# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_a160119e
_audit_block_doi                 10.5517/ccdc.csd.cc1zgcph
_database_code_depnum_ccdc_archive 'CCDC 1831067'
_audit_update_record             
;
2018-03-20 deposited with the CCDC.
2018-04-12 downloaded from the CCDC.
;
_audit_creation_date             2016-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H21 F18 Gd N5 O9'
_chemical_formula_sum            'C25 H21 F18 Gd N5 O9'
_chemical_formula_weight         1034.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0094(3)
_cell_length_b                   12.3115(4)
_cell_length_c                   16.2016(5)
_cell_angle_alpha                105.182(3)
_cell_angle_beta                 103.964(3)
_cell_angle_gamma                99.368(3)
_cell_volume                     1814.66(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    113.00(10)
_cell_measurement_theta_max      28.0470
_cell_measurement_theta_min      3.8470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13737
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.364
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      113.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  84.00   1.00    2.85    --   11.08  38.00-120.00   96
  2  ω    -10.00  30.00   1.00    2.85    --  -11.24-107.00 -14.00   40
  3  ω     36.00  72.00   1.00    2.85    --   11.08-178.00  90.00   36
  4  ω     41.00  98.00   1.00    2.85    --   11.08-178.00  30.00   57
  5  ω    -13.00  85.00   1.00    2.85    --   11.08  38.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0306699000
_diffrn_orient_matrix_UB_12      -0.0163483000
_diffrn_orient_matrix_UB_13      0.0377661000
_diffrn_orient_matrix_UB_21      -0.0301806000
_diffrn_orient_matrix_UB_22      0.0385486000
_diffrn_orient_matrix_UB_23      0.0264781000
_diffrn_orient_matrix_UB_31      -0.0617267000
_diffrn_orient_matrix_UB_32      -0.0450629000
_diffrn_orient_matrix_UB_33      -0.0114562000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5681
_reflns_number_total             6381
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.836
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6381
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0394
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+4.3088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0913
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F11-C20 = F3A-C20 = F12'-C20 = F10'-C20 = F10-C20 = F11'-C20
 1.34 with sigma of 0.01
 C15-C14 = C15'-C14
 1.56 with sigma of 0.01
 F4-C15 = F4'-C15' = F6'-C15' = F6-C15 = F5'-C15' = F5-C15
 1.34 with sigma of 0.01
 F4-F5 \\sim F5-F6
 with sigma of 0.001
 F5-F6 \\sim F6-F4
 with sigma of 0.001
 F4'-F5' \\sim F5'-F6'
 with sigma of 0.001
 F5'-F6' \\sim F6'-F4'
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(F3A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11') \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F10') \\sim Ueq, Uanis(F12') \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(F11) = Uanis(F3A)
Uanis(F12') = Uanis(F10')
Uanis(F10) = Uanis(F11')
Uanis(F4) = Uanis(F4')
Uanis(F5) = Uanis(F5')
Uanis(F6) = Uanis(F6')
Uanis(C15) = Uanis(C15')
4. Others
 Sof(F3A)=Sof(F10')=Sof(F11')=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12')=FVAR(1)
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(C15')=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C15)=FVAR(2)
5.a Rotating group:
 O9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C18(H18), C23(H23)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.49234(2) 0.80423(2) 0.29979(2) 0.01241(9) Uani 1 1 d . . . . .
F1 F 0.8062(5) 0.9017(3) 0.6481(2) 0.0578(11) Uani 1 1 d . U . . .
F2 F 0.9630(4) 0.8596(3) 0.5876(3) 0.0664(13) Uani 1 1 d . U . . .
F3 F 0.8787(4) 1.0052(3) 0.5748(2) 0.0589(12) Uani 1 1 d . . . . .
F7 F 0.7723(4) 1.1796(2) 0.2712(2) 0.0443(10) Uani 1 1 d . . . . .
F8 F 0.7849(4) 1.0882(3) 0.1418(2) 0.0414(9) Uani 1 1 d . . . . .
F9 F 0.5828(4) 1.0944(3) 0.1615(3) 0.0587(11) Uani 1 1 d . U . . .
F13 F 0.1391(5) 1.0016(4) 0.1642(2) 0.0627(12) Uani 1 1 d . . . . .
F14 F 0.0730(5) 0.8838(4) 0.0362(3) 0.0904(17) Uani 1 1 d . U . . .
F15 F 0.2394(6) 1.0267(4) 0.0663(4) 0.0890(16) Uani 1 1 d . U . . .
F16 F 0.4500(5) 0.7186(4) -0.0718(2) 0.0658(13) Uani 1 1 d . . . . .
F17 F 0.5984(4) 0.6635(4) 0.0179(2) 0.0582(11) Uani 1 1 d . . . . .
F18 F 0.3831(5) 0.5694(3) -0.0377(3) 0.0652(12) Uani 1 1 d . . . . .
O1 O 0.2683(4) 0.6622(3) 0.2229(2) 0.0180(7) Uani 1 1 d . . . . .
O2 O 0.1122(4) 0.4215(3) 0.3735(2) 0.0264(8) Uani 1 1 d . . . . .
O3 O 0.6643(3) 0.8704(3) 0.4435(2) 0.0190(7) Uani 1 1 d . . . . .
O4 O 0.5319(3) 0.6332(3) 0.3339(2) 0.0178(7) Uani 1 1 d . . . . .
O5 O 0.6205(4) 0.9674(3) 0.2744(2) 0.0214(8) Uani 1 1 d . . . . .
O6 O 0.7237(4) 0.7735(3) 0.2840(2) 0.0209(8) Uani 1 1 d . . . . .
O7 O 0.4788(4) 0.7246(3) 0.1469(2) 0.0184(7) Uani 1 1 d . . . . .
O8 O 0.3210(3) 0.8815(3) 0.2086(2) 0.0175(7) Uani 1 1 d . . . . .
O9 O 0.4353(4) 0.9724(3) 0.3836(2) 0.0183(7) Uani 1 1 d . . . . .
H9A H 0.3939 1.0070 0.3479 0.027 Uiso 1 1 d GR . . . .
H9B H 0.5120 1.0214 0.4217 0.027 Uiso 1 1 d GR . . . .
N1 N 0.2133(4) 0.5719(3) 0.2401(2) 0.0147(9) Uani 1 1 d . . . . .
N2 N 0.1337(4) 0.4584(3) 0.3104(3) 0.0173(9) Uani 1 1 d . . . . .
N3 N 0.3541(4) 0.7544(3) 0.4143(2) 0.0172(9) Uani 1 1 d . . . . .
N4 N 0.3655(5) 0.8335(3) 0.4948(3) 0.0226(10) Uani 1 1 d . . . . .
N5 N 0.1764(5) 0.6939(3) 0.4627(3) 0.0198(9) Uani 1 1 d . . . . .
C1 C 0.1953(5) 0.5685(4) 0.3180(3) 0.0133(10) Uani 1 1 d . . . . .
C2 C 0.1705(6) 0.4533(4) 0.1703(3) 0.0196(11) Uani 1 1 d . . . . .
C3 C 0.3075(6) 0.4192(5) 0.1633(4) 0.0301(13) Uani 1 1 d . . . . .
H3A H 0.3649 0.4771 0.1483 0.045 Uiso 1 1 calc GR . . . .
H3B H 0.2860 0.3458 0.1176 0.045 Uiso 1 1 calc GR . . . .
H3C H 0.3583 0.4132 0.2197 0.045 Uiso 1 1 calc GR . . . .
C4 C 0.0887(6) 0.4627(5) 0.0819(3) 0.0324(14) Uani 1 1 d . . . . .
H4A H 0.0102 0.4956 0.0895 0.049 Uiso 1 1 calc GR . . . .
H4B H 0.0540 0.3869 0.0383 0.049 Uiso 1 1 calc GR . . . .
H4C H 0.1500 0.5114 0.0619 0.049 Uiso 1 1 calc GR . . . .
C5 C 0.0816(5) 0.3823(4) 0.2143(3) 0.0190(11) Uani 1 1 d . . . . .
C6 C -0.0768(5) 0.3755(4) 0.1842(4) 0.0269(12) Uani 1 1 d . . . . .
H6A H -0.1216 0.3452 0.2224 0.040 Uiso 1 1 calc GR . . . .
H6B H -0.1175 0.3254 0.1235 0.040 Uiso 1 1 calc GR . . . .
H6C H -0.0911 0.4517 0.1879 0.040 Uiso 1 1 calc GR . . . .
C7 C 0.1085(6) 0.2628(4) 0.2091(4) 0.0285(13) Uani 1 1 d . . . . .
H7A H 0.2079 0.2703 0.2346 0.043 Uiso 1 1 calc GR . . . .
H7B H 0.0785 0.2149 0.1476 0.043 Uiso 1 1 calc GR . . . .
H7C H 0.0560 0.2280 0.2419 0.043 Uiso 1 1 calc GR . . . .
C8 C 0.2405(5) 0.6699(4) 0.3977(3) 0.0139(10) Uani 1 1 d . . . . .
C9 C 0.2597(6) 0.7961(4) 0.5211(3) 0.0256(12) Uani 1 1 d . . . . .
H9 H 0.2430 0.8348 0.5738 0.031 Uiso 1 1 calc R . . . .
C10 C 0.0386(7) 0.6358(5) 0.4662(4) 0.0381(15) Uani 1 1 d . . . . .
H10A H -0.0355 0.6610 0.4320 0.057 Uiso 1 1 calc GR . . . .
H10B H 0.0373 0.6551 0.5274 0.057 Uiso 1 1 calc GR . . . .
H10C H 0.0241 0.5534 0.4417 0.057 Uiso 1 1 calc GR . . . .
C11 C 0.8473(6) 0.8983(5) 0.5745(4) 0.0298(13) Uani 1 1 d . . . . .
C12 C 0.7281(5) 0.8188(4) 0.4905(3) 0.0218(11) Uani 1 1 d . . . . .
C13 C 0.7070(6) 0.6995(4) 0.4764(3) 0.0263(12) Uani 1 1 d . . . . .
H13 H 0.7586 0.6739 0.5203 0.032 Uiso 1 1 calc R . . . .
C14 C 0.6120(6) 0.6176(4) 0.3994(4) 0.0250(12) Uani 1 1 d D . . . .
C16 C 0.7111(6) 1.0843(4) 0.2000(3) 0.0266(12) Uani 1 1 d . . . . .
C17 C 0.7053(5) 0.9760(4) 0.2299(3) 0.0195(11) Uani 1 1 d . . . . .
C18 C 0.7918(6) 0.9053(4) 0.2077(3) 0.0238(12) Uani 1 1 d . . . . .
H18 H 0.8467 0.9198 0.1711 0.029 Uiso 1 1 calc R . . . .
C19 C 0.7975(5) 0.8098(4) 0.2407(3) 0.0214(11) Uani 1 1 d . . . . .
C20 C 0.9063(5) 0.7428(4) 0.2226(3) 0.0283(13) Uani 1 1 d D . . . .
C21 C 0.4670(7) 0.6768(5) -0.0044(4) 0.0336(14) Uani 1 1 d . . . . .
C22 C 0.4297(6) 0.7453(4) 0.0762(3) 0.0218(11) Uani 1 1 d . . . . .
C23 C 0.3435(6) 0.8201(4) 0.0614(3) 0.0257(12) Uani 1 1 d . . . . .
H23 H 0.3186 0.8306 0.0054 0.031 Uiso 1 1 calc R . . . .
C24 C 0.2930(6) 0.8805(4) 0.1291(3) 0.0225(11) Uani 1 1 d . . . . .
C25 C 0.1887(7) 0.9517(5) 0.1011(4) 0.0321(13) Uani 1 1 d . . . . .
F4 F 0.6617(9) 0.4704(7) 0.4699(5) 0.058(2) Uani 0.552(10) 1 d D U P A 1
F5 F 0.4489(8) 0.4413(10) 0.3845(6) 0.043(2) Uani 0.552(10) 1 d D U P A 1
F6 F 0.6216(9) 0.4317(11) 0.3271(6) 0.051(2) Uani 0.552(10) 1 d D U P A 1
F10 F 0.9910(8) 0.7374(8) 0.2953(4) 0.0706(18) Uani 0.646(5) 1 d D U P B 1
F11 F 0.9733(9) 0.7699(7) 0.1666(5) 0.076(2) Uani 0.646(5) 1 d D U P B 1
F12' F 0.8398(7) 0.6334(5) 0.1718(5) 0.0698(18) Uani 0.646(5) 1 d D U P B 1
C15 C 0.5856(11) 0.4882(7) 0.3978(7) 0.031(3) Uani 0.552(10) 1 d D . P A 1
F3A F 0.8887(17) 0.6822(13) 0.1393(7) 0.076(2) Uani 0.354(5) 1 d D U P B 2
F4' F 0.7208(11) 0.4696(9) 0.4401(7) 0.058(2) Uani 0.448(10) 1 d D . P A 2
F5' F 0.4957(11) 0.4289(13) 0.3808(7) 0.043(2) Uani 0.448(10) 1 d D . P A 2
F6' F 0.6340(12) 0.4375(15) 0.2991(6) 0.051(2) Uani 0.448(10) 1 d D . P A 2
F10' F 0.9242(16) 0.6652(10) 0.2660(9) 0.0698(18) Uani 0.354(5) 1 d D U P B 2
F11' F 1.0354(10) 0.8137(10) 0.2412(9) 0.0706(18) Uani 0.354(5) 1 d D U P B 2
C15' C 0.6195(13) 0.4878(8) 0.3794(8) 0.031(3) Uani 0.448(10) 1 d D . P A 2


_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 O1 2.423(3) . ?
Gd1 O3 2.380(3) . ?
Gd1 O4 2.382(3) . ?
Gd1 O5 2.388(3) . ?
Gd1 O6 2.468(4) . ?
Gd1 O7 2.375(3) . ?
Gd1 O8 2.465(3) . ?
Gd1 O9 2.397(3) . ?
Gd1 N3 2.701(4) . ?
F1 C11 1.345(7) . ?
F2 C11 1.315(7) . ?
F3 C11 1.302(6) . ?
F7 C16 1.341(6) . ?
F8 C16 1.336(6) . ?
F9 C16 1.328(7) . ?
F13 C25 1.298(7) . ?
F14 C25 1.335(7) . ?
F15 C25 1.299(7) . ?
F16 C21 1.310(6) . ?
F17 C21 1.326(7) . ?
F18 C21 1.338(7) . ?
O1 N1 1.286(5) . ?
O2 N2 1.271(5) . ?
O3 C12 1.241(6) . ?
O4 C14 1.244(6) . ?
O5 C17 1.247(6) . ?
O6 C19 1.242(6) . ?
O7 C22 1.241(6) . ?
O8 C24 1.247(6) . ?
O9 H9A 0.8718 . ?
O9 H9B 0.8721 . ?
N1 C1 1.327(6) . ?
N1 C2 1.514(6) . ?
N2 C1 1.356(6) . ?
N2 C5 1.503(6) . ?
N3 N4 1.374(5) . ?
N3 C8 1.330(6) . ?
N4 C9 1.295(7) . ?
N5 C8 1.354(6) . ?
N5 C9 1.352(6) . ?
