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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# 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. 
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#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1427266'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C52 H24 Cl2 Dy2 F24 N4 O10'
_chemical_formula_sum            'C52 H24 Cl2 Dy2 F24 N4 O10'
_chemical_formula_weight         1716.65
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.347(2)
_cell_length_b                   19.187(4)
_cell_length_c                   13.041(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.15(3)
_cell_angle_gamma                90
_cell_volume                     2827.7(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9451
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9223
_cell_measurement_theta_min      2.1229
_shelx_estimated_absorpt_T_max   0.725
_shelx_estimated_absorpt_T_min   0.599
_exptl_absorpt_coefficient_mu    2.858
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7962
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27956
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.942
_diffrn_reflns_theta_min         2.123
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9678
	          2theta: -19.9519
scan:
	Number of images: 150
	           Slice: -110.0000 - 40.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9678
	          2theta: -19.9519
scan:
	Number of images: 100
	           Slice: -110.0000 - -10.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9678
	          2theta: -19.9519
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             6961
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0163
_diffrn_orient_matrix_UB_12      -0.0028
_diffrn_orient_matrix_UB_13      -0.0869
_diffrn_orient_matrix_UB_21      0.0203
_diffrn_orient_matrix_UB_22      -0.0477
_diffrn_orient_matrix_UB_23      0.0053
_diffrn_orient_matrix_UB_31      -0.0679
_diffrn_orient_matrix_UB_32      -0.0310
_diffrn_orient_matrix_UB_33      -0.0188
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5935
_reflns_number_total             6750
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.000
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6750
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0248
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+0.5979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0611
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-F7 \\sim C22-F8 \\sim C22-F9 \\sim C22-F7' \\sim C22-F8' \\sim C22-F9'
\\sim C22-F7" \\sim C22-F8" ~
 C22-F9"
 with sigma of 0.01
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F7'-F8' \\sim F7'-F9' \\sim F8'-F9' \\sim
F7"-F8" \\sim F7"-F9" \\sim F8"-
 F9"
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F9" \\sim F9 \\sim F9' \\sim F8" \\sim F8 \\sim F8' \\sim F7" \\sim F7 \\sim
F7': within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7') \\sim
Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F7") \\sim Ueq,
Uanis(F8") \\sim Ueq, Uanis(F9") \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F9") \\sim Ueq, Uanis(F8") \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7')+Sof(F8')+Sof(F9')]+1*[Sof(F7")+
 Sof(F8")+Sof(F9")]=1 with esd of 0.0001
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=FVAR(2)
 Sof(F7")=Sof(F8")=Sof(F9")=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.45859(2) 0.09291(2) 0.46871(2) 0.01366(4) Uani 1 1 d . . . . .
Cl1 Cl 0.66515(6) 0.46409(4) 0.40226(7) 0.03899(17) Uani 1 1 d . . . . .
F1 F 0.4204(2) 0.12407(12) 0.84291(15) 0.0580(6) Uani 1 1 d . . . . .
F2 F 0.33425(16) 0.21139(14) 0.76899(15) 0.0638(6) Uani 1 1 d . . . . .
F3 F 0.49739(16) 0.22503(11) 0.86204(13) 0.0467(5) Uani 1 1 d . . . . .
F4 F 0.74244(15) 0.32006(9) 0.60865(18) 0.0521(6) Uani 1 1 d . . . . .
F5 F 0.78645(17) 0.25839(12) 0.48253(14) 0.0543(6) Uani 1 1 d . . . . .
F6 F 0.84718(13) 0.22912(9) 0.63545(14) 0.0401(4) Uani 1 1 d . . . . .
F7 F 0.6479(6) 0.1760(4) 0.1793(6) 0.0429(17) Uani 0.508(3) 1 d D U P A 1
F8 F 0.5207(7) 0.1475(4) 0.0592(5) 0.039(2) Uani 0.508(3) 1 d D U P A 1
F9 F 0.6570(7) 0.0758(3) 0.1106(8) 0.064(3) Uani 0.508(3) 1 d D U P A 1
F7' F 0.6811(7) 0.1502(7) 0.1784(8) 0.069(4) Uani 0.366(3) 1 d D U P A 2
F8' F 0.5221(10) 0.1679(5) 0.0829(8) 0.041(3) Uani 0.366(3) 1 d D U P A 2
F9' F 0.6110(10) 0.0720(4) 0.0742(8) 0.050(3) Uani 0.366(3) 1 d D U P A 2
F7" F 0.5815(19) 0.1895(3) 0.1383(17) 0.043(4) Uani 0.125(3) 1 d D U P A 3
F8" F 0.5516(16) 0.0986(12) 0.0460(7) 0.039(4) Uani 0.125(3) 1 d D U P A 3
F9" F 0.6942(9) 0.1014(11) 0.1618(14) 0.032(4) Uani 0.125(3) 1 d D U P A 3
F10 F 0.15579(14) -0.00656(10) 0.17268(14) 0.0461(5) Uani 1 1 d . . . . .
F11 F 0.22532(16) -0.08297(9) 0.28094(14) 0.0384(4) Uani 1 1 d . . . . .
F12 F 0.29147(17) -0.07726(10) 0.13298(15) 0.0499(5) Uani 1 1 d . . . . .
O1 O 0.39461(13) -0.01193(8) 0.54106(12) 0.0161(3) Uani 1 1 d . . . . .
O2 O 0.46460(14) 0.11971(9) 0.64454(12) 0.0205(3) Uani 1 1 d . . . . .
O3 O 0.61769(14) 0.17019(9) 0.51296(12) 0.0186(3) Uani 1 1 d . . . . .
O4 O 0.51240(14) 0.12265(9) 0.30492(12) 0.0194(3) Uani 1 1 d . . . . .
O5 O 0.33365(14) 0.03398(9) 0.34113(12) 0.0214(3) Uani 1 1 d . . . . .
N1 N 0.25788(17) 0.10228(10) 0.51942(15) 0.0168(4) Uani 1 1 d . . . . .
N2 N 0.36446(17) 0.21683(10) 0.45273(15) 0.0186(4) Uani 1 1 d . . . . .
C1 C 0.21191(19) 0.04516(13) 0.56099(18) 0.0179(5) Uani 1 1 d . . . . .
C2 C 0.28407(19) -0.01578(12) 0.57129(17) 0.0174(5) Uani 1 1 d . . . . .
C3 C 0.2367(2) -0.07424(13) 0.61324(19) 0.0204(5) Uani 1 1 d . . . . .
H3 H 0.2821 -0.1158 0.6198 0.024 Uiso 1 1 calc R . . . .
C4 C 0.1219(2) -0.07330(14) 0.6465(2) 0.0238(5) Uani 1 1 d . . . . .
H4 H 0.0922 -0.1144 0.6757 0.029 Uiso 1 1 calc R . . . .
C5 C 0.0525(2) -0.01565(14) 0.6383(2) 0.0255(5) Uani 1 1 d . . . . .
H5 H -0.0246 -0.0165 0.6613 0.031 Uiso 1 1 calc R . . . .
C6 C 0.09589(19) 0.04551(13) 0.59528(18) 0.0199(5) Uani 1 1 d . . . . .
C7 C 0.0314(2) 0.10830(14) 0.5838(2) 0.0249(5) Uani 1 1 d . . . . .
H7 H -0.0469 0.1104 0.6038 0.030 Uiso 1 1 calc R . . . .
C8 C 0.0809(2) 0.16610(14) 0.5439(2) 0.0239(5) Uani 1 1 d . . . . .
H8 H 0.0382 0.2087 0.5373 0.029 Uiso 1 1 calc R . . . .
C9 C 0.1960(2) 0.16134(13) 0.51280(18) 0.0193(5) Uani 1 1 d . . . . .
C10 C 0.2580(2) 0.22234(13) 0.47828(18) 0.0206(5) Uani 1 1 d . . . . .
H10 H 0.2196 0.2664 0.4746 0.025 Uiso 1 1 calc R . . . .
C11 C 0.4282(2) 0.27947(12) 0.43657(18) 0.0192(5) Uani 1 1 d . . . . .
C12 C 0.4287(2) 0.33451(13) 0.5062(2) 0.0234(5) Uani 1 1 d . . . . .
H12 H 0.3796 0.3326 0.5615 0.028 Uiso 1 1 calc R . . . .
C13 C 0.5004(2) 0.39197(13) 0.4954(2) 0.0278(6) Uani 1 1 d . . . . .
H13 H 0.5016 0.4293 0.5433 0.033 Uiso 1 1 calc R . . . .
C14 C 0.5701(2) 0.39422(13) 0.4143(2) 0.0261(6) Uani 1 1 d . . . . .
C15 C 0.5696(2) 0.34080(13) 0.3436(2) 0.0265(5) Uani 1 1 d . . . . .
H15 H 0.6171 0.3438 0.2873 0.032 Uiso 1 1 calc R . . . .
C16 C 0.4995(2) 0.28277(13) 0.3550(2) 0.0238(5) Uani 1 1 d . . . . .
H16 H 0.5000 0.2453 0.3074 0.029 Uiso 1 1 calc R . . . .
C17 C 0.4393(2) 0.18209(16) 0.7950(2) 0.0302(6) Uani 1 1 d . . . . .
C18 C 0.5024(2) 0.17086(13) 0.69773(18) 0.0195(5) Uani 1 1 d . . . . .
C19 C 0.5904(2) 0.21738(13) 0.67679(18) 0.0210(5) Uani 1 1 d . . . . .
H19 H 0.6130 0.2538 0.7239 0.025 Uiso 1 1 calc R . . . .
C20 C 0.64545(19) 0.21037(12) 0.58628(18) 0.0177(5) Uani 1 1 d . . . . .
C21 C 0.7558(2) 0.25529(13) 0.5766(2) 0.0232(5) Uani 1 1 d . . . . .
C22 C 0.5829(2) 0.12137(13) 0.14001(19) 0.0261(5) Uani 1 1 d D . . . .
C23 C 0.5039(2) 0.09223(12) 0.21958(19) 0.0199(5) Uani 1 1 d . . . . .
C24 C 0.4302(2) 0.03759(14) 0.18794(19) 0.0248(5) Uani 1 1 d . . . . .
H24 H 0.4362 0.0161 0.1230 0.030 Uiso 1 1 calc R . . . .
C25 C 0.3472(2) 0.01437(13) 0.25204(18) 0.0210(5) Uani 1 1 d . . . . .
C26 C 0.2544(2) -0.03914(15) 0.2085(2) 0.0291(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy1 3.7582(7) 3_656 ?
Dy1 O1 2.3636(16) . ?
Dy1 O1 2.2899(15) 3_656 ?
Dy1 O2 2.3449(17) . ?
Dy1 O3 2.3672(16) . ?
Dy1 O4 2.3442(17) . ?
Dy1 O5 2.3734(17) . ?
Dy1 N1 2.435(2) . ?
Dy1 N2 2.607(2) . ?
Cl1 C14 1.737(3) . ?
F1 C17 1.304(4) . ?
F2 C17 1.333(3) . ?
F3 C17 1.332(3) . ?
F4 C21 1.324(3) . ?
F5 C21 1.306(3) . ?
F6 C21 1.332(3) . ?
F7 C22 1.356(5) . ?
F8 C22 1.313(5) . ?
F9 C22 1.295(5) . ?
F7' C22 1.303(6) . ?
F8' C22 1.317(6) . ?
F9' C22 1.335(6) . ?
F7" C22 1.307(6) . ?
F8" C22 1.320(6) . ?
F9" C22 1.326(7) . ?
F10 C26 1.329(3) . ?
F11 C26 1.328(3) . ?
F12 C26 1.325(3) . ?
O1 Dy1 2.2899(15) 3_656 ?
O1 C2 1.350(3) . ?
O2 C18 1.255(3) . ?
O3 C20 1.247(3) . ?
O4 C23 1.253(3) . ?
O5 C25 1.244(3) . ?
N1 C1 1.348(3) . ?
N1 C9 1.332(3) . ?
N2 C10 1.286(3) . ?
N2 C11 1.428(3) . ?
C1 C2 1.427(3) . ?
C1 C6 1.428(3) . ?
C2 C3 1.378(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.409(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.357(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.409(3) . ?
C6 C7 1.410(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.366(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.405(3) . ?
C9 C10 1.458(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(3) . ?
C11 C16 1.395(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.376(4) . ?
C14 C15 1.379(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.527(3) . ?
C18 C19 1.385(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.390(3) . ?
C20 C21 1.534(3) . ?
C22 C23 1.536(3) . ?
C23 C24 1.381(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(3) . ?
C25 C26 1.542(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 Dy1 35.48(4) . 3_656 ?
O1 Dy1 Dy1 36.81(4) 3_656 3_656 ?
O1 Dy1 O1 72.29(6) 3_656 . ?
O1 Dy1 O2 104.23(6) 3_656 . ?
O1 Dy1 O3 84.03(6) 3_656 . ?
O1 Dy1 O3 133.68(6) . . ?
O1 Dy1 O4 82.19(6) 3_656 . ?
O1 Dy1 O5 71.87(6) . . ?
O1 Dy1 O5 91.68(6) 3_656 . ?
O1 Dy1 N1 140.19(6) 3_656 . ?
O1 Dy1 N1 68.04(6) . . ?
O1 Dy1 N2 155.40(6) 3_656 . ?
O1 Dy1 N2 132.04(6) . . ?
O2 Dy1 Dy1 90.63(4) . 3_656 ?
O2 Dy1 O1 77.25(6) . . ?
O2 Dy1 O3 70.72(6) . . ?
O2 Dy1 O5 138.85(6) . . ?
O2 Dy1 N1 70.36(7) . . ?
O2 Dy1 N2 81.60(6) . . ?
O3 Dy1 Dy1 111.78(4) . 3_656 ?
O3 Dy1 O5 149.74(6) . . ?
O3 Dy1 N1 126.81(6) . . ?
O3 Dy1 N2 75.30(6) . . ?
O4 Dy1 Dy1 110.38(4) . 3_656 ?
O4 Dy1 O1 133.26(6) . . ?
O4 Dy1 O2 148.28(6) . . ?
O4 Dy1 O3 79.30(6) . . ?
O4 Dy1 O5 70.44(6) . . ?
O4 Dy1 N1 123.78(7) . . ?
O4 Dy1 N2 81.00(6) . . ?
O5 Dy1 Dy1 79.76(4) . 3_656 ?
O5 Dy1 N1 73.21(6) . . ?
O5 Dy1 N2 99.43(6) . . ?
N1 Dy1 Dy1 103.47(5) . 3_656 ?
N1 Dy1 N2 64.39(6) . . ?
N2 Dy1 Dy1 167.21(4) . 3_656 ?
Dy1 O1 Dy1 107.71(6) 3_656 . ?
C2 O1 Dy1 119.33(13) . . ?
C2 O1 Dy1 132.73(14) . 3_656 ?
C18 O2 Dy1 133.66(16) . . ?
C20 O3 Dy1 135.15(15) . . ?
C23 O4 Dy1 133.66(15) . . ?
C25 O5 Dy1 133.06(15) . . ?
C1 N1 Dy1 117.02(15) . . ?
C9 N1 Dy1 123.09(15) . . ?
C9 N1 C1 119.8(2) . . ?
C10 N2 Dy1 116.22(16) . . ?
C10 N2 C11 118.0(2) . . ?
C11 N2 Dy1 124.76(14) . . ?
N1 C1 C2 117.7(2) . . ?
N1 C1 C6 121.5(2) . . ?
C2 C1 C6 120.8(2) . . ?
O1 C2 C1 117.9(2) . . ?
O1 C2 C3 124.5(2) . . ?
C3 C2 C1 117.6(2) . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.1(2) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 118.9 . . ?
C5 C4 C3 122.1(2) . . ?
C5 C4 H4 118.9 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.3(2) . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 119.1(2) . . ?
C5 C6 C7 123.9(2) . . ?
C7 C6 C1 117.0(2) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.5(2) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.8(2) . . ?
C9 C8 H8 120.6 . . ?
N1 C9 C8 122.4(2) . . ?
N1 C9 C10 115.9(2) . . ?
C8 C9 C10 121.6(2) . . ?
N2 C10 C9 120.3(2) . . ?
N2 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 N2 121.0(2) . . ?
C12 C11 C16 119.6(2) . . ?
C16 C11 N2 119.1(2) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(2) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.1(3) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 Cl1 119.9(2) . . ?
C13 C14 C15 121.5(2) . . ?
C15 C14 Cl1 118.6(2) . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.6(2) . . ?
C16 C15 H15 120.2 . . ?
C11 C16 H16 120.1 . . ?
C15 C16 C11 119.8(2) . . ?
C15 C16 H16 120.1 . . ?
F1 C17 F2 107.5(2) . . ?
F1 C17 F3 107.9(2) . . ?
F1 C17 C18 112.8(2) . . ?
F2 C17 C18 108.9(2) . . ?
F3 C17 F2 106.5(2) . . ?
F3 C17 C18 113.0(2) . . ?
O2 C18 C17 114.0(2) . . ?
O2 C18 C19 127.7(2) . . ?
C19 C18 C17 118.3(2) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.5(2) . . ?
C20 C19 H19 120.3 . . ?
O3 C20 C19 127.5(2) . . ?
O3 C20 C21 115.9(2) . . ?
C19 C20 C21 116.6(2) . . ?
F4 C21 F6 106.1(2) . . ?
F4 C21 C20 112.6(2) . . ?
F5 C21 F4 107.5(2) . . ?
F5 C21 F6 107.4(2) . . ?
F5 C21 C20 113.0(2) . . ?
F6 C21 C20 109.9(2) . . ?
F7 C22 C23 110.9(4) . . ?
F8 C22 F7 104.1(4) . . ?
F8 C22 C23 112.1(5) . . ?
F9 C22 F7 106.8(4) . . ?
F9 C22 F8 109.6(5) . . ?
F9 C22 C23 112.8(4) . . ?
F7' C22 F8' 108.4(6) . . ?
F7' C22 F9' 107.6(5) . . ?
F7' C22 C23 115.2(6) . . ?
F8' C22 F9' 105.1(5) . . ?
F8' C22 C23 108.7(6) . . ?
F9' C22 C23 111.3(5) . . ?
F7" C22 F8" 108.3(6) . . ?
F7" C22 F9" 107.6(6) . . ?
F7" C22 C23 111.6(7) . . ?
F8" C22 F9" 105.9(6) . . ?
F8" C22 C23 112.5(7) . . ?
F9" C22 C23 110.7(8) . . ?
O4 C23 C22 115.3(2) . . ?
O4 C23 C24 128.0(2) . . ?
C24 C23 C22 116.7(2) . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.3(2) . . ?
C25 C24 H24 120.4 . . ?
O5 C25 C24 127.8(2) . . ?
O5 C25 C26 114.1(2) . . ?
C24 C25 C26 118.0(2) . . ?
F10 C26 C25 110.0(2) . . ?
F11 C26 F10 107.0(2) . . ?
F11 C26 C25 111.4(2) . . ?
F12 C26 F10 108.1(2) . . ?
F12 C26 F11 107.1(2) . . ?
F12 C26 C25 112.9(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C2 C1 -2.0(3) . . . . ?
Dy1 O1 C2 C1 -175.88(15) 3_656 . . . ?
Dy1 O1 C2 C3 5.4(3) 3_656 . . . ?
Dy1 O1 C2 C3 179.20(18) . . . . ?
Dy1 O2 C18 C17 152.79(17) . . . . ?
Dy1 O2 C18 C19 -25.7(4) . . . . ?
Dy1 O3 C20 C19 6.9(4) . . . . ?
Dy1 O3 C20 C21 -175.43(14) . . . . ?
Dy1 O4 C23 C22 -162.74(14) . . . . ?
Dy1 O4 C23 C24 19.4(4) . . . . ?
Dy1 O5 C25 C24 -19.5(4) . . . . ?
Dy1 O5 C25 C26 164.24(16) . . . . ?
Dy1 N1 C1 C2 -0.3(3) . . . . ?
Dy1 N1 C1 C6 178.69(17) . . . . ?
Dy1 N1 C9 C8 -178.99(18) . . . . ?
Dy1 N1 C9 C10 -3.3(3) . . . . ?
Dy1 N2 C10 C9 -0.6(3) . . . . ?
Dy1 N2 C11 C12 -121.5(2) . . . . ?
Dy1 N2 C11 C16 52.5(3) . . . . ?
Cl1 C14 C15 C16 176.37(19) . . . . ?
F1 C17 C18 O2 42.3(3) . . . . ?
F1 C17 C18 C19 -139.1(2) . . . . ?
F2 C17 C18 O2 -76.9(3) . . . . ?
F2 C17 C18 C19 101.7(3) . . . . ?
F3 C17 C18 O2 164.9(2) . . . . ?
F3 C17 C18 C19 -16.4(4) . . . . ?
F7 C22 C23 O4 -0.1(5) . . . . ?
F7 C22 C23 C24 178.0(4) . . . . ?
F8 C22 C23 O4 -116.0(4) . . . . ?
F8 C22 C23 C24 62.1(4) . . . . ?
F9 C22 C23 O4 119.6(5) . . . . ?
F9 C22 C23 C24 -62.3(6) . . . . ?
F7' C22 C23 O4 28.9(7) . . . . ?
F7' C22 C23 C24 -152.9(7) . . . . ?
F8' C22 C23 O4 -93.0(6) . . . . ?
F8' C22 C23 C24 85.2(6) . . . . ?
