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

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

data_p140527e
_database_code_depnum_ccdc_archive 'CCDC 1025969'
_audit_update_record             
;
2014-09-24 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_audit_creation_date             2014-09-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '2(C15 H19 N2 O4)'
_chemical_formula_sum            'C30 H38 N4 O8'
_chemical_formula_weight         582.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N'
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'

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

_cell_length_a                   9.5761(6)
_cell_length_b                   10.1949(7)
_cell_length_c                   15.8509(10)
_cell_angle_alpha                102.611(6)
_cell_angle_beta                 96.527(5)
_cell_angle_gamma                96.021(5)
_cell_volume                     1486.88(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    130.65(10)
_cell_measurement_theta_max      28.8820
_cell_measurement_theta_min      3.7510
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10464
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.96
_diffrn_ambient_temperature      130.65(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   57.0000 -150.0000 78

#__ type_ start__ end____ width___ exp.time_
  2 omega  -26.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   19.0000  150.0000 109

#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   81.0000  147.0000 27

#__ type_ start__ end____ width___ exp.time_
  4 omega   -8.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000  -60.0000 66

#__ type_ start__ end____ width___ exp.time_
  5 omega  -46.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -57.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
  6 omega  -35.00   10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1310  -81.0000   24.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0704027000
_diffrn_orient_matrix_UB_12      0.0143439000
_diffrn_orient_matrix_UB_13      0.0030001000
_diffrn_orient_matrix_UB_21      0.0240979000
_diffrn_orient_matrix_UB_22      0.0484752000
_diffrn_orient_matrix_UB_23      0.0398500000
_diffrn_orient_matrix_UB_31      0.0110523000
_diffrn_orient_matrix_UB_32      0.0511847000
_diffrn_orient_matrix_UB_33      -0.0234114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4333
_reflns_number_total             5240
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0440P)²+0.2320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0992
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C24(H24), C28(H28), C9(H9), C13(H13), C27(H27), C25(H25)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C3(H3A,H3B,H3C),
 C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C),
 C30(H30A,H30B,H30C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
O6 O 0.50663(11) 0.42178(12) 0.27934(8) 0.0294(3) Uani 1 1 d . . .
O4 O 0.07599(12) 0.93601(12) 0.13552(7) 0.0280(3) Uani 1 1 d . . .
O1 O -0.21012(12) 0.33447(12) 0.40126(7) 0.0277(3) Uani 1 1 d . . .
O8 O -0.66465(11) 0.77607(13) -0.09964(7) 0.0299(3) Uani 1 1 d . . .
O2 O 0.00677(11) -0.05391(12) 0.37162(7) 0.0287(3) Uani 1 1 d . . .
O3 O -0.13222(12) 0.49202(12) 0.09635(8) 0.0322(3) Uani 1 1 d . . .
N4 N 0.05668(13) 0.81043(14) 0.13700(8) 0.0202(3) Uani 1 1 d . . .
N2 N -0.08765(13) 0.02641(13) 0.38137(8) 0.0188(3) Uani 1 1 d . . .
N1 N -0.19000(13) 0.21152(14) 0.39808(8) 0.0188(3) Uani 1 1 d . . .
O7 O -0.53029(12) 0.92834(14) -0.14939(8) 0.0378(3) Uani 1 1 d . . .
N3 N -0.04401(13) 0.60117(14) 0.12066(8) 0.0217(3) Uani 1 1 d . . .
C8 C 0.06528(15) 0.23819(16) 0.37568(9) 0.0186(3) Uani 1 1 d . . .
C12 C 0.24161(16) 0.43455(17) 0.42627(10) 0.0236(4) Uani 1 1 d . . .
H12 H 0.2767 0.5153 0.4668 0.028 Uiso 1 1 calc . . R
C26 C -0.41896(16) 0.80772(17) -0.05300(9) 0.0215(4) Uani 1 1 d . . .
C10 C 0.26425(16) 0.26556(17) 0.29821(10) 0.0212(4) Uani 1 1 d . . .
H10 H 0.3139 0.2340 0.2524 0.025 Uiso 1 1 calc . . R
C22 C -0.06106(16) 0.72177(17) 0.10165(9) 0.0200(3) Uani 1 1 d . . .
C24 C -0.16853(17) 0.84945(17) 0.00030(10) 0.0234(4) Uani 1 1 d . . .
H24 H -0.0793 0.8964 0.0018 0.028 Uiso 1 1 calc . . R
C28 C -0.32006(16) 0.67961(17) 0.04459(10) 0.0224(4) Uani 1 1 d . . .
H28 H -0.3321 0.6131 0.0760 0.027 Uiso 1 1 calc . . R
C9 C 0.14033(16) 0.18990(17) 0.30742(10) 0.0209(3) Uani 1 1 d . . .
H9 H 0.1073 0.1073 0.2683 0.025 Uiso 1 1 calc . . R
C13 C 0.11669(16) 0.36048(17) 0.43491(10) 0.0221(4) Uani 1 1 d . . .
H13 H 0.0669 0.3926 0.4805 0.027 Uiso 1 1 calc . . R
C7 C -0.06776(15) 0.16014(16) 0.38478(9) 0.0179(3) Uani 1 1 d . . .
C14 C 0.44391(17) 0.47686(18) 0.34760(11) 0.0269(4) Uani 1 1 d . . .
C27 C -0.43553(16) 0.70753(17) -0.00631(10) 0.0226(4) Uani 1 1 d . . .
H27 H -0.5246 0.6591 -0.0093 0.027 Uiso 1 1 calc . . R
C1 C -0.29213(17) 0.14498(18) 0.51733(10) 0.0264(4) Uani 1 1 d . . .
H1A H -0.1984 0.1394 0.5438 0.040 Uiso 1 1 calc . . GR
H1B H -0.3593 0.0822 0.5342 0.040 Uiso 1 1 calc . . GR
H1C H -0.3144 0.2354 0.5364 0.040 Uiso 1 1 calc . . GR
C11 C 0.31480(16) 0.38837(17) 0.35705(10) 0.0207(4) Uani 1 1 d . . .
C23 C -0.18530(16) 0.75108(17) 0.04901(9) 0.0197(3) Uani 1 1 d . . .
O5 O 0.48584(15) 0.58711(14) 0.39396(10) 0.0527(4) Uani 1 1 d . . .
C2 C -0.29893(15) 0.10982(16) 0.41819(9) 0.0190(3) Uani 1 1 d . . .
C16 C 0.04396(17) 0.61950(19) 0.27337(10) 0.0269(4) Uani 1 1 d . . .
H16A H 0.0006 0.7004 0.2894 0.040 Uiso 1 1 calc . . GR
H16B H 0.1255 0.6227 0.3154 0.040 Uiso 1 1 calc . . GR
H16C H -0.0229 0.5417 0.2720 0.040 Uiso 1 1 calc . . GR
C29 C -0.54111(17) 0.84513(18) -0.10626(10) 0.0247(4) Uani 1 1 d . . .
C25 C -0.28486(17) 0.87682(18) -0.05010(10) 0.0253(4) Uani 1 1 d . . .
H25 H -0.2731 0.9422 -0.0824 0.030 Uiso 1 1 calc . . R
C17 C 0.08975(16) 0.60944(17) 0.18273(10) 0.0214(4) Uani 1 1 d . . .
C4 C -0.24113(15) -0.02505(17) 0.38167(9) 0.0190(3) Uani 1 1 d . . .
C19 C 0.17488(16) 0.74173(17) 0.17194(9) 0.0210(4) Uani 1 1 d . . .
C18 C 0.15859(19) 0.48266(19) 0.15556(11) 0.0318(4) Uani 1 1 d . . .