N5 C10 1.468(7) . ?
C1 C8 1.456(6) . ?
C2 C3 1.519(8) . ?
C2 C4 1.511(7) . ?
C2 C5 1.564(7) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.523(7) . ?
C5 C7 1.522(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.540(7) . ?
C12 C13 1.398(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.391(7) . ?
C14 C15 1.564(8) . ?
C14 C15' 1.564(9) . ?
C16 C17 1.530(7) . ?
C17 C18 1.368(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.417(7) . ?
C19 C20 1.508(7) . ?
C20 F10 1.299(7) . ?
C20 F11 1.328(7) . ?
C20 F12' 1.341(7) . ?
C20 F3A 1.312(9) . ?
C20 F10' 1.336(9) . ?
C20 F11' 1.352(9) . ?
C21 C22 1.522(7) . ?
C22 C23 1.387(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.404(7) . ?
C24 C25 1.530(8) . ?
F4 C15 1.324(8) . ?
F5 C15 1.337(8) . ?
F6 C15 1.338(8) . ?
F4' C15' 1.324(9) . ?
F5' C15' 1.339(9) . ?
F6' C15' 1.340(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O6 124.36(11) . . ?
O1 Gd1 O8 68.37(10) . . ?
O1 Gd1 N3 67.68(11) . . ?
O3 Gd1 O1 138.02(10) . . ?
O3 Gd1 O4 74.60(11) . . ?
O3 Gd1 O5 85.31(11) . . ?
O3 Gd1 O6 70.40(11) . . ?
O3 Gd1 O8 137.77(10) . . ?
O3 Gd1 O9 74.05(11) . . ?
O3 Gd1 N3 73.91(11) . . ?
O4 Gd1 O1 75.61(11) . . ?
O4 Gd1 O5 138.98(12) . . ?
O4 Gd1 O6 69.92(11) . . ?
O4 Gd1 O8 143.71(10) . . ?
O4 Gd1 O9 131.31(11) . . ?
O4 Gd1 N3 67.54(12) . . ?
O5 Gd1 O1 135.81(11) . . ?
O5 Gd1 O6 69.73(11) . . ?
O5 Gd1 O8 71.70(11) . . ?
O5 Gd1 O9 73.21(11) . . ?
O5 Gd1 N3 140.10(11) . . ?
O6 Gd1 N3 129.94(11) . . ?
O7 Gd1 O1 71.02(11) . . ?
O7 Gd1 O3 139.18(12) . . ?
O7 Gd1 O4 93.17(11) . . ?
O7 Gd1 O5 79.05(11) . . ?
O7 Gd1 O6 68.83(11) . . ?
O7 Gd1 O8 71.36(11) . . ?
O7 Gd1 O9 134.20(11) . . ?
O7 Gd1 N3 137.52(11) . . ?
O8 Gd1 O6 128.44(11) . . ?
O8 Gd1 N3 101.56(12) . . ?
O9 Gd1 O1 105.75(11) . . ?
O9 Gd1 O6 129.84(11) . . ?
O9 Gd1 O8 65.69(11) . . ?
O9 Gd1 N3 68.52(11) . . ?
N1 O1 Gd1 130.4(3) . . ?
C12 O3 Gd1 132.5(3) . . ?
C14 O4 Gd1 132.4(3) . . ?
C17 O5 Gd1 132.1(3) . . ?
C19 O6 Gd1 130.7(3) . . ?
C22 O7 Gd1 136.0(3) . . ?
C24 O8 Gd1 132.9(3) . . ?
Gd1 O9 H9A 110.4 . . ?
Gd1 O9 H9B 110.5 . . ?
H9A O9 H9B 108.3 . . ?
O1 N1 C1 126.3(4) . . ?
O1 N1 C2 120.6(3) . . ?
C1 N1 C2 112.9(4) . . ?
O2 N2 C1 126.5(4) . . ?
O2 N2 C5 122.0(3) . . ?
C1 N2 C5 111.4(4) . . ?
N4 N3 Gd1 122.9(3) . . ?
C8 N3 Gd1 128.7(3) . . ?
C8 N3 N4 106.1(4) . . ?
C9 N4 N3 107.4(4) . . ?
C8 N5 C10 130.0(4) . . ?
C9 N5 C8 103.9(4) . . ?
C9 N5 C10 125.5(4) . . ?
N1 C1 N2 109.4(4) . . ?
N1 C1 C8 123.1(4) . . ?
N2 C1 C8 127.4(4) . . ?
N1 C2 C3 106.3(4) . . ?
N1 C2 C5 100.3(4) . . ?
C3 C2 C5 115.1(4) . . ?
C4 C2 N1 108.6(4) . . ?
C4 C2 C3 110.2(4) . . ?
C4 C2 C5 115.3(4) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C2 101.4(3) . . ?
N2 C5 C6 105.3(4) . . ?
N2 C5 C7 109.2(4) . . ?
C6 C5 C2 114.0(4) . . ?
C7 C5 C2 114.9(5) . . ?
C7 C5 C6 111.0(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 N5 110.8(4) . . ?
N3 C8 C1 122.1(4) . . ?
N5 C8 C1 127.1(4) . . ?
N4 C9 N5 111.8(4) . . ?
N4 C9 H9 124.1 . . ?
N5 C9 H9 124.1 . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
F1 C11 C12 109.8(5) . . ?
F2 C11 F1 104.7(5) . . ?
F2 C11 C12 112.9(4) . . ?
F3 C11 F1 106.0(4) . . ?
F3 C11 F2 109.7(5) . . ?
F3 C11 C12 113.2(4) . . ?
O3 C12 C11 114.8(4) . . ?
O3 C12 C13 128.6(5) . . ?
C13 C12 C11 116.6(5) . . ?
C12 C13 H13 118.7 . . ?
C14 C13 C12 122.6(5) . . ?
C14 C13 H13 118.7 . . ?
O4 C14 C13 129.0(4) . . ?
O4 C14 C15 113.6(5) . . ?
O4 C14 C15' 111.3(5) . . ?
C13 C14 C15 117.0(5) . . ?
C13 C14 C15' 118.8(6) . . ?
F7 C16 C17 109.9(4) . . ?
F8 C16 F7 106.7(4) . . ?
F8 C16 C17 114.2(5) . . ?
F9 C16 F7 107.1(5) . . ?
F9 C16 F8 106.4(4) . . ?
F9 C16 C17 112.1(4) . . ?
O5 C17 C16 112.5(4) . . ?
O5 C17 C18 129.2(5) . . ?
C18 C17 C16 118.4(5) . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.7(5) . . ?
C19 C18 H18 120.2 . . ?
O6 C19 C18 128.0(5) . . ?
O6 C19 C20 114.7(4) . . ?
C18 C19 C20 117.3(4) . . ?
F10 C20 C19 112.7(5) . . ?
F10 C20 F11 113.4(6) . . ?
F10 C20 F12' 106.9(6) . . ?
F11 C20 C19 115.7(5) . . ?
F11 C20 F12' 97.4(6) . . ?
F12' C20 C19 109.2(5) . . ?
F3A C20 C19 117.8(7) . . ?
F3A C20 F10' 102.7(9) . . ?
F3A C20 F11' 99.9(9) . . ?
F10' C20 C19 115.7(6) . . ?
F10' C20 F11' 107.1(9) . . ?
F11' C20 C19 111.9(6) . . ?
F16 C21 F17 108.5(5) . . ?
F16 C21 F18 105.4(5) . . ?
F16 C21 C22 115.3(5) . . ?
F17 C21 F18 105.6(5) . . ?
F17 C21 C22 111.9(5) . . ?
F18 C21 C22 109.5(5) . . ?
O7 C22 C21 114.9(5) . . ?
O7 C22 C23 128.3(5) . . ?
C23 C22 C21 116.7(5) . . ?
C22 C23 H23 119.2 . . ?
C22 C23 C24 121.6(5) . . ?
C24 C23 H23 119.2 . . ?
O8 C24 C23 127.9(5) . . ?
O8 C24 C25 116.2(5) . . ?
C23 C24 C25 115.9(4) . . ?
F13 C25 F14 103.7(6) . . ?
F13 C25 F15 110.3(5) . . ?
F13 C25 C24 114.1(4) . . ?
F14 C25 C24 110.9(4) . . ?
F15 C25 F14 104.1(5) . . ?
F15 C25 C24 112.9(5) . . ?
F4 C15 C14 114.9(8) . . ?
F4 C15 F5 108.3(6) . . ?
F4 C15 F6 108.3(6) . . ?
F5 C15 C14 112.2(8) . . ?
F5 C15 F6 107.5(6) . . ?
F6 C15 C14 105.3(9) . . ?
F4' C15' C14 113.9(9) . . ?
F4' C15' F5' 107.1(7) . . ?
F4' C15' F6' 107.0(7) . . ?
F5' C15' C14 106.5(11) . . ?
F5' C15' F6' 106.2(7) . . ?
F6' C15' C14 115.6(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 N1 C1 52.5(6) . . . . ?
Gd1 O1 N1 C2 -123.3(4) . . . . ?
Gd1 O3 C12 C11 171.7(3) . . . . ?
Gd1 O3 C12 C13 -7.3(8) . . . . ?
Gd1 O4 C14 C13 0.3(9) . . . . ?
Gd1 O4 C14 C15 172.0(5) . . . . ?
Gd1 O4 C14 C15' -168.2(6) . . . . ?
Gd1 O5 C17 C16 155.2(3) . . . . ?
Gd1 O5 C17 C18 -26.5(8) . . . . ?
Gd1 O6 C19 C18 19.7(7) . . . . ?
Gd1 O6 C19 C20 -160.7(3) . . . . ?
Gd1 O7 C22 C21 172.0(3) . . . . ?
Gd1 O7 C22 C23 -9.7(8) . . . . ?
Gd1 O8 C24 C23 8.2(8) . . . . ?
Gd1 O8 C24 C25 -173.1(3) . . . . ?
Gd1 N3 N4 C9 162.3(3) . . . . ?
Gd1 N3 C8 N5 -160.6(3) . . . . ?
Gd1 N3 C8 C1 18.3(6) . . . . ?
F1 C11 C12 O3 107.0(5) . . . . ?
F1 C11 C12 C13 -73.8(6) . . . . ?
F2 C11 C12 O3 -136.6(5) . . . . ?
F2 C11 C12 C13 42.6(7) . . . . ?
F3 C11 C12 O3 -11.3(7) . . . . ?
F3 C11 C12 C13 167.9(5) . . . . ?
F7 C16 C17 O5 69.1(6) . . . . ?
F7 C16 C17 C18 -109.3(5) . . . . ?
F8 C16 C17 O5 -171.0(4) . . . . ?
F8 C16 C17 C18 10.6(7) . . . . ?
F9 C16 C17 O5 -49.8(6) . . . . ?
F9 C16 C17 C18 131.7(5) . . . . ?
F16 C21 C22 O7 -162.3(5) . . . . ?
F16 C21 C22 C23 19.1(8) . . . . ?
F17 C21 C22 O7 -37.7(6) . . . . ?
F17 C21 C22 C23 143.8(5) . . . . ?
F18 C21 C22 O7 79.0(6) . . . . ?
F18 C21 C22 C23 -99.5(6) . . . . ?
O1 N1 C1 N2 179.8(4) . . . . ?
O1 N1 C1 C8 -1.7(8) . . . . ?
O1 N1 C2 C3 72.1(5) . . . . ?
O1 N1 C2 C4 -46.5(6) . . . . ?
O1 N1 C2 C5 -167.8(4) . . . . ?
O2 N2 C1 N1 173.5(4) . . . . ?
O2 N2 C1 C8 -4.9(8) . . . . ?
O2 N2 C5 C2 -164.2(4) . . . . ?
O2 N2 C5 C6 76.8(5) . . . . ?
O2 N2 C5 C7 -42.5(6) . . . . ?
O3 C12 C13 C14 5.0(9) . . . . ?
O4 C14 C15 F4 -175.1(6) . . . . ?
O4 C14 C15 F5 -50.8(9) . . . . ?
O4 C14 C15 F6 65.9(8) . . . . ?
O4 C14 C15' F4' 169.1(7) . . . . ?
O4 C14 C15' F5' -73.1(8) . . . . ?
O4 C14 C15' F6' 44.5(10) . . . . ?
O5 C17 C18 C19 -3.4(8) . . . . ?
O6 C19 C20 F10 -55.8(7) . . . . ?
O6 C19 C20 F11 171.4(6) . . . . ?
O6 C19 C20 F12' 62.8(7) . . . . ?
O6 C19 C20 F3A 112.3(9) . . . . ?
O6 C19 C20 F10' -9.6(10) . . . . ?
O6 C19 C20 F11' -132.8(7) . . . . ?
O7 C22 C23 C24 -3.6(9) . . . . ?
O8 C24 C25 F13 -2.0(7) . . . . ?
O8 C24 C25 F14 -118.7(5) . . . . ?
O8 C24 C25 F15 125.0(5) . . . . ?
N1 C1 C8 N3 -32.3(7) . . . . ?
N1 C1 C8 N5 146.4(5) . . . . ?
N1 C2 C5 N2 -19.7(4) . . . . ?
N1 C2 C5 C6 93.0(4) . . . . ?
N1 C2 C5 C7 -137.3(4) . . . . ?
N2 C1 C8 N3 145.9(5) . . . . ?
N2 C1 C8 N5 -35.5(8) . . . . ?
N3 N4 C9 N5 0.6(6) . . . . ?
N4 N3 C8 N5 2.1(5) . . . . ?
N4 N3 C8 C1 -179.1(4) . . . . ?
C1 N1 C2 C3 -104.3(5) . . . . ?
C1 N1 C2 C4 137.1(5) . . . . ?
C1 N1 C2 C5 15.9(5) . . . . ?
C1 N2 C5 C2 19.9(5) . . . . ?
C1 N2 C5 C6 -99.2(4) . . . . ?
C1 N2 C5 C7 141.5(4) . . . . ?
C2 N1 C1 N2 -4.1(6) . . . . ?
C2 N1 C1 C8 174.4(4) . . . . ?
C3 C2 C5 N2 93.9(4) . . . . ?
C3 C2 C5 C6 -153.5(4) . . . . ?
C3 C2 C5 C7 -23.7(6) . . . . ?
C4 C2 C5 N2 -136.1(4) . . . . ?
C4 C2 C5 C6 -23.4(6) . . . . ?
C4 C2 C5 C7 106.3(5) . . . . ?
C5 N2 C1 N1 -10.8(5) . . . . ?
C5 N2 C1 C8 170.9(5) . . . . ?
C8 N3 N4 C9 -1.6(5) . . . . ?
C8 N5 C9 N4 0.6(6) . . . . ?
C9 N5 C8 N3 -1.7(5) . . . . ?
C9 N5 C8 C1 179.5(5) . . . . ?
C10 N5 C8 N3 169.9(5) . . . . ?
C10 N5 C8 C1 -8.8(8) . . . . ?
C10 N5 C9 N4 -171.5(5) . . . . ?
C11 C12 C13 C14 -174.1(5) . . . . ?
C12 C13 C14 O4 -1.2(10) . . . . ?
C12 C13 C14 C15 -172.7(6) . . . . ?