F9' C22 C23 O4 151.7(6) . . . . ?
F9' C22 C23 C24 -30.1(6) . . . . ?
F7" C22 C23 O4 -43.6(13) . . . . ?
F7" C22 C23 C24 134.5(13) . . . . ?
F8" C22 C23 O4 -165.6(12) . . . . ?
F8" C22 C23 C24 12.6(12) . . . . ?
F9" C22 C23 O4 76.1(11) . . . . ?
F9" C22 C23 C24 -105.7(11) . . . . ?
O1 C2 C3 C4 177.6(2) . . . . ?
O2 C18 C19 C20 1.5(4) . . . . ?
O3 C20 C21 F4 139.0(2) . . . . ?
O3 C20 C21 F5 16.9(3) . . . . ?
O3 C20 C21 F6 -103.0(2) . . . . ?
O4 C23 C24 C25 5.2(4) . . . . ?
O5 C25 C26 F10 81.7(3) . . . . ?
O5 C25 C26 F11 -36.8(3) . . . . ?
O5 C25 C26 F12 -157.4(2) . . . . ?
N1 C1 C2 O1 1.5(3) . . . . ?
N1 C1 C2 C3 -179.6(2) . . . . ?
N1 C1 C6 C5 -179.9(2) . . . . ?
N1 C1 C6 C7 0.0(4) . . . . ?
N1 C9 C10 N2 2.5(3) . . . . ?
N2 C11 C12 C13 173.3(2) . . . . ?
N2 C11 C16 C15 -174.5(2) . . . . ?
C1 N1 C9 C8 -2.7(4) . . . . ?
C1 N1 C9 C10 173.0(2) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C1 C6 C7 C8 -1.7(4) . . . . ?
C2 C1 C6 C5 -0.9(4) . . . . ?
C2 C1 C6 C7 178.9(2) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C3 C4 C5 C6 -0.1(4) . . . . ?
C4 C5 C6 C1 0.2(4) . . . . ?
C4 C5 C6 C7 -179.6(3) . . . . ?
C5 C6 C7 C8 178.1(3) . . . . ?
C6 C1 C2 O1 -177.5(2) . . . . ?
C6 C1 C2 C3 1.4(3) . . . . ?
C6 C7 C8 C9 1.3(4) . . . . ?
C7 C8 C9 N1 1.0(4) . . . . ?
C7 C8 C9 C10 -174.4(2) . . . . ?
C8 C9 C10 N2 178.2(2) . . . . ?
C9 N1 C1 C2 -176.8(2) . . . . ?
C9 N1 C1 C6 2.2(3) . . . . ?
C10 N2 C11 C12 46.3(3) . . . . ?
C10 N2 C11 C16 -139.7(2) . . . . ?
C11 N2 C10 C9 -169.5(2) . . . . ?
C11 C12 C13 C14 0.7(4) . . . . ?
C12 C11 C16 C15 -0.4(4) . . . . ?
C12 C13 C14 Cl1 -177.4(2) . . . . ?
C12 C13 C14 C15 0.3(4) . . . . ?
C13 C14 C15 C16 -1.3(4) . . . . ?
C14 C15 C16 C11 1.4(4) . . . . ?
C16 C11 C12 C13 -0.7(4) . . . . ?
C17 C18 C19 C20 -176.9(2) . . . . ?
C18 C19 C20 O3 7.8(4) . . . . ?
C18 C19 C20 C21 -169.8(2) . . . . ?
C19 C20 C21 F4 -43.1(3) . . . . ?
C19 C20 C21 F5 -165.2(2) . . . . ?
C19 C20 C21 F6 74.9(3) . . . . ?
C22 C23 C24 C25 -172.6(2) . . . . ?
C23 C24 C25 O5 -4.9(4) . . . . ?
C23 C24 C25 C26 171.2(2) . . . . ?
C24 C25 C26 F10 -95.0(3) . . . . ?
C24 C25 C26 F11 146.5(2) . . . . ?
C24 C25 C26 F12 25.9(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1427267'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C52 H24 Cl2 Er2 F24 N4 O10'
_chemical_formula_sum            'C52 H24 Cl2 Er2 F24 N4 O10'
_chemical_formula_weight         1726.17
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.393(2)
_cell_length_b                   19.181(4)
_cell_length_c                   13.054(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.10(3)
_cell_angle_gamma                90
_cell_volume                     2841.6(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8303
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8864
_cell_measurement_theta_min      1.8922
_shelx_estimated_absorpt_T_max   0.742
_shelx_estimated_absorpt_T_min   0.599
_exptl_absorpt_coefficient_mu    3.168
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.887
_diffrn_reflns_theta_min         1.892
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1288
	          2theta: -29.8619
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1288
	          2theta: -29.8619
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1288
	          2theta: -29.8619
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             6982
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0839
_diffrn_orient_matrix_UB_12      0.0055
_diffrn_orient_matrix_UB_13      -0.0264
_diffrn_orient_matrix_UB_21      -0.0085
_diffrn_orient_matrix_UB_22      0.0377
_diffrn_orient_matrix_UB_23      0.0349
_diffrn_orient_matrix_UB_31      0.0133
_diffrn_orient_matrix_UB_32      0.0530
_diffrn_orient_matrix_UB_33      -0.0541
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5983
_reflns_number_total             6769
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.671
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     217
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0289
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0294P)²+1.6726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F7-C22 \\sim F8-C22 \\sim F9-C22 \\sim F8'-C22 \\sim F9'-C22 \\sim F7'-C22
\\sim F7"-C22 \\sim F8"-C22 ~
 F9"-C22
 with sigma of 0.02
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F8'-F9' \\sim F8'-F7' \\sim F9'-F7' \\sim
F7"-F8" \\sim F7"-F9" \\sim F8"-
 F9"
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7' \\sim F8' \\sim F9' \\sim F7" \\sim F8" \\sim
F9": within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F8') \\sim
Ueq, Uanis(F9') \\sim Ueq, Uanis(F7') \\sim Ueq, Uanis(F7") \\sim Ueq,
Uanis(F8") \\sim Ueq, Uanis(F9") \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.05
4. Others
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7')+Sof(F8')+Sof(F9')]+1*[Sof(F7")+
 Sof(F8")+Sof(F9")]=1 with esd of 0.0001
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=FVAR(2)
 Sof(F7")=Sof(F8")=Sof(F9")=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.45779(2) 0.09234(2) 0.46879(2) 0.01552(5) Uani 1 1 d . . . . .
Cl1 Cl 0.66537(8) 0.46492(4) 0.40233(8) 0.0421(2) Uani 1 1 d . . . . .
F1 F 0.4205(3) 0.12264(14) 0.84329(17) 0.0617(7) Uani 1 1 d . . . . .
F2 F 0.3343(2) 0.21024(17) 0.76987(18) 0.0683(8) Uani 1 1 d . . . . .
F3 F 0.49698(19) 0.22366(13) 0.86219(15) 0.0494(6) Uani 1 1 d . . . . .
F4 F 0.74180(19) 0.31855(11) 0.6076(2) 0.0560(7) Uani 1 1 d . . . . .
F5 F 0.7843(2) 0.25671(15) 0.48085(16) 0.0599(7) Uani 1 1 d . . . . .
F6 F 0.84564(16) 0.22715(12) 0.63330(17) 0.0432(5) Uani 1 1 d . . . . .
F10 F 0.15539(18) -0.00582(13) 0.17329(17) 0.0490(6) Uani 1 1 d . . . . .
F11 F 0.22341(19) -0.08301(11) 0.28145(16) 0.0402(5) Uani 1 1 d . . . . .
F12 F 0.2906(2) -0.07751(13) 0.13354(18) 0.0530(6) Uani 1 1 d . . . . .
O1 O 0.39670(16) -0.01208(10) 0.54110(14) 0.0177(4) Uani 1 1 d . . . . .
O2 O 0.46270(18) 0.11866(11) 0.64373(14) 0.0221(4) Uani 1 1 d . . . . .
O3 O 0.61520(17) 0.16878(10) 0.51200(14) 0.0201(4) Uani 1 1 d . . . . .
O4 O 0.51104(18) 0.12271(11) 0.30683(15) 0.0211(4) Uani 1 1 d . . . . .
O5 O 0.33352(17) 0.03357(11) 0.34282(14) 0.0229(4) Uani 1 1 d . . . . .
N1 N 0.2589(2) 0.10181(12) 0.51857(18) 0.0190(5) Uani 1 1 d . . . . .
N2 N 0.3658(2) 0.21612(13) 0.45184(17) 0.0209(5) Uani 1 1 d . . . . .
C1 C 0.2133(2) 0.04433(15) 0.5605(2) 0.0187(6) Uani 1 1 d . . . . .
C2 C 0.2857(2) -0.01655(15) 0.5711(2) 0.0197(6) Uani 1 1 d . . . . .
C3 C 0.2389(3) -0.07488(16) 0.6141(2) 0.0222(6) Uani 1 1 d . . . . .
H3 H 0.2846 -0.1163 0.6212 0.027 Uiso 1 1 calc R . . . .
C4 C 0.1243(3) -0.07430(17) 0.6478(2) 0.0256(7) Uani 1 1 d . . . . .
H4 H 0.0950 -0.1153 0.6776 0.031 Uiso 1 1 calc R . . . .
C5 C 0.0545(3) -0.01617(17) 0.6385(2) 0.0271(7) Uani 1 1 d . . . . .
H5 H -0.0223 -0.0169 0.6615 0.033 Uiso 1 1 calc R . . . .
C6 C 0.0976(2) 0.04476(16) 0.5947(2) 0.0215(6) Uani 1 1 d . . . . .
C7 C 0.0331(3) 0.10738(17) 0.5831(3) 0.0271(7) Uani 1 1 d . . . . .
H7 H -0.0447 0.1095 0.6038 0.033 Uiso 1 1 calc R . . . .
C8 C 0.0821(3) 0.16539(17) 0.5421(2) 0.0268(7) Uani 1 1 d . . . . .
H8 H 0.0391 0.2078 0.5346 0.032 Uiso 1 1 calc R . . . .
C9 C 0.1970(3) 0.16076(15) 0.5114(2) 0.0208(6) Uani 1 1 d . . . . .
C10 C 0.2596(3) 0.22202(16) 0.4769(2) 0.0225(6) Uani 1 1 d . . . . .
H10 H 0.2217 0.2662 0.4729 0.027 Uiso 1 1 calc R . . . .
C11 C 0.4293(2) 0.27918(15) 0.4359(2) 0.0208(6) Uani 1 1 d . . . . .
C12 C 0.4300(3) 0.33387(16) 0.5063(2) 0.0263(6) Uani 1 1 d . . . . .
H12 H 0.3819 0.3314 0.5620 0.032 Uiso 1 1 calc R . . . .
C13 C 0.5009(3) 0.39205(17) 0.4952(3) 0.0302(7) Uani 1 1 d . . . . .
H13 H 0.5012 0.4295 0.5428 0.036 Uiso 1 1 calc R . . . .
C14 C 0.5710(3) 0.39445(16) 0.4139(3) 0.0281(7) Uani 1 1 d . . . . .
C15 C 0.5700(3) 0.34142(17) 0.3430(2) 0.0291(7) Uani 1 1 d . . . . .
H15 H 0.6169 0.3447 0.2866 0.035 Uiso 1 1 calc R . . . .
C16 C 0.5000(3) 0.28279(17) 0.3541(2) 0.0275(7) Uani 1 1 d . . . . .
H16 H 0.5005 0.2455 0.3062 0.033 Uiso 1 1 calc R . . . .
C17 C 0.4385(3) 0.18079(19) 0.7948(2) 0.0318(7) Uani 1 1 d . . . . .
C18 C 0.5012(2) 0.16972(16) 0.6974(2) 0.0206(6) Uani 1 1 d . . . . .
C19 C 0.5898(3) 0.21610(16) 0.6765(2) 0.0235(6) Uani 1 1 d . . . . .
H19 H 0.6129 0.2523 0.7237 0.028 Uiso 1 1 calc R . . . .
C20 C 0.6444(2) 0.20894(15) 0.5856(2) 0.0198(6) Uani 1 1 d . . . . .
C21 C 0.7545(3) 0.25367(16) 0.5752(2) 0.0244(6) Uani 1 1 d . . . . .
C22 C 0.5809(3) 0.12241(16) 0.1411(2) 0.0279(7) Uani 1 1 d D . . . .
C23 C 0.5024(3) 0.09249(16) 0.2206(2) 0.0220(6) Uani 1 1 d . . . . .
C24 C 0.4294(3) 0.03809(18) 0.1885(2) 0.0276(7) Uani 1 1 d . . . . .
H24 H 0.4356 0.0170 0.1234 0.033 Uiso 1 1 calc R . . . .
C25 C 0.3458(3) 0.01408(16) 0.2530(2) 0.0227(6) Uani 1 1 d . . . . .
C26 C 0.2538(3) -0.03892(19) 0.2094(2) 0.0315(7) Uani 1 1 d . . . . .
F7 F 0.6668(9) 0.1635(6) 0.1802(10) 0.054(4) Uani 0.502(3) 1 d D U P A 1
F8 F 0.5159(10) 0.1616(6) 0.0734(8) 0.035(2) Uani 0.502(3) 1 d D U P A 1
F9 F 0.6260(9) 0.0728(5) 0.0866(9) 0.057(3) Uani 0.502(3) 1 d D U P A 1
F7' F 0.6955(11) 0.1180(15) 0.1704(16) 0.051(5) Uani 0.151(3) 1 d D U P A 2
F8' F 0.552(2) 0.1856(7) 0.1194(18) 0.054(5) Uani 0.151(3) 1 d D U P A 2
F9' F 0.568(2) 0.0852(11) 0.0523(12) 0.041(5) Uani 0.151(3) 1 d D U P A 2
F7" F 0.6348(14) 0.1823(7) 0.1779(16) 0.043(4) Uani 0.347(3) 1 d D U P A 3
F8" F 0.5236(17) 0.1407(8) 0.0549(11) 0.052(5) Uani 0.347(3) 1 d D U P A 3
F9" F 0.6684(12) 0.0805(7) 0.1248(14) 0.060(5) Uani 0.347(3) 1 d D U P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 Er1 3.7413(7) 3_656 ?
Er1 O1 2.3460(19) . ?
Er1 O1 2.2744(18) 3_656 ?
Er1 O2 2.3346(19) . ?
Er1 O3 2.346(2) . ?
Er1 O4 2.3250(19) . ?
Er1 O5 2.359(2) . ?
Er1 N1 2.419(2) . ?
Er1 N2 2.597(2) . ?
Cl1 C14 1.742(3) . ?
F1 C17 1.308(4) . ?
F2 C17 1.329(4) . ?
F3 C17 1.338(4) . ?
F4 C21 1.326(4) . ?
F5 C21 1.308(4) . ?
F6 C21 1.331(4) . ?
F10 C26 1.337(4) . ?
F11 C26 1.333(4) . ?
F12 C26 1.334(4) . ?
O1 Er1 2.2743(18) 3_656 ?
O1 C2 1.359(3) . ?
O2 C18 1.260(3) . ?
O3 C20 1.253(3) . ?
O4 C23 1.262(4) . ?
O5 C25 1.251(3) . ?
N1 C1 1.355(4) . ?
N1 C9 1.332(4) . ?
N2 C10 1.285(4) . ?
N2 C11 1.434(4) . ?
C1 C2 1.430(4) . ?
C1 C6 1.428(4) . ?
C2 C3 1.380(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.415(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.409(4) . ?
C6 C7 1.410(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.375(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.405(4) . ?
C9 C10 1.467(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(4) . ?
C11 C16 1.395(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(5) . ?
C14 C15 1.375(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.393(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.528(4) . ?
C18 C19 1.391(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.395(4) . ?
C20 C21 1.535(4) . ?
C22 C23 1.540(4) . ?
C22 F7 1.323(8) . ?
C22 F8 1.334(7) . ?
C22 F9 1.320(7) . ?
C22 F7' 1.331(11) . ?
C22 F8' 1.282(11) . ?
C22 F9' 1.358(10) . ?
C22 F7" 1.369(10) . ?
C22 F8" 1.298(11) . ?
C22 F9" 1.312(10) . ?
C23 C24 1.376(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.403(4) . ?
C25 C26 1.533(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Er1 Er1 35.29(4) . 3_656 ?
O1 Er1 Er1 36.58(5) 3_656 3_656 ?
O1 Er1 O1 71.87(7) 3_656 . ?
O1 Er1 O2 104.34(7) 3_656 . ?
O1 Er1 O3 83.76(7) 3_656 . ?
O1 Er1 O3 133.20(7) . . ?
O1 Er1 O4 82.39(7) 3_656 . ?
O1 Er1 O5 72.02(7) . . ?
O1 Er1 O5 91.85(7) 3_656 . ?
O1 Er1 N1 140.45(7) 3_656 . ?
O1 Er1 N1 68.75(7) . . ?
O1 Er1 N2 154.79(7) 3_656 . ?
O1 Er1 N2 133.07(7) . . ?
O2 Er1 Er1 90.48(5) . 3_656 ?
O2 Er1 O1 76.89(7) . . ?
O2 Er1 O3 71.24(7) . . ?
O2 Er1 O5 138.24(7) . . ?
O2 Er1 N1 70.28(8) . . ?
O2 Er1 N2 81.95(7) . . ?
O3 Er1 Er1 111.29(5) . 3_656 ?
O3 Er1 O5 149.86(7) . . ?
O3 Er1 N1 127.06(7) . . ?
O3 Er1 N2 75.13(7) . . ?
O4 Er1 Er1 110.64(5) . 3_656 ?
O4 Er1 O1 133.67(7) . . ?
O4 Er1 O2 148.19(7) . . ?
O4 Er1 O3 78.84(7) . . ?
O4 Er1 O5 71.02(7) . . ?
O4 Er1 N1 123.49(8) . . ?
O4 Er1 N2 80.18(7) . . ?
O5 Er1 Er1 79.99(5) . 3_656 ?
O5 Er1 N1 72.83(7) . . ?
O5 Er1 N2 99.48(8) . . ?
N1 Er1 Er1 103.97(6) . 3_656 ?
N1 Er1 N2 64.75(8) . . ?
N2 Er1 Er1 168.01(5) . 3_656 ?
Er1 O1 Er1 108.13(7) 3_656 . ?
C2 O1 Er1 119.11(17) . . ?
C2 O1 Er1 132.47(17) . 3_656 ?
C18 O2 Er1 133.55(18) . . ?
C20 O3 Er1 135.55(18) . . ?
C23 O4 Er1 133.62(19) . . ?
C25 O5 Er1 133.32(19) . . ?
C1 N1 Er1 116.74(18) . . ?
C9 N1 Er1 123.26(19) . . ?
C9 N1 C1 119.9(2) . . ?
C10 N2 Er1 116.1(2) . . ?
C10 N2 C11 117.5(3) . . ?
C11 N2 Er1 125.32(17) . . ?
N1 C1 C2 117.7(2) . . ?
N1 C1 C6 121.3(3) . . ?
C6 C1 C2 121.0(3) . . ?
O1 C2 C1 117.7(2) . . ?
O1 C2 C3 124.8(3) . . ?
C3 C2 C1 117.4(3) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.4(3) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.6(3) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.4(3) . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 123.6(3) . . ?
C7 C6 C1 117.3(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.3(3) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.7(3) . . ?
C9 C8 H8 120.6 . . ?
N1 C9 C8 122.4(3) . . ?
N1 C9 C10 115.6(3) . . ?
C8 C9 C10 121.9(3) . . ?
N2 C10 C9 120.1(3) . . ?
N2 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 N2 120.8(3) . . ?
C12 C11 C16 119.8(3) . . ?
C16 C11 N2 119.1(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.0(3) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 Cl1 119.7(3) . . ?
C15 C14 Cl1 118.9(3) . . ?
C15 C14 C13 121.4(3) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(3) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 120.2 . . ?
C15 C16 C11 119.6(3) . . ?
C15 C16 H16 120.2 . . ?
F1 C17 F2 107.8(3) . . ?
F1 C17 F3 107.3(3) . . ?
F1 C17 C18 112.9(3) . . ?
F2 C17 F3 106.4(3) . . ?
F2 C17 C18 109.2(3) . . ?
F3 C17 C18 113.0(3) . . ?
O2 C18 C17 113.9(3) . . ?
O2 C18 C19 127.6(3) . . ?
C19 C18 C17 118.4(3) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
O3 C20 C19 127.2(3) . . ?
O3 C20 C21 116.1(2) . . ?
C19 C20 C21 116.7(3) . . ?
F4 C21 F6 106.2(3) . . ?
F4 C21 C20 112.6(2) . . ?
F5 C21 F4 107.6(3) . . ?
F5 C21 F6 107.4(3) . . ?
F5 C21 C20 113.0(3) . . ?
F6 C21 C20 109.8(2) . . ?
F7 C22 C23 114.5(7) . . ?
F7 C22 F8 105.6(7) . . ?
F8 C22 C23 109.6(6) . . ?
F9 C22 C23 111.8(5) . . ?
F9 C22 F7 109.1(6) . . ?
F9 C22 F8 105.7(6) . . ?
F7' C22 C23 113.4(9) . . ?
F7' C22 F9' 103.8(9) . . ?
F8' C22 C23 110.2(8) . . ?
F8' C22 F7' 110.8(10) . . ?
F8' C22 F9' 107.6(10) . . ?