H18A H 0.1001 0.4061 0.1647 0.048 Uiso 1 1 calc . . GR
H18B H 0.2501 0.4930 0.1898 0.048 Uiso 1 1 calc . . GR
H18C H 0.1693 0.4685 0.0949 0.048 Uiso 1 1 calc . . GR
C3 C -0.44549(16) 0.12390(19) 0.37515(11) 0.0264(4) Uani 1 1 d . . .
H3A H -0.4705 0.2112 0.4007 0.040 Uiso 1 1 calc . . GR
H3B H -0.5139 0.0541 0.3840 0.040 Uiso 1 1 calc . . GR
H3C H -0.4444 0.1153 0.3137 0.040 Uiso 1 1 calc . . GR
C6 C -0.30050(17) -0.09235(18) 0.28652(10) 0.0267(4) Uani 1 1 d . . .
H6A H -0.2939 -0.0262 0.2519 0.040 Uiso 1 1 calc . . GR
H6B H -0.3980 -0.1292 0.2829 0.040 Uiso 1 1 calc . . GR
H6C H -0.2468 -0.1639 0.2651 0.040 Uiso 1 1 calc . . GR
C20 C 0.25713(17) 0.83332(18) 0.25540(10) 0.0256(4) Uani 1 1 d . . .
H20A H 0.3089 0.9102 0.2419 0.038 Uiso 1 1 calc . . GR
H20B H 0.3222 0.7837 0.2820 0.038 Uiso 1 1 calc . . GR
H20C H 0.1922 0.8639 0.2950 0.038 Uiso 1 1 calc . . GR
C5 C -0.24942(17) -0.12900(18) 0.43757(11) 0.0269(4) Uani 1 1 d . . .
H5A H -0.2048 -0.2053 0.4123 0.040 Uiso 1 1 calc . . GR
H5B H -0.3470 -0.1587 0.4402 0.040 Uiso 1 1 calc . . GR
H5C H -0.2017 -0.0885 0.4955 0.040 Uiso 1 1 calc . . GR
C21 C 0.27197(18) 0.7190(2) 0.10123(11) 0.0301(4) Uani 1 1 d . . .
H21A H 0.2192 0.6630 0.0482 0.045 Uiso 1 1 calc . . GR
H21B H 0.3496 0.6750 0.1201 0.045 Uiso 1 1 calc . . GR
H21C H 0.3080 0.8048 0.0910 0.045 Uiso 1 1 calc . . GR
C30 C -0.79040(18) 0.8042(2) -0.14959(12) 0.0370(5) Uani 1 1 d . . .
H30A H -0.7830 0.7793 -0.2108 0.055 Uiso 1 1 calc . . GR
H30B H -0.7983 0.8992 -0.1330 0.055 Uiso 1 1 calc . . GR
H30C H -0.8729 0.7527 -0.1380 0.055 Uiso 1 1 calc . . GR
C15 C 0.63303(19) 0.5029(2) 0.26698(13) 0.0372(5) Uani 1 1 d . . .
H15A H 0.6649 0.4605 0.2136 0.056 Uiso 1 1 calc . . GR
H15B H 0.7062 0.5100 0.3151 0.056 Uiso 1 1 calc . . GR
H15C H 0.6117 0.5918 0.2640 0.056 Uiso 1 1 calc . . GR


_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
O6 C14 1.342(2) . ?
O6 C15 1.450(2) . ?
O4 N4 1.2800(17) . ?
O1 N1 1.2790(17) . ?
O8 C29 1.3388(19) . ?
O8 C30 1.4540(18) . ?
O2 N2 1.2821(16) . ?
O3 N3 1.2814(17) . ?
N4 C22 1.350(2) . ?
N4 C19 1.5072(19) . ?
N2 C7 1.345(2) . ?
N2 C4 1.5087(19) . ?
N1 C7 1.3511(19) . ?
N1 C2 1.5026(19) . ?
O7 C29 1.2036(18) . ?
N3 C22 1.350(2) . ?
N3 C17 1.5068(18) . ?
C8 C9 1.396(2) . ?
C8 C13 1.390(2) . ?
C8 C7 1.468(2) . ?
C12 C13 1.383(2) . ?
C12 C11 1.391(2) . ?
C26 C27 1.392(2) . ?
C26 C29 1.495(2) . ?
C26 C25 1.389(2) . ?
C10 C9 1.386(2) . ?
C10 C11 1.390(2) . ?
C22 C23 1.469(2) . ?
C24 C23 1.400(2) . ?
C24 C25 1.385(2) . ?
C28 C27 1.385(2) . ?
C28 C23 1.400(2) . ?
C14 C11 1.494(2) . ?
C14 O5 1.201(2) . ?
C1 C2 1.526(2) . ?
C2 C4 1.555(2) . ?
C2 C3 1.524(2) . ?
C16 C17 1.535(2) . ?
C17 C19 1.554(2) . ?
C17 C18 1.514(2) . ?
C4 C6 1.530(2) . ?
C4 C5 1.524(2) . ?
C19 C20 1.521(2) . ?
C19 C21 1.531(2) . ?

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
C14 O6 C15 115.18(14) . . ?
C29 O8 C30 116.41(12) . . ?
O4 N4 C22 126.28(13) . . ?
O4 N4 C19 121.42(12) . . ?
C22 N4 C19 111.99(13) . . ?
O2 N2 C7 125.94(13) . . ?
O2 N2 C4 121.81(13) . . ?
C7 N2 C4 112.01(12) . . ?
O1 N1 C7 125.57(13) . . ?
O1 N1 C2 122.38(12) . . ?
C7 N1 C2 111.79(12) . . ?
O3 N3 C22 126.56(12) . . ?
O3 N3 C17 121.24(12) . . ?
C22 N3 C17 112.01(12) . . ?
C9 C8 C7 120.06(14) . . ?
C13 C8 C9 119.83(14) . . ?
C13 C8 C7 120.11(14) . . ?
C13 C12 C11 120.06(16) . . ?
C27 C26 C29 122.36(14) . . ?
C25 C26 C27 119.43(14) . . ?
C25 C26 C29 118.20(13) . . ?
C9 C10 C11 120.37(15) . . ?
N4 C22 C23 125.44(14) . . ?
N3 C22 N4 108.77(12) . . ?
N3 C22 C23 125.76(14) . . ?
C25 C24 C23 119.99(15) . . ?
C27 C28 C23 120.31(14) . . ?
C10 C9 C8 119.71(15) . . ?
C12 C13 C8 120.25(15) . . ?
N2 C7 N1 109.05(13) . . ?
N2 C7 C8 125.63(14) . . ?
N1 C7 C8 125.31(14) . . ?
O6 C14 C11 112.62(15) . . ?
O5 C14 O6 123.00(16) . . ?
O5 C14 C11 124.35(16) . . ?
C28 C27 C26 120.32(15) . . ?
C12 C11 C14 117.75(15) . . ?
C10 C11 C12 119.76(14) . . ?
C10 C11 C14 122.46(15) . . ?
C24 C23 C22 119.62(14) . . ?
C24 C23 C28 119.16(14) . . ?
C28 C23 C22 121.19(13) . . ?
N1 C2 C1 105.75(12) . . ?
N1 C2 C4 101.09(11) . . ?
N1 C2 C3 109.55(11) . . ?
C1 C2 C4 113.76(12) . . ?
C3 C2 C1 110.13(13) . . ?
C3 C2 C4 115.66(13) . . ?
O8 C29 C26 111.99(13) . . ?
O7 C29 O8 123.80(14) . . ?
O7 C29 C26 124.21(15) . . ?
C24 C25 C26 120.75(14) . . ?
N3 C17 C16 106.12(12) . . ?
N3 C17 C19 101.04(11) . . ?
N3 C17 C18 109.31(13) . . ?
C16 C17 C19 114.07(14) . . ?
C18 C17 C16 110.70(13) . . ?
C18 C17 C19 114.72(13) . . ?
N2 C4 C2 100.77(12) . . ?
N2 C4 C6 105.78(12) . . ?
N2 C4 C5 109.29(12) . . ?