C12 C13 C14 C15' 166.5(7) . . . . ?
C13 C14 C15 F4 -2.3(10) . . . . ?
C13 C14 C15 F5 122.0(7) . . . . ?
C13 C14 C15 F6 -121.3(7) . . . . ?
C13 C14 C15' F4' -0.7(11) . . . . ?
C13 C14 C15' F5' 117.1(7) . . . . ?
C13 C14 C15' F6' -125.2(8) . . . . ?
C16 C17 C18 C19 174.7(4) . . . . ?
C17 C18 C19 O6 6.1(8) . . . . ?
C17 C18 C19 C20 -173.5(4) . . . . ?
C18 C19 C20 F10 123.8(6) . . . . ?
C18 C19 C20 F11 -9.0(8) . . . . ?
C18 C19 C20 F12' -117.5(6) . . . . ?
C18 C19 C20 F3A -68.0(10) . . . . ?
C18 C19 C20 F10' 170.0(8) . . . . ?
C18 C19 C20 F11' 46.9(9) . . . . ?
C21 C22 C23 C24 174.8(5) . . . . ?
C22 C23 C24 O8 3.8(8) . . . . ?
C22 C23 C24 C25 -174.9(5) . . . . ?
C23 C24 C25 F13 176.8(5) . . . . ?
C23 C24 C25 F14 60.2(7) . . . . ?
C23 C24 C25 F15 -56.2(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.374
_oxdiff_exptl_absorpt_empirical_full_min 0.699
####################################################################### 
# 
# 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_a160629f_sqd
_audit_block_doi                 10.5517/ccdc.csd.cc1zgcrk
_database_code_depnum_ccdc_archive 'CCDC 1831069'
_audit_update_record             
;
2018-03-20 deposited with the CCDC.
2018-04-12 downloaded from the CCDC.
;
_audit_creation_date             2016-07-04
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H34 Dy F12 N10 O8, C20 H4 Dy F24 O8, C H Cl3'
_chemical_formula_sum            'C51 H39 Cl3 Dy2 F36 N10 O16'
_chemical_formula_weight         2163.27
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.4350(4)
_cell_length_b                   21.3325(7)
_cell_length_c                   23.0646(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.183(2)
_cell_angle_gamma                90
_cell_volume                     8511.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10569
_cell_measurement_temperature    156.9(7)
_cell_measurement_theta_max      73.7690
_cell_measurement_theta_min      3.9550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.432
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.261
_diffrn_reflns_theta_min         3.649
_diffrn_ambient_temperature      156.9(7)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13016
_reflns_number_total             16830
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         16830
_refine_ls_number_restraints     201
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0739
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1159P)²+14.0975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2060
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F10-C30 = F10'-C30 = F11-C30 = F11'-C30 = F12-C30 = F12'-C30
 1.33 with sigma of 0.01
 F5-C25 = F5'-C25 = F4-C25 = F4'-C25 = F6-C25 = F6'-C25
 1.33 with sigma of 0.01
 F10'-F11' \\sim F11'-F12'
 with sigma of 0.001
 F11'-F12' \\sim F12'-F10'
 with sigma of 0.001
 F11-F12 \\sim F12-F10
 with sigma of 0.001
 F12-F10 \\sim F10-F11
 with sigma of 0.001
 F4'-F6' \\sim F6'-F5'
 with sigma of 0.001
 F6'-F5' \\sim F5'-F4'
 with sigma of 0.001
 F6-F5 \\sim F5-F4
 with sigma of 0.001
 F5-F4 \\sim F4-F6
 with sigma of 0.001
3. Rigid bond restraints
 F2, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F34, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F35, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(F28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F4') \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F5)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6') \\sim Ueq, Uanis(F11') \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F10') \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12')
\\sim Ueq, Uanis(F12) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(F3) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F32)
\\sim Ueq, Uanis(F35) \\sim Ueq, Uanis(F27) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.002
Uanis(F16) \\sim Ueq, Uanis(F30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F6') = Uanis(F6)
Uanis(F5') = Uanis(F5)
Uanis(F4) = Uanis(F4')
5. Others
 Sof(F10')=Sof(F11')=Sof(F12')=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C51(H51)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C23(H23), C28(H28), C33(H33), C38(H38), C43(H43), C48(H48)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.70201(2) 0.29182(2) 0.69374(2) 0.02639(12) Uani 1 1 d . . . . .
F1 F 0.5794(5) 0.4473(4) 0.5447(4) 0.099(2) Uani 1 1 d . U . . .
F2 F 0.4635(5) 0.4454(4) 0.5732(4) 0.093(2) Uani 1 1 d . U . . .
F3 F 0.5101(4) 0.3688(4) 0.5327(3) 0.0807(19) Uani 1 1 d . U . . .
F7 F 0.8482(4) 0.4041(4) 0.8683(2) 0.084(2) Uani 1 1 d . . . . .
F8 F 0.9071(4) 0.3180(4) 0.8553(3) 0.078(2) Uani 1 1 d . . . . .
F9 F 0.9563(4) 0.4050(4) 0.8349(2) 0.075(2) Uani 1 1 d . . . . .
O1 O 0.6976(3) 0.2097(3) 0.7584(2) 0.0326(11) Uani 1 1 d . . . . .
O2 O 0.9316(4) 0.1666(5) 0.8671(3) 0.070(2) Uani 1 1 d . . . . .
O3 O 0.7072(3) 0.2263(3) 0.61451(19) 0.0336(12) Uani 1 1 d . . . . .
O4 O 0.4744(3) 0.2226(4) 0.4942(3) 0.061(2) Uani 1 1 d . . . . .
O5 O 0.6225(3) 0.3521(3) 0.6255(2) 0.0367(12) Uani 1 1 d . . . . .
O6 O 0.6233(3) 0.3496(3) 0.7471(2) 0.0381(12) Uani 1 1 d . . . . .
O7 O 0.7847(3) 0.3357(3) 0.77052(19) 0.0345(11) Uani 1 1 d . . . . .
O8 O 0.7793(3) 0.3615(3) 0.6514(2) 0.0368(12) Uani 1 1 d . . . . .
N1 N 0.7483(3) 0.1939(3) 0.8011(2) 0.0320(13) Uani 1 1 d . . . . .
N2 N 0.8591(4) 0.1714(4) 0.8530(3) 0.0454(17) Uani 1 1 d . . . . .
N3 N 0.8296(3) 0.2332(3) 0.7036(2) 0.0299(13) Uani 1 1 d . . . . .
N4 N 0.8759(3) 0.2310(3) 0.6603(2) 0.0327(13) Uani 1 1 d . . . . .
N5 N 0.9249(3) 0.1677(3) 0.7304(3) 0.0368(14) Uani 1 1 d . . . . .
N6 N 0.6565(3) 0.2247(4) 0.5677(2) 0.0346(15) Uani 1 1 d . . . . .
N7 N 0.5468(4) 0.2206(4) 0.5106(3) 0.0417(17) Uani 1 1 d . . . . .
N8 N 0.5739(3) 0.2362(3) 0.6700(2) 0.0296(12) Uani 1 1 d . . . . .
N9 N 0.5256(3) 0.2215(4) 0.7105(2) 0.0374(15) Uani 1 1 d . . . . .
N10 N 0.4752(4) 0.1825(4) 0.6257(3) 0.0423(16) Uani 1 1 d . . . . .
C1 C 0.8235(4) 0.1859(4) 0.7986(3) 0.0333(15) Uani 1 1 d . . . . .
C2 C 0.7269(5) 0.1885(5) 0.8623(3) 0.045(2) Uani 1 1 d . . . . .
C3 C 0.7134(7) 0.2558(6) 0.8819(4) 0.065(3) Uani 1 1 d . . . . .
H3A H 0.7583 0.2807 0.8778 0.097 Uiso 1 1 calc GR . . . .
H3B H 0.7041 0.2557 0.9220 0.097 Uiso 1 1 calc GR . . . .
H3C H 0.6695 0.2731 0.8580 0.097 Uiso 1 1 calc GR . . . .
C4 C 0.6527(5) 0.1512(6) 0.8600(4) 0.058(3) Uani 1 1 d . . . . .
H4A H 0.6112 0.1743 0.8385 0.087 Uiso 1 1 calc GR . . . .
H4B H 0.6410 0.1438 0.8990 0.087 Uiso 1 1 calc GR . . . .
H4C H 0.6588 0.1118 0.8410 0.087 Uiso 1 1 calc GR . . . .
C5 C 0.8002(5) 0.1555(6) 0.8933(4) 0.058(3) Uani 1 1 d . . . . .
C6 C 0.8272(8) 0.1843(7) 0.9545(6) 0.076(3) Uani 1 1 d . U . . .
H6A H 0.8720 0.1623 0.9724 0.114 Uiso 1 1 calc GR . . . .
H6B H 0.7864 0.1808 0.9787 0.114 Uiso 1 1 calc GR . . . .
H6C H 0.8398 0.2278 0.9502 0.114 Uiso 1 1 calc GR . . . .
C7 C 0.7967(9) 0.0841(7) 0.8954(6) 0.086(4) Uani 1 1 d . U . . .
H7A H 0.7895 0.0678 0.8563 0.129 Uiso 1 1 calc GR . . . .
H7B H 0.7542 0.0715 0.9154 0.129 Uiso 1 1 calc GR . . . .
H7C H 0.8441 0.0682 0.9157 0.129 Uiso 1 1 calc GR . . . .
C8 C 0.8594(4) 0.1955(4) 0.7464(3) 0.0326(15) Uani 1 1 d . . . . .
C9 C 0.9315(4) 0.1911(4) 0.6771(3) 0.0378(17) Uani 1 1 d . . . . .
H9 H 0.9706 0.1804 0.6549 0.045 Uiso 1 1 calc R . . . .
C10 C 0.9743(5) 0.1194(5) 0.7602(4) 0.050(2) Uani 1 1 d . . . . .
H10A H 1.0127 0.1387 0.7880 0.074 Uiso 1 1 calc GR . . . .
H10B H 0.9993 0.0964 0.7320 0.074 Uiso 1 1 calc GR . . . .
H10C H 0.9435 0.0913 0.7801 0.074 Uiso 1 1 calc GR . . . .
C11 C 0.5430(4) 0.2123(4) 0.6193(3) 0.0330(16) Uani 1 1 d . . . . .
C12 C 0.4681(4) 0.1900(5) 0.6832(3) 0.0398(18) Uani 1 1 d . . . . .
H12 H 0.4269 0.1746 0.7009 0.048 Uiso 1 1 calc R . . . .
C13 C 0.4231(7) 0.1440(6) 0.5846(5) 0.064(3) Uani 1 1 d . U . . .
H13A H 0.3973 0.1704 0.5545 0.096 Uiso 1 1 calc GR . . . .
H13B H 0.3855 0.1238 0.6053 0.096 Uiso 1 1 calc GR . . . .
H13C H 0.4527 0.1128 0.5672 0.096 Uiso 1 1 calc GR . . . .
C14 C 0.5809(4) 0.2178(4) 0.5665(3) 0.0329(16) Uani 1 1 d . . . . .
C15 C 0.6821(4) 0.2366(5) 0.5089(3) 0.043(2) Uani 1 1 d . . . . .
C16 C 0.7009(5) 0.3069(5) 0.5068(4) 0.054(2) Uani 1 1 d . . . . .
H16A H 0.6562 0.3308 0.5134 0.081 Uiso 1 1 calc GR . . . .
H16B H 0.7155 0.3172 0.4692 0.081 Uiso 1 1 calc GR . . . .
H16C H 0.7428 0.3165 0.5366 0.081 Uiso 1 1 calc GR . . . .
C17 C 0.7522(5) 0.1962(6) 0.5031(4) 0.059(3) Uani 1 1 d . . . . .
H17A H 0.7948 0.2100 0.5306 0.088 Uiso 1 1 calc GR . . . .
H17B H 0.7658 0.1998 0.4641 0.088 Uiso 1 1 calc GR . . . .
H17C H 0.7405 0.1533 0.5108 0.088 Uiso 1 1 calc GR . . . .
C18 C 0.6067(5) 0.2177(5) 0.4683(3) 0.048(2) Uani 1 1 d . . . . .
C19 C 0.5835(6) 0.2610(7) 0.4175(4) 0.074(4) Uani 1 1 d . . . . .
H19A H 0.5343 0.2483 0.3976 0.110 Uiso 1 1 calc GR . . . .
H19B H 0.6217 0.2593 0.3909 0.110 Uiso 1 1 calc GR . . . .
H19C H 0.5798 0.3031 0.4316 0.110 Uiso 1 1 calc GR . . . .
C20 C 0.6049(6) 0.1495(7) 0.4477(5) 0.077(4) Uani 1 1 d . . . . .
H20A H 0.6213 0.1226 0.4802 0.116 Uiso 1 1 calc GR . . . .
H20B H 0.6391 0.1446 0.4184 0.116 Uiso 1 1 calc GR . . . .
H20C H 0.5533 0.1386 0.4314 0.116 Uiso 1 1 calc GR . . . .
C21 C 0.5295(7) 0.4149(6) 0.5710(4) 0.061(2) Uani 1 1 d . U . . .
C22 C 0.5672(4) 0.3884(4) 0.6298(3) 0.0371(16) Uani 1 1 d . . . . .
C23 C 0.5366(5) 0.4077(5) 0.6793(4) 0.046(2) Uani 1 1 d . . . . .
H23 H 0.4949 0.4353 0.6762 0.055 Uiso 1 1 calc R . . . .
C24 C 0.5689(4) 0.3855(4) 0.7347(3) 0.0382(17) Uani 1 1 d . . . . .
C25 C 0.5321(4) 0.4119(3) 0.7866(3) 0.045(2) Uani 1 1 d D . . . .
C26 C 0.8904(5) 0.3740(5) 0.8327(4) 0.050(2) Uani 1 1 d . . . . .
C27 C 0.8449(4) 0.3674(4) 0.7722(3) 0.0350(16) Uani 1 1 d . . . . .
C28 C 0.8757(4) 0.3961(4) 0.7259(4) 0.0428(19) Uani 1 1 d . . . . .
H28 H 0.9210 0.4193 0.7335 0.051 Uiso 1 1 calc R . . . .
C29 C 0.8401(4) 0.3909(4) 0.6685(3) 0.0388(17) Uani 1 1 d . . . . .
C30 C 0.8752(4) 0.4250(4) 0.6203(4) 0.055(2) Uani 1 1 d D . . . .
