9(3) . . ?
C47 C46 C45 121.8(3) . . ?
C46 C47 C42 117.9(2) . . ?
C46 C47 C48 121.4(2) . . ?
C42 C47 C48 120.7(2) . . ?
O12 C48 O11 121.8(2) . . ?
O12 C48 C47 117.9(2) . . ?
O11 C48 C47 120.3(2) . . ?
O12 C48 Gd1 54.00(14) . 2_657 ?
O11 C48 Gd1 68.42(14) . 2_657 ?
C47 C48 Gd1 168.22(19) . 2_657 ?
C1 N1 C12 117.7(3) . . ?
C1 N1 Gd1 121.94(19) . . ?
C12 N1 Gd1 120.08(18) . . ?
C10 N2 C11 117.9(2) . . ?
C10 N2 Gd1 122.44(18) . . ?
C11 N2 Gd1 118.75(17) . . ?
C13 N3 C24 118.0(3) . . ?
C13 N3 Gd2 121.2(2) . . ?
C24 N3 Gd2 120.85(19) . . ?
C22 N4 C23 117.8(3) . . ?
C22 N4 Gd2 123.4(2) . . ?
C23 N4 Gd2 118.60(19) . . ?
C25 O1 Gd1 152.8(2) . . ?
C25 O2 Gd2 155.60(19) . . ?
C32 O3 Gd1 145.28(18) . 2_657 ?
C33 O5 Gd2 91.98(17) . . ?
C33 O6 Gd2 95.17(16) . . ?
C40 O7 Gd2 167.6(2) . 2_666 ?
C41 O9 Gd2 155.32(19) . . ?
C41 O10 Gd1 125.22(16) . . ?
C48 O11 Gd1 138.83(17) . . ?
C48 O11 Gd1 86.09(15) . 2_657 ?
Gd1 O11 Gd1 118.09(7) . 2_657 ?
C48 O12 Gd1 101.31(17) . 2_657 ?
Gd1 O13 H13A 117.4 . . ?
Gd1 O13 H13B 112.7 . . ?
H13A O13 H13B 117.2 . . ?
Gd2 O14 H14A 122.7 . . ?
Gd2 O14 H14B 121.6 . . ?
H14A O14 H14B 115.6 . . ?
H15A O15 H15B 111.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.7(6) . . . . ?
C1 C2 C3 C4 0.6(6) . . . . ?
C2 C3 C4 C12 1.2(5) . . . . ?
C2 C3 C4 C5 -178.3(3) . . . . ?
C3 C4 C5 C6 -179.5(3) . . . . ?
C12 C4 C5 C6 0.9(5) . . . . ?
C4 C5 C6 C7 1.9(5) . . . . ?
C5 C6 C7 C8 176.0(3) . . . . ?
C5 C6 C7 C11 -2.6(5) . . . . ?
C11 C7 C8 C9 1.4(5) . . . . ?
C6 C7 C8 C9 -177.3(3) . . . . ?
C7 C8 C9 C10 -3.6(5) . . . . ?
C8 C9 C10 N2 3.5(5) . . . . ?
C8 C7 C11 N2 1.4(4) . . . . ?
C6 C7 C11 N2 -179.9(3) . . . . ?
C8 C7 C11 C12 -178.2(3) . . . . ?
C6 C7 C11 C12 0.5(4) . . . . ?
C3 C4 C12 N1 -3.2(4) . . . . ?
C5 C4 C12 N1 176.3(3) . . . . ?
C3 C4 C12 C11 177.5(3) . . . . ?
C5 C4 C12 C11 -3.0(4) . . . . ?
N2 C11 C12 N1 3.3(4) . . . . ?
C7 C11 C12 N1 -177.1(2) . . . . ?
N2 C11 C12 C4 -177.3(2) . . . . ?
C7 C11 C12 C4 2.2(4) . . . . ?
N3 C13 C14 C15 0.1(6) . . . . ?
C13 C14 C15 C16 0.3(6) . . . . ?
C14 C15 C16 C24 -1.0(5) . . . . ?
C14 C15 C16 C17 177.5(4) . . . . ?
C15 C16 C17 C18 -179.9(4) . . . . ?
C24 C16 C17 C18 -1.5(7) . . . . ?
C16 C17 C18 C19 -0.3(8) . . . . ?
C17 C18 C19 C20 -178.8(5) . . . . ?
C17 C18 C19 C23 0.7(7) . . . . ?
C23 C19 C20 C21 -0.3(7) . . . . ?
C18 C19 C20 C21 179.2(5) . . . . ?
C19 C20 C21 C22 0.5(7) . . . . ?
C20 C21 C22 N4 -0.2(7) . . . . ?
C20 C19 C23 N4 -0.1(5) . . . . ?
C18 C19 C23 N4 -179.6(4) . . . . ?
C20 C19 C23 C24 -179.7(3) . . . . ?
C18 C19 C23 C24 0.8(5) . . . . ?
C15 C16 C24 N3 1.2(5) . . . . ?
C17 C16 C24 N3 -177.3(3) . . . . ?