C6 C4 C2 114.27(12) . . ?
C5 C4 C2 115.54(13) . . ?
C5 C4 C6 110.21(14) . . ?
N4 C19 C17 100.71(12) . . ?
N4 C19 C20 110.08(14) . . ?
N4 C19 C21 105.90(12) . . ?
C20 C19 C17 115.62(12) . . ?
C20 C19 C21 109.65(13) . . ?
C21 C19 C17 114.05(14) . . ?

####################################################################### 
# 
# 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_p131204f
_database_code_depnum_ccdc_archive 'CCDC 1025970'
_audit_update_record             
;
2014-09-24 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H41 F18 Gd N4 O14'
_chemical_formula_weight         1361.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.0143(8)
_cell_length_b                   10.4711(5)
_cell_length_c                   21.5686(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.242(3)
_cell_angle_gamma                90.00
_cell_volume                     5419.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2708
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10343
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4766
_reflns_number_gt                4386
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0165P)²+2.0315P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4766
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.5000 0.83796(2) 0.2500 0.01511(7) Uani 1 2 d S . .
F1 F 0.55057(10) 1.3412(2) 0.15951(11) 0.0619(7) Uani 1 1 d . . .
O2 O 0.55107(9) 0.6592(2) 0.29128(9) 0.0267(5) Uani 1 1 d . . .
O42 O 0.79921(11) 0.6879(3) 0.11932(10) 0.0445(7) Uani 1 1 d . . .
F2 F 0.55110(9) 1.1740(2) 0.10206(8) 0.0500(6) Uani 1 1 d . . .
O1 O 0.57061(8) 0.9173(2) 0.31782(8) 0.0229(5) Uani 1 1 d . . .
O3 O 0.55635(8) 0.7611(2) 0.17113(8) 0.0223(5) Uani 1 1 d . . .
F6 F 0.65350(10) 0.5762(3) 0.09700(9) 0.0746(9) Uani 1 1 d . . .
F4 F 0.56993(10) 0.6034(3) 0.06272(8) 0.0677(8) Uani 1 1 d . . .
F8 F 0.56870(10) 0.4466(3) 0.35444(11) 0.0707(8) Uani 1 1 d . . .
F5 F 0.62420(9) 0.7624(2) 0.07499(8) 0.0513(6) Uani 1 1 d . . .
F9 F 0.62644(11) 0.3781(2) 0.29000(9) 0.0631(7) Uani 1 1 d . . .
O4 O 0.53769(8) 1.0212(2) 0.20083(8) 0.0192(5) Uani 1 1 d . . .
F7 F 0.64876(10) 0.5305(2) 0.35152(9) 0.0573(6) Uani 1 1 d . . .
F3 F 0.61719(8) 1.2064(2) 0.16911(9) 0.0513(6) Uani 1 1 d . . .
O5 O 0.73685(9) 0.8277(3) 0.42394(9) 0.0488(8) Uani 1 1 d . . .
O40 O 0.76263(9) 0.8743(2) 0.08570(9) 0.0310(6) Uani 1 1 d . . .
N1 N 0.60687(9) 0.8912(2) 0.36241(10) 0.0195(6) Uani 1 1 d . . .
N2 N 0.68541(10) 0.8491(3) 0.41289(11) 0.0291(7) Uani 1 1 d . . .
C3 C 0.5000 1.2049(5) 0.2500 0.0285(11) Uani 1 2 d S . .
H3 H 0.5000 1.2937 0.2500 0.034 Uiso 1 2 calc SR . .
C23 C 0.66006(12) 0.8617(3) 0.35573(12) 0.0225(7) Uani 1 1 d . . .
C17 C 0.53719(13) 0.8449(4) 0.44011(13) 0.0347(9) Uani 1 1 d . . .
H17A H 0.5077 0.8880 0.4173 0.052 Uiso 1 1 calc R . .
H17B H 0.5300 0.8468 0.4836 0.052 Uiso 1 1 calc R . .
H17C H 0.5392 0.7578 0.4264 0.052 Uiso 1 1 calc R . .
C19 C 0.63723(14) 0.7137(4) 0.48413(14) 0.0353(8) Uani 1 1 d . . .
H19A H 0.6229 0.6639 0.4497 0.053 Uiso 1 1 calc R . .
H19B H 0.6117 0.7098 0.5173 0.053 Uiso 1 1 calc R . .
H19C H 0.6727 0.6801 0.4982 0.053 Uiso 1 1 calc R . .
C8 C 0.60737(14) 0.4829(3) 0.31631(14) 0.0334(8) Uani 1 1 d . . .
C11 C 0.69895(12) 0.8967(3) 0.18937(13) 0.0223(7) Uani 1 1 d . . .
H11 H 0.6896 0.9467 0.1549 0.027 Uiso 1 1 calc R . .
C7 C 0.58565(12) 0.5842(3) 0.26976(13) 0.0225(7) Uani 1 1 d . . .
C21 C 0.59232(12) 0.9116(3) 0.42907(12) 0.0243(7) Uani 1 1 d . . .
C10 C 0.67204(11) 0.9162(3) 0.24428(12) 0.0204(7) Uani 1 1 d . . .
H10 H 0.6440 0.9772 0.2465 0.024 Uiso 1 1 calc R . .
C12 C 0.73939(12) 0.8040(3) 0.18537(13) 0.0245(7) Uani 1 1 d . . .
C6 C 0.60640(13) 0.5819(3) 0.21043(13) 0.0259(7) Uani 1 1 d . . .
H6 H 0.6323 0.5200 0.2005 0.031 Uiso 1 1 calc R . .
C1 C 0.53103(12) 1.1385(3) 0.20671(13) 0.0229(7) Uani 1 1 d . . .
C9 C 0.68761(12) 0.8431(3) 0.29633(13) 0.0222(7) Uani 1 1 d . . .
C5 C 0.58929(12) 0.6697(3) 0.16600(13) 0.0222(7) Uani 1 1 d . . .
C18 C 0.58618(13) 1.0555(3) 0.43699(14) 0.0327(8) Uani 1 1 d . . .
H18A H 0.6209 1.0965 0.4289 0.049 Uiso 1 1 calc R . .
H18B H 0.5761 1.0740 0.4787 0.049 Uiso 1 1 calc R . .
H18C H 0.5577 1.0867 0.4084 0.049 Uiso 1 1 calc R . .
C2 C 0.56238(14) 1.2177(3) 0.15950(14) 0.0316(8) Uani 1 1 d . . .
C15 C 0.77029(13) 0.7795(4) 0.12709(14) 0.0290(8) Uani 1 1 d . . .
C22 C 0.64414(12) 0.8520(3) 0.46387(12) 0.0241(7) Uani 1 1 d . . .
C13 C 0.75396(13) 0.7299(4) 0.23693(14) 0.0340(8) Uani 1 1 d . . .
H13 H 0.7809 0.6667 0.2340 0.041 Uiso 1 1 calc R . .
C20 C 0.66845(13) 0.9318(4) 0.51744(13) 0.0361(9) Uani 1 1 d . . .
H20A H 0.7012 0.8906 0.5349 0.054 Uiso 1 1 calc R . .
H20B H 0.6413 0.9403 0.5487 0.054 Uiso 1 1 calc R . .
H20C H 0.6782 1.0149 0.5025 0.054 Uiso 1 1 calc R . .
C14 C 0.72861(13) 0.7497(4) 0.29245(13) 0.0320(8) Uani 1 1 d . . .
H14 H 0.7389 0.7009 0.3271 0.038 Uiso 1 1 calc R . .
C16 C 0.79743(14) 0.8676(4) 0.03198(13) 0.0393(10) Uani 1 1 d . . .
H16A H 0.7859 0.9320 0.0025 0.059 Uiso 1 1 calc R . .
H16B H 0.7937 0.7849 0.0131 0.059 Uiso 1 1 calc R . .