F9' C22 C23 110.8(8) . . ?
F7" C22 C23 110.2(9) . . ?
F8" C22 C23 114.0(11) . . ?
F8" C22 F7" 104.6(9) . . ?
F8" C22 F9" 110.9(9) . . ?
F9" C22 C23 112.1(8) . . ?
F9" C22 F7" 104.3(8) . . ?
O4 C23 C22 115.2(3) . . ?
O4 C23 C24 128.1(3) . . ?
C24 C23 C22 116.7(3) . . ?
C23 C24 H24 120.3 . . ?
C23 C24 C25 119.4(3) . . ?
C25 C24 H24 120.3 . . ?
O5 C25 C24 127.1(3) . . ?
O5 C25 C26 114.6(3) . . ?
C24 C25 C26 118.3(3) . . ?
F10 C26 C25 109.9(3) . . ?
F11 C26 F10 106.8(3) . . ?
F11 C26 F12 106.9(3) . . ?
F11 C26 C25 111.8(2) . . ?
F12 C26 F10 108.1(3) . . ?
F12 C26 C25 113.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O1 C2 C1 -2.5(3) . . . . ?
Er1 O1 C2 C1 -175.50(17) 3_656 . . . ?
Er1 O1 C2 C3 179.7(2) . . . . ?
Er1 O1 C2 C3 6.7(4) 3_656 . . . ?
Er1 O2 C18 C17 153.4(2) . . . . ?
Er1 O2 C18 C19 -25.1(5) . . . . ?
Er1 O3 C20 C19 6.1(5) . . . . ?
Er1 O3 C20 C21 -175.65(18) . . . . ?
Er1 O4 C23 C22 -163.06(18) . . . . ?
Er1 O4 C23 C24 19.1(5) . . . . ?
Er1 O5 C25 C24 -18.7(5) . . . . ?
Er1 O5 C25 C26 164.8(2) . . . . ?
Er1 N1 C1 C2 -0.3(3) . . . . ?
Er1 N1 C1 C6 178.6(2) . . . . ?
Er1 N1 C9 C8 -179.1(2) . . . . ?
Er1 N1 C9 C10 -3.6(3) . . . . ?
Er1 N2 C10 C9 -0.7(3) . . . . ?
Er1 N2 C11 C12 -120.6(3) . . . . ?
Er1 N2 C11 C16 53.2(3) . . . . ?
Cl1 C14 C15 C16 176.5(2) . . . . ?
F1 C17 C18 O2 43.2(4) . . . . ?
F1 C17 C18 C19 -138.1(3) . . . . ?
F2 C17 C18 O2 -76.7(4) . . . . ?
F2 C17 C18 C19 101.9(3) . . . . ?
F3 C17 C18 O2 165.2(3) . . . . ?
F3 C17 C18 C19 -16.2(4) . . . . ?
O1 C2 C3 C4 177.0(3) . . . . ?
O2 C18 C19 C20 1.4(5) . . . . ?
O3 C20 C21 F4 138.7(3) . . . . ?
O3 C20 C21 F5 16.6(4) . . . . ?
O3 C20 C21 F6 -103.2(3) . . . . ?
O4 C23 C24 C25 5.4(5) . . . . ?
O5 C25 C26 F10 82.4(3) . . . . ?
O5 C25 C26 F11 -35.9(4) . . . . ?
O5 C25 C26 F12 -156.7(3) . . . . ?
N1 C1 C2 O1 1.9(4) . . . . ?
N1 C1 C2 C3 179.8(3) . . . . ?
N1 C1 C6 C5 -179.5(3) . . . . ?
N1 C1 C6 C7 -0.1(4) . . . . ?
N1 C9 C10 N2 2.7(4) . . . . ?
N2 C11 C12 C13 173.8(3) . . . . ?
N2 C11 C16 C15 -174.5(3) . . . . ?
C1 N1 C9 C8 -2.8(4) . . . . ?
C1 N1 C9 C10 172.7(2) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C1 C6 C7 C8 -1.1(5) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
C2 C1 C6 C7 178.8(3) . . . . ?
C2 C3 C4 C5 0.5(5) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C4 C5 C6 C1 0.2(4) . . . . ?
C4 C5 C6 C7 -179.1(3) . . . . ?
C5 C6 C7 C8 178.2(3) . . . . ?
C6 C1 C2 O1 -177.1(2) . . . . ?
C6 C1 C2 C3 0.9(4) . . . . ?
C6 C7 C8 C9 0.4(5) . . . . ?
C7 C8 C9 N1 1.5(5) . . . . ?
C7 C8 C9 C10 -173.7(3) . . . . ?
C8 C9 C10 N2 178.3(3) . . . . ?
C9 N1 C1 C2 -176.9(3) . . . . ?
C9 N1 C1 C6 2.0(4) . . . . ?
C10 N2 C11 C12 47.0(4) . . . . ?
C10 N2 C11 C16 -139.1(3) . . . . ?
C11 N2 C10 C9 -169.5(2) . . . . ?
C11 C12 C13 C14 -0.4(5) . . . . ?
C12 C11 C16 C15 -0.6(4) . . . . ?
C12 C13 C14 Cl1 -177.0(3) . . . . ?
C12 C13 C14 C15 1.4(5) . . . . ?
C13 C14 C15 C16 -1.9(5) . . . . ?
C14 C15 C16 C11 1.5(5) . . . . ?
C16 C11 C12 C13 0.0(5) . . . . ?
C17 C18 C19 C20 -177.0(3) . . . . ?
C18 C19 C20 O3 8.1(5) . . . . ?
C18 C19 C20 C21 -170.2(3) . . . . ?
C19 C20 C21 F4 -42.8(4) . . . . ?
C19 C20 C21 F5 -165.0(3) . . . . ?
C19 C20 C21 F6 75.2(3) . . . . ?
C22 C23 C24 C25 -172.4(3) . . . . ?
C23 C24 C25 O5 -5.3(5) . . . . ?
C23 C24 C25 C26 171.1(3) . . . . ?
C24 C25 C26 F10 -94.4(3) . . . . ?
C24 C25 C26 F11 147.2(3) . . . . ?
C24 C25 C26 F12 26.5(4) . . . . ?
F7 C22 C23 O4 15.9(7) . . . . ?
F7 C22 C23 C24 -166.0(7) . . . . ?
F8 C22 C23 O4 -102.5(6) . . . . ?
F8 C22 C23 C24 75.6(6) . . . . ?
F9 C22 C23 O4 140.7(6) . . . . ?
F9 C22 C23 C24 -41.2(7) . . . . ?
F7' C22 C23 O4 61.8(14) . . . . ?
F7' C22 C23 C24 -120.1(14) . . . . ?
F8' C22 C23 O4 -63.0(14) . . . . ?
F8' C22 C23 C24 115.1(14) . . . . ?
F9' C22 C23 O4 178.1(13) . . . . ?
F9' C22 C23 C24 -3.8(13) . . . . ?
F7" C22 C23 O4 -7.3(8) . . . . ?
F7" C22 C23 C24 170.8(8) . . . . ?
F8" C22 C23 O4 -124.5(8) . . . . ?
F8" C22 C23 C24 53.6(8) . . . . ?
F9" C22 C23 O4 108.4(9) . . . . ?
F9" C22 C23 C24 -73.5(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1427268'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C52 H24 Cl2 F24 Gd2 N4 O10'
_chemical_formula_sum            'C52 H24 Cl2 F24 Gd2 N4 O10'
_chemical_formula_weight         1706.15
_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'
Cl Cl 0.1484 0.1585 '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      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                   11.348(2)
_cell_length_b                   19.320(4)
_cell_length_c                   13.115(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.21(3)
_cell_angle_gamma                90
_cell_volume                     2863.6(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8987
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9103
_cell_measurement_theta_min      1.8821
_shelx_estimated_absorpt_T_max   0.786
_shelx_estimated_absorpt_T_min   0.632
_exptl_absorpt_coefficient_mu    2.529
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25700
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.928
_diffrn_reflns_theta_min         1.882
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0982
	          2theta: -19.8909
scan:
	Number of images: 140
	           Slice: -110.0000 - 30.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0982
	          2theta: -19.8909
scan:
	Number of images: 70
	           Slice: -110.0000 - -40.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0982
	          2theta: -19.8909
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             7040
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0213
_diffrn_orient_matrix_UB_12      -0.0848
_diffrn_orient_matrix_UB_13      -0.0136
_diffrn_orient_matrix_UB_21      0.0363
_diffrn_orient_matrix_UB_22      0.0146
_diffrn_orient_matrix_UB_23      -0.0339
_diffrn_orient_matrix_UB_31      0.0528
_diffrn_orient_matrix_UB_32      -0.0029
_diffrn_orient_matrix_UB_33      0.0554
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5667
_reflns_number_total             6827
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         3.665
_refine_diff_density_min         -2.046
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6827
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0468
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0628P)²+0.0106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1176
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-F7 \\sim C22-F8 \\sim C22-F9 \\sim C22-F7' \\sim C22-F8' \\sim C22-F9'
\\sim C22-F7" \\sim C22-F8" ~
 C22-F9"
 with sigma of 0.01
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F7'-F8' \\sim F7'-F9' \\sim F8'-F9' \\sim
F7"-F8" \\sim F7"-F9" \\sim F8"-
 F9"
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F7 \\sim F7" \\sim F8' \\sim F8 \\sim F8" \\sim F9' \\sim F9 \\sim F9" \\sim
F7': within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7') \\sim
Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq, Uanis(F7") \\sim Ueq,
Uanis(F8") \\sim Ueq, Uanis(F9") \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.02
4. Others
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7')+Sof(F8')+Sof(F9')]+1*[Sof(F7")+
 Sof(F8")+Sof(F9")]=1 with esd of 0.0001
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=FVAR(2)
 Sof(F7")=Sof(F8")=Sof(F9")=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
Highest peak    3.66  at  0.6230  0.0940  0.5937  [  1.82 A from O3 ]
Deepest hole   -2.05  at  0.4023  0.0951  0.5012  [  0.81 A from GD1 ]
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.45958(2) 0.09362(2) 0.46861(2) 0.02265(9) Uani 1 1 d . . . . .
Cl1 Cl 0.66361(12) 0.46331(6) 0.40103(12) 0.0515(3) Uani 1 1 d . . . . .
F1 F 0.4201(4) 0.1260(2) 0.8438(2) 0.0703(11) Uani 1 1 d . . . . .
F2 F 0.3352(3) 0.2126(2) 0.7704(3) 0.0773(11) Uani 1 1 d . . . . .
F3 F 0.4976(3) 0.22573(18) 0.8632(2) 0.0614(9) Uani 1 1 d . . . . .
F4 F 0.7413(3) 0.32132(15) 0.6104(3) 0.0684(11) Uani 1 1 d . . . . .
F5 F 0.7874(3) 0.2607(2) 0.4854(2) 0.0681(11) Uani 1 1 d . . . . .
F6 F 0.8480(2) 0.23140(16) 0.6369(2) 0.0520(8) Uani 1 1 d . . . . .
F7 F 0.6484(9) 0.1760(5) 0.1782(8) 0.049(3) Uani 0.447(3) 1 d D U P A 1
F8 F 0.5258(10) 0.1442(6) 0.0566(7) 0.047(3) Uani 0.447(3) 1 d D U P A 1
F9 F 0.6647(10) 0.0757(5) 0.1135(11) 0.073(4) Uani 0.447(3) 1 d D U P A 1
F7' F 0.6841(9) 0.1501(9) 0.1784(10) 0.067(5) Uani 0.351(3) 1 d D U P A 2
F8' F 0.5254(11) 0.1663(6) 0.0817(9) 0.036(3) Uani 0.351(3) 1 d D U P A 2
F9' F 0.6154(12) 0.0707(5) 0.0760(10) 0.048(3) Uani 0.351(3) 1 d D U P A 2
F7" F 0.575(2) 0.1879(4) 0.1317(18) 0.064(5) Uani 0.201(3) 1 d D U P A 3
F8" F 0.5622(18) 0.0931(12) 0.0476(9) 0.054(5) Uani 0.201(3) 1 d D U P A 3
F9" F 0.6989(9) 0.1066(12) 0.1675(14) 0.049(5) Uani 0.201(3) 1 d D U P A 3
F10 F 0.1565(3) -0.00669(17) 0.1720(3) 0.0590(9) Uani 1 1 d . . . . .
F11 F 0.2272(3) -0.08298(15) 0.2789(2) 0.0483(7) Uani 1 1 d . . . . .
F12 F 0.2939(3) -0.07638(18) 0.1320(3) 0.0645(10) Uani 1 1 d . . . . .
O1 O 0.3928(2) -0.01113(14) 0.5406(2) 0.0252(6) Uani 1 1 d . . . . .
O2 O 0.4649(3) 0.12135(16) 0.6460(2) 0.0306(6) Uani 1 1 d . . . . .
O3 O 0.6200(2) 0.17152(14) 0.5145(2) 0.0279(6) Uani 1 1 d . . . . .
O4 O 0.5141(3) 0.12287(15) 0.3031(2) 0.0307(6) Uani 1 1 d . . . . .
O5 O 0.3330(3) 0.03515(15) 0.3391(2) 0.0312(6) Uani 1 1 d . . . . .
N1 N 0.2560(3) 0.10294(17) 0.5201(3) 0.0256(7) Uani 1 1 d . . . . .
N2 N 0.3624(3) 0.21754(17) 0.4535(3) 0.0281(7) Uani 1 1 d . . . . .
C1 C 0.2097(4) 0.0464(2) 0.5611(3) 0.0268(8) Uani 1 1 d . . . . .
C2 C 0.2816(3) -0.0149(2) 0.5705(3) 0.0258(8) Uani 1 1 d . . . . .
C3 C 0.2344(4) -0.0728(2) 0.6113(3) 0.0288(9) Uani 1 1 d . . . . .
H3 H 0.2797 -0.1142 0.6170 0.035 Uiso 1 1 calc R . . . .
C4 C 0.1188(4) -0.0722(3) 0.6453(4) 0.0350(10) Uani 1 1 d . . . . .
H4 H 0.0891 -0.1132 0.6738 0.042 Uiso 1 1 calc R . . . .
C5 C 0.0494(4) -0.0144(2) 0.6380(3) 0.0357(10) Uani 1 1 d . . . . .
H5 H -0.0275 -0.0150 0.6613 0.043 Uiso 1 1 calc R . . . .
C6 C 0.0938(4) 0.0462(2) 0.5953(3) 0.0290(9) Uani 1 1 d . . . . .
C7 C 0.0292(4) 0.1089(2) 0.5852(4) 0.0353(10) Uani 1 1 d . . . . .
H7 H -0.0488 0.1111 0.6058 0.042 Uiso 1 1 calc R . . . .
C8 C 0.0795(4) 0.1666(2) 0.5457(4) 0.0345(10) Uani 1 1 d . . . . .
H8 H 0.0372 0.2090 0.5398 0.041 Uiso 1 1 calc R . . . .
C9 C 0.1943(4) 0.1619(2) 0.5142(3) 0.0288(8) Uani 1 1 d . . . . .
C10 C 0.2575(4) 0.2223(2) 0.4798(3) 0.0288(9) Uani 1 1 d . . . . .
H10 H 0.2194 0.2662 0.4770 0.035 Uiso 1 1 calc R . . . .
C11 C 0.4275(4) 0.2801(2) 0.4377(3) 0.0292(9) Uani 1 1 d . . . . .
C12 C 0.4271(4) 0.3350(2) 0.5056(4) 0.0346(10) Uani 1 1 d . . . . .
H12 H 0.3779 0.3334 0.5604 0.042 Uiso 1 1 calc R . . . .
C13 C 0.4987(5) 0.3927(2) 0.4937(4) 0.0375(10) Uani 1 1 d . . . . .
H13 H 0.4987 0.4305 0.5401 0.045 Uiso 1 1 calc R . . . .
C14 C 0.5690(4) 0.3937(2) 0.4139(4) 0.0375(11) Uani 1 1 d . . . . .
C15 C 0.5692(4) 0.3400(2) 0.3442(4) 0.0364(10) Uani 1 1 d . . . . .
H15 H 0.6172 0.3425 0.2886 0.044 Uiso 1 1 calc R . . . .
C16 C 0.4986(4) 0.2827(2) 0.3563(3) 0.0329(9) Uani 1 1 d . . . . .
H16 H 0.4986 0.2452 0.3093 0.039 Uiso 1 1 calc R . . . .
C17 C 0.4391(4) 0.1835(3) 0.7956(4) 0.0414(11) Uani 1 1 d . . . . .
C18 C 0.5032(4) 0.1722(2) 0.6995(3) 0.0287(9) Uani 1 1 d . . . . .
C19 C 0.5911(4) 0.2182(2) 0.6778(3) 0.0308(9) Uani 1 1 d . . . . .
H19 H 0.6136 0.2544 0.7247 0.037 Uiso 1 1 calc R . . . .
C20 C 0.6466(3) 0.2120(2) 0.5882(3) 0.0265(8) Uani 1 1 d . . . . .
C21 C 0.7568(4) 0.2574(2) 0.5790(4) 0.0329(9) Uani 1 1 d . . . . .
C22 C 0.5862(4) 0.1202(2) 0.1400(3) 0.0354(10) Uani 1 1 d D . . . .
C23 C 0.5060(4) 0.0919(2) 0.2183(3) 0.0296(9) Uani 1 1 d . . . . .
C24 C 0.4321(4) 0.0379(2) 0.1870(3) 0.0356(10) Uani 1 1 d . . . . .
H24 H 0.4384 0.0164 0.1226 0.043 Uiso 1 1 calc R . . . .
C25 C 0.3468(4) 0.0147(2) 0.2511(3) 0.0317(9) Uani 1 1 d . . . . .
C26 C 0.2557(4) -0.0381(3) 0.2069(4) 0.0401(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Gd1 3.8040(8) 3_656 ?
Gd1 O1 2.386(3) . ?
Gd1 O1 2.323(3) 3_656 ?
Gd1 O2 2.383(3) . ?
Gd1 O3 2.396(3) . ?
Gd1 O4 2.378(3) . ?
Gd1 O5 2.404(3) . ?
Gd1 N1 2.471(4) . ?
Gd1 N2 2.636(3) . ?
Cl1 C14 1.738(5) . ?
F1 C17 1.307(6) . ?
F2 C17 1.321(6) . ?
F3 C17 1.336(5) . ?
F4 C21 1.320(5) . ?
F5 C21 1.307(5) . ?
F6 C21 1.325(5) . ?
F7 C22 1.359(6) . ?
F8 C22 1.321(6) . ?
F9 C22 1.308(6) . ?
F7' C22 1.312(7) . ?
F8' C22 1.326(6) . ?
F9' C22 1.334(6) . ?
F7" C22 1.317(7) . ?
F8" C22 1.325(7) . ?
F9" C22 1.324(7) . ?
F10 C26 1.324(6) . ?
F11 C26 1.343(6) . ?
F12 C26 1.333(5) . ?
O1 Gd1 2.323(3) 3_656 ?
O1 C2 1.357(4) . ?
O2 C18 1.262(5) . ?
O3 C20 1.259(5) . ?
O4 C23 1.259(5) . ?
O5 C25 1.243(5) . ?
N1 C1 1.346(5) . ?
N1 C9 1.336(5) . ?
N2 C10 1.272(5) . ?
N2 C11 1.441(5) . ?
C1 C2 1.436(5) . ?
C1 C6 1.428(5) . ?
C2 C3 1.371(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.423(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.364(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.412(6) . ?
C6 C7 1.416(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.374(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.405(6) . ?
C9 C10 1.463(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(6) . ?
C11 C16 1.397(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.395(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.373(7) . ?
C14 C15 1.383(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.527(6) . ?
C18 C19 1.385(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.389(5) . ?
C20 C21 1.540(6) . ?
C22 C23 1.533(6) . ?
C23 C24 1.378(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.411(6) . ?
C25 C26 1.529(6) . ?

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 Gd1 35.57(6) . 3_656 ?
O1 Gd1 Gd1 36.68(7) 3_656 3_656 ?
O1 Gd1 O1 72.25(10) 3_656 . ?
O1 Gd1 O2 104.51(10) 3_656 . ?
O1 Gd1 O3 84.77(10) 3_656 . ?
O1 Gd1 O3 134.02(10) . . ?
O1 Gd1 O4 82.36(10) 3_656 . ?
O1 Gd1 O5 71.94(10) . . ?
O1 Gd1 O5 91.63(10) 3_656 . ?
O1 Gd1 N1 139.50(10) 3_656 . ?
O1 Gd1 N1 67.37(10) . . ?
O1 Gd1 N2 156.62(10) 3_656 . ?
O1 Gd1 N2 130.88(10) . . ?
O2 Gd1 Gd1 91.05(8) . 3_656 ?
O2 Gd1 O1 77.59(10) . . ?
O2 Gd1 O3 70.28(10) . . ?
O2 Gd1 O5 139.09(10) . . ?
O2 Gd1 N1 70.02(11) . . ?
O2 Gd1 N2 80.94(11) . . ?
O3 Gd1 Gd1 112.35(7) . 3_656 ?
O3 Gd1 O5 149.77(9) . . ?
O3 Gd1 N1 126.40(10) . . ?
O3 Gd1 N2 75.62(10) . . ?
O4 Gd1 Gd1 110.23(7) . 3_656 ?
O4 Gd1 O1 132.92(10) . . ?