C15 C16 C24 C23 -178.6(3) . . . . ?
C17 C16 C24 C23 2.9(5) . . . . ?
N4 C23 C24 N3 -2.0(4) . . . . ?
C19 C23 C24 N3 177.6(3) . . . . ?
N4 C23 C24 C16 177.8(3) . . . . ?
C19 C23 C24 C16 -2.6(5) . . . . ?
O1 C25 C26 C27 -63.2(4) . . . . ?
O2 C25 C26 C27 118.0(3) . . . . ?
O1 C25 C26 C31 115.4(3) . . . . ?
O2 C25 C26 C31 -63.5(3) . . . . ?
C31 C26 C27 F1 178.0(3) . . . . ?
C25 C26 C27 F1 -3.5(4) . . . . ?
C31 C26 C27 C28 -1.5(4) . . . . ?
C25 C26 C27 C28 177.0(3) . . . . ?
F1 C27 C28 F2 3.1(5) . . . . ?
C26 C27 C28 F2 -177.4(3) . . . . ?
F1 C27 C28 C29 -178.5(3) . . . . ?
C26 C27 C28 C29 1.0(5) . . . . ?
F2 C28 C29 F3 -1.1(5) . . . . ?
C27 C28 C29 F3 -179.5(3) . . . . ?
F2 C28 C29 C30 178.2(3) . . . . ?
C27 C28 C29 C30 -0.2(5) . . . . ?
F3 C29 C30 F4 1.0(5) . . . . ?
C28 C29 C30 F4 -178.2(3) . . . . ?
F3 C29 C30 C31 179.2(3) . . . . ?
C28 C29 C30 C31 0.0(5) . . . . ?
F4 C30 C31 C26 177.7(3) . . . . ?
C29 C30 C31 C26 -0.5(5) . . . . ?
F4 C30 C31 C32 -0.4(4) . . . . ?
C29 C30 C31 C32 -178.6(3) . . . . ?
C27 C26 C31 C30 1.3(4) . . . . ?
C25 C26 C31 C30 -177.3(3) . . . . ?
C27 C26 C31 C32 179.4(3) . . . . ?
C25 C26 C31 C32 0.8(4) . . . . ?
C30 C31 C32 O4 -73.7(4) . . . . ?
C26 C31 C32 O4 108.3(3) . . . . ?
C30 C31 C32 O3 106.4(3) . . . . ?
C26 C31 C32 O3 -71.7(3) . . . . ?
O6 C33 C34 C35 166.3(3) . . . . ?
O5 C33 C34 C35 -13.7(4) . . . . ?
O6 C33 C34 C39 -13.6(4) . . . . ?
O5 C33 C34 C39 166.4(3) . . . . ?
C39 C34 C35 F5 176.9(3) . . . . ?
C33 C34 C35 F5 -3.0(5) . . . . ?
C39 C34 C35 C36 0.3(5) . . . . ?
C33 C34 C35 C36 -179.6(3) . . . . ?
F5 C35 C36 F6 2.5(5) . . . . ?
C34 C35 C36 F6 179.3(3) . . . . ?
F5 C35 C36 C37 -178.0(3) . . . . ?
C34 C35 C36 C37 -1.2(5) . . . . ?
F6 C36 C37 F7 -1.4(5) . . . . ?
C35 C36 C37 F7 179.0(3) . . . . ?
F6 C36 C37 C38 -179.6(3) . . . . ?
C35 C36 C37 C38 0.8(5) . . . . ?
F7 C37 C38 F8 0.8(5) . . . . ?
C36 C37 C38 F8 179.0(3) . . . . ?
F7 C37 C38 C39 -177.8(3) . . . . ?
C36 C37 C38 C39 0.4(5) . . . . ?
F8 C38 C39 C34 -179.8(3) . . . . ?
C37 C38 C39 C34 -1.2(5) . . . . ?
F8 C38 C39 C40 0.3(4) . . . . ?
C37 C38 C39 C40 178.9(3) . . . . ?
C35 C34 C39 C38 0.9(4) . . . . ?
C33 C34 C39 C38 -179.3(3) . . . . ?
C35 C34 C39 C40 -179.3(3) . . . . ?
C33 C34 C39 C40 0.6(4) . . . . ?
C38 C39 C40 O8 85.1(3) . . . . ?
C34 C39 C40 O8 -94.8(4) . . . . ?
C38 C39 C40 O7 -89.8(3) . . . . ?
C34 C39 C40 O7 90.3(3) . . . . ?
O9 C41 C42 C43 -89.5(3) . . . . ?
O10 C41 C42 C43 87.6(3) . . . . ?
O9 C41 C42 C47 89.9(3) . . . . ?
O10 C41 C42 C47 -93.0(3) . . . . ?
C47 C42 C43 F12 -178.8(2) . . . . ?
C41 C42 C43 F12 0.7(4) . . . . ?
C47 C42 C43 C44 1.6(4) . . . . ?
C41 C42 C43 C44 -178.9(3) . . . . ?