F4 F 0.5640(6) 0.4650(4) 0.8057(5) 0.076(3) Uani 0.549(8) 1 d D U P A 1
F5 F 0.4565(5) 0.4226(5) 0.7754(6) 0.084(3) Uani 0.549(8) 1 d D U P A 1
F6 F 0.5405(7) 0.3722(5) 0.8313(5) 0.079(3) Uani 0.549(8) 1 d D U P A 1
F10 F 0.8210(6) 0.4489(6) 0.5806(5) 0.073(4) Uani 0.533(18) 1 d D U P B 1
F11 F 0.9209(7) 0.4727(5) 0.6391(6) 0.081(4) Uani 0.533(18) 1 d D U P B 1
F12 F 0.9165(8) 0.3862(6) 0.5929(6) 0.100(6) Uani 0.533(18) 1 d D U P B 1
F4' F 0.5864(7) 0.4317(6) 0.8281(5) 0.076(3) Uani 0.451(8) 1 d D U P A 2
F5' F 0.4843(7) 0.4598(5) 0.7748(7) 0.084(3) Uani 0.451(8) 1 d D U P A 2
F6' F 0.4929(7) 0.3682(6) 0.8105(6) 0.079(3) Uani 0.451(8) 1 d D U P A 2
F10' F 0.8339(8) 0.4758(6) 0.6051(7) 0.095(6) Uani 0.467(18) 1 d D U P B 2
F11' F 0.9476(6) 0.4425(6) 0.6345(6) 0.068(4) Uani 0.467(18) 1 d D U P B 2
F12' F 0.8733(8) 0.3897(6) 0.5720(5) 0.073(5) Uani 0.467(18) 1 d D U P B 2
Dy2 Dy 0.69072(2) 0.36729(2) 1.16785(2) 0.02561(12) Uani 1 1 d . . . . .
F13 F 0.6465(6) 0.4010(4) 1.3767(3) 0.095(3) Uani 1 1 d . . . . .
F14 F 0.6020(5) 0.4793(4) 1.3319(3) 0.085(2) Uani 1 1 d . U . . .
F15 F 0.7076(4) 0.4870(4) 1.3889(3) 0.0787(18) Uani 1 1 d . U . . .
F16 F 0.9233(5) 0.5150(4) 1.2896(4) 0.095(2) Uani 1 1 d . U . . .
F17 F 0.9647(5) 0.4241(4) 1.2790(4) 0.092(2) Uani 1 1 d . U . . .
F18 F 0.9288(5) 0.4803(5) 1.2064(4) 0.102(3) Uani 1 1 d . U . . .
F19 F 0.7636(4) 0.5846(4) 1.1281(4) 0.096(3) Uani 1 1 d . . . . .
F20 F 0.6959(5) 0.6082(3) 1.1947(3) 0.083(2) Uani 1 1 d . . . . .
F21 F 0.6529(5) 0.6267(3) 1.1069(4) 0.091(3) Uani 1 1 d . . . . .
F22 F 0.4386(3) 0.5030(3) 1.0470(2) 0.0551(13) Uani 1 1 d . . . . .
F23 F 0.4111(3) 0.4378(3) 1.1121(2) 0.0526(13) Uani 1 1 d . . . . .
F24 F 0.4586(3) 0.4054(3) 1.0359(2) 0.0640(16) Uani 1 1 d . . . . .
F25 F 0.7364(4) 0.4977(4) 1.0046(3) 0.081(2) Uani 1 1 d . . . . .
F26 F 0.7113(4) 0.4345(4) 0.9322(2) 0.075(2) Uani 1 1 d . . . . .
F27 F 0.8158(4) 0.4251(3) 0.9904(3) 0.0707(16) Uani 1 1 d . U . . .
F28 F 0.4948(5) 0.2546(4) 1.0412(3) 0.087(2) Uani 1 1 d . U . . .
F29 F 0.5063(6) 0.2956(4) 0.9609(4) 0.112(3) Uani 1 1 d . . . . .
F30 F 0.5774(5) 0.2190(4) 0.9885(4) 0.097(2) Uani 1 1 d . U . . .
F31 F 0.8507(7) 0.1999(5) 1.1073(4) 0.126(4) Uani 1 1 d . . . . .
F32 F 0.8114(6) 0.1218(5) 1.1549(4) 0.103(3) Uani 1 1 d . U . . .
F33 F 0.8876(4) 0.1845(5) 1.1961(5) 0.118(4) Uani 1 1 d . . . . .
F34 F 0.5325(6) 0.1608(5) 1.2006(4) 0.103(2) Uani 1 1 d . U . . .
F35 F 0.6112(5) 0.1480(4) 1.2806(4) 0.095(2) Uani 1 1 d . U . . .
F36 F 0.5307(4) 0.2235(3) 1.2669(3) 0.0732(19) Uani 1 1 d . . . . .
O9 O 0.6716(3) 0.3985(2) 1.26157(19) 0.0299(10) Uani 1 1 d . . . . .
O10 O 0.8119(3) 0.3988(3) 1.2131(2) 0.0319(10) Uani 1 1 d . . . . .
O11 O 0.6959(3) 0.4796(3) 1.1670(2) 0.0352(11) Uani 1 1 d . . . . .
O12 O 0.5672(3) 0.4064(2) 1.1359(2) 0.0293(10) Uani 1 1 d . . . . .
O13 O 0.7317(3) 0.3966(3) 1.0805(2) 0.0380(12) Uani 1 1 d . . . . .
O14 O 0.6266(3) 0.3025(3) 1.0916(2) 0.0395(12) Uani 1 1 d . . . . .
O15 O 0.7725(3) 0.2807(3) 1.1651(2) 0.0390(12) Uani 1 1 d . . . . .
O16 O 0.6309(3) 0.2862(2) 1.2125(2) 0.0339(11) Uani 1 1 d . . . . .
C31 C 0.6674(5) 0.4510(4) 1.3507(3) 0.0422(18) Uani 1 1 d . . . . .
C32 C 0.7113(4) 0.4341(4) 1.2988(3) 0.0321(15) Uani 1 1 d . . . . .
C33 C 0.7852(4) 0.4556(4) 1.2972(3) 0.0397(17) Uani 1 1 d . . . . .
H33 H 0.8063 0.4836 1.3257 0.048 Uiso 1 1 calc R . . . .
C34 C 0.8288(4) 0.4369(4) 1.2547(3) 0.0376(17) Uani 1 1 d . . . . .
C35 C 0.9119(5) 0.4644(5) 1.2571(4) 0.053(2) Uani 1 1 d . . . . .
C36 C 0.6918(6) 0.5850(5) 1.1418(4) 0.048(2) Uani 1 1 d . . . . .
C37 C 0.6562(4) 0.5200(4) 1.1382(3) 0.0324(15) Uani 1 1 d . . . . .
C38 C 0.5839(4) 0.5117(4) 1.1051(3) 0.0303(14) Uani 1 1 d . . . . .
H38 H 0.5625 0.5439 1.0811 0.036 Uiso 1 1 calc R . . . .
C39 C 0.5440(4) 0.4557(4) 1.1079(3) 0.0267(14) Uani 1 1 d . . . . .
C40 C 0.4618(4) 0.4513(4) 1.0748(3) 0.0355(16) Uani 1 1 d . . . . .
C41 C 0.7426(5) 0.4386(6) 0.9881(3) 0.055(3) Uani 1 1 d . . . . .
C42 C 0.7032(4) 0.3938(5) 1.0274(3) 0.0401(19) Uani 1 1 d . . . . .
C43 C 0.6419(5) 0.3567(5) 1.0042(3) 0.047(2) Uani 1 1 d . . . . .
H43 H 0.6220 0.3614 0.9651 0.056 Uiso 1 1 calc R . . . .
C44 C 0.6095(5) 0.3126(5) 1.0381(3) 0.0424(19) Uani 1 1 d . . . . .
C45 C 0.5457(6) 0.2696(5) 1.0074(4) 0.058(3) Uani 1 1 d . . . . .
C46 C 0.8268(7) 0.1820(5) 1.1540(7) 0.071(3) Uani 1 1 d . . . . .
C47 C 0.7615(5) 0.2234(4) 1.1720(4) 0.0435(19) Uani 1 1 d . . . . .
C48 C 0.7018(4) 0.1942(4) 1.1949(3) 0.0406(18) Uani 1 1 d . . . . .
H48 H 0.7016 0.1507 1.1976 0.049 Uiso 1 1 calc R . . . .
C49 C 0.6415(4) 0.2283(4) 1.2144(3) 0.0343(16) Uani 1 1 d . . . . .
C50 C 0.5805(7) 0.1910(5) 1.2426(5) 0.0639(19) Uani 1 1 d . U . . .
Cl1 Cl 0.43946(15) 0.22714(17) 0.82410(11) 0.0705(8) Uani 1 1 d . . . . .
Cl2 Cl 0.3878(2) 0.15651(17) 0.91797(13) 0.0839(9) Uani 1 1 d . . . . .
Cl3 Cl 0.27752(13) 0.22132(13) 0.83690(10) 0.0576(6) Uani 1 1 d . . . . .
C51 C 0.3723(5) 0.2207(5) 0.8740(3) 0.047(2) Uani 1 1 d . . . . .
H51 H 0.3780 0.2579 0.8991 0.057 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.307(5) . ?
Dy1 O3 2.311(5) . ?
Dy1 O5 2.347(5) . ?
Dy1 O6 2.311(5) . ?
Dy1 O7 2.334(5) . ?
Dy1 O8 2.304(5) . ?
Dy1 N3 2.537(6) . ?
Dy1 N8 2.527(6) . ?
F1 C21 1.317(14) . ?
F2 C21 1.329(14) . ?
F3 C21 1.336(13) . ?
F7 C26 1.334(12) . ?
F8 C26 1.323(13) . ?
F9 C26 1.322(11) . ?
O1 N1 1.284(7) . ?
O2 N2 1.270(9) . ?
O3 N6 1.308(7) . ?
O4 N7 1.272(9) . ?
O5 C22 1.249(9) . ?
O6 C24 1.224(10) . ?
O7 C27 1.247(10) . ?
O8 C29 1.252(10) . ?
N1 C1 1.330(10) . ?
N1 C2 1.510(9) . ?
N2 C1 1.363(9) . ?
N2 C5 1.507(12) . ?
N3 N4 1.361(8) . ?
N3 C8 1.328(10) . ?
N4 C9 1.312(10) . ?
N5 C8 1.377(9) . ?
N5 C9 1.345(11) . ?
N5 C10 1.459(11) . ?
N6 C14 1.323(9) . ?
N6 C15 1.501(9) . ?
N7 C14 1.354(9) . ?
N7 C18 1.515(10) . ?
N8 N9 1.371(8) . ?
N8 C11 1.327(9) . ?
N9 C12 1.303(10) . ?
N10 C11 1.366(10) . ?
N10 C12 1.356(10) . ?
N10 C13 1.478(12) . ?
C1 C8 1.441(10) . ?
C2 C3 1.532(15) . ?
C2 C4 1.514(13) . ?
C2 C5 1.553(13) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.559(16) . ?
C5 C7 1.525(18) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C14 1.460(10) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 C16 1.536(15) . ?
C15 C17 1.516(12) . ?
C15 C18 1.569(11) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.508(14) . ?
C18 C20 1.528(16) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.540(12) . ?
C22 C23 1.383(11) . ?
C23 H23 0.9300 . ?
C23 C24 1.413(12) . ?
C24 C25 1.535(10) . ?
C25 F4 1.313(8) . ?
C25 F5 1.331(8) . ?
C25 F6 1.327(8) . ?
C25 F4' 1.327(9) . ?
C25 F5' 1.325(9) . ?
C25 F6' 1.316(9) . ?
C26 C27 1.522(10) . ?
C27 C28 1.395(12) . ?
C28 H28 0.9300 . ?
C28 C29 1.395(11) . ?
C29 C30 1.519(12) . ?
C30 F10 1.333(8) . ?
C30 F11 1.331(9) . ?
C30 F12 1.310(9) . ?
C30 F10' 1.325(9) . ?
C30 F11' 1.317(9) . ?
C30 F12' 1.341(9) . ?
Dy2 O9 2.325(4) . ?
Dy2 O10 2.335(4) . ?
Dy2 O11 2.399(6) . ?
Dy2 O12 2.341(5) . ?
Dy2 O13 2.307(5) . ?
Dy2 O14 2.400(5) . ?
Dy2 O15 2.339(6) . ?
Dy2 O16 2.326(5) . ?
F13 C31 1.298(12) . ?
F14 C31 1.315(11) . ?
F15 C31 1.305(10) . ?
F16 C35 1.317(13) . ?
F17 C35 1.313(13) . ?
F18 C35 1.286(13) . ?
F19 C36 1.329(12) . ?
F20 C36 1.311(11) . ?
F21 C36 1.327(11) . ?
F22 C40 1.314(9) . ?
F23 C40 1.340(9) . ?
F24 C40 1.325(10) . ?
F25 C41 1.325(14) . ?
F26 C41 1.339(10) . ?
F27 C41 1.302(11) . ?
F28 C45 1.294(14) . ?
F29 C45 1.322(13) . ?
F30 C45 1.313(13) . ?
F31 C46 1.262(16) . ?
F32 C46 1.313(14) . ?
F33 C46 1.345(16) . ?
F34 C50 1.361(15) . ?
F35 C50 1.334(14) . ?
F36 C50 1.292(12) . ?
O9 C32 1.282(9) . ?
O10 C34 1.264(10) . ?
O11 C37 1.245(9) . ?
O12 C39 1.273(8) . ?
O13 C42 1.264(9) . ?
O14 C44 1.251(9) . ?
O15 C47 1.251(11) . ?
O16 C49 1.249(10) . ?
C31 C32 1.542(10) . ?
C32 C33 1.373(11) . ?
C33 H33 0.9300 . ?
C33 C34 1.373(12) . ?
C34 C35 1.558(11) . ?
C36 C37 1.515(12) . ?
C37 C38 1.402(10) . ?
C38 H38 0.9300 . ?
C38 C39 1.388(11) . ?
C39 C40 1.539(9) . ?
C41 C42 1.535(13) . ?
C42 C43 1.383(13) . ?
C43 H43 0.9300 . ?
C43 C44 1.387(14) . ?
C44 C45 1.543(13) . ?
C46 C47 1.538(13) . ?
C47 C48 1.374(13) . ?
C48 H48 0.9300 . ?
C48 C49 1.398(11) . ?
C49 C50 1.537(12) . ?
Cl1 C51 1.746(9) . ?
Cl2 C51 1.706(11) . ?
Cl3 C51 1.763(9) . ?
C51 H51 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O3 93.42(19) . . ?
O1 Dy1 O5 141.67(18) . . ?
O1 Dy1 O6 89.4(2) . . ?
O1 Dy1 O7 83.19(19) . . ?
O1 Dy1 N3 70.59(19) . . ?
O1 Dy1 N8 71.55(18) . . ?
O3 Dy1 O5 83.06(19) . . ?
O3 Dy1 O6 145.91(17) . . ?
O3 Dy1 O7 139.51(16) . . ?
O3 Dy1 N3 69.67(17) . . ?
O3 Dy1 N8 70.48(18) . . ?
O5 Dy1 N3 140.19(17) . . ?
O5 Dy1 N8 71.3(2) . . ?
O6 Dy1 O5 74.02(18) . . ?
O6 Dy1 O7 74.56(18) . . ?
O6 Dy1 N3 141.94(17) . . ?
O6 Dy1 N8 78.34(19) . . ?
O7 Dy1 O5 123.1(2) . . ?
O7 Dy1 N3 71.22(18) . . ?
O7 Dy1 N8 142.86(17) . . ?
O8 Dy1 O1 146.28(17) . . ?
O8 Dy1 O3 88.40(19) . . ?
O8 Dy1 O5 71.98(19) . . ?
O8 Dy1 O6 107.5(2) . . ?