H16C H 0.8357 0.8815 0.0449 0.059 Uiso 1 1 calc R . .
C4 C 0.60957(15) 0.6522(3) 0.09943(14) 0.0330(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.3475(19) . ?
Gd1 O1 2.3475(19) 2_655 ?
Gd1 O3 2.3564(17) . ?
Gd1 O3 2.3564(17) 2_655 ?
Gd1 O4 2.3875(19) . ?
Gd1 O4 2.3875(19) 2_655 ?
Gd1 O2 2.390(2) 2_655 ?
Gd1 O2 2.390(2) . ?
F1 C2 1.324(4) . ?
O2 C7 1.246(3) . ?
O42 C15 1.200(4) . ?
F2 C2 1.338(4) . ?
O1 N1 1.301(3) . ?
O3 C5 1.249(4) . ?
F6 C4 1.324(4) . ?
F4 C4 1.317(4) . ?
F8 C8 1.320(4) . ?
F5 C4 1.322(4) . ?
F9 C8 1.325(4) . ?
O4 C1 1.246(4) . ?
F7 C8 1.324(4) . ?
F3 C2 1.330(4) . ?
O5 N2 1.269(3) . ?
O40 C15 1.343(4) . ?
O40 C16 1.457(3) . ?
N1 C23 1.328(4) . ?
N1 C21 1.508(3) . ?
N2 C23 1.360(4) . ?
N2 C22 1.509(3) . ?
C3 C1 1.402(4) . ?
C3 C1 1.402(4) 2_655 ?
C23 C9 1.478(4) . ?
C17 C21 1.524(4) . ?
C19 C22 1.524(5) . ?
C8 C7 1.538(4) . ?
C11 C12 1.378(4) . ?
C11 C10 1.386(4) . ?
C7 C6 1.392(4) . ?
C21 C18 1.525(5) . ?
C21 C22 1.558(4) . ?
C10 C9 1.398(4) . ?
C12 C13 1.389(4) . ?
C12 C15 1.506(4) . ?
C6 C5 1.379(4) . ?
C1 C2 1.533(4) . ?
C9 C14 1.393(4) . ?
C5 C4 1.545(4) . ?
C22 C20 1.524(4) . ?
C13 C14 1.380(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 Gd1 O1 138.54(11) . 2_655 ?
O1 Gd1 O3 98.60(6) . . ?
O1 Gd1 O3 95.29(6) 2_655 . ?
O1 Gd1 O3 95.29(6) . 2_655 ?
O1 Gd1 O3 98.60(6) 2_655 2_655 ?
O3 Gd1 O3 140.06(10) . 2_655 ?
O1 Gd1 O4 73.45(7) . . ?
O1 Gd1 O4 73.50(7) 2_655 . ?
O3 Gd1 O4 73.47(7) . . ?
O3 Gd1 O4 146.46(7) 2_655 . ?
O1 Gd1 O4 73.50(7) . 2_655 ?
O1 Gd1 O4 73.45(7) 2_655 2_655 ?
O3 Gd1 O4 146.46(7) . 2_655 ?
O3 Gd1 O4 73.47(7) 2_655 2_655 ?
O4 Gd1 O4 73.04(9) . 2_655 ?
O1 Gd1 O2 148.95(8) . 2_655 ?
O1 Gd1 O2 72.39(7) 2_655 2_655 ?
O3 Gd1 O2 76.38(7) . 2_655 ?
O3 Gd1 O2 72.58(7) 2_655 2_655 ?
O4 Gd1 O2 131.43(6) . 2_655 ?
O4 Gd1 O2 126.64(7) 2_655 2_655 ?
O1 Gd1 O2 72.39(7) . . ?
O1 Gd1 O2 148.95(8) 2_655 . ?
O3 Gd1 O2 72.58(7) . . ?
O3 Gd1 O2 76.38(7) 2_655 . ?
O4 Gd1 O2 126.64(7) . . ?
O4 Gd1 O2 131.43(6) 2_655 . ?
O2 Gd1 O2 76.94(11) 2_655 . ?
C7 O2 Gd1 134.01(18) . . ?
N1 O1 Gd1 146.36(18) . . ?
C5 O3 Gd1 135.17(18) . . ?
C1 O4 Gd1 134.01(18) . . ?
C15 O40 C16 115.1(3) . . ?
O1 N1 C23 126.0(2) . . ?
O1 N1 C21 120.1(2) . . ?
C23 N1 C21 113.3(2) . . ?
O5 N2 C23 125.8(2) . . ?
O5 N2 C22 121.9(2) . . ?
C23 N2 C22 112.0(2) . . ?
C1 C3 C1 120.6(4) . 2_655 ?
N1 C23 N2 108.8(2) . . ?
N1 C23 C9 126.2(3) . . ?
N2 C23 C9 125.0(3) . . ?
F8 C8 F7 106.4(3) . . ?
F8 C8 F9 107.0(3) . . ?
F7 C8 F9 107.0(3) . . ?
F8 C8 C7 112.1(3) . . ?
F7 C8 C7 110.0(3) . . ?
F9 C8 C7 113.9(2) . . ?
C12 C11 C10 120.7(3) . . ?
O2 C7 C6 128.4(3) . . ?
O2 C7 C8 113.9(2) . . ?
C6 C7 C8 117.7(3) . . ?
N1 C21 C17 108.6(2) . . ?
N1 C21 C18 105.9(2) . . ?
C17 C21 C18 110.3(3) . . ?
N1 C21 C22 101.1(2) . . ?
C17 C21 C22 115.1(3) . . ?
C18 C21 C22 114.9(3) . . ?
C11 C10 C9 119.1(3) . . ?
C11 C12 C13 119.9(3) . . ?
C11 C12 C15 122.9(3) . . ?
C13 C12 C15 117.1(3) . . ?
C5 C6 C7 121.3(3) . . ?
O4 C1 C3 129.1(3) . . ?
O4 C1 C2 113.4(3) . . ?
C3 C1 C2 117.5(3) . . ?
C14 C9 C10 120.3(3) . . ?
C14 C9 C23 119.1(3) . . ?
C10 C9 C23 120.6(3) . . ?
O3 C5 C6 128.4(3) . . ?
O3 C5 C4 113.4(3) . . ?
C6 C5 C4 118.1(3) . . ?
F1 C2 F3 107.3(3) . . ?
F1 C2 F2 107.4(3) . . ?
F3 C2 F2 106.1(3) . . ?
F1 C2 C1 114.7(3) . . ?
F3 C2 C1 110.9(3) . . ?
F2 C2 C1 110.1(3) . . ?
O42 C15 O40 124.3(3) . . ?
O42 C15 C12 124.0(3) . . ?
O40 C15 C12 111.7(3) . . ?
N2 C22 C20 108.7(2) . . ?
N2 C22 C19 105.8(3) . . ?
C20 C22 C19 110.3(3) . . ?
N2 C22 C21 101.1(2) . . ?
C20 C22 C21 114.9(3) . . ?
C19 C22 C21 115.1(3) . . ?
C14 C13 C12 120.3(3) . . ?
C13 C14 C9 119.6(3) . . ?
F4 C4 F5 107.2(3) . . ?
F4 C4 F6 107.5(3) . . ?
F5 C4 F6 106.5(3) . . ?
F4 C4 C5 111.0(3) . . ?
F5 C4 C5 111.4(3) . . ?
F6 C4 C5 112.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_p131219b
_database_code_depnum_ccdc_archive 'CCDC 1025971'
_audit_update_record             
;
2014-09-24 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H41 F18 N4 O14 Tb'
_chemical_formula_weight         1362.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9249(4)
_cell_length_b                   16.9590(4)
_cell_length_c                   26.6066(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.593(3)
_cell_angle_gamma                90.00
_cell_volume                     5459.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2712
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26307
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.01
_reflns_number_total             9603
_reflns_number_gt                7590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0136P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9603
_refine_ls_number_parameters     777
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0678
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.153808(16) 0.685762(11) 0.873416(8) 0.01649(7) Uani 1 1 d . . .