F12 C43 C44 F11 -0.2(4) . . . . ?
C42 C43 C44 F11 179.4(3) . . . . ?
F12 C43 C44 C45 179.3(3) . . . . ?
C42 C43 C44 C45 -1.1(4) . . . . ?
F11 C44 C45 F10 -1.2(5) . . . . ?
C43 C44 C45 F10 179.3(3) . . . . ?
F11 C44 C45 C46 178.9(3) . . . . ?
C43 C44 C45 C46 -0.6(5) . . . . ?
F10 C45 C46 F9 0.5(4) . . . . ?
C44 C45 C46 F9 -179.6(3) . . . . ?
F10 C45 C46 C47 -178.1(3) . . . . ?
C44 C45 C46 C47 1.9(5) . . . . ?
F9 C46 C47 C42 -179.8(3) . . . . ?
C45 C46 C47 C42 -1.4(4) . . . . ?
F9 C46 C47 C48 -0.4(4) . . . . ?
C45 C46 C47 C48 178.0(3) . . . . ?
C43 C42 C47 C46 -0.4(4) . . . . ?
C41 C42 C47 C46 -179.8(2) . . . . ?
C43 C42 C47 C48 -179.8(2) . . . . ?
C41 C42 C47 C48 0.8(4) . . . . ?
C46 C47 C48 O12 26.1(4) . . . . ?
C42 C47 C48 O12 -154.4(3) . . . . ?
C46 C47 C48 O11 -153.7(3) . . . . ?
C42 C47 C48 O11 25.8(4) . . . . ?
C46 C47 C48 Gd1 -17.9(11) . . . 2_657 ?
C42 C47 C48 Gd1 161.5(8) . . . 2_657 ?
C2 C1 N1 C12 -1.3(5) . . . . ?
C2 C1 N1 Gd1 173.0(3) . . . . ?
C4 C12 N1 C1 3.2(4) . . . . ?
C11 C12 N1 C1 -177.5(3) . . . . ?
C4 C12 N1 Gd1 -171.2(2) . . . . ?
C11 C12 N1 Gd1 8.1(3) . . . . ?
C9 C10 N2 C11 -0.8(4) . . . . ?
C9 C10 N2 Gd1 -169.5(2) . . . . ?
C7 C11 N2 C10 -1.6(4) . . . . ?
C12 C11 N2 C10 177.9(2) . . . . ?
C7 C11 N2 Gd1 167.5(2) . . . . ?
C12 C11 N2 Gd1 -12.9(3) . . . . ?
C14 C13 N3 C24 0.1(5) . . . . ?
C14 C13 N3 Gd2 -178.7(3) . . . . ?
C16 C24 N3 C13 -0.8(4) . . . . ?
C23 C24 N3 C13 179.0(3) . . . . ?
C16 C24 N3 Gd2 178.0(2) . . . . ?
C23 C24 N3 Gd2 -2.2(3) . . . . ?
C21 C22 N4 C23 -0.1(5) . . . . ?
C21 C22 N4 Gd2 174.4(3) . . . . ?
C19 C23 N4 C22 0.3(5) . . . . ?
C24 C23 N4 C22 179.9(3) . . . . ?
C19 C23 N4 Gd2 -174.5(3) . . . . ?
C24 C23 N4 Gd2 5.1(3) . . . . ?
O2 C25 O1 Gd1 59.8(6) . . . . ?
C26 C25 O1 Gd1 -118.9(4) . . . . ?
O1 C25 O2 Gd2 32.9(7) . . . . ?
C26 C25 O2 Gd2 -148.4(4) . . . . ?
O4 C32 O3 Gd1 -23.5(5) . . . 2_657 ?
C31 C32 O3 Gd1 156.4(2) . . . 2_657 ?
O6 C33 O5 Gd2 1.6(3) . . . . ?
C34 C33 O5 Gd2 -178.5(2) . . . . ?
O5 C33 O6 Gd2 -1.6(3) . . . . ?
C34 C33 O6 Gd2 178.4(2) . . . . ?
O8 C40 O7 Gd2 -169.8(7) . . . 2_666 ?
C39 C40 O7 Gd2 4.5(11) . . . 2_666 ?
O10 C41 O9 Gd2 111.0(5) . . . . ?
C42 C41 O9 Gd2 -72.2(5) . . . . ?
O9 C41 O10 Gd1 -100.1(3) . . . . ?
C42 C41 O10 Gd1 83.0(3) . . . . ?
O12 C48 O11 Gd1 -138.3(2) . . . . ?
C47 C48 O11 Gd1 41.5(4) . . . . ?
Gd1 C48 O11 Gd1 -129.7(2) 2_657 . . . ?
O12 C48 O11 Gd1 -8.6(3) . . . 2_657 ?
C47 C48 O11 Gd1 171.2(2) . . . 2_657 ?
O11 C48 O12 Gd1 9.9(3) . . . 2_657 ?
C47 C48 O12 Gd1 -169.90(19) . . . 2_657 ?

_refine_diff_density_max         1.242
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.153