O8 Dy1 O7 74.00(18) . . ?
O8 Dy1 N3 78.6(2) . . ?
O8 Dy1 N8 139.39(18) . . ?
N8 Dy1 N3 122.0(2) . . ?
N1 O1 Dy1 128.3(4) . . ?
N6 O3 Dy1 125.4(4) . . ?
C22 O5 Dy1 133.1(5) . . ?
C24 O6 Dy1 134.7(5) . . ?
C27 O7 Dy1 132.8(4) . . ?
C29 O8 Dy1 135.0(5) . . ?
O1 N1 C1 126.0(6) . . ?
O1 N1 C2 120.7(6) . . ?
C1 N1 C2 113.0(6) . . ?
O2 N2 C1 125.3(7) . . ?
O2 N2 C5 123.9(7) . . ?
C1 N2 C5 110.6(6) . . ?
N4 N3 Dy1 123.0(4) . . ?
C8 N3 Dy1 128.5(4) . . ?
C8 N3 N4 108.2(6) . . ?
C9 N4 N3 106.8(6) . . ?
C8 N5 C10 129.7(7) . . ?
C9 N5 C8 104.7(6) . . ?
C9 N5 C10 125.5(7) . . ?
O3 N6 C14 126.0(6) . . ?
O3 N6 C15 119.7(6) . . ?
C14 N6 C15 114.1(6) . . ?
O4 N7 C14 125.8(6) . . ?
O4 N7 C18 123.3(6) . . ?
C14 N7 C18 110.9(6) . . ?
N9 N8 Dy1 124.1(4) . . ?
C11 N8 Dy1 128.5(4) . . ?
C11 N8 N9 107.3(6) . . ?
C12 N9 N8 106.8(6) . . ?
C11 N10 C13 131.3(7) . . ?
C12 N10 C11 103.7(6) . . ?
C12 N10 C13 124.7(8) . . ?
N1 C1 N2 109.1(6) . . ?
N1 C1 C8 123.5(6) . . ?
N2 C1 C8 127.3(7) . . ?
N1 C2 C3 105.6(7) . . ?
N1 C2 C4 108.5(7) . . ?
N1 C2 C5 100.3(7) . . ?
C3 C2 C5 115.9(9) . . ?
C4 C2 C3 110.0(9) . . ?
C4 C2 C5 115.4(9) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C2 101.5(7) . . ?
N2 C5 C6 108.6(9) . . ?
N2 C5 C7 106.1(10) . . ?
C2 C5 C6 112.1(10) . . ?
C7 C5 C2 115.6(9) . . ?
C7 C5 C6 112.0(10) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 N5 108.8(6) . . ?
N3 C8 C1 122.4(6) . . ?
N5 C8 C1 128.7(7) . . ?
N4 C9 N5 111.5(6) . . ?
N4 C9 H9 124.2 . . ?
N5 C9 H9 124.2 . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N8 C11 N10 110.2(6) . . ?
N8 C11 C14 121.8(6) . . ?
N10 C11 C14 128.0(7) . . ?
N9 C12 N10 112.1(6) . . ?
N9 C12 H12 124.0 . . ?
N10 C12 H12 124.0 . . ?
N10 C13 H13A 109.5 . . ?
N10 C13 H13B 109.5 . . ?
N10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N6 C14 N7 109.4(6) . . ?
N6 C14 C11 123.1(6) . . ?
N7 C14 C11 127.5(6) . . ?
N6 C15 C16 106.4(6) . . ?
N6 C15 C17 108.5(7) . . ?
N6 C15 C18 100.0(6) . . ?
C16 C15 C18 113.6(8) . . ?
C17 C15 C16 111.9(8) . . ?
C17 C15 C18 115.2(7) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N7 C18 C15 101.4(5) . . ?
N7 C18 C20 104.6(8) . . ?
C19 C18 N7 109.6(7) . . ?
C19 C18 C15 115.4(9) . . ?
C19 C18 C20 110.4(9) . . ?
C20 C18 C15 114.4(8) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
F1 C21 F2 112.7(10) . . ?
F1 C21 F3 102.1(9) . . ?
F1 C21 C22 111.3(9) . . ?
F2 C21 F3 103.8(9) . . ?
F2 C21 C22 115.0(9) . . ?
F3 C21 C22 110.9(9) . . ?
O5 C22 C21 114.0(7) . . ?
O5 C22 C23 129.2(8) . . ?
C23 C22 C21 116.9(8) . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.6(7) . . ?
C24 C23 H23 120.2 . . ?
O6 C24 C23 129.2(7) . . ?
O6 C24 C25 115.8(7) . . ?
C23 C24 C25 115.0(7) . . ?
F4 C25 C24 112.1(8) . . ?
F4 C25 F5 106.5(6) . . ?
F4 C25 F6 106.8(6) . . ?
F5 C25 C24 114.4(8) . . ?
F6 C25 C24 110.8(8) . . ?
F6 C25 F5 105.8(6) . . ?
F4' C25 C24 110.4(8) . . ?
F5' C25 C24 115.8(9) . . ?
F5' C25 F4' 106.0(7) . . ?
F6' C25 C24 110.9(9) . . ?
F6' C25 F4' 106.6(7) . . ?
F6' C25 F5' 106.7(7) . . ?
F7 C26 C27 110.2(7) . . ?
F8 C26 F7 107.7(9) . . ?
F8 C26 C27 109.9(8) . . ?
F9 C26 F7 106.2(8) . . ?
F9 C26 F8 106.8(8) . . ?
F9 C26 C27 115.6(8) . . ?
O7 C27 C26 114.8(7) . . ?
O7 C27 C28 128.1(6) . . ?
C28 C27 C26 117.1(7) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 C27 121.6(7) . . ?
C29 C28 H28 119.2 . . ?
O8 C29 C28 126.6(8) . . ?
O8 C29 C30 114.4(6) . . ?
C28 C29 C30 119.0(7) . . ?
F10 C30 C29 111.7(8) . . ?
F11 C30 C29 114.1(9) . . ?
F11 C30 F10 106.0(7) . . ?
F12 C30 C29 110.3(10) . . ?
F12 C30 F10 107.2(7) . . ?
F12 C30 F11 107.3(7) . . ?
F10' C30 C29 109.2(10) . . ?
F10' C30 F12' 106.4(7) . . ?
F11' C30 C29 114.6(9) . . ?
F11' C30 F10' 107.8(7) . . ?
F11' C30 F12' 106.8(7) . . ?
F12' C30 C29 111.6(9) . . ?
O9 Dy2 O10 74.26(17) . . ?
O9 Dy2 O11 74.42(18) . . ?
O9 Dy2 O12 87.61(16) . . ?
O9 Dy2 O14 137.58(19) . . ?
O9 Dy2 O15 114.16(18) . . ?
O9 Dy2 O16 71.11(18) . . ?
O10 Dy2 O11 71.52(18) . . ?
O10 Dy2 O12 141.61(18) . . ?
O10 Dy2 O14 143.68(19) . . ?
O10 Dy2 O15 73.65(19) . . ?
O11 Dy2 O14 125.73(18) . . ?
O12 Dy2 O11 71.09(17) . . ?
O12 Dy2 O14 69.39(18) . . ?
O13 Dy2 O9 146.2(2) . . ?
O13 Dy2 O10 87.20(18) . . ?
O13 Dy2 O11 72.9(2) . . ?
O13 Dy2 O12 90.06(17) . . ?
O13 Dy2 O14 71.5(2) . . ?
O13 Dy2 O15 86.2(2) . . ?
O13 Dy2 O16 142.5(2) . . ?
O15 Dy2 O11 139.91(19) . . ?
O15 Dy2 O12 144.36(19) . . ?
O15 Dy2 O14 75.85(19) . . ?
O16 Dy2 O10 116.51(18) . . ?
O16 Dy2 O11 139.99(18) . . ?
O16 Dy2 O12 87.64(18) . . ?
O16 Dy2 O14 72.74(19) . . ?
O16 Dy2 O15 74.5(2) . . ?
C32 O9 Dy2 131.6(4) . . ?
C34 O10 Dy2 129.6(5) . . ?
C37 O11 Dy2 132.6(5) . . ?
C39 O12 Dy2 132.5(4) . . ?
C42 O13 Dy2 135.0(5) . . ?
C44 O14 Dy2 131.0(6) . . ?
C47 O15 Dy2 131.7(5) . . ?
C49 O16 Dy2 132.7(5) . . ?
F13 C31 F14 104.4(8) . . ?
F13 C31 F15 109.2(8) . . ?
F13 C31 C32 111.2(7) . . ?
F14 C31 C32 110.2(7) . . ?
F15 C31 F14 108.8(8) . . ?
F15 C31 C32 112.6(7) . . ?
O9 C32 C31 112.3(6) . . ?
O9 C32 C33 127.6(7) . . ?
C33 C32 C31 120.1(7) . . ?
C32 C33 H33 119.1 . . ?
C32 C33 C34 121.8(7) . . ?
C34 C33 H33 119.1 . . ?
O10 C34 C33 129.1(7) . . ?
O10 C34 C35 113.4(7) . . ?
C33 C34 C35 117.5(8) . . ?
F16 C35 C34 113.7(9) . . ?
F17 C35 F16 105.5(8) . . ?
F17 C35 C34 111.8(9) . . ?
F18 C35 F16 105.4(10) . . ?
F18 C35 F17 107.2(10) . . ?
F18 C35 C34 112.6(8) . . ?
F19 C36 C37 111.8(8) . . ?
F20 C36 F19 106.2(9) . . ?
F20 C36 F21 106.0(9) . . ?
F20 C36 C37 111.8(7) . . ?
F21 C36 F19 106.6(8) . . ?
F21 C36 C37 113.9(8) . . ?
O11 C37 C36 114.0(7) . . ?
O11 C37 C38 127.3(7) . . ?
C38 C37 C36 118.7(7) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.4(6) . . ?
C39 C38 H38 119.8 . . ?
O12 C39 C38 127.3(6) . . ?
O12 C39 C40 114.7(6) . . ?
C38 C39 C40 118.0(6) . . ?
F22 C40 F23 107.9(6) . . ?
F22 C40 F24 107.8(6) . . ?
F22 C40 C39 113.7(7) . . ?
F23 C40 C39 110.1(6) . . ?
F24 C40 F23 107.4(7) . . ?
F24 C40 C39 109.8(6) . . ?
F25 C41 F26 107.4(8) . . ?
F25 C41 C42 111.3(7) . . ?
F26 C41 C42 111.6(9) . . ?
F27 C41 F25 108.3(10) . . ?
F27 C41 F26 107.7(7) . . ?
F27 C41 C42 110.3(8) . . ?
O13 C42 C41 113.1(8) . . ?
O13 C42 C43 126.2(8) . . ?
C43 C42 C41 120.6(7) . . ?
C42 C43 H43 119.3 . . ?
C42 C43 C44 121.4(7) . . ?
C44 C43 H43 119.3 . . ?
O14 C44 C43 127.4(8) . . ?
O14 C44 C45 114.8(9) . . ?
C43 C44 C45 117.8(7) . . ?
F28 C45 F29 105.5(10) . . ?
F28 C45 F30 110.2(10) . . ?
F28 C45 C44 112.3(7) . . ?
F29 C45 C44 113.3(9) . . ?
F30 C45 F29 105.9(8) . . ?
F30 C45 C44 109.4(9) . . ?
F31 C46 F32 113.6(12) . . ?
F31 C46 F33 106.8(11) . . ?
F31 C46 C47 113.0(11) . . ?
F32 C46 F33 99.8(11) . . ?
F32 C46 C47 113.4(10) . . ?
F33 C46 C47 109.0(10) . . ?
O15 C47 C46 113.3(8) . . ?
O15 C47 C48 128.9(8) . . ?
C48 C47 C46 117.8(9) . . ?
C47 C48 H48 119.2 . . ?
C47 C48 C49 121.6(8) . . ?
C49 C48 H48 119.2 . . ?
O16 C49 C48 128.2(8) . . ?
O16 C49 C50 114.8(7) . . ?
C48 C49 C50 117.1(8) . . ?
F34 C50 C49 109.8(8) . . ?
F35 C50 F34 107.6(9) . . ?
F35 C50 C49 113.1(10) . . ?
F36 C50 F34 100.1(11) . . ?
F36 C50 F35 108.8(9) . . ?
F36 C50 C49 116.3(8) . . ?
Cl1 C51 Cl3 110.2(5) . . ?
Cl1 C51 H51 107.5 . . ?
Cl2 C51 Cl1 112.7(6) . . ?
Cl2 C51 Cl3 111.3(5) . . ?
Cl2 C51 H51 107.5 . . ?
Cl3 C51 H51 107.5 . . ?

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
Dy1 O1 N1 C1 -50.0(10) . . . . ?
Dy1 O1 N1 C2 124.0(7) . . . . ?
Dy1 O3 N6 C14 -53.2(11) . . . . ?
Dy1 O3 N6 C15 121.6(7) . . . . ?
Dy1 O5 C22 C21 -176.7(6) . . . . ?
Dy1 O5 C22 C23 3.8(15) . . . . ?
Dy1 O6 C24 C23 -4.0(14) . . . . ?
Dy1 O6 C24 C25 178.1(5) . . . . ?
Dy1 O7 C27 C26 -166.9(6) . . . . ?
Dy1 O7 C27 C28 11.9(13) . . . . ?
Dy1 O8 C29 C28 -9.9(14) . . . . ?
Dy1 O8 C29 C30 171.8(5) . . . . ?
Dy1 N3 N4 C9 -172.5(5) . . . . ?
Dy1 N3 C8 N5 172.4(5) . . . . ?
Dy1 N3 C8 C1 -5.3(11) . . . . ?
Dy1 N8 N9 C12 -176.2(5) . . . . ?
Dy1 N8 C11 N10 176.0(5) . . . . ?
Dy1 N8 C11 C14 -2.7(11) . . . . ?
F1 C21 C22 O5 -60.5(12) . . . . ?
F1 C21 C22 C23 119.1(11) . . . . ?
F2 C21 C22 O5 169.8(9) . . . . ?
F2 C21 C22 C23 -10.6(14) . . . . ?
F3 C21 C22 O5 52.5(12) . . . . ?
F3 C21 C22 C23 -127.9(10) . . . . ?
F7 C26 C27 O7 -62.7(11) . . . . ?
F7 C26 C27 C28 118.4(10) . . . . ?
F8 C26 C27 O7 56.0(10) . . . . ?
F8 C26 C27 C28 -123.0(9) . . . . ?
F9 C26 C27 O7 176.9(8) . . . . ?
F9 C26 C27 C28 -2.1(13) . . . . ?
O1 N1 C1 N2 177.9(8) . . . . ?
O1 N1 C1 C8 1.3(13) . . . . ?
O1 N1 C2 C3 -70.7(10) . . . . ?
O1 N1 C2 C4 47.2(11) . . . . ?
O1 N1 C2 C5 168.5(8) . . . . ?
O2 N2 C1 N1 -173.0(9) . . . . ?
O2 N2 C1 C8 3.5(16) . . . . ?
O2 N2 C5 C2 163.2(9) . . . . ?
O2 N2 C5 C6 45.0(15) . . . . ?