O4 Gd1 O2 148.43(11) . . ?
O4 Gd1 O3 79.93(10) . . ?
O4 Gd1 O5 69.84(10) . . ?
O4 Gd1 N1 123.98(11) . . ?
O4 Gd1 N2 81.79(10) . . ?
O5 Gd1 Gd1 79.80(7) . 3_656 ?
O5 Gd1 N1 73.37(11) . . ?
O5 Gd1 N2 98.89(10) . . ?
N1 Gd1 Gd1 102.90(8) . 3_656 ?
N1 Gd1 N2 63.85(11) . . ?
N2 Gd1 Gd1 166.20(8) . 3_656 ?
Gd1 O1 Gd1 107.75(10) 3_656 . ?
C2 O1 Gd1 119.8(2) . . ?
C2 O1 Gd1 132.3(2) . 3_656 ?
C18 O2 Gd1 134.0(3) . . ?
C20 O3 Gd1 135.0(3) . . ?
C23 O4 Gd1 133.5(3) . . ?
C25 O5 Gd1 133.4(3) . . ?
C1 N1 Gd1 117.3(3) . . ?
C9 N1 Gd1 123.0(3) . . ?
C9 N1 C1 119.6(4) . . ?
C10 N2 Gd1 116.2(3) . . ?
C10 N2 C11 118.9(4) . . ?
C11 N2 Gd1 123.8(3) . . ?
N1 C1 C2 117.7(4) . . ?
N1 C1 C6 122.1(4) . . ?
C6 C1 C2 120.2(4) . . ?
O1 C2 C1 117.9(3) . . ?
O1 C2 C3 124.3(4) . . ?
C3 C2 C1 117.8(4) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.4(4) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.8(4) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C1 119.9(4) . . ?
C5 C6 C7 123.1(4) . . ?
C7 C6 C1 116.9(4) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(4) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.1(4) . . ?
C9 C8 H8 120.4 . . ?
N1 C9 C8 122.2(4) . . ?
N1 C9 C10 115.4(4) . . ?
C8 C9 C10 122.3(4) . . ?
N2 C10 C9 121.5(4) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C12 C11 N2 121.2(4) . . ?
C12 C11 C16 119.9(4) . . ?
C16 C11 N2 118.7(4) . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.3(4) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(5) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 Cl1 119.5(4) . . ?
C13 C14 C15 121.9(4) . . ?
C15 C14 Cl1 118.6(4) . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.3(4) . . ?
C16 C15 H15 120.3 . . ?
C11 C16 H16 120.1 . . ?
C15 C16 C11 119.8(4) . . ?
C15 C16 H16 120.1 . . ?
F1 C17 F2 107.5(4) . . ?
F1 C17 F3 107.0(4) . . ?
F1 C17 C18 113.0(4) . . ?
F2 C17 F3 106.5(4) . . ?
F2 C17 C18 109.7(4) . . ?
F3 C17 C18 112.9(4) . . ?
O2 C18 C17 113.9(4) . . ?
O2 C18 C19 127.2(4) . . ?
C19 C18 C17 118.9(4) . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
O3 C20 C19 127.5(4) . . ?
O3 C20 C21 115.7(4) . . ?
C19 C20 C21 116.8(4) . . ?
F4 C21 F6 107.1(4) . . ?
F4 C21 C20 112.1(4) . . ?
F5 C21 F4 107.5(4) . . ?
F5 C21 F6 107.3(4) . . ?
F5 C21 C20 112.8(4) . . ?
F6 C21 C20 109.7(4) . . ?
F7 C22 C23 110.9(5) . . ?
F8 C22 F7 103.9(5) . . ?
F8 C22 C23 112.7(7) . . ?
F9 C22 F7 106.0(5) . . ?
F9 C22 F8 109.0(6) . . ?
F9 C22 C23 113.8(6) . . ?
F7' C22 F8' 107.7(6) . . ?
F7' C22 F9' 107.8(6) . . ?
F7' C22 C23 115.7(7) . . ?
F8' C22 F9' 105.3(6) . . ?
F8' C22 C23 108.5(7) . . ?
F9' C22 C23 111.2(6) . . ?
F7" C22 F8" 107.8(7) . . ?
F7" C22 F9" 107.6(7) . . ?
F7" C22 C23 110.6(8) . . ?
F8" C22 C23 112.7(8) . . ?
F9" C22 F8" 106.5(6) . . ?
F9" C22 C23 111.3(8) . . ?
O4 C23 C22 114.9(4) . . ?
O4 C23 C24 128.1(4) . . ?
C24 C23 C22 116.9(4) . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.7(4) . . ?
C25 C24 H24 120.2 . . ?
O5 C25 C24 127.1(4) . . ?
O5 C25 C26 115.2(4) . . ?
C24 C25 C26 117.6(4) . . ?
F10 C26 F11 106.7(4) . . ?
F10 C26 F12 108.8(4) . . ?
F10 C26 C25 110.5(4) . . ?
F11 C26 C25 111.2(4) . . ?
F12 C26 F11 105.9(4) . . ?
F12 C26 C25 113.3(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 C2 C1 -2.5(5) . . . . ?
Gd1 O1 C2 C1 -176.5(2) 3_656 . . . ?
Gd1 O1 C2 C3 5.1(6) 3_656 . . . ?
Gd1 O1 C2 C3 179.1(3) . . . . ?
Gd1 O2 C18 C17 152.9(3) . . . . ?
Gd1 O2 C18 C19 -24.5(7) . . . . ?
Gd1 O3 C20 C19 8.1(6) . . . . ?
Gd1 O3 C20 C21 -174.8(3) . . . . ?
Gd1 O4 C23 C22 -161.9(2) . . . . ?
Gd1 O4 C23 C24 20.4(7) . . . . ?
Gd1 O5 C25 C24 -21.0(7) . . . . ?
Gd1 O5 C25 C26 163.1(3) . . . . ?
Gd1 N1 C1 C2 -0.7(5) . . . . ?
Gd1 N1 C1 C6 178.8(3) . . . . ?
Gd1 N1 C9 C8 -178.7(3) . . . . ?
Gd1 N1 C9 C10 -3.0(5) . . . . ?
Gd1 N2 C10 C9 -1.3(5) . . . . ?
Gd1 N2 C11 C12 -122.8(4) . . . . ?
Gd1 N2 C11 C16 52.6(5) . . . . ?
Cl1 C14 C15 C16 176.9(3) . . . . ?
F1 C17 C18 O2 43.1(6) . . . . ?
F1 C17 C18 C19 -139.3(4) . . . . ?
F2 C17 C18 O2 -76.7(5) . . . . ?
F2 C17 C18 C19 100.9(5) . . . . ?
F3 C17 C18 O2 164.7(4) . . . . ?
F3 C17 C18 C19 -17.7(6) . . . . ?
F7 C22 C23 O4 -2.1(7) . . . . ?
F7 C22 C23 C24 175.9(6) . . . . ?
F8 C22 C23 O4 -118.0(6) . . . . ?
F8 C22 C23 C24 59.9(7) . . . . ?
F9 C22 C23 O4 117.3(8) . . . . ?
F9 C22 C23 C24 -64.7(8) . . . . ?
F7' C22 C23 O4 27.9(10) . . . . ?
F7' C22 C23 C24 -154.2(9) . . . . ?
F8' C22 C23 O4 -93.2(7) . . . . ?
F8' C22 C23 C24 84.7(8) . . . . ?
F9' C22 C23 O4 151.4(7) . . . . ?
F9' C22 C23 C24 -30.7(8) . . . . ?
F7" C22 C23 O4 -49.8(13) . . . . ?
F7" C22 C23 C24 128.2(13) . . . . ?
F8" C22 C23 O4 -170.5(13) . . . . ?
F8" C22 C23 C24 7.4(13) . . . . ?
F9" C22 C23 O4 69.9(12) . . . . ?
F9" C22 C23 C24 -112.2(12) . . . . ?
O1 C2 C3 C4 177.2(4) . . . . ?
O2 C18 C19 C20 1.0(7) . . . . ?
O3 C20 C21 F4 138.9(4) . . . . ?
O3 C20 C21 F5 17.4(5) . . . . ?
O3 C20 C21 F6 -102.2(4) . . . . ?
O4 C23 C24 C25 4.8(7) . . . . ?
O5 C25 C26 F10 79.8(5) . . . . ?
O5 C25 C26 F11 -38.5(6) . . . . ?
O5 C25 C26 F12 -157.7(4) . . . . ?
N1 C1 C2 O1 2.1(5) . . . . ?
N1 C1 C2 C3 -179.4(4) . . . . ?
N1 C1 C6 C5 -179.8(4) . . . . ?
N1 C1 C6 C7 -0.7(6) . . . . ?
N1 C9 C10 N2 2.8(6) . . . . ?
N2 C11 C12 C13 174.5(4) . . . . ?
N2 C11 C16 C15 -174.9(4) . . . . ?
C1 N1 C9 C8 -2.6(6) . . . . ?
C1 N1 C9 C10 173.0(4) . . . . ?
C1 C2 C3 C4 -1.3(6) . . . . ?
C1 C6 C7 C8 -1.1(7) . . . . ?
C2 C1 C6 C5 -0.4(6) . . . . ?
C2 C1 C6 C7 178.8(4) . . . . ?
C2 C3 C4 C5 0.7(7) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
C4 C5 C6 C1 -0.3(7) . . . . ?
C4 C5 C6 C7 -179.4(5) . . . . ?
C5 C6 C7 C8 178.0(5) . . . . ?
C6 C1 C2 O1 -177.4(4) . . . . ?
C6 C1 C2 C3 1.1(6) . . . . ?
C6 C7 C8 C9 1.0(7) . . . . ?
C7 C8 C9 N1 0.9(7) . . . . ?
C7 C8 C9 C10 -174.5(4) . . . . ?
C8 C9 C10 N2 178.5(4) . . . . ?
C9 N1 C1 C2 -177.0(4) . . . . ?
C9 N1 C1 C6 2.5(6) . . . . ?
C10 N2 C11 C12 44.1(6) . . . . ?
C10 N2 C11 C16 -140.5(4) . . . . ?
C11 N2 C10 C9 -169.2(4) . . . . ?
C11 C12 C13 C14 0.0(7) . . . . ?
C12 C11 C16 C15 0.5(6) . . . . ?
C12 C13 C14 Cl1 -177.2(4) . . . . ?
C12 C13 C14 C15 1.2(8) . . . . ?
C13 C14 C15 C16 -1.5(7) . . . . ?
C14 C15 C16 C11 0.7(7) . . . . ?
C16 C11 C12 C13 -0.8(7) . . . . ?
C17 C18 C19 C20 -176.2(4) . . . . ?
C18 C19 C20 O3 7.1(7) . . . . ?
C18 C19 C20 C21 -170.0(4) . . . . ?
C19 C20 C21 F4 -43.7(5) . . . . ?
C19 C20 C21 F5 -165.2(4) . . . . ?
C19 C20 C21 F6 75.2(5) . . . . ?
C22 C23 C24 C25 -172.9(4) . . . . ?
C23 C24 C25 O5 -4.3(7) . . . . ?
C23 C24 C25 C26 171.5(4) . . . . ?
C24 C25 C26 F10 -96.5(5) . . . . ?
C24 C25 C26 F11 145.2(4) . . . . ?
C24 C25 C26 F12 26.0(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r140630f1
_database_code_depnum_ccdc_archive 'CCDC 1427269'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C52 H24 Cl2 F24 Ho2 N4 O10'
_chemical_formula_sum            'C52 H24 Cl2 F24 Ho2 N4 O10'
_chemical_formula_weight         1721.51
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   11.361(2)
_cell_length_b                   19.160(4)
_cell_length_c                   13.035(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.15(3)
_cell_angle_gamma                90
_cell_volume                     2825.9(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8522
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8944
_cell_measurement_theta_min      1.8951
_shelx_estimated_absorpt_T_max   0.714
_shelx_estimated_absorpt_T_min   0.557
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7915
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28448
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.936
_diffrn_reflns_theta_min         1.895
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
scan:
	Number of images: 90
	           Slice: -110.0000 - 70.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9871
	          2theta: -19.9345
scan:
	Number of images: 70
	           Slice: -110.0000 - 30.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9871
	          2theta: -19.9345
scan:
	Number of images: 60
	           Slice: -110.0000 - 10.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9871
	          2theta: -19.9345
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             13298
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0589
_diffrn_orient_matrix_UB_12      -0.0032
_diffrn_orient_matrix_UB_13      -0.0658
_diffrn_orient_matrix_UB_21      -0.0508
_diffrn_orient_matrix_UB_22      0.0470
_diffrn_orient_matrix_UB_23      0.0339
_diffrn_orient_matrix_UB_31      0.0229
_diffrn_orient_matrix_UB_32      0.0411
_diffrn_orient_matrix_UB_33      -0.0226
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5606
_reflns_number_total             6763
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0670
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-F7 \\sim C22-F8 \\sim C22-F9 \\sim C22-F9' \\sim C22-F7' \\sim C22-F8'
\\sim C22-F7" \\sim C22-F8" ~
 C22-F9"
 with sigma of 0.01
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F9'-F7' \\sim F9'-F8' \\sim F7'-F8' \\sim
F7"-F8" \\sim F7"-F9" \\sim F8"-
 F9"
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F8') \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F8") \\sim Ueq, Uanis(F7')
\\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7") \\sim Ueq, Uanis(F9') \\sim Ueq,
Uanis(F9) \\sim Ueq, Uanis(F9") \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 F8', F8, F8", F7', F7, F7", F9', F9, F9"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7')+Sof(F8')+Sof(F9')]+1*[Sof(F7")+
 Sof(F8")+Sof(F9")]=1 with esd of 0.0001
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=FVAR(2)
 Sof(F7")=Sof(F8")=Sof(F9")=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.45807(2) 0.09261(2) 0.46876(2) 0.01462(5) Uani 1 1 d . . . . .
Cl1 Cl 0.66527(8) 0.46452(5) 0.40224(8) 0.0404(2) Uani 1 1 d . . . . .
F1 F 0.4198(3) 0.12361(15) 0.84322(17) 0.0598(8) Uani 1 1 d . . . . .
F2 F 0.3343(2) 0.21123(18) 0.76971(17) 0.0659(9) Uani 1 1 d . . . . .
F3 F 0.49721(19) 0.22428(14) 0.86198(15) 0.0475(6) Uani 1 1 d . . . . .
F4 F 0.74200(19) 0.31923(12) 0.6077(2) 0.0541(7) Uani 1 1 d . . . . .
F5 F 0.7859(2) 0.25724(15) 0.48176(16) 0.0567(8) Uani 1 1 d . . . . .
F6 F 0.84615(16) 0.22804(12) 0.63408(17) 0.0412(5) Uani 1 1 d . . . . .
F10 F 0.15590(18) -0.00632(13) 0.17239(16) 0.0467(6) Uani 1 1 d . . . . .
F11 F 0.2240(2) -0.08312(11) 0.28080(16) 0.0396(5) Uani 1 1 d . . . . .
F12 F 0.2913(2) -0.07736(13) 0.13311(18) 0.0529(7) Uani 1 1 d . . . . .
O1 O 0.39593(16) -0.01196(11) 0.54093(14) 0.0165(4) Uani 1 1 d . . . . .
O2 O 0.46343(18) 0.11927(12) 0.64414(15) 0.0207(5) Uani 1 1 d . . . . .
O3 O 0.61630(18) 0.16937(11) 0.51231(15) 0.0199(5) Uani 1 1 d . . . . .
O4 O 0.51147(18) 0.12273(12) 0.30597(15) 0.0199(5) Uani 1 1 d . . . . .
O5 O 0.33343(18) 0.03391(12) 0.34203(14) 0.0222(5) Uani 1 1 d . . . . .
N1 N 0.2585(2) 0.10205(13) 0.51887(18) 0.0176(5) Uani 1 1 d . . . . .
N2 N 0.3654(2) 0.21654(14) 0.45211(18) 0.0194(5) Uani 1 1 d . . . . .
C1 C 0.2126(2) 0.04486(17) 0.5604(2) 0.0169(6) Uani 1 1 d . . . . .
C2 C 0.2845(2) -0.01626(16) 0.5714(2) 0.0174(6) Uani 1 1 d . . . . .
C3 C 0.2381(3) -0.07458(17) 0.6138(2) 0.0218(7) Uani 1 1 d . . . . .
H3 H 0.2840 -0.1160 0.6208 0.026 Uiso 1 1 calc R . . . .
C4 C 0.1231(3) -0.07387(18) 0.6472(3) 0.0249(7) Uani 1 1 d . . . . .
H4 H 0.0935 -0.1149 0.6767 0.030 Uiso 1 1 calc R . . . .
C5 C 0.0538(3) -0.01606(18) 0.6382(2) 0.0265(7) Uani 1 1 d . . . . .
H5 H -0.0232 -0.0169 0.6611 0.032 Uiso 1 1 calc R . . . .
C6 C 0.0967(3) 0.04508(17) 0.5950(2) 0.0215(7) Uani 1 1 d . . . . .
C7 C 0.0324(3) 0.10790(18) 0.5833(3) 0.0256(7) Uani 1 1 d . . . . .
H7 H -0.0458 0.1099 0.6034 0.031 Uiso 1 1 calc R . . . .
C8 C 0.0812(3) 0.16604(18) 0.5432(2) 0.0242(7) Uani 1 1 d . . . . .
H8 H 0.0385 0.2087 0.5366 0.029 Uiso 1 1 calc R . . . .
C9 C 0.1965(3) 0.16105(17) 0.5121(2) 0.0202(6) Uani 1 1 d . . . . .
C10 C 0.2585(3) 0.22198(17) 0.4777(2) 0.0207(6) Uani 1 1 d . . . . .
H10 H 0.2201 0.2661 0.4739 0.025 Uiso 1 1 calc R . . . .
C11 C 0.4287(3) 0.27944(17) 0.4364(2) 0.0202(6) Uani 1 1 d . . . . .
C12 C 0.4294(3) 0.33428(17) 0.5059(2) 0.0241(7) Uani 1 1 d . . . . .
H12 H 0.3807 0.3323 0.5614 0.029 Uiso 1 1 calc R . . . .
C13 C 0.5005(3) 0.39177(18) 0.4949(3) 0.0283(7) Uani 1 1 d . . . . .
H13 H 0.5010 0.4292 0.5426 0.034 Uiso 1 1 calc R . . . .
C14 C 0.5707(3) 0.39441(17) 0.4138(3) 0.0267(7) Uani 1 1 d . . . . .
C15 C 0.5696(3) 0.34090(18) 0.3430(3) 0.0273(7) Uani 1 1 d . . . . .
H15 H 0.6165 0.3439 0.2864 0.033 Uiso 1 1 calc R . . . .
C16 C 0.4998(3) 0.28280(18) 0.3546(2) 0.0247(7) Uani 1 1 d . . . . .
H16 H 0.5002 0.2453 0.3070 0.030 Uiso 1 1 calc R . . . .
C17 C 0.4384(3) 0.1817(2) 0.7950(2) 0.0307(8) Uani 1 1 d . . . . .
C18 C 0.5018(3) 0.17022(18) 0.6977(2) 0.0206(7) Uani 1 1 d . . . . .
C19 C 0.5895(3) 0.21667(18) 0.6765(2) 0.0231(7) Uani 1 1 d . . . . .
H19 H 0.6117 0.2533 0.7234 0.028 Uiso 1 1 calc R . . . .
C20 C 0.6452(3) 0.20943(17) 0.5860(2) 0.0192(6) Uani 1 1 d . . . . .
C21 C 0.7553(3) 0.25442(17) 0.5756(2) 0.0236(7) Uani 1 1 d . . . . .
C22 C 0.5817(3) 0.12205(16) 0.1404(2) 0.0255(7) Uani 1 1 d D . . . .
C23 C 0.5027(3) 0.09247(17) 0.2201(2) 0.0204(6) Uani 1 1 d . . . . .
C24 C 0.4301(3) 0.03776(18) 0.1888(2) 0.0252(7) Uani 1 1 d . . . . .
H24 H 0.4371 0.0160 0.1242 0.030 Uiso 1 1 calc R . . . .
C25 C 0.3461(3) 0.01431(18) 0.2524(2) 0.0215(7) Uani 1 1 d . . . . .
C26 C 0.2541(3) -0.0394(2) 0.2088(2) 0.0306(8) Uani 1 1 d . . . . .
F7 F 0.6494(5) 0.1758(3) 0.1802(4) 0.0397(14) Uani 0.576(3) 1 d D U P A 1
F8 F 0.5177(6) 0.1495(3) 0.0610(4) 0.0385(17) Uani 0.576(3) 1 d D U P A 1
F9 F 0.6536(6) 0.0755(3) 0.1083(7) 0.060(2) Uani 0.576(3) 1 d D U P A 1
F7' F 0.585(2) 0.1910(4) 0.1412(17) 0.044(5) Uani 0.135(3) 1 d D U P A 2
F8' F 0.5502(16) 0.1015(12) 0.0446(7) 0.039(5) Uani 0.135(3) 1 d D U P A 2
F9' F 0.6930(9) 0.1002(12) 0.1619(14) 0.029(4) Uani 0.135(3) 1 d D U P A 2
F7" F 0.6835(7) 0.1462(7) 0.1796(8) 0.046(3) Uani 0.290(3) 1 d D U P A 3
F8" F 0.5236(10) 0.1719(5) 0.0877(9) 0.033(3) Uani 0.290(3) 1 d D U P A 3
F9" F 0.6041(10) 0.0731(4) 0.0702(8) 0.033(3) Uani 0.290(3) 1 d D U P A 3


_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
Ho1 Ho1 3.7451(7) 3_656 ?