F11 F 0.1282(2) 0.97993(15) 0.90951(13) 0.0597(9) Uani 1 1 d . . .
F7 F 0.5601(2) 0.73981(17) 0.95456(12) 0.0540(8) Uani 1 1 d . . .
F9 F 0.5541(2) 0.82268(17) 1.01415(13) 0.0659(10) Uani 1 1 d . . .
F8 F 0.5144(2) 0.70096(17) 1.02006(12) 0.0524(8) Uani 1 1 d . . .
F12 F 0.1868(3) 0.97602(16) 0.84552(14) 0.0837(13) Uani 1 1 d . . .
F10 F 0.2929(3) 1.00800(17) 0.92264(17) 0.0959(14) Uani 1 1 d . . .
F1 F -0.0437(2) 0.86202(16) 0.68073(11) 0.0466(8) Uani 1 1 d . . .
F2 F -0.0698(2) 0.89629(15) 0.75317(11) 0.0488(8) Uani 1 1 d . . .
F3 F -0.1404(2) 0.78903(15) 0.71346(10) 0.0390(7) Uani 1 1 d . . .
F15 F 0.1997(3) 0.53484(16) 1.03981(11) 0.0597(9) Uani 1 1 d . . .
F17 F -0.2195(2) 0.56401(16) 0.82158(13) 0.0615(10) Uani 1 1 d . . .
F16 F -0.1721(2) 0.44234(15) 0.83904(11) 0.0458(8) Uani 1 1 d . . .
F18 F -0.1471(2) 0.49998(15) 0.77260(11) 0.0443(7) Uani 1 1 d . . .
F14 F 0.2618(2) 0.44759(18) 0.99941(12) 0.0619(9) Uani 1 1 d . . .
F13 F 0.1036(3) 0.43339(16) 1.00669(12) 0.0577(9) Uani 1 1 d . . .
O8 O 0.3259(2) 0.71321(16) 0.93803(11) 0.0233(7) Uani 1 1 d . . .
O7 O 0.1632(2) 0.82579(15) 0.88654(11) 0.0255(7) Uani 1 1 d . . .
O5 O 0.2686(2) 0.72954(15) 0.82620(11) 0.0245(7) Uani 1 1 d . . .
O6 O 0.0369(2) 0.74441(15) 0.79461(11) 0.0211(7) Uani 1 1 d . . .
O1 O 0.2187(2) 0.57157(15) 0.84413(11) 0.0203(7) Uani 1 1 d . . .
O9 O 0.4203(3) 0.5206(2) 0.73434(13) 0.0464(10) Uani 1 1 d . . .
O14 O -0.1389(2) 0.71054(18) 0.61181(12) 0.0361(8) Uani 1 1 d . . .
O13 O -0.0244(3) 0.74546(19) 0.56909(13) 0.0404(9) Uani 1 1 d . . .
O2 O 0.0300(2) 0.71619(15) 0.91591(11) 0.0215(7) Uani 1 1 d . . .
O10 O -0.0443(2) 0.92586(16) 1.00913(12) 0.0314(8) Uani 1 1 d . . .
O12 O 0.5064(3) 0.88367(19) 1.14291(14) 0.0468(9) Uani 1 1 d . . .
O11 O 0.5174(3) 0.7529(2) 1.13863(15) 0.0524(10) Uani 1 1 d . . .
O4 O 0.0042(2) 0.59768(15) 0.83945(10) 0.0188(6) Uani 1 1 d . . .
O3 O 0.1768(2) 0.58943(15) 0.94106(11) 0.0196(7) Uani 1 1 d . . .
N31 N 0.2976(3) 0.55084(18) 0.82684(13) 0.0197(8) Uani 1 1 d . . .
N34 N 0.3942(3) 0.5276(2) 0.77603(14) 0.0269(9) Uani 1 1 d . . .
N52 N -0.0185(3) 0.77654(18) 0.92879(13) 0.0192(8) Uani 1 1 d . . .
N55 N -0.0541(3) 0.87579(19) 0.97204(14) 0.0236(9) Uani 1 1 d . . .
C5 C 0.2123(4) 0.9594(3) 0.8960(2) 0.0380(13) Uani 1 1 d . . .
C4 C 0.2422(4) 0.8720(2) 0.90777(18) 0.0269(11) Uani 1 1 d . . .
C3 C 0.3505(4) 0.8531(2) 0.93879(18) 0.0292(11) Uani 1 1 d . . .
H3 H 0.4025 0.8931 0.9512 0.035 Uiso 1 1 calc R . .
C2 C 0.3822(3) 0.7748(3) 0.95161(17) 0.0255(10) Uani 1 1 d . . .
C1 C 0.5026(4) 0.7604(3) 0.9858(2) 0.0364(12) Uani 1 1 d . . .
C7 C 0.2514(4) 0.7764(2) 0.78744(19) 0.0304(12) Uani 1 1 d . A .
C8 C 0.1520(4) 0.8084(2) 0.75481(18) 0.0319(12) Uani 1 1 d . . .
H8 H 0.1517 0.8428 0.7275 0.038 Uiso 1 1 calc R . .
C9 C 0.0524(4) 0.7908(2) 0.76142(17) 0.0241(10) Uani 1 1 d . . .
C10 C -0.0508(4) 0.8343(3) 0.72631(18) 0.0320(12) Uani 1 1 d . . .
C23 C 0.2089(3) 0.5911(2) 0.73148(16) 0.0210(10) Uani 1 1 d . . .
C24 C 0.2334(4) 0.6305(2) 0.69093(17) 0.0278(11) Uani 1 1 d . . .
H24 H 0.3059 0.6318 0.6917 0.033 Uiso 1 1 calc R . .
C25 C 0.1519(4) 0.6670(2) 0.65016(17) 0.0292(11) Uani 1 1 d . . .
H25 H 0.1697 0.6940 0.6239 0.035 Uiso 1 1 calc R . .
C26 C 0.0427(4) 0.6642(2) 0.64745(17) 0.0252(10) Uani 1 1 d . . .
C27 C 0.0164(3) 0.6225(2) 0.68635(17) 0.0245(10) Uani 1 1 d . . .
H27 H -0.0569 0.6186 0.6841 0.029 Uiso 1 1 calc R . .
C28 C 0.0984(3) 0.5869(2) 0.72810(17) 0.0226(10) Uani 1 1 d . . .
H28 H 0.0803 0.5599 0.7543 0.027 Uiso 1 1 calc R . .
C22 C 0.2955(3) 0.5580(2) 0.77677(17) 0.0219(10) Uani 1 1 d . . .
C20 C 0.3927(3) 0.5020(2) 0.86209(17) 0.0218(10) Uani 1 1 d . . .
C17 C 0.4746(4) 0.5123(2) 0.83134(18) 0.0272(11) Uani 1 1 d . . .
C21 C 0.3491(4) 0.4182(2) 0.8604(2) 0.0360(13) Uani 1 1 d . . .
H21A H 0.3286 0.3979 0.8245 0.054 Uiso 1 1 calc R . .
H21B H 0.2856 0.4185 0.8711 0.054 Uiso 1 1 calc R . .
H21C H 0.4055 0.3854 0.8844 0.054 Uiso 1 1 calc R . .
C19 C 0.4332(3) 0.5329(3) 0.91914(17) 0.0349(12) Uani 1 1 d . . .
H19A H 0.4984 0.5045 0.9401 0.052 Uiso 1 1 calc R . .
H19B H 0.3766 0.5257 0.9344 0.052 Uiso 1 1 calc R . .
H19C H 0.4502 0.5880 0.9191 0.052 Uiso 1 1 calc R . .
C16 C 0.5459(3) 0.5871(2) 0.84843(19) 0.0351(12) Uani 1 1 d . . .