O2 N2 C5 C7 -75.5(12) . . . . ?
O3 N6 C14 N7 177.9(8) . . . . ?
O3 N6 C14 C11 1.4(14) . . . . ?
O3 N6 C15 C16 -71.5(9) . . . . ?
O3 N6 C15 C17 49.1(11) . . . . ?
O3 N6 C15 C18 170.1(7) . . . . ?
O4 N7 C14 N6 -171.9(9) . . . . ?
O4 N7 C14 C11 4.4(16) . . . . ?
O4 N7 C18 C15 163.6(9) . . . . ?
O4 N7 C18 C19 41.2(13) . . . . ?
O4 N7 C18 C20 -77.2(11) . . . . ?
O5 C22 C23 C24 0.0(16) . . . . ?
O6 C24 C25 F4 91.1(9) . . . . ?
O6 C24 C25 F5 -147.6(8) . . . . ?
O6 C24 C25 F6 -28.1(10) . . . . ?
O6 C24 C25 F4' 46.5(10) . . . . ?
O6 C24 C25 F5' 166.9(8) . . . . ?
O6 C24 C25 F6' -71.4(9) . . . . ?
O7 C27 C28 C29 -1.2(15) . . . . ?
O8 C29 C30 F10 36.9(10) . . . . ?
O8 C29 C30 F11 157.0(8) . . . . ?
O8 C29 C30 F12 -82.1(10) . . . . ?
O8 C29 C30 F10' 75.2(10) . . . . ?
O8 C29 C30 F11' -163.8(8) . . . . ?
O8 C29 C30 F12' -42.2(10) . . . . ?
N1 C1 C8 N3 25.0(12) . . . . ?
N1 C1 C8 N5 -152.2(8) . . . . ?
N1 C2 C5 N2 21.5(10) . . . . ?
N1 C2 C5 C6 137.2(9) . . . . ?
N1 C2 C5 C7 -92.9(10) . . . . ?
N2 C1 C8 N3 -150.9(8) . . . . ?
N2 C1 C8 N5 31.8(14) . . . . ?
N3 N4 C9 N5 -1.3(9) . . . . ?
N4 N3 C8 N5 -1.0(8) . . . . ?
N4 N3 C8 C1 -178.7(7) . . . . ?
N6 C15 C18 N7 18.6(9) . . . . ?
N6 C15 C18 C19 136.9(8) . . . . ?
N6 C15 C18 C20 -93.3(9) . . . . ?
N8 N9 C12 N10 0.2(10) . . . . ?
N8 C11 C14 N6 25.7(13) . . . . ?
N8 C11 C14 N7 -150.1(9) . . . . ?
N9 N8 C11 N10 0.3(9) . . . . ?
N9 N8 C11 C14 -178.3(7) . . . . ?
N10 C11 C14 N6 -152.7(9) . . . . ?
N10 C11 C14 N7 31.5(15) . . . . ?
C1 N1 C2 C3 104.0(9) . . . . ?
C1 N1 C2 C4 -138.1(8) . . . . ?
C1 N1 C2 C5 -16.7(10) . . . . ?
C1 N2 C5 C2 -22.1(11) . . . . ?
C1 N2 C5 C6 -140.3(9) . . . . ?
C1 N2 C5 C7 99.2(10) . . . . ?
C2 N1 C1 N2 3.5(10) . . . . ?
C2 N1 C1 C8 -173.1(8) . . . . ?
C3 C2 C5 N2 -91.6(9) . . . . ?
C3 C2 C5 C6 24.1(12) . . . . ?
C3 C2 C5 C7 154.1(9) . . . . ?
C4 C2 C5 N2 137.8(8) . . . . ?
C4 C2 C5 C6 -106.5(11) . . . . ?
C4 C2 C5 C7 23.4(12) . . . . ?
C5 N2 C1 N1 12.4(11) . . . . ?
C5 N2 C1 C8 -171.1(9) . . . . ?
C8 N3 N4 C9 1.4(8) . . . . ?
C8 N5 C9 N4 0.6(9) . . . . ?
C9 N5 C8 N3 0.2(9) . . . . ?
C9 N5 C8 C1 177.8(8) . . . . ?
C10 N5 C8 N3 -174.8(8) . . . . ?
C10 N5 C8 C1 2.7(14) . . . . ?
C10 N5 C9 N4 176.0(8) . . . . ?
C11 N8 N9 C12 -0.3(9) . . . . ?
C11 N10 C12 N9 0.0(11) . . . . ?
C12 N10 C11 N8 -0.2(10) . . . . ?
C12 N10 C11 C14 178.4(8) . . . . ?
C13 N10 C11 N8 -173.7(9) . . . . ?
C13 N10 C11 C14 4.9(16) . . . . ?
C13 N10 C12 N9 174.1(9) . . . . ?
C14 N6 C15 C16 103.8(8) . . . . ?
C14 N6 C15 C17 -135.5(8) . . . . ?
C14 N6 C15 C18 -14.5(10) . . . . ?
C14 N7 C18 C15 -19.4(11) . . . . ?
C14 N7 C18 C19 -141.8(9) . . . . ?
C14 N7 C18 C20 99.9(9) . . . . ?
C15 N6 C14 N7 2.9(11) . . . . ?
C15 N6 C14 C11 -173.6(8) . . . . ?
C16 C15 C18 N7 -94.3(8) . . . . ?
C16 C15 C18 C19 24.0(10) . . . . ?
C16 C15 C18 C20 153.7(8) . . . . ?
C17 C15 C18 N7 134.7(8) . . . . ?
C17 C15 C18 C19 -106.9(11) . . . . ?
C17 C15 C18 C20 22.8(12) . . . . ?
C18 N7 C14 N6 11.2(11) . . . . ?
C18 N7 C14 C11 -172.5(9) . . . . ?
C21 C22 C23 C24 -179.6(9) . . . . ?
C22 C23 C24 O6 0.1(15) . . . . ?
C22 C23 C24 C25 178.0(8) . . . . ?
C23 C24 C25 F4 -87.1(9) . . . . ?
C23 C24 C25 F5 34.3(10) . . . . ?
C23 C24 C25 F6 153.7(8) . . . . ?
C23 C24 C25 F4' -131.7(9) . . . . ?
C23 C24 C25 F5' -11.3(11) . . . . ?
C23 C24 C25 F6' 110.4(9) . . . . ?
C26 C27 C28 C29 177.6(8) . . . . ?
C27 C28 C29 O8 -0.1(15) . . . . ?
C27 C28 C29 C30 178.1(8) . . . . ?
C28 C29 C30 F10 -141.5(9) . . . . ?
C28 C29 C30 F11 -21.4(11) . . . . ?
C28 C29 C30 F12 99.4(10) . . . . ?
C28 C29 C30 F10' -103.3(10) . . . . ?
C28 C29 C30 F11' 17.8(12) . . . . ?
C28 C29 C30 F12' 139.4(9) . . . . ?
Dy2 O9 C32 C31 169.0(5) . . . . ?
Dy2 O9 C32 C33 -12.7(11) . . . . ?
Dy2 O10 C34 C33 23.2(12) . . . . ?
Dy2 O10 C34 C35 -158.1(6) . . . . ?
Dy2 O11 C37 C36 -166.2(5) . . . . ?
Dy2 O11 C37 C38 15.3(10) . . . . ?
Dy2 O12 C39 C38 -24.5(10) . . . . ?
Dy2 O12 C39 C40 156.6(4) . . . . ?
Dy2 O13 C42 C41 161.4(6) . . . . ?
Dy2 O13 C42 C43 -17.2(14) . . . . ?
Dy2 O14 C44 C43 20.4(13) . . . . ?
Dy2 O14 C44 C45 -160.5(6) . . . . ?
Dy2 O15 C47 C46 168.2(7) . . . . ?
Dy2 O15 C47 C48 -14.6(13) . . . . ?
Dy2 O16 C49 C48 9.0(11) . . . . ?
Dy2 O16 C49 C50 -172.0(6) . . . . ?
F13 C31 C32 O9 56.7(10) . . . . ?
F13 C31 C32 C33 -121.7(9) . . . . ?
F14 C31 C32 O9 -58.6(10) . . . . ?
F14 C31 C32 C33 123.0(9) . . . . ?
F15 C31 C32 O9 179.7(7) . . . . ?
F15 C31 C32 C33 1.2(12) . . . . ?
F19 C36 C37 O11 53.3(10) . . . . ?
F19 C36 C37 C38 -128.1(8) . . . . ?
F20 C36 C37 O11 -65.7(10) . . . . ?
F20 C36 C37 C38 113.0(9) . . . . ?
F21 C36 C37 O11 174.2(8) . . . . ?
F21 C36 C37 C38 -7.2(11) . . . . ?
F25 C41 C42 O13 -60.1(9) . . . . ?
F25 C41 C42 C43 118.6(9) . . . . ?
F26 C41 C42 O13 179.9(8) . . . . ?
F26 C41 C42 C43 -1.4(12) . . . . ?
F27 C41 C42 O13 60.2(11) . . . . ?
F27 C41 C42 C43 -121.2(9) . . . . ?
F31 C46 C47 O15 -41.7(15) . . . . ?
F31 C46 C47 C48 140.8(11) . . . . ?
F32 C46 C47 O15 -172.8(10) . . . . ?
F32 C46 C47 C48 9.7(16) . . . . ?
F33 C46 C47 O15 77.0(12) . . . . ?
F33 C46 C47 C48 -100.6(11) . . . . ?
O9 C32 C33 C34 -4.4(13) . . . . ?
O10 C34 C35 F16 163.5(8) . . . . ?
O10 C34 C35 F17 -77.1(10) . . . . ?
O10 C34 C35 F18 43.6(12) . . . . ?
O11 C37 C38 C39 8.5(11) . . . . ?
O12 C39 C40 F22 179.0(6) . . . . ?
O12 C39 C40 F23 57.8(8) . . . . ?
O12 C39 C40 F24 -60.2(8) . . . . ?
O13 C42 C43 C44 -6.6(14) . . . . ?
O14 C44 C45 F28 33.4(13) . . . . ?
O14 C44 C45 F29 152.9(9) . . . . ?
O14 C44 C45 F30 -89.3(10) . . . . ?
O15 C47 C48 C49 0.5(14) . . . . ?
O16 C49 C50 F34 105.4(9) . . . . ?
O16 C49 C50 F35 -134.4(8) . . . . ?
O16 C49 C50 F36 -7.4(14) . . . . ?
C31 C32 C33 C34 173.8(8) . . . . ?
C32 C33 C34 O10 -1.4(14) . . . . ?
C32 C33 C34 C35 179.9(8) . . . . ?
C33 C34 C35 F16 -17.7(12) . . . . ?
C33 C34 C35 F17 101.7(10) . . . . ?
C33 C34 C35 F18 -137.6(10) . . . . ?
C36 C37 C38 C39 -170.0(6) . . . . ?
C37 C38 C39 O12 -4.2(10) . . . . ?
C37 C38 C39 C40 174.7(6) . . . . ?
C38 C39 C40 F22 0.0(9) . . . . ?
C38 C39 C40 F23 -121.2(7) . . . . ?
C38 C39 C40 F24 120.8(7) . . . . ?
C41 C42 C43 C44 174.9(8) . . . . ?
C42 C43 C44 O14 3.9(14) . . . . ?
C42 C43 C44 C45 -175.2(8) . . . . ?
C43 C44 C45 F28 -147.4(9) . . . . ?
C43 C44 C45 F29 -27.9(13) . . . . ?
C43 C44 C45 F30 90.0(11) . . . . ?
C46 C47 C48 C49 177.7(9) . . . . ?
C47 C48 C49 O16 2.5(12) . . . . ?
C47 C48 C49 C50 -176.4(9) . . . . ?
C48 C49 C50 F34 -75.5(12) . . . . ?
C48 C49 C50 F35 44.7(12) . . . . ?
C48 C49 C50 F36 171.7(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_details          ?
# SQUEEZE RESULTS (Version = 50315)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.500 0.500 227 50 ' '
2 0.000 0.500 1.000 363 121 ' '
3 0.012 0.935 0.067 6 0 ' '
4 0.500 0.000 0.500 363 121 ' '
5 0.500 1.000 1.000 227 50 ' '
6 0.488 0.435 0.433 6 0 ' '
7 0.512 0.565 0.567 6 0 ' '
8 0.988 0.065 0.933 6 0 ' '

_platon_squeeze_void_probe_radius 1.20
####################################################################### 
# 
# 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_a160122a
_audit_block_doi                 10.5517/ccdc.csd.cc1zgcqj
_database_code_depnum_ccdc_archive 'CCDC 1831068'
_audit_update_record             
;
2018-03-20 deposited with the CCDC.
2018-04-12 downloaded from the CCDC.
;
_audit_creation_date             2016-01-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H21 F18 N5 O9 Tb'
_chemical_formula_sum            'C25 H21 F18 N5 O9 Tb'
_chemical_formula_weight         1036.39
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9958(3)
_cell_length_b                   12.3076(4)
_cell_length_c                   16.1878(6)
_cell_angle_alpha                105.052(3)
_cell_angle_beta                 103.900(3)
_cell_angle_gamma                99.476(3)
_cell_volume                     1811.27(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7346
_cell_measurement_temperature    113.01(10)
_cell_measurement_theta_max      73.6970
_cell_measurement_theta_min      3.8270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13161
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.833
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      113.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  31.00   1.00    1.00    --  -41.49  51.00 -11.00   99
  2  ω    -70.00  32.00   1.00    1.00    --  -41.49  57.00  90.00  102
  3  ω    -70.00  32.00   1.00    1.00    --  -41.49  57.00 120.00  102
  4  ω   -116.00 -17.00   1.00    1.00    --  -41.49 -38.00-180.00   99
  5  ω     23.00  98.00   1.00    1.00    --   41.49-125.00-180.00   75
  6  ω     31.00 135.00   1.00    1.00    --  107.08 -30.00 -90.00  104
  7  ω     94.00 133.00   1.00    1.00    --  107.08 -45.00-180.00   39
  8  ω     42.00 117.00   1.00    1.00    --  107.08 -30.00  90.00   75
  9  ω     36.00  81.00   1.00    1.00    --  107.08 -45.00-180.00   45
 10  ω     43.00 121.00   1.00    1.00    --  107.08-125.00  90.00   78
 11  ω     98.00 178.00   1.00    1.00    --  107.08  45.00 -90.00   80
 12  ω     34.00  83.00   1.00    1.00    --  107.08 -95.00 150.00   49
 13  ω     35.00 142.00   1.00    1.00    --  107.08 -15.00 -90.00  107
 14  ω     55.00 119.00   1.00    1.00    --  107.08-125.00-120.00   64
 15  ω     56.00 140.00   1.00    1.00    --  107.08 -77.00-120.00   84
 16  ω    104.00 175.00   1.00    1.00    --  107.08 125.00-150.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0191863000
_diffrn_orient_matrix_UB_12      -0.1232065000
_diffrn_orient_matrix_UB_13      -0.0060610000
_diffrn_orient_matrix_UB_21      0.1520187000
_diffrn_orient_matrix_UB_22      0.0515563000
_diffrn_orient_matrix_UB_23      0.0642222000
_diffrn_orient_matrix_UB_31      -0.0574546000
_diffrn_orient_matrix_UB_32      0.0031213000
_diffrn_orient_matrix_UB_33      0.0805664000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5851
_reflns_number_total             6434
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6434
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0701P)²+1.9294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1205
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F9-C16 = F8-C16 = F7-C16
 1.34 with sigma of 0.001
 F9'-C16 = F7'-C16 = F8'-C16
 1.34 with sigma of 0.001
 C11'-C12 = C11-C12
 1.52 with sigma of 0.01
 F3'-C11' = F3-C11 = F1-C11 = F1'-C11' = F2-C11 = F2'-C11'
 1.34 with sigma of 0.001
 F9-F7 \\sim F7-F8
 with sigma of 0.001
 F7-F8 \\sim F8-F9
 with sigma of 0.001
 F9'-F7' \\sim F7'-F8'
 with sigma of 0.001
 F7'-F8' \\sim F8'-F9'
 with sigma of 0.001
 F3'-F1' \\sim F1'-F2'
 with sigma of 0.001
 F1'-F2' \\sim F2'-F3'
 with sigma of 0.001
 F3-F1 \\sim F1-F2
 with sigma of 0.001
 F1-F2 \\sim F2-F3
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F8) \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7')
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F15) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F16) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(F9') = Uanis(F9)
Uanis(F7') = Uanis(F7)
Uanis(F8') = Uanis(F8)
Uanis(F3') = Uanis(F3)
Uanis(F1) = Uanis(F1')
Uanis(F2) = Uanis(F2')
Uanis(C11) = Uanis(C11')
4. Others
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C11')=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C11)=FVAR(2)
5.a Rotating group:
 O9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C18(H18), C23(H23)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.50809(3) 0.19558(2) 0.70047(2) 0.00948(11) Uani 1 1 d . . . . .