Ho1 O1 2.349(2) . ?
Ho1 O1 2.2788(19) 3_656 ?
Ho1 O2 2.338(2) . ?
Ho1 O3 2.352(2) . ?
Ho1 O4 2.331(2) . ?
Ho1 O5 2.362(2) . ?
Ho1 N1 2.422(2) . ?
Ho1 N2 2.599(3) . ?
Cl1 C14 1.735(3) . ?
F1 C17 1.305(4) . ?
F2 C17 1.326(4) . ?
F3 C17 1.330(4) . ?
F4 C21 1.323(4) . ?
F5 C21 1.303(4) . ?
F6 C21 1.327(4) . ?
F10 C26 1.333(4) . ?
F11 C26 1.325(4) . ?
F12 C26 1.325(4) . ?
O1 Ho1 2.2788(19) 3_656 ?
O1 C2 1.363(3) . ?
O2 C18 1.255(4) . ?
O3 C20 1.250(4) . ?
O4 C23 1.257(4) . ?
O5 C25 1.247(3) . ?
N1 C1 1.348(4) . ?
N1 C9 1.331(4) . ?
N2 C10 1.292(4) . ?
N2 C11 1.427(4) . ?
C1 C2 1.428(4) . ?
C1 C6 1.429(4) . ?
C2 C3 1.373(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.414(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.358(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.406(4) . ?
C6 C7 1.409(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.369(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.408(4) . ?
C9 C10 1.455(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(5) . ?
C11 C16 1.396(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.381(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.381(5) . ?
C14 C15 1.379(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.530(4) . ?
C18 C19 1.382(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.395(4) . ?
C20 C21 1.535(4) . ?
C22 C23 1.541(4) . ?
C22 F7 1.360(5) . ?
C22 F8 1.320(5) . ?
C22 F9 1.303(5) . ?
C22 F7' 1.322(7) . ?
C22 F8' 1.326(7) . ?
C22 F9' 1.338(7) . ?
C22 F7" 1.307(6) . ?
C22 F8" 1.318(6) . ?
C22 F9" 1.350(6) . ?
C23 C24 1.373(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(4) . ?
C25 C26 1.538(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ho1 Ho1 35.35(5) . 3_656 ?
O1 Ho1 Ho1 36.61(5) 3_656 3_656 ?
O1 Ho1 O1 71.96(8) 3_656 . ?
O1 Ho1 O2 104.31(7) 3_656 . ?
O1 Ho1 O3 83.86(7) 3_656 . ?
O1 Ho1 O3 133.42(7) . . ?
O1 Ho1 O4 82.36(7) 3_656 . ?
O1 Ho1 O5 72.00(7) . . ?
O1 Ho1 O5 91.83(7) 3_656 . ?
O1 Ho1 N1 140.29(8) 3_656 . ?
O1 Ho1 N1 68.49(8) . . ?
O1 Ho1 N2 155.01(8) 3_656 . ?
O1 Ho1 N2 132.76(7) . . ?
O2 Ho1 Ho1 90.61(6) . 3_656 ?
O2 Ho1 O1 77.12(7) . . ?
O2 Ho1 O3 71.05(7) . . ?
O2 Ho1 O5 138.53(7) . . ?
O2 Ho1 N1 70.29(8) . . ?
O2 Ho1 N2 81.76(8) . . ?
O3 Ho1 Ho1 111.47(5) . 3_656 ?
O3 Ho1 O5 149.73(7) . . ?
O3 Ho1 N1 127.00(8) . . ?
O3 Ho1 N2 75.16(7) . . ?
O4 Ho1 Ho1 110.52(6) . 3_656 ?
O4 Ho1 O1 133.46(7) . . ?
O4 Ho1 O2 148.20(8) . . ?
O4 Ho1 O3 79.00(7) . . ?
O4 Ho1 O5 70.73(7) . . ?
O4 Ho1 N1 123.61(8) . . ?
O4 Ho1 N2 80.47(8) . . ?
O5 Ho1 Ho1 79.96(6) . 3_656 ?
O5 Ho1 N1 72.98(8) . . ?
O5 Ho1 N2 99.43(8) . . ?
N1 Ho1 Ho1 103.78(6) . 3_656 ?
N1 Ho1 N2 64.68(8) . . ?
N2 Ho1 Ho1 167.77(5) . 3_656 ?
Ho1 O1 Ho1 108.05(8) 3_656 . ?
C2 O1 Ho1 119.25(18) . . ?
C2 O1 Ho1 132.45(19) . 3_656 ?
C18 O2 Ho1 133.7(2) . . ?
C20 O3 Ho1 135.37(19) . . ?
C23 O4 Ho1 133.7(2) . . ?
C25 O5 Ho1 133.32(19) . . ?
C1 N1 Ho1 116.97(19) . . ?
C9 N1 Ho1 123.3(2) . . ?
C9 N1 C1 119.7(3) . . ?
C10 N2 Ho1 115.8(2) . . ?
C10 N2 C11 117.8(3) . . ?
C11 N2 Ho1 125.32(19) . . ?
N1 C1 C2 117.9(3) . . ?
N1 C1 C6 121.7(3) . . ?
C2 C1 C6 120.4(3) . . ?
O1 C2 C1 117.4(3) . . ?
O1 C2 C3 124.5(3) . . ?
C3 C2 C1 118.1(3) . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.7(3) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.7(3) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 124.1(3) . . ?
C7 C6 C1 116.9(3) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.8(3) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.9 . . ?
C7 C8 C9 118.3(3) . . ?
C9 C8 H8 120.9 . . ?
N1 C9 C8 122.6(3) . . ?
N1 C9 C10 115.7(3) . . ?
C8 C9 C10 121.5(3) . . ?
N2 C10 C9 120.5(3) . . ?
N2 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 N2 121.3(3) . . ?
C12 C11 C16 119.6(3) . . ?
C16 C11 N2 118.8(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.5(3) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 Cl1 120.0(3) . . ?
C15 C14 Cl1 119.1(3) . . ?
C15 C14 C13 120.9(3) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.7(3) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 120.1 . . ?
C15 C16 C11 119.8(3) . . ?
C15 C16 H16 120.1 . . ?
F1 C17 F2 107.7(3) . . ?
F1 C17 F3 107.5(3) . . ?
F1 C17 C18 112.7(3) . . ?
F2 C17 F3 106.6(3) . . ?
F2 C17 C18 109.4(3) . . ?
F3 C17 C18 112.8(3) . . ?
O2 C18 C17 114.0(3) . . ?
O2 C18 C19 127.7(3) . . ?
C19 C18 C17 118.3(3) . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
O3 C20 C19 127.1(3) . . ?
O3 C20 C21 115.9(3) . . ?
C19 C20 C21 117.0(3) . . ?
F4 C21 F6 106.3(3) . . ?
F4 C21 C20 112.5(3) . . ?
F5 C21 F4 107.8(3) . . ?
F5 C21 F6 107.2(3) . . ?
F5 C21 C20 113.2(3) . . ?
F6 C21 C20 109.5(3) . . ?
F7 C22 C23 111.4(3) . . ?
F8 C22 C23 111.2(4) . . ?
F8 C22 F7 104.5(4) . . ?
F9 C22 C23 112.6(4) . . ?
F9 C22 F7 106.9(4) . . ?
F9 C22 F8 109.8(4) . . ?
F7' C22 C23 112.3(8) . . ?
F7' C22 F8' 108.0(6) . . ?
F7' C22 F9' 106.7(7) . . ?
F8' C22 C23 113.6(7) . . ?
F8' C22 F9' 106.0(6) . . ?
F9' C22 C23 109.9(8) . . ?
F7" C22 C23 114.5(6) . . ?
F7" C22 F8" 109.3(6) . . ?
F7" C22 F9" 107.3(5) . . ?
F8" C22 C23 108.9(6) . . ?
F8" C22 F9" 105.4(5) . . ?
F9" C22 C23 111.0(5) . . ?
O4 C23 C22 115.3(3) . . ?
O4 C23 C24 127.9(3) . . ?
C24 C23 C22 116.8(3) . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.7(3) . . ?
C25 C24 H24 120.2 . . ?
O5 C25 C24 127.0(3) . . ?
O5 C25 C26 114.6(3) . . ?
C24 C25 C26 118.3(3) . . ?
F10 C26 C25 109.4(3) . . ?
F11 C26 F10 106.9(3) . . ?
F11 C26 C25 111.8(3) . . ?
F12 C26 F10 107.9(3) . . ?
F12 C26 F11 107.5(3) . . ?
F12 C26 C25 113.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O1 C2 C1 -2.0(3) . . . . ?
Ho1 O1 C2 C1 -175.59(18) 3_656 . . . ?
Ho1 O1 C2 C3 6.0(4) 3_656 . . . ?
Ho1 O1 C2 C3 179.5(2) . . . . ?
Ho1 O2 C18 C17 153.0(2) . . . . ?
Ho1 O2 C18 C19 -24.7(5) . . . . ?
Ho1 O3 C20 C19 5.6(5) . . . . ?
Ho1 O3 C20 C21 -175.44(19) . . . . ?
Ho1 O4 C23 C22 -162.88(18) . . . . ?
Ho1 O4 C23 C24 18.6(5) . . . . ?
Ho1 O5 C25 C24 -18.6(5) . . . . ?
Ho1 O5 C25 C26 164.0(2) . . . . ?
Ho1 N1 C1 C2 -0.1(3) . . . . ?
Ho1 N1 C1 C6 178.5(2) . . . . ?
Ho1 N1 C9 C8 -178.9(2) . . . . ?
Ho1 N1 C9 C10 -3.4(4) . . . . ?
Ho1 N2 C10 C9 -0.7(4) . . . . ?
Ho1 N2 C11 C12 -121.0(3) . . . . ?
Ho1 N2 C11 C16 53.0(3) . . . . ?
Cl1 C14 C15 C16 176.3(3) . . . . ?
F1 C17 C18 O2 43.1(4) . . . . ?
F1 C17 C18 C19 -139.1(3) . . . . ?
F2 C17 C18 O2 -76.7(4) . . . . ?
F2 C17 C18 C19 101.2(4) . . . . ?
F3 C17 C18 O2 164.9(3) . . . . ?
F3 C17 C18 C19 -17.2(5) . . . . ?
O1 C2 C3 C4 177.4(3) . . . . ?
O2 C18 C19 C20 0.4(5) . . . . ?
O3 C20 C21 F4 138.5(3) . . . . ?
O3 C20 C21 F5 16.0(4) . . . . ?
O3 C20 C21 F6 -103.5(3) . . . . ?
O4 C23 C24 C25 6.5(5) . . . . ?
O5 C25 C26 F10 82.6(3) . . . . ?
O5 C25 C26 F11 -35.7(4) . . . . ?
O5 C25 C26 F12 -157.1(3) . . . . ?
N1 C1 C2 O1 1.4(4) . . . . ?
N1 C1 C2 C3 179.9(3) . . . . ?
N1 C1 C6 C5 -179.6(3) . . . . ?
N1 C1 C6 C7 0.2(4) . . . . ?
N1 C9 C10 N2 2.6(4) . . . . ?
N2 C11 C12 C13 173.5(3) . . . . ?
N2 C11 C16 C15 -174.6(3) . . . . ?
C1 N1 C9 C8 -2.5(4) . . . . ?
C1 N1 C9 C10 173.0(3) . . . . ?
C1 C2 C3 C4 -1.0(5) . . . . ?
C1 C6 C7 C8 -1.8(5) . . . . ?
C2 C1 C6 C5 -1.1(4) . . . . ?
C2 C1 C6 C7 178.8(3) . . . . ?
C2 C3 C4 C5 0.4(5) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C4 C5 C6 C1 0.5(5) . . . . ?
C4 C5 C6 C7 -179.3(3) . . . . ?
C5 C6 C7 C8 178.1(3) . . . . ?
C6 C1 C2 O1 -177.2(2) . . . . ?
C6 C1 C2 C3 1.3(4) . . . . ?
C6 C7 C8 C9 1.3(5) . . . . ?
C7 C8 C9 N1 0.9(5) . . . . ?
C7 C8 C9 C10 -174.3(3) . . . . ?
C8 C9 C10 N2 178.1(3) . . . . ?
C9 N1 C1 C2 -176.7(3) . . . . ?
C9 N1 C1 C6 1.9(4) . . . . ?
C10 N2 C11 C12 46.4(4) . . . . ?
C10 N2 C11 C16 -139.6(3) . . . . ?
C11 N2 C10 C9 -169.3(3) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C11 C16 C15 -0.5(5) . . . . ?
C12 C13 C14 Cl1 -177.2(3) . . . . ?
C12 C13 C14 C15 0.9(5) . . . . ?
C13 C14 C15 C16 -1.9(5) . . . . ?
C14 C15 C16 C11 1.6(5) . . . . ?
C16 C11 C12 C13 -0.4(5) . . . . ?
C17 C18 C19 C20 -177.1(3) . . . . ?
C18 C19 C20 O3 9.0(5) . . . . ?
C18 C19 C20 C21 -169.9(3) . . . . ?
C19 C20 C21 F4 -42.5(4) . . . . ?
C19 C20 C21 F5 -165.0(3) . . . . ?
C19 C20 C21 F6 75.5(4) . . . . ?
C22 C23 C24 C25 -172.0(3) . . . . ?
C23 C24 C25 O5 -6.3(5) . . . . ?
C23 C24 C25 C26 171.0(3) . . . . ?
C24 C25 C26 F10 -95.1(3) . . . . ?
C24 C25 C26 F11 146.7(3) . . . . ?
C24 C25 C26 F12 25.2(5) . . . . ?
F7 C22 C23 O4 1.4(5) . . . . ?
F7 C22 C23 C24 -179.9(4) . . . . ?
F8 C22 C23 O4 -114.8(4) . . . . ?
F8 C22 C23 C24 63.9(5) . . . . ?
F9 C22 C23 O4 121.5(5) . . . . ?
F9 C22 C23 C24 -59.8(6) . . . . ?
F7' C22 C23 O4 -41.1(13) . . . . ?
F7' C22 C23 C24 137.5(13) . . . . ?
F8' C22 C23 O4 -164.0(12) . . . . ?
F8' C22 C23 C24 14.6(12) . . . . ?
F9' C22 C23 O4 77.4(11) . . . . ?
F9' C22 C23 C24 -103.9(11) . . . . ?
F7" C22 C23 O4 33.5(8) . . . . ?
F7" C22 C23 C24 -147.8(7) . . . . ?
F8" C22 C23 O4 -89.2(7) . . . . ?
F8" C22 C23 C24 89.5(7) . . . . ?
F9" C22 C23 O4 155.2(6) . . . . ?
F9" C22 C23 C24 -26.1(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1427270'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C52 H24 Cl2 F24 Lu2 N4 O10'
_chemical_formula_sum            'C52 H24 Cl2 F24 Lu2 N4 O10'
_chemical_formula_weight         1741.59
_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'
Cl Cl 0.1484 0.1585 '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'
Lu Lu -0.4720 5.8584 '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      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                   11.416(2)
_cell_length_b                   19.038(4)
_cell_length_c                   12.998(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.99(3)
_cell_angle_gamma                90
_cell_volume                     2814.1(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7724
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8664
_cell_measurement_theta_min      1.9021
_shelx_estimated_absorpt_T_max   0.663
_shelx_estimated_absorpt_T_min   0.523
_exptl_absorpt_coefficient_mu    3.725
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23448
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         1.902
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
scan:
	Number of images: 90
	           Slice: -110.0000 - 70.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0482
	          2theta: -19.8967
scan:
	Number of images: 70
	           Slice: -110.0000 - 30.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0482
	          2theta: -19.8967
scan:
	Number of images: 60
	           Slice: -110.0000 - 10.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0482
	          2theta: -19.8967
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             6948
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0120
_diffrn_orient_matrix_UB_12      -0.0849
_diffrn_orient_matrix_UB_13      -0.0194
_diffrn_orient_matrix_UB_21      -0.0331
_diffrn_orient_matrix_UB_22      -0.0046
_diffrn_orient_matrix_UB_23      0.0405
_diffrn_orient_matrix_UB_31      -0.0597
_diffrn_orient_matrix_UB_32      0.0123
_diffrn_orient_matrix_UB_33      -0.0474
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4241
_reflns_number_total             4979
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.083
_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)+(0.0379P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0694
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.45700(2) 0.09164(2) 0.46877(2) 0.01493(7) Uani 1 1 d . . . . .
Cl1 Cl 0.66638(12) 0.46598(7) 0.40236(12) 0.0424(3) Uani 1 1 d . . . . .
F1 F 0.4212(4) 0.12077(18) 0.8423(2) 0.0611(11) Uani 1 1 d . . . . .
F2 F 0.3342(3) 0.2085(2) 0.7691(3) 0.0686(12) Uani 1 1 d . . . . .
F3 F 0.4966(3) 0.22247(17) 0.8611(2) 0.0477(9) Uani 1 1 d . . . . .
F4 F 0.7417(3) 0.31707(15) 0.6054(3) 0.0551(10) Uani 1 1 d . . . . .
F5 F 0.7824(3) 0.25539(19) 0.4778(2) 0.0600(11) Uani 1 1 d . . . . .
F6 F 0.8444(2) 0.22481(16) 0.6295(2) 0.0443(8) Uani 1 1 d . . . . .
F7 F 0.6528(4) 0.1717(3) 0.1804(3) 0.0896(16) Uani 1 1 d . . . . .
F8 F 0.5162(3) 0.1567(2) 0.0694(3) 0.0754(13) Uani 1 1 d . . . . .
F9 F 0.6375(5) 0.07767(19) 0.0986(4) 0.110(2) Uani 1 1 d . U . . .
F10 F 0.1554(3) -0.00496(17) 0.1742(2) 0.0471(8) Uani 1 1 d . . . . .
F11 F 0.2212(3) -0.08298(14) 0.2828(2) 0.0389(8) Uani 1 1 d . . . . .
F12 F 0.2894(3) -0.07762(17) 0.1345(2) 0.0513(9) Uani 1 1 d . . . . .
O1 O 0.3984(2) -0.01294(14) 0.5413(2) 0.0166(6) Uani 1 1 d . . . . .
O2 O 0.4621(3) 0.11716(16) 0.6417(2) 0.0203(7) Uani 1 1 d . . . . .
O3 O 0.6126(3) 0.16744(15) 0.5100(2) 0.0198(7) Uani 1 1 d . . . . .
O4 O 0.5094(3) 0.12290(15) 0.3086(2) 0.0196(7) Uani 1 1 d . . . . .
O5 O 0.3345(3) 0.03277(15) 0.3450(2) 0.0215(7) Uani 1 1 d . . . . .
N1 N 0.2610(3) 0.10123(18) 0.5173(3) 0.0172(8) Uani 1 1 d . . . . .
N2 N 0.3681(3) 0.21591(18) 0.4502(3) 0.0198(8) Uani 1 1 d . . . . .
C1 C 0.2150(4) 0.0436(2) 0.5601(3) 0.0179(9) Uani 1 1 d . . . . .
C2 C 0.2883(4) -0.0172(2) 0.5717(3) 0.0174(9) Uani 1 1 d . . . . .
C3 C 0.2420(4) -0.0757(2) 0.6150(3) 0.0220(10) Uani 1 1 d . . . . .
H3 H 0.2879 -0.1173 0.6226 0.026 Uiso 1 1 calc R . . . .
C4 C 0.1272(4) -0.0753(2) 0.6486(4) 0.0235(11) Uani 1 1 d . . . . .
H4 H 0.0984 -0.1165 0.6788 0.028 Uiso 1 1 calc R . . . .
C5 C 0.0572(4) -0.0176(2) 0.6389(3) 0.0258(11) Uani 1 1 d . . . . .
H5 H -0.0196 -0.0185 0.6619 0.031 Uiso 1 1 calc R . . . .
C6 C 0.1005(4) 0.0438(2) 0.5940(3) 0.0214(10) Uani 1 1 d . . . . .
C7 C 0.0345(4) 0.1065(2) 0.5809(4) 0.0269(11) Uani 1 1 d . . . . .
H7 H -0.0437 0.1083 0.6005 0.032 Uiso 1 1 calc R . . . .
C8 C 0.0838(4) 0.1648(2) 0.5399(3) 0.0252(11) Uani 1 1 d . . . . .
H8 H 0.0408 0.2074 0.5323 0.030 Uiso 1 1 calc R . . . .
C9 C 0.1981(4) 0.1605(2) 0.5094(3) 0.0203(10) Uani 1 1 d . . . . .
C10 C 0.2610(4) 0.2214(2) 0.4746(3) 0.0218(10) Uani 1 1 d . . . . .
H10 H 0.2229 0.2658 0.4698 0.026 Uiso 1 1 calc R . . . .
C11 C 0.4320(4) 0.2789(2) 0.4349(4) 0.0212(10) Uani 1 1 d . . . . .
C12 C 0.4318(4) 0.3339(2) 0.5060(4) 0.0259(11) Uani 1 1 d . . . . .
H12 H 0.3832 0.3315 0.5617 0.031 Uiso 1 1 calc R . . . .