H16A H 0.5803 0.5985 0.8226 0.053 Uiso 1 1 calc R . .
H16B H 0.6019 0.5788 0.8830 0.053 Uiso 1 1 calc R . .
H16C H 0.5000 0.6307 0.8503 0.053 Uiso 1 1 calc R . .
C18 C 0.5451(3) 0.4410(3) 0.83163(19) 0.0358(12) Uani 1 1 d . . .
H18A H 0.4985 0.3958 0.8189 0.054 Uiso 1 1 calc R . .
H18B H 0.5950 0.4314 0.8675 0.054 Uiso 1 1 calc R . .
H18C H 0.5867 0.4506 0.8086 0.054 Uiso 1 1 calc R . .
C29 C -0.0411(4) 0.7100(3) 0.60451(18) 0.0292(11) Uani 1 1 d . . .
C30 C -0.2209(4) 0.7639(3) 0.57690(19) 0.0492(15) Uani 1 1 d . . .
H30A H -0.2446 0.7446 0.5407 0.074 Uiso 1 1 calc R . .
H30B H -0.1890 0.8154 0.5785 0.074 Uiso 1 1 calc R . .
H30C H -0.2832 0.7670 0.5885 0.074 Uiso 1 1 calc R . .
C38 C 0.1386(3) 0.8208(2) 1.00907(16) 0.0190(9) Uani 1 1 d . . .
C43 C 0.1932(3) 0.8913(2) 1.02985(17) 0.0234(10) Uani 1 1 d . . .
H43 H 0.1580 0.9395 1.0188 0.028 Uiso 1 1 calc R . .
C42 C 0.2996(3) 0.8890(2) 1.06682(17) 0.0235(10) Uani 1 1 d . . .
H42 H 0.3358 0.9358 1.0807 0.028 Uiso 1 1 calc R . .
C44 C 0.3530(3) 0.8175(2) 1.08359(17) 0.0228(10) Uani 1 1 d . . .
C40 C 0.2985(3) 0.7478(2) 1.06181(17) 0.0245(10) Uani 1 1 d . . .
H40 H 0.3344 0.6998 1.0721 0.029 Uiso 1 1 calc R . .
C39 C 0.1926(3) 0.7490(2) 1.02540(17) 0.0232(10) Uani 1 1 d . . .
H39 H 0.1568 0.7020 1.0116 0.028 Uiso 1 1 calc R . .
C37 C 0.0252(3) 0.8235(2) 0.97072(16) 0.0191(10) Uani 1 1 d . . .
C32 C -0.1415(3) 0.7874(2) 0.90133(17) 0.0209(10) Uani 1 1 d . . .
C35 C -0.1544(3) 0.8720(2) 0.92177(17) 0.0217(10) Uani 1 1 d . . .
C33 C -0.1949(3) 0.7226(2) 0.92360(18) 0.0290(11) Uani 1 1 d . . .
H33A H -0.1700 0.6721 0.9162 0.044 Uiso 1 1 calc R . .
H33B H -0.2738 0.7257 0.9069 0.044 Uiso 1 1 calc R . .
H33C H -0.1746 0.7292 0.9617 0.044 Uiso 1 1 calc R . .
C31 C -0.1723(4) 0.7798(3) 0.84160(17) 0.0315(11) Uani 1 1 d . . .
H31A H -0.1286 0.8158 0.8295 0.047 Uiso 1 1 calc R . .
H31B H -0.2492 0.7920 0.8243 0.047 Uiso 1 1 calc R . .
H31C H -0.1586 0.7268 0.8329 0.047 Uiso 1 1 calc R . .
C36 C -0.1422(4) 0.9382(2) 0.88531(18) 0.0324(12) Uani 1 1 d . . .
H36A H -0.1337 0.9877 0.9039 0.049 Uiso 1 1 calc R . .
H36B H -0.2069 0.9401 0.8534 0.049 Uiso 1 1 calc R . .
H36C H -0.0784 0.9285 0.8757 0.049 Uiso 1 1 calc R . .
C34 C -0.2577(3) 0.8838(2) 0.93585(18) 0.0302(11) Uani 1 1 d . . .
H34A H -0.2612 0.8436 0.9606 0.045 Uiso 1 1 calc R . .
H34B H -0.3219 0.8805 0.9038 0.045 Uiso 1 1 calc R . .
H34C H -0.2551 0.9347 0.9520 0.045 Uiso 1 1 calc R . .
C45 C 0.4669(4) 0.8132(3) 1.12396(19) 0.0310(11) Uani 1 1 d . . .
C46 C 0.6148(4) 0.8850(3) 1.1843(2) 0.0633(17) Uani 1 1 d . . .
H46A H 0.6685 0.8657 1.1700 0.095 Uiso 1 1 calc R . .
H46B H 0.6148 0.8522 1.2137 0.095 Uiso 1 1 calc R . .
H46C H 0.6331 0.9381 1.1968 0.095 Uiso 1 1 calc R . .
C15 C 0.1715(4) 0.4860(3) 0.99771(19) 0.0364(13) Uani 1 1 d . . .
C14 C 0.1211(3) 0.5311(2) 0.94489(17) 0.0206(10) Uani 1 1 d . . .
C13 C 0.0227(4) 0.5026(2) 0.90777(18) 0.0266(11) Uani 1 1 d . . .
H13 H -0.0093 0.4577 0.9160 0.032 Uiso 1 1 calc R . .
C12 C -0.0281(3) 0.5395(2) 0.85921(18) 0.0218(10) Uani 1 1 d . . .
C11 C -0.1424(4) 0.5109(3) 0.8225(2) 0.0340(12) Uani 1 1 d . . .
F4A F 0.3314(13) 0.8152(8) 0.7230(4) 0.061(3) Uani 0.52(3) 1 d PU A 1
F5A F 0.4274(15) 0.7505(12) 0.7899(10) 0.108(7) Uani 0.52(3) 1 d PU A 1
C6 C 0.3577(5) 0.8025(3) 0.7781(3) 0.0497(15) Uani 1 1 d U . .
F6A F 0.3890(14) 0.8690(7) 0.7974(10) 0.082(5) Uani 0.52(3) 1 d PU A 1
F6B F 0.430(2) 0.834(2) 0.8259(10) 0.126(10) Uani 0.48(3) 1 d PU A 2
F4B F 0.3504(17) 0.852(2) 0.7432(16) 0.150(11) Uani 0.48(3) 1 d PU A 2
F5B F 0.4197(15) 0.7423(9) 0.7727(8) 0.062(4) Uani 0.48(3) 1 d PU A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O2 2.319(2) . ?
Tb1 O8 2.331(3) . ?
Tb1 O6 2.333(3) . ?
Tb1 O1 2.350(2) . ?
Tb1 O4 2.357(3) . ?
Tb1 O3 2.371(2) . ?
Tb1 O5 2.375(2) . ?
Tb1 O7 2.397(3) . ?
F11 C5 1.307(5) . ?
F7 C1 1.342(5) . ?
F9 C1 1.331(5) . ?
F8 C1 1.331(5) . ?
F12 C5 1.295(6) . ?
F10 C5 1.322(5) . ?
F1 C10 1.334(5) . ?
F2 C10 1.342(5) . ?
F3 C10 1.330(5) . ?
F15 C15 1.336(5) . ?
F17 C11 1.337(5) . ?
F16 C11 1.346(5) . ?
F18 C11 1.321(5) . ?
F14 C15 1.324(5) . ?
F13 C15 1.331(5) . ?
O8 C2 1.251(5) . ?
O7 C4 1.252(5) . ?
O5 C7 1.258(5) . ?
O6 C9 1.250(4) . ?
O1 N31 1.305(3) . ?
O9 N34 1.273(4) . ?
O14 C29 1.345(5) . ?
O14 C30 1.453(5) . ?
O13 C29 1.200(5) . ?
O2 N52 1.307(4) . ?
O10 N55 1.274(4) . ?