F4 F 0.1948(5) 0.0986(4) 0.3529(2) 0.0473(10) Uani 1 1 d . . . . .
F5 F 0.1229(5) -0.0064(3) 0.4259(3) 0.0497(11) Uani 1 1 d . U . . .
F6 F 0.0360(4) 0.1396(4) 0.4141(3) 0.0566(12) Uani 1 1 d . U . . .
F10 F 0.2282(5) -0.1799(3) 0.7289(2) 0.0413(10) Uani 1 1 d . . . . .
F11 F 0.2163(4) -0.0885(3) 0.8585(2) 0.0356(9) Uani 1 1 d . . . . .
F12 F 0.4180(4) -0.0945(4) 0.8378(3) 0.0533(12) Uani 1 1 d . . . . .
F13 F 0.4002(5) 0.3368(4) 0.9808(2) 0.0508(11) Uani 1 1 d . . . . .
F14 F 0.6181(6) 0.4316(4) 1.0369(3) 0.0584(12) Uani 1 1 d . U . . .
F15 F 0.5485(6) 0.2809(4) 1.0708(2) 0.0583(13) Uani 1 1 d . U . . .
F16 F 0.7626(6) -0.0252(5) 0.9347(4) 0.0762(16) Uani 1 1 d . U . . .
F17 F 0.9273(5) 0.1159(5) 0.9631(3) 0.0778(17) Uani 1 1 d . U . . .
F18 F 0.8597(5) -0.0022(4) 0.8347(2) 0.0529(12) Uani 1 1 d . U . . .
O1 O 0.7317(4) 0.3370(3) 0.7770(2) 0.0151(7) Uani 1 1 d . . . . .
O2 O 0.8872(4) 0.5787(3) 0.6262(2) 0.0192(8) Uani 1 1 d . . . . .
O3 O 0.4699(4) 0.3663(3) 0.6672(2) 0.0147(7) Uani 1 1 d . . . . .
O4 O 0.3369(4) 0.1294(3) 0.5573(2) 0.0146(7) Uani 1 1 d . . . . .
O5 O 0.2768(4) 0.2264(3) 0.7161(2) 0.0165(7) Uani 1 1 d . . . . .
O6 O 0.3814(4) 0.0337(3) 0.7258(2) 0.0162(7) Uani 1 1 d . . . . .
O7 O 0.5214(4) 0.2754(3) 0.8527(2) 0.0149(7) Uani 1 1 d . . . . .
O8 O 0.6784(4) 0.1186(3) 0.7910(2) 0.0136(7) Uani 1 1 d . . . . .
O9 O 0.5643(4) 0.0272(3) 0.6165(2) 0.0158(7) Uani 1 1 d . . . . .
H9A H 0.6118 -0.0035 0.6525 0.024 Uiso 1 1 d GR . . . .
H9B H 0.6150 0.0459 0.5837 0.024 Uiso 1 1 d GR . . . .
N1 N 0.7861(4) 0.4281(3) 0.7601(3) 0.0119(8) Uani 1 1 d . . . . .
N2 N 0.8641(5) 0.5415(3) 0.6888(3) 0.0137(8) Uani 1 1 d . . . . .
N3 N 0.6450(5) 0.2456(3) 0.5852(2) 0.0132(8) Uani 1 1 d . . . . .
N4 N 0.6330(5) 0.1666(4) 0.5054(3) 0.0174(9) Uani 1 1 d . . . . .
N5 N 0.8221(5) 0.3060(4) 0.5370(3) 0.0167(9) Uani 1 1 d . . . . .
C1 C 0.8044(5) 0.4322(4) 0.6819(3) 0.0104(9) Uani 1 1 d . . . . .
C2 C 0.8298(6) 0.5463(4) 0.8293(3) 0.0163(10) Uani 1 1 d . . . . .
C3 C 0.6930(6) 0.5816(5) 0.8374(4) 0.0261(12) Uani 1 1 d . . . . .
H3A H 0.6414 0.5875 0.7811 0.039 Uiso 1 1 calc GR . . . .
H3B H 0.7157 0.6552 0.8829 0.039 Uiso 1 1 calc GR . . . .
H3C H 0.6357 0.5242 0.8531 0.039 Uiso 1 1 calc GR . . . .
C4 C 0.9136(7) 0.5364(5) 0.9181(3) 0.0260(13) Uani 1 1 d . . . . .
H4A H 0.8532 0.4864 0.9380 0.039 Uiso 1 1 calc GR . . . .
H4B H 0.9475 0.6119 0.9620 0.039 Uiso 1 1 calc GR . . . .
H4C H 0.9929 0.5048 0.9100 0.039 Uiso 1 1 calc GR . . . .
C5 C 0.9184(5) 0.6179(4) 0.7856(3) 0.0145(10) Uani 1 1 d . . . . .
C6 C 0.8912(7) 0.7372(4) 0.7911(4) 0.0251(12) Uani 1 1 d . . . . .
H6A H 0.9444 0.7728 0.7589 0.038 Uiso 1 1 calc GR . . . .
H6B H 0.9202 0.7846 0.8526 0.038 Uiso 1 1 calc GR . . . .
H6C H 0.7917 0.7295 0.7651 0.038 Uiso 1 1 calc GR . . . .
C7 C 1.0770(6) 0.6239(5) 0.8156(4) 0.0246(12) Uani 1 1 d . . . . .
H7A H 1.0907 0.5478 0.8131 0.037 Uiso 1 1 calc GR . . . .
H7B H 1.1184 0.6751 0.8759 0.037 Uiso 1 1 calc GR . . . .
H7C H 1.1218 0.6526 0.7766 0.037 Uiso 1 1 calc GR . . . .
C8 C 0.7590(5) 0.3297(4) 0.6029(3) 0.0107(9) Uani 1 1 d . . . . .
C9 C 0.7392(6) 0.2039(4) 0.4784(3) 0.0214(12) Uani 1 1 d . . . . .
H9 H 0.7558 0.1653 0.4257 0.026 Uiso 1 1 calc R . . . .
C10 C 0.9611(7) 0.3656(5) 0.5339(4) 0.0311(14) Uani 1 1 d . . . . .
H10A H 0.9701 0.4478 0.5517 0.047 Uiso 1 1 calc GR . . . .
H10B H 0.9675 0.3396 0.4740 0.047 Uiso 1 1 calc GR . . . .
H10C H 1.0360 0.3480 0.5740 0.047 Uiso 1 1 calc GR . . . .
C12 C 0.3896(6) 0.3826(4) 0.6018(4) 0.0214(11) Uani 1 1 d D . . . .
C13 C 0.2931(6) 0.2998(5) 0.5249(3) 0.0208(11) Uani 1 1 d . . . . .
H13 H 0.2403 0.3253 0.4813 0.025 Uiso 1 1 calc R . . . .
C14 C 0.2725(6) 0.1806(5) 0.5107(3) 0.0174(10) Uani 1 1 d . . . . .
C15 C 0.1536(6) 0.1012(5) 0.4264(3) 0.0240(12) Uani 1 1 d . . . . .
C16 C 0.0948(4) 0.2578(4) 0.7784(2) 0.0262(12) Uani 1 1 d D . . . .
C17 C 0.2021(6) 0.1894(5) 0.7591(3) 0.0195(11) Uani 1 1 d . . . . .
C18 C 0.2082(6) 0.0954(5) 0.7923(3) 0.0200(11) Uani 1 1 d . . . . .
H18 H 0.1525 0.0810 0.8286 0.024 Uiso 1 1 calc R . . . .
C19 C 0.2963(6) 0.0244(4) 0.7714(3) 0.0171(10) Uani 1 1 d . . . . .
C20 C 0.2902(6) -0.0838(5) 0.8004(4) 0.0222(11) Uani 1 1 d . . . . .
C21 C 0.5310(7) 0.3239(5) 1.0039(3) 0.0289(13) Uani 1 1 d . . . . .
C22 C 0.5694(6) 0.2539(4) 0.9232(3) 0.0189(11) Uani 1 1 d . . . . .
C23 C 0.6568(6) 0.1802(5) 0.9384(3) 0.0218(11) Uani 1 1 d . . . . .
H23 H 0.6830 0.1708 0.9948 0.026 Uiso 1 1 calc R . . . .
C24 C 0.7068(6) 0.1192(4) 0.8705(3) 0.0179(11) Uani 1 1 d . . . . .
C25 C 0.8114(7) 0.0481(5) 0.8980(4) 0.0290(14) Uani 1 1 d . . . . .
F1 F 0.3367(10) 0.5295(8) 0.5327(5) 0.049(2) Uani 0.527(10) 1 d D U P A 1
F2 F 0.3818(10) 0.5680(12) 0.6759(5) 0.041(2) Uani 0.527(10) 1 d D U P A 1
F3 F 0.5518(8) 0.5582(10) 0.6155(6) 0.0352(19) Uani 0.527(10) 1 d D U P A 1
F7 F -0.0051(7) 0.2513(7) 0.7043(4) 0.068(2) Uani 0.565(6) 1 d D U P B 1
F8 F 0.0249(8) 0.2299(7) 0.8338(4) 0.063(2) Uani 0.565(6) 1 d D U P B 1
F9 F 0.1604(8) 0.3705(4) 0.8167(5) 0.084(3) Uani 0.565(6) 1 d D U P B 1
C11 C 0.4157(8) 0.5103(7) 0.6045(5) 0.026(3) Uani 0.527(10) 1 d D . P A 1
F1' F 0.2836(10) 0.5299(10) 0.5586(6) 0.049(2) Uani 0.473(10) 1 d D . P A 2
F2' F 0.3666(11) 0.5627(14) 0.6999(5) 0.041(2) Uani 0.473(10) 1 d D . P A 2
F3' F 0.5083(10) 0.5701(12) 0.6201(7) 0.0352(19) Uani 0.473(10) 1 d D . P A 2
F7' F 0.0611(11) 0.3182(7) 0.7217(5) 0.068(2) Uani 0.435(6) 1 d D U P B 2
F8' F -0.0290(6) 0.1874(7) 0.7692(6) 0.063(2) Uani 0.435(6) 1 d D U P B 2
F9' F 0.1281(12) 0.3351(7) 0.8600(4) 0.084(3) Uani 0.435(6) 1 d D U P B 2
C11' C 0.3839(9) 0.5107(7) 0.6209(5) 0.026(3) Uani 0.473(10) 1 d D . P A 2


_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 O1 2.415(4) . ?
Tb1 O3 2.367(3) . ?
Tb1 O4 2.370(3) . ?
Tb1 O5 2.465(4) . ?
Tb1 O6 2.364(3) . ?
Tb1 O7 2.366(3) . ?
Tb1 O8 2.449(3) . ?
Tb1 O9 2.397(3) . ?
Tb1 N3 2.698(4) . ?
F4 C15 1.344(7) . ?
F5 C15 1.306(7) . ?
F6 C15 1.329(7) . ?
F10 C20 1.352(7) . ?
F11 C20 1.334(6) . ?
F12 C20 1.320(7) . ?
F13 C21 1.318(7) . ?
F14 C21 1.352(8) . ?
F15 C21 1.310(6) . ?
F16 C25 1.296(7) . ?
F17 C25 1.337(8) . ?
F18 C25 1.294(7) . ?
O1 N1 1.287(5) . ?
O2 N2 1.268(5) . ?
O3 C12 1.249(6) . ?
O4 C14 1.235(6) . ?
O5 C17 1.245(6) . ?
O6 C19 1.263(6) . ?
O7 C22 1.241(6) . ?
O8 C24 1.247(6) . ?
O9 H9A 0.8648 . ?
O9 H9B 0.8651 . ?
N1 C1 1.334(6) . ?
N1 C2 1.507(6) . ?
N2 C1 1.343(6) . ?
N2 C5 1.514(6) . ?
N3 N4 1.365(5) . ?
N3 C8 1.324(6) . ?
N4 C9 1.301(7) . ?
N5 C8 1.357(6) . ?
N5 C9 1.352(7) . ?
N5 C10 1.479(7) . ?
C1 C8 1.459(7) . ?
C2 C3 1.526(8) . ?
C2 C4 1.525(7) . ?
C2 C5 1.559(7) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.521(7) . ?
C5 C7 1.525(8) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 C13 1.400(8) . ?
C12 C11 1.537(8) . ?
C12 C11' 1.539(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.397(7) . ?
C14 C15 1.542(7) . ?
C16 C17 1.510(7) . ?
C16 F7 1.3385(10) . ?
C16 F8 1.3397(10) . ?
C16 F9 1.3407(11) . ?
C16 F7' 1.3399(10) . ?
C16 F8' 1.3404(11) . ?
C16 F9' 1.3392(11) . ?
C17 C18 1.400(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.378(8) . ?
C19 C20 1.519(7) . ?
C21 C22 1.537(7) . ?
C22 C23 1.385(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.408(7) . ?
C24 C25 1.529(7) . ?
F1 C11 1.3398(10) . ?
F2 C11 1.3401(10) . ?
F3 C11 1.3401(11) . ?
F1' C11' 1.3399(10) . ?
F2' C11' 1.3401(10) . ?
F3' C11' 1.3401(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O5 124.32(12) . . ?
O1 Tb1 O8 68.37(11) . . ?
O1 Tb1 N3 67.97(11) . . ?
O3 Tb1 O1 75.36(11) . . ?
O3 Tb1 O4 75.05(11) . . ?
O3 Tb1 O5 69.88(11) . . ?