C13 C 0.5030(5) 0.3918(2) 0.4949(4) 0.0307(12) Uani 1 1 d . . . . .
H13 H 0.5042 0.4291 0.5435 0.037 Uiso 1 1 calc R . . . .
C14 C 0.5719(4) 0.3952(2) 0.4132(4) 0.0272(11) Uani 1 1 d . . . . .
C15 C 0.5706(4) 0.3421(2) 0.3414(4) 0.0287(11) Uani 1 1 d . . . . .
H15 H 0.6176 0.3455 0.2848 0.034 Uiso 1 1 calc R . . . .
C16 C 0.5004(4) 0.2834(2) 0.3520(4) 0.0244(11) Uani 1 1 d . . . . .
H16 H 0.4992 0.2465 0.3027 0.029 Uiso 1 1 calc R . . . .
C17 C 0.4385(5) 0.1791(3) 0.7936(4) 0.0324(12) Uani 1 1 d . . . . .
C18 C 0.5012(4) 0.1681(2) 0.6964(3) 0.0212(10) Uani 1 1 d . . . . .
C19 C 0.5895(4) 0.2148(2) 0.6749(4) 0.0245(11) Uani 1 1 d . . . . .
H19 H 0.6133 0.2511 0.7223 0.029 Uiso 1 1 calc R . . . .
C20 C 0.6423(4) 0.2076(2) 0.5837(3) 0.0195(10) Uani 1 1 d . . . . .
C21 C 0.7535(4) 0.2520(2) 0.5728(4) 0.0252(11) Uani 1 1 d . . . . .
C22 C 0.5786(5) 0.1230(3) 0.1423(4) 0.0265(11) Uani 1 1 d . . . . .
C23 C 0.5021(4) 0.0930(2) 0.2219(3) 0.0194(10) Uani 1 1 d . . . . .
C24 C 0.4284(4) 0.0385(2) 0.1892(4) 0.0261(11) Uani 1 1 d . . . . .
H24 H 0.4338 0.0177 0.1233 0.031 Uiso 1 1 calc R . . . .
C25 C 0.3455(4) 0.0139(2) 0.2542(3) 0.0219(10) Uani 1 1 d . . . . .
C26 C 0.2527(4) -0.0390(3) 0.2104(4) 0.0306(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 Lu1 3.6958(8) 3_656 ?
Lu1 O1 2.326(3) . ?
Lu1 O1 2.241(3) 3_656 ?
Lu1 O2 2.296(3) . ?
Lu1 O3 2.315(3) . ?
Lu1 O4 2.294(3) . ?
Lu1 O5 2.325(3) . ?
Lu1 N1 2.384(4) . ?
Lu1 N2 2.577(4) . ?
Cl1 C14 1.739(5) . ?
F1 C17 1.302(6) . ?
F2 C17 1.328(6) . ?
F3 C17 1.337(5) . ?
F4 C21 1.320(5) . ?
F5 C21 1.307(5) . ?
F6 C21 1.325(5) . ?
F7 C22 1.324(6) . ?
F8 C22 1.304(6) . ?
F9 C22 1.259(6) . ?
F10 C26 1.336(6) . ?
F11 C26 1.333(6) . ?
F12 C26 1.327(5) . ?
O1 Lu1 2.242(3) 3_656 ?
O1 C2 1.353(5) . ?
O2 C18 1.261(5) . ?
O3 C20 1.249(5) . ?
O4 C23 1.258(5) . ?
O5 C25 1.250(5) . ?
N1 C1 1.357(5) . ?
N1 C9 1.337(5) . ?
N2 C10 1.294(6) . ?
N2 C11 1.427(6) . ?
C1 C2 1.428(6) . ?
C1 C6 1.415(6) . ?
C2 C3 1.376(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.416(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.357(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.415(6) . ?
C6 C7 1.414(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.372(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.399(6) . ?
C9 C10 1.457(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(6) . ?
C11 C16 1.387(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.377(7) . ?
C14 C15 1.376(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.519(6) . ?
C18 C19 1.391(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(6) . ?
C20 C21 1.541(6) . ?
C22 C23 1.522(6) . ?
C23 C24 1.379(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.402(6) . ?
C25 C26 1.536(6) . ?

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 Lu1 Lu1 36.77(7) 3_656 3_656 ?
O1 Lu1 Lu1 35.23(7) . 3_656 ?
O1 Lu1 O1 71.99(11) 3_656 . ?
O1 Lu1 O2 104.05(11) 3_656 . ?
O1 Lu1 O3 82.88(10) 3_656 . ?
O1 Lu1 O4 82.45(10) 3_656 . ?
O1 Lu1 O5 92.22(10) 3_656 . ?
O1 Lu1 N1 141.22(11) 3_656 . ?
O1 Lu1 N1 69.42(11) . . ?
O1 Lu1 N2 134.34(10) . . ?
O1 Lu1 N2 153.38(11) 3_656 . ?
O2 Lu1 Lu1 90.06(8) . 3_656 ?
O2 Lu1 O1 76.57(10) . . ?
O2 Lu1 O3 71.81(10) . . ?
O2 Lu1 O5 137.89(10) . . ?
O2 Lu1 N1 70.66(12) . . ?
O2 Lu1 N2 82.76(11) . . ?
O3 Lu1 Lu1 110.71(7) . 3_656 ?
O3 Lu1 O1 132.96(10) . . ?
O3 Lu1 O5 149.73(10) . . ?
O3 Lu1 N1 127.58(11) . . ?
O3 Lu1 N2 74.79(11) . . ?
O4 Lu1 Lu1 111.03(7) . 3_656 ?
O4 Lu1 O1 134.18(10) . . ?
O4 Lu1 O2 147.92(11) . . ?
O4 Lu1 O3 78.05(10) . . ?
O4 Lu1 O5 71.70(10) . . ?
O4 Lu1 N1 123.06(12) . . ?
O4 Lu1 N2 78.96(11) . . ?
O5 Lu1 Lu1 80.16(8) . 3_656 ?
O5 Lu1 O1 72.01(10) . . ?
O5 Lu1 N1 72.45(11) . . ?
O5 Lu1 N2 99.75(11) . . ?
N1 Lu1 Lu1 104.57(8) . 3_656 ?
N1 Lu1 N2 65.39(11) . . ?
N2 Lu1 Lu1 169.15(8) . 3_656 ?
Lu1 O1 Lu1 108.01(11) 3_656 . ?
C2 O1 Lu1 133.3(2) . 3_656 ?
C2 O1 Lu1 118.5(2) . . ?
C18 O2 Lu1 133.8(3) . . ?
C20 O3 Lu1 135.3(3) . . ?
C23 O4 Lu1 133.8(3) . . ?
C25 O5 Lu1 133.4(3) . . ?
C1 N1 Lu1 116.9(3) . . ?
C9 N1 Lu1 123.7(3) . . ?
C9 N1 C1 119.3(4) . . ?
C10 N2 Lu1 115.1(3) . . ?
C10 N2 C11 118.1(4) . . ?
C11 N2 Lu1 125.7(3) . . ?
N1 C1 C2 117.0(4) . . ?
N1 C1 C6 121.8(4) . . ?
C6 C1 C2 121.2(4) . . ?
O1 C2 C1 118.2(4) . . ?
O1 C2 C3 124.6(4) . . ?
C3 C2 C1 117.2(4) . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.3(4) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 119.0 . . ?
C5 C4 C3 122.0(4) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.8(4) . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C5 119.5(4) . . ?
C7 C6 C1 117.5(4) . . ?
C7 C6 C5 123.1(4) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.8(4) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.2(4) . . ?
C9 C8 H8 120.4 . . ?
N1 C9 C8 122.4(4) . . ?
N1 C9 C10 114.8(4) . . ?
C8 C9 C10 122.6(4) . . ?
N2 C10 C9 120.9(4) . . ?
N2 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 N2 120.5(4) . . ?
C16 C11 N2 119.3(4) . . ?
C16 C11 C12 120.1(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.9(5) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 Cl1 120.0(4) . . ?
C13 C14 C15 121.0(4) . . ?
C15 C14 Cl1 119.0(4) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(4) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 120.1 . . ?
C15 C16 C11 119.7(4) . . ?
C15 C16 H16 120.1 . . ?
F1 C17 F2 107.7(5) . . ?
F1 C17 F3 107.1(4) . . ?
F1 C17 C18 112.8(4) . . ?
F2 C17 F3 106.3(4) . . ?
F2 C17 C18 109.7(4) . . ?
F3 C17 C18 112.8(4) . . ?
O2 C18 C17 114.0(4) . . ?
O2 C18 C19 127.3(4) . . ?
C19 C18 C17 118.7(4) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 C18 119.2(4) . . ?
C20 C19 H19 120.4 . . ?
O3 C20 C19 127.5(4) . . ?
O3 C20 C21 115.8(4) . . ?
C19 C20 C21 116.7(4) . . ?
F4 C21 F6 106.6(4) . . ?
F4 C21 C20 112.2(4) . . ?
F5 C21 F4 107.4(4) . . ?
F5 C21 F6 107.1(4) . . ?
F5 C21 C20 113.0(4) . . ?
F6 C21 C20 110.3(4) . . ?
F7 C22 C23 113.3(4) . . ?
F8 C22 F7 102.6(4) . . ?
F8 C22 C23 111.7(4) . . ?
F9 C22 F7 107.4(5) . . ?
F9 C22 F8 106.8(5) . . ?
F9 C22 C23 114.2(4) . . ?
O4 C23 C22 116.2(4) . . ?
O4 C23 C24 127.4(4) . . ?
C24 C23 C22 116.3(4) . . ?
C23 C24 H24 120.3 . . ?
C23 C24 C25 119.3(4) . . ?
C25 C24 H24 120.3 . . ?
O5 C25 C24 127.0(4) . . ?
O5 C25 C26 114.6(4) . . ?
C24 C25 C26 118.4(4) . . ?
F10 C26 C25 109.8(4) . . ?
F11 C26 F10 106.6(4) . . ?
F11 C26 C25 111.7(4) . . ?
F12 C26 F10 108.3(4) . . ?
F12 C26 F11 107.4(4) . . ?
F12 C26 C25 112.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Lu1 O1 C2 C1 -1.7(5) . . . . ?
Lu1 O1 C2 C1 -175.0(3) 3_656 . . . ?
Lu1 O1 C2 C3 6.3(6) 3_656 . . . ?
Lu1 O1 C2 C3 179.5(3) . . . . ?
Lu1 O2 C18 C17 153.2(3) . . . . ?
Lu1 O2 C18 C19 -24.2(7) . . . . ?
Lu1 O3 C20 C19 6.2(7) . . . . ?
Lu1 O3 C20 C21 -176.5(3) . . . . ?
Lu1 O4 C23 C22 -163.0(3) . . . . ?
Lu1 O4 C23 C24 20.5(7) . . . . ?
Lu1 O5 C25 C24 -17.2(7) . . . . ?
Lu1 O5 C25 C26 166.1(3) . . . . ?
Lu1 N1 C1 C2 -0.1(5) . . . . ?
Lu1 N1 C1 C6 178.6(3) . . . . ?
Lu1 N1 C9 C8 -179.1(3) . . . . ?
Lu1 N1 C9 C10 -3.8(5) . . . . ?
Lu1 N2 C10 C9 -0.2(5) . . . . ?
Lu1 N2 C11 C12 -120.3(4) . . . . ?
Lu1 N2 C11 C16 55.7(5) . . . . ?
Cl1 C14 C15 C16 176.6(4) . . . . ?
F1 C17 C18 O2 44.5(6) . . . . ?
F1 C17 C18 C19 -137.9(5) . . . . ?
F2 C17 C18 O2 -75.6(5) . . . . ?
F2 C17 C18 C19 102.0(5) . . . . ?
F3 C17 C18 O2 166.1(4) . . . . ?
F3 C17 C18 C19 -16.3(7) . . . . ?
F7 C22 C23 O4 7.5(6) . . . . ?
F7 C22 C23 C24 -175.6(5) . . . . ?
F8 C22 C23 O4 -107.8(5) . . . . ?
F8 C22 C23 C24 69.2(6) . . . . ?
F9 C22 C23 O4 130.9(5) . . . . ?
F9 C22 C23 C24 -52.2(7) . . . . ?
O1 C2 C3 C4 177.5(4) . . . . ?
O2 C18 C19 C20 1.0(7) . . . . ?
O3 C20 C21 F4 138.9(4) . . . . ?
O3 C20 C21 F5 17.4(6) . . . . ?
O3 C20 C21 F6 -102.5(4) . . . . ?
O4 C23 C24 C25 4.1(7) . . . . ?
O5 C25 C26 F10 83.5(5) . . . . ?
O5 C25 C26 F11 -34.5(6) . . . . ?
O5 C25 C26 F12 -155.6(4) . . . . ?
N1 C1 C2 O1 1.2(6) . . . . ?
N1 C1 C2 C3 -180.0(4) . . . . ?
N1 C1 C6 C5 -179.5(4) . . . . ?
N1 C1 C6 C7 0.4(6) . . . . ?
N1 C9 C10 N2 2.5(6) . . . . ?
N2 C11 C12 C13 174.0(4) . . . . ?
N2 C11 C16 C15 -174.6(4) . . . . ?
C1 N1 C9 C8 -2.7(6) . . . . ?
C1 N1 C9 C10 172.6(4) . . . . ?
C1 C2 C3 C4 -1.2(7) . . . . ?
C1 C6 C7 C8 -2.1(7) . . . . ?
C2 C1 C6 C5 -0.8(7) . . . . ?
C2 C1 C6 C7 179.1(4) . . . . ?
C2 C3 C4 C5 0.6(7) . . . . ?
C3 C4 C5 C6 -0.1(7) . . . . ?
C4 C5 C6 C1 0.1(7) . . . . ?
C4 C5 C6 C7 -179.7(5) . . . . ?
C5 C6 C7 C8 177.8(5) . . . . ?
C6 C1 C2 O1 -177.5(4) . . . . ?
C6 C1 C2 C3 1.3(6) . . . . ?
C6 C7 C8 C9 1.4(7) . . . . ?
C7 C8 C9 N1 1.0(7) . . . . ?
C7 C8 C9 C10 -173.9(4) . . . . ?
C8 C9 C10 N2 177.8(4) . . . . ?
C9 N1 C1 C2 -176.8(4) . . . . ?
C9 N1 C1 C6 2.0(6) . . . . ?
C10 N2 C11 C12 47.0(6) . . . . ?
C10 N2 C11 C16 -137.0(4) . . . . ?
C11 N2 C10 C9 -168.8(4) . . . . ?
C11 C12 C13 C14 0.9(7) . . . . ?
C12 C11 C16 C15 1.4(7) . . . . ?
C12 C13 C14 Cl1 -177.0(4) . . . . ?
C12 C13 C14 C15 0.6(8) . . . . ?
C13 C14 C15 C16 -1.1(7) . . . . ?
C14 C15 C16 C11 0.1(7) . . . . ?
C16 C11 C12 C13 -1.9(7) . . . . ?
C17 C18 C19 C20 -176.2(4) . . . . ?
C18 C19 C20 O3 7.8(7) . . . . ?
C18 C19 C20 C21 -169.5(4) . . . . ?
C19 C20 C21 F4 -43.4(6) . . . . ?
C19 C20 C21 F5 -165.0(4) . . . . ?
C19 C20 C21 F6 75.2(5) . . . . ?
C22 C23 C24 C25 -172.4(4) . . . . ?
C23 C24 C25 O5 -5.5(7) . . . . ?
C23 C24 C25 C26 171.1(4) . . . . ?
C24 C25 C26 F10 -93.5(5) . . . . ?
C24 C25 C26 F11 148.5(4) . . . . ?
C24 C25 C26 F12 27.4(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1427271'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C52 H24 Cl2 F24 N4 O10 Tb2'
_chemical_formula_sum            'C52 H24 Cl2 F24 N4 O10 Tb2'
_chemical_formula_weight         1709.49
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.345(2)
_cell_length_b                   19.264(4)
_cell_length_c                   13.074(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.17(3)
_cell_angle_gamma                90
_cell_volume                     2845.7(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8375
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8267
_cell_measurement_theta_min      1.8878
_shelx_estimated_absorpt_T_max   0.774
_shelx_estimated_absorpt_T_min   0.614
_exptl_absorpt_coefficient_mu    2.699
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8553
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29090
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.009
_diffrn_reflns_theta_min         1.888
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
scan:
	Number of images: 90
	           Slice: -110.0000 - 70.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0396
	          2theta: -19.9087
scan:
	Number of images: 70
	           Slice: -110.0000 - 30.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0396
	          2theta: -19.9087
scan:
	Number of images: 60
	           Slice: -110.0000 - 10.0000
	     Image width: 2.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0396
	          2theta: -19.9087
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             7004
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0212
_diffrn_orient_matrix_UB_12      0.0489
_diffrn_orient_matrix_UB_13      -0.0707
_diffrn_orient_matrix_UB_21      0.0243
_diffrn_orient_matrix_UB_22      -0.0408
_diffrn_orient_matrix_UB_23      -0.0209
_diffrn_orient_matrix_UB_31      -0.0634
_diffrn_orient_matrix_UB_32      -0.0174
_diffrn_orient_matrix_UB_33      -0.0397
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5664
_reflns_number_total             6792
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         2.058
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0349P)²+2.1450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0883
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-F7 \\sim C22-F8 \\sim C22-F9 \\sim C22-F7' \\sim C22-F8' \\sim C22-F9'
 with sigma of 0.01
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F7'-F8' \\sim F7'-F9' \\sim F8'-F9'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7') \\sim
Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
Highest peak    2.06  at  0.6231  0.0937  0.5908  [  1.78 A from O3 ]
Deepest hole   -1.32  at  0.5171  0.1169  0.5007  [  0.87 A from TB1 ]
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.45922(2) 0.09310(2) 0.46919(2) 0.01679(7) Uani 1 1 d . . . . .
Cl1 Cl 0.66479(11) 0.46364(6) 0.40219(11) 0.0419(3) Uani 1 1 d . . . . .
F1 F 0.4202(3) 0.12563(18) 0.8434(2) 0.0604(10) Uani 1 1 d . . . . .
F2 F 0.3347(3) 0.2127(2) 0.7694(3) 0.0681(11) Uani 1 1 d . . . . .
F3 F 0.4979(3) 0.22606(17) 0.8625(2) 0.0499(8) Uani 1 1 d . . . . .
F4 F 0.7423(3) 0.32071(14) 0.6089(3) 0.0543(9) Uani 1 1 d . . . . .
F5 F 0.7882(3) 0.25865(18) 0.4838(2) 0.0568(9) Uani 1 1 d . . . . .
F6 F 0.8481(2) 0.23030(15) 0.6370(2) 0.0421(7) Uani 1 1 d . . . . .
F7 F 0.6596(5) 0.1683(3) 0.1794(3) 0.075(3) Uani 0.810(11) 1 d D U P A 1
F8 F 0.5202(3) 0.1542(3) 0.0666(4) 0.0573(18) Uani 0.810(11) 1 d D U P A 1
F9 F 0.6429(6) 0.0741(2) 0.0979(6) 0.093(3) Uani 0.810(11) 1 d D U P A 1
F7' F 0.6949(7) 0.1096(11) 0.1675(12) 0.043(6) Uani 0.190(11) 1 d D U P A 2
F8' F 0.5708(18) 0.1873(4) 0.1264(16) 0.066(9) Uani 0.190(11) 1 d D U P A 2
F9' F 0.5633(16) 0.0924(10) 0.0489(8) 0.059(8) Uani 0.190(11) 1 d D U P A 2
F10 F 0.1567(2) -0.00699(16) 0.1720(2) 0.0492(8) Uani 1 1 d . . . . .
F11 F 0.2261(3) -0.08332(14) 0.2801(2) 0.0412(7) Uani 1 1 d . . . . .
F12 F 0.2928(3) -0.07728(17) 0.1321(2) 0.0539(9) Uani 1 1 d . . . . .
O1 O 0.3941(2) -0.01163(13) 0.5416(2) 0.0189(6) Uani 1 1 d . . . . .
O2 O 0.4649(2) 0.12052(15) 0.6455(2) 0.0223(6) Uani 1 1 d . . . . .
O3 O 0.6189(2) 0.17044(14) 0.5140(2) 0.0211(6) Uani 1 1 d . . . . .
O4 O 0.5129(2) 0.12266(15) 0.3050(2) 0.0219(6) Uani 1 1 d . . . . .
O5 O 0.3338(2) 0.03381(15) 0.3408(2) 0.0248(6) Uani 1 1 d . . . . .
N1 N 0.2572(3) 0.10264(16) 0.5201(3) 0.0183(7) Uani 1 1 d . . . . .
N2 N 0.3640(3) 0.21732(18) 0.4535(3) 0.0218(7) Uani 1 1 d . . . . .
C1 C 0.2107(3) 0.0457(2) 0.5616(3) 0.0207(9) Uani 1 1 d . . . . .
C2 C 0.2825(3) -0.0153(2) 0.5718(3) 0.0202(8) Uani 1 1 d . . . . .
C3 C 0.2353(4) -0.0737(2) 0.6129(3) 0.0221(9) Uani 1 1 d . . . . .
H3 H 0.2808 -0.1151 0.6191 0.026 Uiso 1 1 calc R . . . .
C4 C 0.1204(4) -0.0729(2) 0.6458(4) 0.0263(10) Uani 1 1 d . . . . .