O12 C45 1.327(5) . ?
O12 C46 1.447(6) . ?
O11 C45 1.202(5) . ?
O4 C12 1.257(4) . ?
O3 C14 1.248(4) . ?
N31 C22 1.328(5) . ?
N31 C20 1.506(5) . ?
N34 C22 1.382(5) . ?
N34 C17 1.495(5) . ?
N52 C37 1.325(5) . ?
N52 C32 1.510(5) . ?
N55 C37 1.365(4) . ?
N55 C35 1.501(5) . ?
C5 C4 1.537(6) . ?
C4 C3 1.389(6) . ?
C3 C2 1.396(6) . ?
C3 H3 0.9300 . ?
C2 C1 1.522(6) . ?
C7 C8 1.383(6) . ?
C7 C6 1.545(6) . ?
C8 C9 1.392(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.523(6) . ?
C23 C24 1.396(5) . ?
C23 C28 1.401(5) . ?
C23 C22 1.440(6) . ?
C24 C25 1.366(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.388(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.391(5) . ?
C26 C29 1.487(6) . ?
C27 C28 1.376(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C20 C19 1.514(6) . ?
C20 C21 1.524(5) . ?
C20 C17 1.558(5) . ?
C17 C18 1.513(5) . ?
C17 C16 1.540(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C38 C39 1.394(5) . ?
C38 C43 1.400(5) . ?
C38 C37 1.462(6) . ?
C43 C42 1.382(6) . ?
C43 H43 0.9300 . ?
C42 C44 1.388(5) . ?
C42 H42 0.9300 . ?
C44 C40 1.394(5) . ?
C44 C45 1.488(6) . ?
C40 C39 1.371(6) . ?
C40 H40 0.9300 . ?
C39 H39 0.9300 . ?
C32 C31 1.502(5) . ?
C32 C33 1.525(5) . ?
C32 C35 1.563(5) . ?
C35 C34 1.522(5) . ?
C35 C36 1.527(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C15 C14 1.529(6) . ?
C14 C13 1.394(6) . ?
C13 C12 1.376(6) . ?
C13 H13 0.9300 . ?
C12 C11 1.535(6) . ?
F4A C6 1.402(12) . ?
F5A C6 1.221(17) . ?
C6 F4B 1.226(14) . ?
C6 F6A 1.246(13) . ?
C6 F5B 1.337(16) . ?
C6 F6B 1.395(18) . ?

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
O2 Tb1 O8 103.84(9) . . ?
O2 Tb1 O6 90.19(9) . . ?
O8 Tb1 O6 136.60(9) . . ?
O2 Tb1 O1 137.15(8) . . ?
O8 Tb1 O1 92.85(9) . . ?
O6 Tb1 O1 104.32(9) . . ?
O2 Tb1 O4 73.40(9) . . ?
O8 Tb1 O4 148.30(9) . . ?
O6 Tb1 O4 74.98(9) . . ?
O1 Tb1 O4 72.00(8) . . ?
O2 Tb1 O3 72.97(8) . . ?
O8 Tb1 O3 75.24(9) . . ?
O6 Tb1 O3 147.67(9) . . ?
O1 Tb1 O3 73.72(8) . . ?
O4 Tb1 O3 73.82(9) . . ?
O2 Tb1 O5 148.74(9) . . ?
O8 Tb1 O5 73.49(9) . . ?
O6 Tb1 O5 73.69(9) . . ?
O1 Tb1 O5 73.74(8) . . ?
O4 Tb1 O5 125.17(9) . . ?
O3 Tb1 O5 132.99(9) . . ?
O2 Tb1 O7 73.55(8) . . ?
O8 Tb1 O7 73.04(10) . . ?
O6 Tb1 O7 72.07(9) . . ?
O1 Tb1 O7 149.22(8) . . ?
O4 Tb1 O7 132.55(9) . . ?
O3 Tb1 O7 125.85(9) . . ?
O5 Tb1 O7 76.01(9) . . ?
C2 O8 Tb1 133.4(3) . . ?
C4 O7 Tb1 132.6(3) . . ?
C7 O5 Tb1 131.9(3) . . ?
C9 O6 Tb1 133.5(3) . . ?
N31 O1 Tb1 138.8(2) . . ?
C29 O14 C30 115.0(3) . . ?
N52 O2 Tb1 141.1(2) . . ?
C45 O12 C46 116.3(4) . . ?
C12 O4 Tb1 133.3(3) . . ?
C14 O3 Tb1 133.3(3) . . ?
O1 N31 C22 125.9(3) . . ?
O1 N31 C20 119.8(3) . . ?
C22 N31 C20 113.5(3) . . ?
O9 N34 C22 125.1(4) . . ?
O9 N34 C17 122.4(3) . . ?
C22 N34 C17 112.1(3) . . ?
O2 N52 C37 126.1(4) . . ?
O2 N52 C32 119.3(3) . . ?
C37 N52 C32 113.5(3) . . ?
O10 N55 C37 125.6(4) . . ?
O10 N55 C35 122.6(3) . . ?
C37 N55 C35 111.7(3) . . ?
F12 C5 F11 107.2(4) . . ?
F12 C5 F10 106.6(4) . . ?
F11 C5 F10 105.2(4) . . ?
F12 C5 C4 112.0(4) . . ?
F11 C5 C4 112.0(3) . . ?
F10 C5 C4 113.4(4) . . ?
O7 C4 C3 128.0(4) . . ?
O7 C4 C5 113.9(4) . . ?
C3 C4 C5 118.1(4) . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
O8 C2 C3 129.3(4) . . ?
O8 C2 C1 114.1(4) . . ?
C3 C2 C1 116.7(4) . . ?
F9 C1 F8 107.4(4) . . ?
F9 C1 F7 106.4(4) . . ?
F8 C1 F7 105.8(4) . . ?
F9 C1 C2 114.5(4) . . ?
F8 C1 C2 112.2(4) . . ?
F7 C1 C2 110.1(4) . . ?
O5 C7 C8 128.3(4) . . ?
O5 C7 C6 113.7(4) . . ?
C8 C7 C6 118.0(4) . . ?
C7 C8 C9 122.2(4) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
O6 C9 C8 127.6(4) . . ?
O6 C9 C10 114.5(4) . . ?
C8 C9 C10 117.9(4) . . ?
F3 C10 F1 107.6(4) . . ?
F3 C10 F2 106.4(3) . . ?
F1 C10 F2 107.0(4) . . ?
F3 C10 C9 112.0(3) . . ?
F1 C10 C9 113.8(4) . . ?
F2 C10 C9 109.8(4) . . ?
C24 C23 C28 118.5(4) . . ?
C24 C23 C22 120.8(4) . . ?
C28 C23 C22 120.6(3) . . ?
C25 C24 C23 120.6(4) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 120.8(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 119.2(4) . . ?
C25 C26 C29 118.3(4) . . ?
C27 C26 C29 122.3(4) . . ?
C28 C27 C26 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C23 120.5(4) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
N31 C22 N34 106.7(4) . . ?
N31 C22 C23 127.6(3) . . ?
N34 C22 C23 125.7(3) . . ?
N31 C20 C19 110.6(3) . . ?
N31 C20 C21 106.3(3) . . ?
C19 C20 C21 110.3(4) . . ?
N31 C20 C17 99.7(3) . . ?
C19 C20 C17 115.4(4) . . ?
C21 C20 C17 113.7(3) . . ?
N34 C17 C18 110.6(3) . . ?
N34 C17 C16 106.5(3) . . ?
C18 C17 C16 111.1(4) . . ?
N34 C17 C20 99.9(3) . . ?
C18 C17 C20 115.3(3) . . ?
C16 C17 C20 112.6(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O13 C29 O14 123.3(4) . . ?
O13 C29 C26 125.5(4) . . ?
O14 C29 C26 111.1(4) . . ?
O14 C30 H30A 109.5 . . ?