O3 Tb1 O8 143.43(11) . . ?
O3 Tb1 O9 131.53(11) . . ?
O3 Tb1 N3 67.43(12) . . ?
O4 Tb1 O1 138.10(11) . . ?
O4 Tb1 O5 70.43(11) . . ?
O4 Tb1 O8 137.59(11) . . ?
O4 Tb1 O9 73.79(12) . . ?
O4 Tb1 N3 73.58(12) . . ?
O5 Tb1 N3 129.51(11) . . ?
O6 Tb1 O1 135.69(11) . . ?
O6 Tb1 O3 139.29(12) . . ?
O6 Tb1 O4 85.31(11) . . ?
O6 Tb1 O5 70.02(11) . . ?
O6 Tb1 O7 79.28(12) . . ?
O6 Tb1 O8 71.54(11) . . ?
O6 Tb1 O9 72.94(12) . . ?
O6 Tb1 N3 139.96(12) . . ?
O7 Tb1 O1 70.92(11) . . ?
O7 Tb1 O3 92.68(11) . . ?
O7 Tb1 O4 139.20(12) . . ?
O7 Tb1 O5 68.82(11) . . ?
O7 Tb1 O8 71.60(11) . . ?
O7 Tb1 O9 134.46(11) . . ?
O7 Tb1 N3 137.60(12) . . ?
O8 Tb1 O5 128.60(10) . . ?
O8 Tb1 N3 101.85(11) . . ?
O9 Tb1 O1 105.94(12) . . ?
O9 Tb1 O5 129.69(12) . . ?
O9 Tb1 O8 65.75(11) . . ?
O9 Tb1 N3 68.68(11) . . ?
N1 O1 Tb1 130.3(3) . . ?
C12 O3 Tb1 132.4(3) . . ?
C14 O4 Tb1 132.5(3) . . ?
C17 O5 Tb1 130.5(3) . . ?
C19 O6 Tb1 132.2(3) . . ?
C22 O7 Tb1 135.8(3) . . ?
C24 O8 Tb1 133.2(3) . . ?
Tb1 O9 H9A 110.1 . . ?
Tb1 O9 H9B 110.2 . . ?
H9A O9 H9B 108.7 . . ?
O1 N1 C1 126.1(4) . . ?
O1 N1 C2 121.4(4) . . ?
C1 N1 C2 112.4(4) . . ?
O2 N2 C1 127.0(4) . . ?
O2 N2 C5 121.5(4) . . ?
C1 N2 C5 111.2(4) . . ?
N4 N3 Tb1 122.7(3) . . ?
C8 N3 Tb1 127.8(3) . . ?
C8 N3 N4 107.0(4) . . ?
C9 N4 N3 107.4(4) . . ?
C8 N5 C10 129.2(4) . . ?
C9 N5 C8 104.4(4) . . ?
C9 N5 C10 125.7(4) . . ?
N1 C1 N2 109.9(4) . . ?
N1 C1 C8 122.1(4) . . ?
N2 C1 C8 128.0(4) . . ?
N1 C2 C3 106.6(4) . . ?
N1 C2 C4 108.4(4) . . ?
N1 C2 C5 101.0(4) . . ?
C3 C2 C5 114.8(4) . . ?
C4 C2 C3 110.4(4) . . ?
C4 C2 C5 114.8(4) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C2 100.8(4) . . ?
N2 C5 C6 109.1(4) . . ?
N2 C5 C7 105.8(4) . . ?
C6 C5 C2 115.0(4) . . ?
C6 C5 C7 111.4(4) . . ?
C7 C5 C2 113.7(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 N5 110.1(4) . . ?
N3 C8 C1 123.1(4) . . ?
N5 C8 C1 126.8(4) . . ?
N4 C9 N5 111.1(4) . . ?
N4 C9 H9 124.4 . . ?
N5 C9 H9 124.4 . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C12 C13 128.3(4) . . ?
O3 C12 C11 113.4(5) . . ?
O3 C12 C11' 111.6(5) . . ?
C13 C12 C11 117.9(4) . . ?
C13 C12 C11' 119.2(5) . . ?
C12 C13 H13 118.5 . . ?
C14 C13 C12 122.9(4) . . ?
C14 C13 H13 118.5 . . ?
O4 C14 C13 128.6(5) . . ?
O4 C14 C15 115.0(5) . . ?
C13 C14 C15 116.5(4) . . ?
F4 C15 C14 110.0(5) . . ?
F5 C15 F4 106.0(5) . . ?
F5 C15 F6 109.5(5) . . ?
F5 C15 C14 113.0(4) . . ?
F6 C15 F4 105.4(4) . . ?
F6 C15 C14 112.5(4) . . ?
F7 C16 C17 113.0(5) . . ?
F7 C16 F8 105.9(3) . . ?
F7 C16 F9 105.8(3) . . ?
F8 C16 C17 116.2(5) . . ?
F8 C16 F9 105.7(3) . . ?
F9 C16 C17 109.5(5) . . ?
F7' C16 C17 113.5(6) . . ?
F7' C16 F8' 104.6(4) . . ?
F8' C16 C17 111.1(6) . . ?
F9' C16 C17 117.3(6) . . ?
F9' C16 F7' 104.6(4) . . ?
F9' C16 F8' 104.6(4) . . ?
O5 C17 C16 114.4(4) . . ?
O5 C17 C18 128.2(5) . . ?
C18 C17 C16 117.4(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.2(5) . . ?
C19 C18 H18 119.9 . . ?
O6 C19 C18 128.1(5) . . ?
O6 C19 C20 112.6(5) . . ?
C18 C19 C20 119.2(5) . . ?
F10 C20 C19 110.5(4) . . ?
F11 C20 F10 106.3(4) . . ?
F11 C20 C19 114.1(5) . . ?
F12 C20 F10 106.6(5) . . ?
F12 C20 F11 106.9(4) . . ?
F12 C20 C19 112.0(4) . . ?
F13 C21 F14 106.7(5) . . ?
F13 C21 C22 111.7(5) . . ?
F14 C21 C22 108.9(5) . . ?
F15 C21 F13 109.5(5) . . ?
F15 C21 F14 105.8(5) . . ?
F15 C21 C22 113.8(5) . . ?
O7 C22 C21 114.3(5) . . ?
O7 C22 C23 128.4(5) . . ?
C23 C22 C21 117.3(4) . . ?
C22 C23 H23 119.2 . . ?
C22 C23 C24 121.5(5) . . ?
C24 C23 H23 119.2 . . ?
O8 C24 C23 127.6(5) . . ?
O8 C24 C25 116.2(5) . . ?
C23 C24 C25 116.2(4) . . ?
F16 C25 F17 102.5(5) . . ?
F16 C25 C24 112.9(5) . . ?
F17 C25 C24 110.9(5) . . ?
F18 C25 F16 110.9(5) . . ?
F18 C25 F17 104.4(6) . . ?
F18 C25 C24 114.2(4) . . ?
F1 C11 C12 114.8(7) . . ?
F1 C11 F2 107.4(4) . . ?
F1 C11 F3 107.4(4) . . ?
F2 C11 C12 106.6(9) . . ?
F2 C11 F3 107.3(4) . . ?
F3 C11 C12 113.0(8) . . ?
F1' C11' C12 113.9(8) . . ?
F1' C11' F2' 106.1(5) . . ?
F1' C11' F3' 106.1(5) . . ?
F2' C11' C12 116.5(10) . . ?
F3' C11' C12 107.4(9) . . ?
F3' C11' F2' 106.1(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 N1 C1 -53.2(6) . . . . ?
Tb1 O1 N1 C2 123.4(4) . . . . ?
Tb1 O3 C12 C13 0.2(9) . . . . ?
Tb1 O3 C12 C11 -172.6(4) . . . . ?
Tb1 O3 C12 C11' 168.9(5) . . . . ?
Tb1 O4 C14 C13 7.9(8) . . . . ?
Tb1 O4 C14 C15 -171.8(3) . . . . ?
Tb1 O5 C17 C16 160.0(3) . . . . ?
Tb1 O5 C17 C18 -18.6(8) . . . . ?
Tb1 O6 C19 C18 28.1(8) . . . . ?
Tb1 O6 C19 C20 -155.4(3) . . . . ?
Tb1 O7 C22 C21 -171.7(4) . . . . ?
Tb1 O7 C22 C23 11.6(9) . . . . ?
Tb1 O8 C24 C23 -8.6(8) . . . . ?
Tb1 O8 C24 C25 173.3(4) . . . . ?
Tb1 N3 N4 C9 -162.0(3) . . . . ?
Tb1 N3 C8 N5 160.8(3) . . . . ?
Tb1 N3 C8 C1 -20.0(6) . . . . ?
F13 C21 C22 O7 38.4(7) . . . . ?
F13 C21 C22 C23 -144.5(5) . . . . ?
F14 C21 C22 O7 -79.2(6) . . . . ?
F14 C21 C22 C23 97.9(6) . . . . ?
F15 C21 C22 O7 163.1(5) . . . . ?
F15 C21 C22 C23 -19.9(8) . . . . ?
O1 N1 C1 N2 180.0(4) . . . . ?
O1 N1 C1 C8 1.8(7) . . . . ?
O1 N1 C2 C3 -72.5(5) . . . . ?
O1 N1 C2 C4 46.4(6) . . . . ?
O1 N1 C2 C5 167.4(4) . . . . ?
O2 N2 C1 N1 -174.5(4) . . . . ?
O2 N2 C1 C8 3.6(8) . . . . ?
O2 N2 C5 C2 165.3(4) . . . . ?
O2 N2 C5 C6 43.9(6) . . . . ?
O2 N2 C5 C7 -76.1(5) . . . . ?
O3 C12 C13 C14 0.2(10) . . . . ?
O3 C12 C11 F1 176.3(5) . . . . ?
O3 C12 C11 F2 -65.0(6) . . . . ?
O3 C12 C11 F3 52.7(7) . . . . ?
O3 C12 C11' F1' -170.5(6) . . . . ?
O3 C12 C11' F2' -46.4(7) . . . . ?
O3 C12 C11' F3' 72.3(6) . . . . ?
O4 C14 C15 F4 -106.6(5) . . . . ?
O4 C14 C15 F5 11.6(7) . . . . ?
O4 C14 C15 F6 136.2(5) . . . . ?
O5 C17 C18 C19 -6.3(9) . . . . ?
O6 C19 C20 F10 -68.8(6) . . . . ?
O6 C19 C20 F11 171.5(4) . . . . ?
O6 C19 C20 F12 49.9(6) . . . . ?
O7 C22 C23 C24 1.6(9) . . . . ?
O8 C24 C25 F16 -126.6(6) . . . . ?
O8 C24 C25 F17 119.0(6) . . . . ?
O8 C24 C25 F18 1.4(8) . . . . ?
N1 C1 C8 N3 33.6(7) . . . . ?
N1 C1 C8 N5 -147.3(5) . . . . ?
N1 C2 C5 N2 20.0(4) . . . . ?
N1 C2 C5 C6 137.1(4) . . . . ?
N1 C2 C5 C7 -92.8(5) . . . . ?
N2 C1 C8 N3 -144.2(5) . . . . ?
N2 C1 C8 N5 34.9(8) . . . . ?
N3 N4 C9 N5 -0.5(6) . . . . ?
N4 N3 C8 N5 -1.0(5) . . . . ?
N4 N3 C8 C1 178.1(4) . . . . ?
C1 N1 C2 C3 104.6(5) . . . . ?
C1 N1 C2 C4 -136.6(4) . . . . ?
C1 N1 C2 C5 -15.6(5) . . . . ?
C1 N2 C5 C2 -20.6(5) . . . . ?
C1 N2 C5 C6 -142.0(5) . . . . ?
C1 N2 C5 C7 98.0(5) . . . . ?
C2 N1 C1 N2 3.1(6) . . . . ?
C2 N1 C1 C8 -175.0(4) . . . . ?
C3 C2 C5 N2 -94.2(5) . . . . ?
C3 C2 C5 C6 22.9(6) . . . . ?
C3 C2 C5 C7 153.1(4) . . . . ?
C4 C2 C5 N2 136.3(4) . . . . ?
C4 C2 C5 C6 -106.6(5) . . . . ?
C4 C2 C5 C7 23.5(6) . . . . ?
C5 N2 C1 N1 11.8(6) . . . . ?
C5 N2 C1 C8 -170.2(5) . . . . ?
C8 N3 N4 C9 1.0(5) . . . . ?
C8 N5 C9 N4 -0.1(6) . . . . ?
C9 N5 C8 N3 0.7(5) . . . . ?
C9 N5 C8 C1 -178.4(4) . . . . ?
C10 N5 C8 N3 -170.6(5) . . . . ?
C10 N5 C8 C1 10.3(8) . . . . ?
C10 N5 C9 N4 171.6(5) . . . . ?
C12 C13 C14 O4 -4.5(9) . . . . ?
C12 C13 C14 C15 175.1(5) . . . . ?
C13 C12 C11 F1 2.7(8) . . . . ?
C13 C12 C11 F2 121.4(6) . . . . ?
C13 C12 C11 F3 -120.9(6) . . . . ?
C13 C12 C11' F1' -0.7(9) . . . . ?
C13 C12 C11' F2' 123.4(6) . . . . ?
C13 C12 C11' F3' -117.9(6) . . . . ?
C13 C14 C15 F4 73.7(6) . . . . ?
C13 C14 C15 F5 -168.1(5) . . . . ?
C13 C14 C15 F6 -43.5(7) . . . . ?
C16 C17 C18 C19 175.2(4) . . . . ?
C17 C18 C19 O6 2.4(9) . . . . ?
C17 C18 C19 C20 -173.9(5) . . . . ?
C18 C19 C20 F10 108.1(6) . . . . ?
C18 C19 C20 F11 -11.6(7) . . . . ?
C18 C19 C20 F12 -133.2(5) . . . . ?
C21 C22 C23 C24 -175.0(5) . . . . ?
C22 C23 C24 O8 -2.6(9) . . . . ?
C22 C23 C24 C25 175.5(5) . . . . ?
C23 C24 C25 F16 55.1(7) . . . . ?
C23 C24 C25 F17 -59.3(7) . . . . ?
C23 C24 C25 F18 -176.9(5) . . . . ?
F7 C16 C17 O5 65.4(6) . . . . ?
F7 C16 C17 C18 -115.9(6) . . . . ?
F8 C16 C17 O5 -171.9(5) . . . . ?
F8 C16 C17 C18 6.8(7) . . . . ?
F9 C16 C17 O5 -52.3(6) . . . . ?
F9 C16 C17 C18 126.4(5) . . . . ?
C11 C12 C13 C14 172.8(6) . . . . ?
F7' C16 C17 O5 22.6(6) . . . . ?
F7' C16 C17 C18 -158.7(6) . . . . ?
F8' C16 C17 O5 140.1(5) . . . . ?
F8' C16 C17 C18 -41.2(6) . . . . ?
F9' C16 C17 O5 -99.7(6) . . . . ?
F9' C16 C17 C18 79.0(7) . . . . ?
C11' C12 C13 C14 -167.7(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-22
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 11.542
_oxdiff_exptl_absorpt_empirical_full_min 0.672