H4 H 0.0903 -0.1141 0.6738 0.032 Uiso 1 1 calc R . . . .
C5 C 0.0510(4) -0.0149(2) 0.6388(3) 0.0277(10) Uani 1 1 d . . . . .
H5 H -0.0257 -0.0155 0.6626 0.033 Uiso 1 1 calc R . . . .
C6 C 0.0952(4) 0.0458(2) 0.5956(3) 0.0229(9) Uani 1 1 d . . . . .
C7 C 0.0313(4) 0.1086(2) 0.5850(4) 0.0275(10) Uani 1 1 d . . . . .
H7 H -0.0465 0.1109 0.6061 0.033 Uiso 1 1 calc R . . . .
C8 C 0.0805(4) 0.1663(2) 0.5446(3) 0.0252(9) Uani 1 1 d . . . . .
H8 H 0.0374 0.2086 0.5372 0.030 Uiso 1 1 calc R . . . .
C9 C 0.1953(4) 0.1617(2) 0.5145(3) 0.0221(9) Uani 1 1 d . . . . .
C10 C 0.2581(4) 0.2222(2) 0.4796(3) 0.0225(9) Uani 1 1 d . . . . .
H10 H 0.2197 0.2661 0.4761 0.027 Uiso 1 1 calc R . . . .
C11 C 0.4279(4) 0.2795(2) 0.4373(3) 0.0216(9) Uani 1 1 d . . . . .
C12 C 0.4275(4) 0.3348(2) 0.5062(4) 0.0255(9) Uani 1 1 d . . . . .
H12 H 0.3779 0.3333 0.5609 0.031 Uiso 1 1 calc R . . . .
C13 C 0.4994(4) 0.3922(2) 0.4950(4) 0.0306(10) Uani 1 1 d . . . . .
H13 H 0.4998 0.4298 0.5421 0.037 Uiso 1 1 calc R . . . .
C14 C 0.5703(4) 0.3938(2) 0.4147(4) 0.0294(10) Uani 1 1 d . . . . .
C15 C 0.5697(4) 0.3402(2) 0.3450(3) 0.0271(10) Uani 1 1 d . . . . .
H15 H 0.6174 0.3428 0.2890 0.033 Uiso 1 1 calc R . . . .
C16 C 0.4998(4) 0.2827(2) 0.3566(3) 0.0253(9) Uani 1 1 d . . . . .
H16 H 0.5007 0.2452 0.3095 0.030 Uiso 1 1 calc R . . . .
C17 C 0.4395(4) 0.1834(3) 0.7948(4) 0.0328(11) Uani 1 1 d . . . . .
C18 C 0.5027(4) 0.1718(2) 0.6987(3) 0.0216(9) Uani 1 1 d . . . . .
C19 C 0.5910(4) 0.2181(2) 0.6770(3) 0.0248(9) Uani 1 1 d . . . . .
H19 H 0.6134 0.2547 0.7235 0.030 Uiso 1 1 calc R . . . .
C20 C 0.6466(3) 0.2107(2) 0.5870(3) 0.0210(9) Uani 1 1 d . . . . .
C21 C 0.7569(4) 0.2559(2) 0.5772(3) 0.0264(10) Uani 1 1 d . . . . .
C22 C 0.5833(4) 0.1212(2) 0.1402(3) 0.0286(10) Uani 1 1 d D . . . .
C23 C 0.5049(4) 0.0920(2) 0.2198(3) 0.0223(9) Uani 1 1 d . . . . .
C24 C 0.4318(4) 0.0373(2) 0.1875(3) 0.0268(10) Uani 1 1 d . . . . .
H24 H 0.4386 0.0159 0.1229 0.032 Uiso 1 1 calc R . . . .
C25 C 0.3475(4) 0.0138(2) 0.2518(3) 0.0228(9) Uani 1 1 d . . . . .
C26 C 0.2558(4) -0.0397(3) 0.2081(4) 0.0322(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb1 3.7731(8) 3_656 ?
Tb1 O1 2.375(3) . ?
Tb1 O1 2.301(3) 3_656 ?
Tb1 O2 2.361(3) . ?
Tb1 O3 2.378(3) . ?
Tb1 O4 2.354(3) . ?
Tb1 O5 2.391(3) . ?
Tb1 N1 2.450(3) . ?
Tb1 N2 2.626(3) . ?
Cl1 C14 1.737(4) . ?
F1 C17 1.310(6) . ?
F2 C17 1.331(6) . ?
F3 C17 1.340(5) . ?
F4 C21 1.330(5) . ?
F5 C21 1.302(5) . ?
F6 C21 1.335(5) . ?
F7 C22 1.325(5) . ?
F8 C22 1.311(5) . ?
F9 C22 1.286(5) . ?
F7' C22 1.304(7) . ?
F8' C22 1.291(7) . ?
F9' C22 1.318(7) . ?
F10 C26 1.337(5) . ?
F11 C26 1.328(5) . ?
F12 C26 1.328(5) . ?
O1 Tb1 2.301(3) 3_656 ?
O1 C2 1.361(5) . ?
O2 C18 1.261(5) . ?
O3 C20 1.248(5) . ?
O4 C23 1.256(5) . ?
O5 C25 1.249(5) . ?
N1 C1 1.352(5) . ?
N1 C9 1.336(5) . ?
N2 C10 1.281(5) . ?
N2 C11 1.426(5) . ?
C1 C2 1.430(6) . ?
C1 C6 1.421(5) . ?
C2 C3 1.375(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.409(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.365(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.411(6) . ?
C6 C7 1.410(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.371(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.396(6) . ?
C9 C10 1.460(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(6) . ?
C11 C16 1.392(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(7) . ?
C14 C15 1.377(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.379(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.518(6) . ?
C18 C19 1.389(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.392(6) . ?
C20 C21 1.540(6) . ?
C22 C23 1.536(6) . ?
C23 C24 1.383(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.403(6) . ?
C25 C26 1.538(6) . ?

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 Tb1 35.54(6) . 3_656 ?
O1 Tb1 Tb1 36.87(7) 3_656 3_656 ?
O1 Tb1 O1 72.41(10) 3_656 . ?
O1 Tb1 O2 104.87(10) 3_656 . ?
O1 Tb1 O3 133.75(9) . . ?
O1 Tb1 O3 84.45(10) 3_656 . ?
O1 Tb1 O4 82.00(10) 3_656 . ?
O1 Tb1 O5 71.79(9) . . ?
O1 Tb1 O5 91.09(10) 3_656 . ?
O1 Tb1 N1 140.11(10) 3_656 . ?
O1 Tb1 N1 67.87(10) . . ?
O1 Tb1 N2 131.67(10) . . ?
O1 Tb1 N2 155.70(10) 3_656 . ?
O2 Tb1 Tb1 91.13(7) . 3_656 ?
O2 Tb1 O1 77.44(9) . . ?
O2 Tb1 O3 70.49(10) . . ?
O2 Tb1 O5 139.00(10) . . ?
O2 Tb1 N1 70.23(11) . . ?
O2 Tb1 N2 81.20(10) . . ?
O3 Tb1 Tb1 112.10(7) . 3_656 ?
O3 Tb1 O5 149.81(10) . . ?
O3 Tb1 N1 126.63(10) . . ?
O3 Tb1 N2 75.36(10) . . ?
O4 Tb1 Tb1 110.25(7) . 3_656 ?
O4 Tb1 O1 133.21(9) . . ?
O4 Tb1 O2 148.25(10) . . ?
O4 Tb1 O3 79.59(10) . . ?
O4 Tb1 O5 70.22(10) . . ?
O4 Tb1 N1 123.68(11) . . ?
O4 Tb1 N2 81.19(10) . . ?
O5 Tb1 Tb1 79.33(7) . 3_656 ?
O5 Tb1 N1 73.40(10) . . ?
O5 Tb1 N2 99.55(10) . . ?
N1 Tb1 Tb1 103.34(8) . 3_656 ?
N1 Tb1 N2 64.18(10) . . ?
N2 Tb1 Tb1 166.96(7) . 3_656 ?
Tb1 O1 Tb1 107.59(10) 3_656 . ?
C2 O1 Tb1 119.4(2) . . ?
C2 O1 Tb1 132.7(2) . 3_656 ?
C18 O2 Tb1 133.8(3) . . ?
C20 O3 Tb1 135.4(3) . . ?
C23 O4 Tb1 133.7(3) . . ?
C25 O5 Tb1 133.3(3) . . ?
C1 N1 Tb1 117.2(2) . . ?
C9 N1 Tb1 123.3(3) . . ?
C9 N1 C1 119.4(3) . . ?
C10 N2 Tb1 115.8(3) . . ?
C10 N2 C11 118.6(4) . . ?
C11 N2 Tb1 124.5(2) . . ?
N1 C1 C2 117.7(3) . . ?
N1 C1 C6 121.9(4) . . ?
C6 C1 C2 120.4(4) . . ?
O1 C2 C1 117.8(3) . . ?
O1 C2 C3 124.1(4) . . ?
C3 C2 C1 118.0(4) . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 118.9 . . ?
C5 C4 C3 122.1(4) . . ?
C5 C4 H4 118.9 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.8(4) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C1 119.6(4) . . ?
C7 C6 C1 116.8(4) . . ?
C7 C6 C5 123.5(4) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(4) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.6(4) . . ?
C9 C8 H8 120.7 . . ?
N1 C9 C8 122.5(4) . . ?
N1 C9 C10 115.3(4) . . ?
C8 C9 C10 122.1(4) . . ?
N2 C10 C9 121.3(4) . . ?
N2 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C12 C11 N2 120.9(4) . . ?
C16 C11 N2 119.4(4) . . ?
C16 C11 C12 119.5(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.2(4) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.1(4) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 Cl1 119.8(4) . . ?
C15 C14 Cl1 119.0(4) . . ?
C15 C14 C13 121.2(4) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.9(4) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 120.0 . . ?
C15 C16 C11 120.1(4) . . ?
C15 C16 H16 120.0 . . ?
F1 C17 F2 107.3(4) . . ?
F1 C17 F3 107.1(4) . . ?
F1 C17 C18 112.9(4) . . ?
F2 C17 F3 106.4(4) . . ?
F2 C17 C18 109.6(4) . . ?
F3 C17 C18 113.2(4) . . ?
O2 C18 C17 114.1(4) . . ?
O2 C18 C19 127.3(4) . . ?
C19 C18 C17 118.6(4) . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.9(4) . . ?
C20 C19 H19 120.1 . . ?
O3 C20 C19 127.4(4) . . ?
O3 C20 C21 116.0(4) . . ?
C19 C20 C21 116.5(4) . . ?
F4 C21 F6 106.0(4) . . ?
F4 C21 C20 112.3(4) . . ?
F5 C21 F4 107.9(4) . . ?
F5 C21 F6 107.6(4) . . ?
F5 C21 C20 113.1(4) . . ?
F6 C21 C20 109.6(4) . . ?
F7 C22 C23 112.7(4) . . ?
F8 C22 F7 104.3(4) . . ?
F8 C22 C23 111.4(4) . . ?
F9 C22 F7 107.4(4) . . ?
F9 C22 F8 107.5(4) . . ?
F9 C22 C23 113.0(4) . . ?
F7' C22 F9' 105.0(6) . . ?
F7' C22 C23 111.0(7) . . ?
F8' C22 F7' 107.5(7) . . ?
F8' C22 F9' 106.4(7) . . ?
F8' C22 C23 113.2(8) . . ?
F9' C22 C23 113.3(8) . . ?
O4 C23 C22 115.4(4) . . ?
O4 C23 C24 128.5(4) . . ?
C24 C23 C22 116.1(4) . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.0(4) . . ?
C25 C24 H24 120.5 . . ?
O5 C25 C24 127.4(4) . . ?
O5 C25 C26 114.5(4) . . ?
C24 C25 C26 118.0(4) . . ?
F10 C26 C25 109.5(4) . . ?
F11 C26 F10 106.9(4) . . ?
F11 C26 F12 107.6(4) . . ?
F11 C26 C25 111.6(4) . . ?
F12 C26 F10 107.7(4) . . ?
F12 C26 C25 113.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C2 C1 -175.5(3) 3_656 . . . ?
Tb1 O1 C2 C1 -2.3(5) . . . . ?
Tb1 O1 C2 C3 178.8(3) . . . . ?
Tb1 O1 C2 C3 5.7(6) 3_656 . . . ?
Tb1 O2 C18 C17 152.6(3) . . . . ?
Tb1 O2 C18 C19 -25.4(7) . . . . ?
Tb1 O3 C20 C19 6.9(6) . . . . ?
Tb1 O3 C20 C21 -174.9(3) . . . . ?
Tb1 O4 C23 C22 -162.8(2) . . . . ?
Tb1 O4 C23 C24 19.9(7) . . . . ?
Tb1 O5 C25 C24 -19.7(7) . . . . ?
Tb1 O5 C25 C26 163.8(3) . . . . ?
Tb1 N1 C1 C2 -0.5(5) . . . . ?
Tb1 N1 C1 C6 178.8(3) . . . . ?
Tb1 N1 C9 C8 -179.5(3) . . . . ?
Tb1 N1 C9 C10 -2.5(5) . . . . ?
Tb1 N2 C10 C9 -0.7(5) . . . . ?
Tb1 N2 C11 C12 -122.5(4) . . . . ?
Tb1 N2 C11 C16 51.9(5) . . . . ?
Cl1 C14 C15 C16 176.7(3) . . . . ?
F1 C17 C18 O2 42.5(5) . . . . ?
F1 C17 C18 C19 -139.3(4) . . . . ?
F2 C17 C18 O2 -77.0(5) . . . . ?
F2 C17 C18 C19 101.2(5) . . . . ?
F3 C17 C18 O2 164.4(4) . . . . ?
F3 C17 C18 C19 -17.4(6) . . . . ?
F7 C22 C23 O4 9.1(6) . . . . ?
F7 C22 C23 C24 -173.3(5) . . . . ?
F8 C22 C23 O4 -107.8(5) . . . . ?
F8 C22 C23 C24 69.8(5) . . . . ?
F9 C22 C23 O4 131.1(5) . . . . ?
F9 C22 C23 C24 -51.3(6) . . . . ?
F7' C22 C23 O4 68.8(11) . . . . ?
F7' C22 C23 C24 -113.6(11) . . . . ?
F8' C22 C23 O4 -52.1(12) . . . . ?
F8' C22 C23 C24 125.5(12) . . . . ?
F9' C22 C23 O4 -173.3(11) . . . . ?
F9' C22 C23 C24 4.3(12) . . . . ?
O1 C2 C3 C4 177.7(4) . . . . ?
O2 C18 C19 C20 1.0(7) . . . . ?
O3 C20 C21 F4 138.8(4) . . . . ?
O3 C20 C21 F5 16.4(5) . . . . ?
O3 C20 C21 F6 -103.6(4) . . . . ?
O4 C23 C24 C25 5.2(7) . . . . ?
O5 C25 C26 F10 81.6(5) . . . . ?
O5 C25 C26 F11 -36.6(5) . . . . ?
O5 C25 C26 F12 -158.2(4) . . . . ?
N1 C1 C2 O1 1.8(6) . . . . ?
N1 C1 C2 C3 -179.3(4) . . . . ?
N1 C1 C6 C5 -179.8(4) . . . . ?
N1 C1 C6 C7 -0.7(6) . . . . ?
N1 C9 C10 N2 2.0(6) . . . . ?
N2 C11 C12 C13 173.5(4) . . . . ?
N2 C11 C16 C15 -174.6(4) . . . . ?
C1 N1 C9 C8 -3.8(6) . . . . ?
C1 N1 C9 C10 173.2(4) . . . . ?
C1 C2 C3 C4 -1.2(6) . . . . ?
C1 C6 C7 C8 -0.6(6) . . . . ?
C2 C1 C6 C5 -0.5(6) . . . . ?
C2 C1 C6 C7 178.6(4) . . . . ?
C2 C3 C4 C5 -0.1(7) . . . . ?
C3 C4 C5 C6 1.0(7) . . . . ?
C4 C5 C6 C1 -0.7(6) . . . . ?
C4 C5 C6 C7 -179.7(4) . . . . ?
C5 C6 C7 C8 178.4(4) . . . . ?
C6 C1 C2 O1 -177.4(4) . . . . ?
C6 C1 C2 C3 1.5(6) . . . . ?
C6 C7 C8 C9 -0.2(7) . . . . ?
C7 C8 C9 N1 2.5(7) . . . . ?
C7 C8 C9 C10 -174.3(4) . . . . ?
C8 C9 C10 N2 179.0(4) . . . . ?
C9 N1 C1 C2 -176.4(4) . . . . ?
C9 N1 C1 C6 2.9(6) . . . . ?
C10 N2 C11 C12 45.1(6) . . . . ?
C10 N2 C11 C16 -140.6(4) . . . . ?
C11 N2 C10 C9 -169.3(4) . . . . ?
C11 C12 C13 C14 0.5(7) . . . . ?
C12 C11 C16 C15 -0.2(6) . . . . ?
C12 C13 C14 Cl1 -177.6(4) . . . . ?
C12 C13 C14 C15 0.8(7) . . . . ?
C13 C14 C15 C16 -1.8(7) . . . . ?
C14 C15 C16 C11 1.5(7) . . . . ?
C16 C11 C12 C13 -0.8(6) . . . . ?
C17 C18 C19 C20 -176.9(4) . . . . ?
C18 C19 C20 O3 8.2(7) . . . . ?
C18 C19 C20 C21 -170.0(4) . . . . ?
C19 C20 C21 F4 -42.8(5) . . . . ?
C19 C20 C21 F5 -165.2(4) . . . . ?
C19 C20 C21 F6 74.7(5) . . . . ?
C22 C23 C24 C25 -172.1(4) . . . . ?
C23 C24 C25 O5 -5.0(7) . . . . ?
C23 C24 C25 C26 171.4(4) . . . . ?
C24 C25 C26 F10 -95.3(5) . . . . ?
C24 C25 C26 F11 146.6(4) . . . . ?
C24 C25 C26 F12 25.0(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1427272'
_audit_update_record             
;
2016-01-01 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H24 Cl2 F24 N4 O10 Y2'
_chemical_formula_sum            'C52 H24 Cl2 F24 N4 O10 Y2'
_chemical_formula_weight         1569.47
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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                   11.380(2)
_cell_length_b                   19.207(4)
_cell_length_c                   13.089(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.04(3)
_cell_angle_gamma                90
_cell_volume                     2849.9(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7554
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      34.8566
_cell_measurement_theta_min      1.8878
_shelx_estimated_absorpt_T_max   0.773
_shelx_estimated_absorpt_T_min   0.661
_exptl_absorpt_coefficient_mu    2.260
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8476
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.015
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         1.888
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1239
	          2theta: -29.8668
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1239
	          2theta: -29.8668
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1239
	          2theta: -29.8668
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_number_total             11062
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0846
_diffrn_orient_matrix_UB_12      0.0249
_diffrn_orient_matrix_UB_13      0.0032
_diffrn_orient_matrix_UB_21      -0.0124
_diffrn_orient_matrix_UB_22      -0.0379
_diffrn_orient_matrix_UB_23      -0.0334
_diffrn_orient_matrix_UB_31      -0.0183
_diffrn_orient_matrix_UB_32      -0.0458
_diffrn_orient_matrix_UB_33      0.0587
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4499
_reflns_number_total             5026
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5026
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0373
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+2.7731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0873
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-F7 \\sim C22-F8 \\sim C22-F9 \\sim C22-F7' \\sim C22-F8' \\sim C22-F9'
\\sim C22-F7" \\sim C22-F8" ~
 C22-F9"
 with sigma of 0.01
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F7'-F8' \\sim F7'-F9' \\sim F8'-F9' \\sim
F7"-F8" \\sim F7"-F9" \\sim F8"-
 F9"
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.05
Uanis(F9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F9) = Uanis(F9') = Uanis(F9")
Uanis(F8) = Uanis(F8') = Uanis(F8")
Uanis(F7) = Uanis(F7') = Uanis(F7")
4. Others
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7')+Sof(F8')+Sof(F9')]+1*[Sof(F7")+
 Sof(F8")+Sof(F9")]=1 with esd of 0.0001
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F7')=Sof(F8')=Sof(F9')=FVAR(2)
 Sof(F7")=Sof(F8")=Sof(F9")=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C19(H19), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.45831(2) 0.09249(2) 0.46854(2) 0.01718(9) Uani 1 1 d . . . . .
Cl1 Cl 0.66479(8) 0.46459(4) 0.40166(8) 0.0447(2) Uani 1 1 d . . . . .
F1 F 0.4207(2) 0.12284(13) 0.84304(16) 0.0641(7) Uani 1 1 d . . . . .
F2 F 0.33433(19) 0.21035(16) 0.76985(17) 0.0699(8) Uani 1 1 d . . . . .
F3 F 0.49718(18) 0.22404(12) 0.86164(15) 0.0509(6) Uani 1 1 d . . . . .
F4 F 0.74165(18) 0.31935(11) 0.6077(2) 0.0590(7) Uani 1 1 d . . . . .
F5 F 0.7852(2) 0.25775(14) 0.48123(15) 0.0621(7) Uani 1 1 d . . . . .
F6 F 0.84620(15) 0.22826(11) 0.63336(16) 0.0449(5) Uani 1 1 d . . . . .
F10 F 0.15588(17) -0.00569(12) 0.17272(16) 0.0511(6) Uani 1 1 d . . . . .
F11 F 0.22442(18) -0.08275(10) 0.28040(15) 0.0433(5) Uani 1 1 d . . . . .
F12 F 0.2915(2) -0.07672(12) 0.13265(17) 0.0563(6) Uani 1 1 d . . . . .
O1 O 0.39568(15) -0.01201(10) 0.54094(14) 0.0190(4) Uani 1 1 d . . . . .
O2 O 0.46318(17) 0.11913(11) 0.64364(14) 0.0236(4) Uani 1 1 d . . . . .
O3 O 0.61591(16) 0.16957(10) 0.51195(14) 0.0222(4) Uani 1 1 d . . . . .
O4 O 0.51213(17) 0.12258(10) 0.30633(14) 0.0232(4) Uani 1 1 d . . . . .
O5 O 0.33393(17) 0.03383(11) 0.34172(14) 0.0243(4) Uani 1 1 d . . . . .
N1 N 0.2580(2) 0.10200(12) 0.51866(17) 0.0202(5) Uani 1 1 d . . . . .
N2 N 0.3647(2) 0.21648(12) 0.45171(17) 0.0222(5) Uani 1 1 d . . . . .
C1 C 0.2119(2) 0.04461(15) 0.5605(2) 0.0208(6) Uani 1 1 d . . . . .
C2 C 0.2846(2) -0.01600(15) 0.5710(2) 0.0201(6) Uani 1 1 d . . . . .
C3 C 0.2380(3) -0.07464(16) 0.6138(2) 0.0238(6) Uani 1 1 d . . . . .
H3 H 0.2840 -0.1159 0.6212 0.029 Uiso 1 1 calc R . . . .
C4 C 0.1227(3) -0.07395(17) 0.6467(2) 0.0276(7) Uani 1 1 d . . . . .
H4 H 0.0928 -0.1150 0.6755 0.033 Uiso 1 1 calc R . . . .
C5 C 0.0531(3) -0.01571(17) 0.6380(2) 0.0286(7) Uani 1 1 d . . . . .
H5 H -0.0237 -0.0165 0.6611 0.034 Uiso 1 1 calc R . . . .
C6 C 0.0962(2) 0.04521(16) 0.5948(2) 0.0254(6) Uani 1 1 d . . . . .
C7 C 0.0315(3) 0.10785(17) 0.5829(2) 0.0292(7) Uani 1 1 d . . . . .
H7 H -0.0466 0.1099 0.6030 0.035 Uiso 1 1 calc R . . . .
C8 C 0.0809(3) 0.16589(16) 0.5425(2) 0.0277(7) Uani 1 1 d . . . . .
H8 H 0.0383 0.2084 0.5356 0.033 Uiso 1 1 calc R . . . .
C9 C 0.1960(2) 0.16100(15) 0.5115(2) 0.0229(6) Uani 1 1 d . . . . .
C10 C 0.2587(2) 0.22187(15) 0.4768(2) 0.0239(6) Uani 1 1 d . . . . .
H10 H 0.2204 0.2659 0.4727 0.029 Uiso 1 1 calc R . . . .
C11 C 0.4285(3) 0.27932(15) 0.4360(2) 0.0240(6) Uani 1 1 d . . . . .
C12 C 0.4293(3) 0.33452(16) 0.5056(2) 0.0285(7) Uani 1 1 d . . . . .
H12 H 0.3806 0.3326 0.5609 0.034 Uiso 1 1 calc R . . . .
C13 C 0.5000(3) 0.39143(16) 0.4946(3) 0.0323(7) Uani 1 1 d . . . . .
H13 H 0.5007 0.4287 0.5423 0.039 Uiso 1 1 calc R . . . .
C14 C 0.5703(3) 0.39428(16) 0.4133(3) 0.0298(7) Uani 1 1 d . . . . .
C15 C 0.5690(3) 0.34136(16) 0.3427(2) 0.0308(7) Uani 1 1 d . . . . .
H15 H 0.6157 0.3447 0.2862 0.037 Uiso 1 1 calc R . . . .
C16 C 0.4995(3) 0.28308(16) 0.3542(2) 0.0287(7) Uani 1 1 d . . . . .
H16 H 0.5001 0.2458 0.3065 0.034 Uiso 1 1 calc R . . . .
C17 C 0.4389(3) 0.18139(18) 0.7946(2) 0.0325(7) Uani 1 1 d . . . . .
C18 C 0.5018(2) 0.17018(16) 0.6973(2) 0.0227(6) Uani 1 1 d . . . . .
C19 C 0.5898(2) 0.21645(16) 0.6762(2) 0.0256(6) Uani 1 1 d . . . . .
H19 H 0.6129 0.2526 0.7232 0.031 Uiso 1 1 calc R . . . .
C20 C 0.6443(2) 0.20939(15) 0.5852(2) 0.0214(6) Uani 1 1 d . . . . .
C21 C 0.7547(3) 0.25456(16) 0.5755(2) 0.0278(7) Uani 1 1 d . . . . .
C22 C 0.5820(3) 0.12233(14) 0.1408(2) 0.0286(7) Uani 1 1 d D . . . .
C23 C 0.5037(3) 0.09287(15) 0.2200(2) 0.0225(6) Uani 1 1 d . . . . .
C24 C 0.4294(3) 0.03831(17) 0.1880(2) 0.0286(7) Uani 1 1 d . . . . .
H24 H 0.4348 0.0175 0.1227 0.034 Uiso 1 1 calc R . . . .
C25 C 0.3469(2) 0.01437(16) 0.2520(2) 0.0234(6) Uani 1 1 d . . . . .
C26 C 0.2545(3) -0.03853(18) 0.2080(2) 0.0323(7) Uani 1 1 d . . . . .
F7 F 0.6537(4) 0.1746(2) 0.1810(3) 0.0451(11) Uani 0.611(3) 1 d D U P A 1
F8 F 0.5177(3) 0.1529(2) 0.0624(3) 0.0375(10) Uani 0.611(3) 1 d D U P A 1
F9 F 0.6492(4) 0.0749(2) 0.1025(4) 0.0692(18) Uani 0.611(3) 1 d D U P A 1
F7' F 0.6893(6) 0.1392(6) 0.1775(7) 0.0451(11) Uani 0.236(3) 1 d D . P A 2
F8' F 0.5293(9) 0.1767(4) 0.0969(8) 0.0375(10) Uani 0.236(3) 1 d D . P A 2
F9' F 0.5932(11) 0.0753(5) 0.0656(9) 0.0692(18) Uani 0.236(3) 1 d D . P A 2
F7" F 0.5939(13) 0.1911(4) 0.1519(10) 0.0451(11) Uani 0.153(2) 1 d D . P A 3
F8" F 0.5439(12) 0.1108(7) 0.0437(6) 0.0375(10) Uani 0.153(2) 1 d D . P A 3
F9" F 0.6896(9) 0.0954(8) 0.1565(12) 0.0692(18) Uani 0.153(2) 1 d D . P A 3


_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
Y1 Y1 3.7502(9) 3_656 ?
Y1 O1 2.3564(19) . ?
Y1 O1 2.2808(18) 3_656 ?
Y1 O2 2.3443(19) . ?
Y1 O3 2.3564(19) . ?
Y1 O4 2.3335(19) . ?
Y1 O5 2.370(2) . ?
Y1 N1 2.434(2) . ?
Y1 N2 2.610(2) . ?
Cl1 C14 1.741(3) . ?
F1 C17 1.317(4) . ?
F2 C17 1.328(4) . ?
F3 C17 1.334(4) . ?
F4 C21 1.326(4) . ?
F5 C21 1.312(4) . ?
F6 C21 1.332(3) . ?
F10 C26 1.334(4) . ?
F11 C26 1.339(4) . ?
F12 C26 1.327(4) . ?
O1 Y1 2.2808(18) 3_656 ?
O1 C2 1.359(3) . ?
O2 C18 1.262(3) . ?
O3 C20 1.247(3) . ?
O4 C23 1.262(3) . ?
O5 C25 1.254(3) . ?
N1 C1 1.357(4) . ?
N1 C9 1.334(4) . ?
N2 C10 1.282(4) . ?
N2 C11 1.433(4) . ?
C1 C2 1.428(4) . ?
C1 C6 1.427(4) . ?
C2 C3 1.384(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.417(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.406(4) . ?
C6 C7 1.412(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.375(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.408(4) . ?
C9 C10 1.463(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.398(4) . ?
C11 C16 1.399(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(5) . ?
C14 C15 1.373(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.530(4) . ?
C18 C19 1.385(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.397(4) . ?
C20 C21 1.542(4) . ?
C22 C23 1.533(4) . ?
C22 F7 1.368(4) . ?
C22 F8 1.342(4) . ?
C22 F9 1.316(4) . ?
C22 F7' 1.312(6) . ?
C22 F8' 1.311(6) . ?
C22 F9' 1.350(6) . ?
C22 F7" 1.335(6) . ?
C22 F8" 1.326(6) . ?
C22 F9" 1.328(7) . ?
C23 C24 1.388(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(4) . ?
C25 C26 1.537(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 Y1 36.71(5) 3_656 3_656 ?
O1 Y1 Y1 35.36(4) . 3_656 ?
O1 Y1 O1 72.07(7) 3_656 . ?
O1 Y1 O2 104.26(7) 3_656 . ?
O1 Y1 O3 84.04(7) 3_656 . ?
O1 Y1 O4 82.40(7) 3_656 . ?
O1 Y1 O5 72.16(7) . . ?
O1 Y1 O5 91.88(7) 3_656 . ?
O1 Y1 N1 68.41(7) . . ?
O1 Y1 N1 140.32(7) 3_656 . ?
O1 Y1 N2 132.48(7) . . ?
O1 Y1 N2 155.18(7) 3_656 . ?
O2 Y1 Y1 90.47(5) . 3_656 ?
O2 Y1 O1 76.98(7) . . ?
O2 Y1 O3 71.03(7) . . ?
O2 Y1 O5 138.59(7) . . ?
O2 Y1 N1 70.27(7) . . ?
O2 Y1 N2 81.82(7) . . ?
O3 Y1 Y1 111.70(5) . 3_656 ?
O3 Y1 O1 133.53(7) . . ?
O3 Y1 O5 149.63(7) . . ?
O3 Y1 N1 126.79(7) . . ?
O3 Y1 N2 75.14(7) . . ?
O4 Y1 Y1 110.66(5) . 3_656 ?
O4 Y1 O1 133.61(7) . . ?
O4 Y1 O2 148.20(7) . . ?
O4 Y1 O3 78.97(7) . . ?
O4 Y1 O5 70.66(7) . . ?
O4 Y1 N1 123.61(7) . . ?
O4 Y1 N2 80.51(7) . . ?
O5 Y1 Y1 80.07(5) . 3_656 ?
O5 Y1 N1 73.05(7) . . ?
O5 Y1 N2 99.23(7) . . ?
N1 Y1 Y1 103.70(6) . 3_656 ?
N1 Y1 N2 64.48(7) . . ?
N2 Y1 Y1 167.52(5) . 3_656 ?
Y1 O1 Y1 107.93(7) 3_656 . ?
C2 O1 Y1 119.11(16) . . ?
C2 O1 Y1 132.71(17) . 3_656 ?
C18 O2 Y1 133.68(18) . . ?
C20 O3 Y1 135.32(18) . . ?
C23 O4 Y1 134.21(18) . . ?
C25 O5 Y1 133.30(18) . . ?
C1 N1 Y1 116.92(18) . . ?
C9 N1 Y1 123.18(18) . . ?
C9 N1 C1 119.8(2) . . ?
C10 N2 Y1 116.01(19) . . ?
C10 N2 C11 118.0(2) . . ?
C11 N2 Y1 124.91(17) . . ?
N1 C1 C2 117.4(2) . . ?
N1 C1 C6 121.4(3) . . ?
C6 C1 C2 121.3(3) . . ?
O1 C2 C1 118.2(2) . . ?
O1 C2 C3 124.2(3) . . ?
C3 C2 C1 117.6(2) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.9(3) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.8(3) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C7 123.8(3) . . ?
C7 C6 C1 117.3(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.6(3) . . ?
C9 C8 H8 120.7 . . ?
N1 C9 C8 122.4(3) . . ?
N1 C9 C10 115.6(2) . . ?
C8 C9 C10 121.8(3) . . ?
N2 C10 C9 120.7(3) . . ?
N2 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 N2 121.3(3) . . ?
C12 C11 C16 119.3(3) . . ?
C16 C11 N2 119.2(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.7(3) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 Cl1 120.0(3) . . ?
C15 C14 Cl1 119.0(3) . . ?
C15 C14 C13 120.9(3) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(3) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 120.1 . . ?
C15 C16 C11 119.8(3) . . ?
C15 C16 H16 120.1 . . ?
F1 C17 F2 107.4(3) . . ?
F1 C17 F3 107.3(3) . . ?
F1 C17 C18 112.7(3) . . ?
F2 C17 F3 106.6(3) . . ?
F2 C17 C18 109.3(3) . . ?
F3 C17 C18 113.1(2) . . ?
O2 C18 C17 114.0(2) . . ?
O2 C18 C19 127.6(3) . . ?
C19 C18 C17 118.3(3) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
O3 C20 C19 127.7(3) . . ?
O3 C20 C21 116.1(3) . . ?
C19 C20 C21 116.2(3) . . ?
F4 C21 F6 106.2(3) . . ?
F4 C21 C20 112.7(2) . . ?
F5 C21 F4 107.5(3) . . ?
F5 C21 F6 107.2(3) . . ?
F5 C21 C20 112.9(2) . . ?
F6 C21 C20 110.0(2) . . ?
F7 C22 C23 111.9(3) . . ?
F8 C22 C23 111.6(3) . . ?
F8 C22 F7 103.9(3) . . ?
F9 C22 C23 113.2(3) . . ?
F9 C22 F7 107.9(3) . . ?
F9 C22 F8 107.8(3) . . ?
F7' C22 C23 115.0(5) . . ?
F7' C22 F9' 106.7(5) . . ?
F8' C22 C23 108.6(5) . . ?
F8' C22 F7' 109.8(5) . . ?
F8' C22 F9' 106.4(5) . . ?
F9' C22 C23 110.1(6) . . ?
F7" C22 C23 110.6(6) . . ?
F8" C22 C23 115.2(6) . . ?
F8" C22 F7" 106.9(6) . . ?
F8" C22 F9" 107.6(6) . . ?
F9" C22 C23 109.6(7) . . ?
F9" C22 F7" 106.6(6) . . ?
O4 C23 C22 115.8(2) . . ?
O4 C23 C24 127.5(3) . . ?
C24 C23 C22 116.7(2) . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.6(3) . . ?
C25 C24 H24 120.2 . . ?
O5 C25 C24 127.4(3) . . ?
O5 C25 C26 114.5(2) . . ?
C24 C25 C26 118.0(3) . . ?
F10 C26 F11 106.6(3) . . ?
F10 C26 C25 110.1(3) . . ?
F11 C26 C25 111.3(2) . . ?
F12 C26 F10 108.5(3) . . ?
F12 C26 F11 107.0(3) . . ?
F12 C26 C25 113.1(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C2 C1 -2.2(3) . . . . ?
Y1 O1 C2 C1 -175.65(17) 3_656 . . . ?
Y1 O1 C2 C3 179.6(2) . . . . ?
Y1 O1 C2 C3 6.1(4) 3_656 . . . ?
Y1 O2 C18 C17 153.4(2) . . . . ?
Y1 O2 C18 C19 -24.7(4) . . . . ?
Y1 O3 C20 C19 6.1(5) . . . . ?
Y1 O3 C20 C21 -175.83(18) . . . . ?
Y1 O4 C23 C22 -163.09(17) . . . . ?
Y1 O4 C23 C24 19.0(4) . . . . ?
Y1 O5 C25 C24 -19.5(5) . . . . ?
Y1 O5 C25 C26 164.75(19) . . . . ?
Y1 N1 C1 C2 -0.2(3) . . . . ?
Y1 N1 C1 C6 178.4(2) . . . . ?
Y1 N1 C9 C8 -178.9(2) . . . . ?
Y1 N1 C9 C10 -3.4(3) . . . . ?
Y1 N2 C10 C9 -0.5(3) . . . . ?
Y1 N2 C11 C12 -121.0(2) . . . . ?
Y1 N2 C11 C16 53.4(3) . . . . ?
Cl1 C14 C15 C16 176.3(2) . . . . ?
F1 C17 C18 O2 43.2(4) . . . . ?
F1 C17 C18 C19 -138.5(3) . . . . ?
F2 C17 C18 O2 -76.2(4) . . . . ?
F2 C17 C18 C19 102.1(3) . . . . ?
F3 C17 C18 O2 165.2(3) . . . . ?
F3 C17 C18 C19 -16.5(4) . . . . ?
O1 C2 C3 C4 177.7(3) . . . . ?
O2 C18 C19 C20 1.3(5) . . . . ?
O3 C20 C21 F4 138.6(3) . . . . ?
O3 C20 C21 F5 16.5(4) . . . . ?
O3 C20 C21 F6 -103.1(3) . . . . ?
O4 C23 C24 C25 5.0(5) . . . . ?
O5 C25 C26 F10 81.7(3) . . . . ?
O5 C25 C26 F11 -36.3(4) . . . . ?
O5 C25 C26 F12 -156.8(3) . . . . ?
N1 C1 C2 O1 1.6(4) . . . . ?
N1 C1 C2 C3 179.9(2) . . . . ?
N1 C1 C6 C5 -179.7(3) . . . . ?
N1 C1 C6 C7 0.3(4) . . . . ?
N1 C9 C10 N2 2.5(4) . . . . ?
N2 C11 C12 C13 173.6(3) . . . . ?
N2 C11 C16 C15 -174.9(3) . . . . ?
C1 N1 C9 C8 -2.5(4) . . . . ?
C1 N1 C9 C10 173.0(2) . . . . ?
C1 C2 C3 C4 -0.6(4) . . . . ?
C1 C6 C7 C8 -1.8(4) . . . . ?
C2 C1 C6 C5 -1.1(4) . . . . ?
C2 C1 C6 C7 178.9(3) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C3 C4 C5 C6 0.4(5) . . . . ?
C4 C5 C6 C1 0.3(4) . . . . ?
C4 C5 C6 C7 -179.8(3) . . . . ?
C5 C6 C7 C8 178.2(3) . . . . ?
C6 C1 C2 O1 -177.1(2) . . . . ?
C6 C1 C2 C3 1.3(4) . . . . ?
C6 C7 C8 C9 1.2(5) . . . . ?
C7 C8 C9 N1 1.0(4) . . . . ?
C7 C8 C9 C10 -174.2(3) . . . . ?
C8 C9 C10 N2 178.0(3) . . . . ?
C9 N1 C1 C2 -176.9(2) . . . . ?
C9 N1 C1 C6 1.8(4) . . . . ?
C10 N2 C11 C12 46.5(4) . . . . ?
C10 N2 C11 C16 -139.1(3) . . . . ?
C11 N2 C10 C9 -169.1(2) . . . . ?
C11 C12 C13 C14 0.5(5) . . . . ?
C12 C11 C16 C15 -0.3(4) . . . . ?
C12 C13 C14 Cl1 -177.4(2) . . . . ?
C12 C13 C14 C15 1.0(5) . . . . ?
C13 C14 C15 C16 -2.1(5) . . . . ?
C14 C15 C16 C11 1.7(5) . . . . ?
C16 C11 C12 C13 -0.8(4) . . . . ?
C17 C18 C19 C20 -176.7(3) . . . . ?
C18 C19 C20 O3 7.9(5) . . . . ?
C18 C19 C20 C21 -170.1(3) . . . . ?
C19 C20 C21 F4 -43.2(4) . . . . ?
C19 C20 C21 F5 -165.2(3) . . . . ?
C19 C20 C21 F6 75.2(3) . . . . ?
C22 C23 C24 C25 -172.9(3) . . . . ?
C23 C24 C25 O5 -4.4(5) . . . . ?
C23 C24 C25 C26 171.2(3) . . . . ?
C24 C25 C26 F10 -94.5(3) . . . . ?
C24 C25 C26 F11 147.5(3) . . . . ?
C24 C25 C26 F12 27.0(4) . . . . ?
F7 C22 C23 O4 3.4(4) . . . . ?
F7 C22 C23 C24 -178.5(3) . . . . ?
F8 C22 C23 O4 -112.5(3) . . . . ?
F8 C22 C23 C24 65.6(4) . . . . ?
F9 C22 C23 O4 125.6(4) . . . . ?
F9 C22 C23 C24 -56.3(4) . . . . ?
F7' C22 C23 O4 40.8(7) . . . . ?
F7' C22 C23 C24 -141.0(6) . . . . ?
F8' C22 C23 O4 -82.6(6) . . . . ?
F8' C22 C23 C24 95.6(6) . . . . ?
F9' C22 C23 O4 161.3(6) . . . . ?
F9' C22 C23 C24 -20.5(7) . . . . ?
F7" C22 C23 O4 -34.3(8) . . . . ?
F7" C22 C23 C24 143.8(7) . . . . ?
F8" C22 C23 O4 -155.7(8) . . . . ?
F8" C22 C23 C24 22.5(8) . . . . ?
F9" C22 C23 O4 82.9(8) . . . . ?
F9" C22 C23 C24 -98.9(8) . . . . ?

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