O14 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O14 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C39 C38 C43 119.7(4) . . ?
C39 C38 C37 120.9(4) . . ?
C43 C38 C37 119.4(4) . . ?
C42 C43 C38 119.5(4) . . ?
C42 C43 H43 120.2 . . ?
C38 C43 H43 120.2 . . ?
C43 C42 C44 120.8(4) . . ?
C43 C42 H42 119.6 . . ?
C44 C42 H42 119.6 . . ?
C42 C44 C40 119.0(4) . . ?
C42 C44 C45 121.9(4) . . ?
C40 C44 C45 119.1(4) . . ?
C39 C40 C44 120.9(4) . . ?
C39 C40 H40 119.5 . . ?
C44 C40 H40 119.5 . . ?
C40 C39 C38 119.9(4) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
N52 C37 N55 108.1(4) . . ?
N52 C37 C38 126.5(3) . . ?
N55 C37 C38 125.5(4) . . ?
C31 C32 N52 110.0(3) . . ?
C31 C32 C33 111.2(4) . . ?
N52 C32 C33 105.5(3) . . ?
C31 C32 C35 115.2(3) . . ?
N52 C32 C35 99.6(3) . . ?
C33 C32 C35 114.1(3) . . ?
N55 C35 C34 109.4(3) . . ?
N55 C35 C36 106.6(3) . . ?
C34 C35 C36 110.8(3) . . ?
N55 C35 C32 100.7(3) . . ?
C34 C35 C32 114.6(3) . . ?
C36 C35 C32 114.0(3) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O11 C45 O12 123.4(5) . . ?
O11 C45 C44 124.2(4) . . ?
O12 C45 C44 112.4(4) . . ?
O12 C46 H46A 109.5 . . ?
O12 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
O12 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
F14 C15 F13 107.0(4) . . ?
F14 C15 F15 107.4(4) . . ?
F13 C15 F15 105.5(3) . . ?
F14 C15 C14 111.3(3) . . ?
F13 C15 C14 113.9(4) . . ?
F15 C15 C14 111.3(4) . . ?
O3 C14 C13 128.7(4) . . ?
O3 C14 C15 113.6(4) . . ?
C13 C14 C15 117.7(4) . . ?
C12 C13 C14 121.6(4) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
O4 C12 C13 129.0(4) . . ?
O4 C12 C11 111.7(4) . . ?
C13 C12 C11 119.3(4) . . ?
F18 C11 F17 107.8(4) . . ?
F18 C11 F16 106.9(4) . . ?
F17 C11 F16 107.0(3) . . ?
F18 C11 C12 112.2(3) . . ?
F17 C11 C12 110.1(4) . . ?
F16 C11 C12 112.7(4) . . ?
F5A C6 F4B 122.6(12) . . ?
F5A C6 F6A 116.5(13) . . ?
F4B C6 F6A 68.1(16) . . ?
F5A C6 F5B 19.8(15) . . ?
F4B C6 F5B 109.0(14) . . ?
F6A C6 F5B 128.0(11) . . ?
F5A C6 F6B 81.2(13) . . ?
F4B C6 F6B 106.1(13) . . ?
F6A C6 F6B 42.1(11) . . ?
F5B C6 F6B 99.1(16) . . ?
F5A C6 F4A 105.4(12) . . ?
F4B C6 F4A 35(2) . . ?
F6A C6 F4A 102.5(10) . . ?
F5B C6 F4A 86.5(11) . . ?
F6B C6 F4A 137.1(11) . . ?
F5A C6 C7 111.6(9) . . ?
F4B C6 C7 118.7(9) . . ?
F6A C6 C7 111.8(7) . . ?
F5B C6 C7 113.5(9) . . ?
F6B C6 C7 108.3(7) . . ?
F4A C6 C7 108.1(8) . . ?

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
O2 Tb1 O8 C2 -85.1(3) . . . . ?
O6 Tb1 O8 C2 20.3(4) . . . . ?
O1 Tb1 O8 C2 134.7(3) . . . . ?
O4 Tb1 O8 C2 -165.8(3) . . . . ?
O3 Tb1 O8 C2 -152.9(3) . . . . ?
O5 Tb1 O8 C2 62.6(3) . . . . ?
O7 Tb1 O8 C2 -17.4(3) . . . . ?
O2 Tb1 O7 C4 127.0(4) . . . . ?
O8 Tb1 O7 C4 16.5(3) . . . . ?
O6 Tb1 O7 C4 -137.3(4) . . . . ?
O1 Tb1 O7 C4 -49.3(4) . . . . ?
O4 Tb1 O7 C4 174.5(3) . . . . ?
O3 Tb1 O7 C4 73.2(4) . . . . ?
O5 Tb1 O7 C4 -60.2(3) . . . . ?
O2 Tb1 O5 C7 -46.7(5) . . . . ?
O8 Tb1 O5 C7 -136.3(4) . . . . ?
O6 Tb1 O5 C7 14.9(4) . . . . ?
O1 Tb1 O5 C7 125.7(4) . . . . ?
O4 Tb1 O5 C7 72.5(4) . . . . ?
O3 Tb1 O5 C7 173.5(3) . . . . ?
O7 Tb1 O5 C7 -60.1(4) . . . . ?
O2 Tb1 O6 C9 134.9(3) . . . . ?
O8 Tb1 O6 C9 24.3(4) . . . . ?
O1 Tb1 O6 C9 -85.8(3) . . . . ?
O4 Tb1 O6 C9 -152.3(3) . . . . ?
O3 Tb1 O6 C9 -167.9(3) . . . . ?
O5 Tb1 O6 C9 -17.9(3) . . . . ?
O7 Tb1 O6 C9 62.3(3) . . . . ?
O2 Tb1 O1 N31 -168.1(3) . . . . ?
O8 Tb1 O1 N31 -54.2(4) . . . . ?
O6 Tb1 O1 N31 85.6(4) . . . . ?
O4 Tb1 O1 N31 154.3(4) . . . . ?
O3 Tb1 O1 N31 -127.9(4) . . . . ?
O5 Tb1 O1 N31 17.7(3) . . . . ?
O7 Tb1 O1 N31 6.7(5) . . . . ?
O8 Tb1 O2 N52 79.1(4) . . . . ?
O6 Tb1 O2 N52 -59.4(4) . . . . ?
O1 Tb1 O2 N52 -170.9(3) . . . . ?
O4 Tb1 O2 N52 -133.6(4) . . . . ?
O3 Tb1 O2 N52 148.7(4) . . . . ?
O5 Tb1 O2 N52 -1.8(5) . . . . ?
O7 Tb1 O2 N52 11.9(4) . . . . ?
O2 Tb1 O4 C12 -71.5(3) . . . . ?
O8 Tb1 O4 C12 18.1(4) . . . . ?
O6 Tb1 O4 C12 -166.3(3) . . . . ?
O1 Tb1 O4 C12 82.8(3) . . . . ?
O3 Tb1 O4 C12 5.1(3) . . . . ?
O5 Tb1 O4 C12 136.7(3) . . . . ?
O7 Tb1 O4 C12 -119.1(3) . . . . ?
O2 Tb1 O3 C14 75.1(3) . . . . ?
O8 Tb1 O3 C14 -175.1(3) . . . . ?
O6 Tb1 O3 C14 13.6(4) . . . . ?
O1 Tb1 O3 C14 -77.6(3) . . . . ?
O4 Tb1 O3 C14 -2.1(3) . . . . ?
O5 Tb1 O3 C14 -125.4(3) . . . . ?
O7 Tb1 O3 C14 129.2(3) . . . . ?
Tb1 O1 N31 C22 -82.7(5) . . . . ?
Tb1 O1 N31 C20 108.5(4) . . . . ?
Tb1 O2 N52 C37 -81.2(5) . . . . ?
Tb1 O2 N52 C32 111.4(4) . . . . ?
Tb1 O7 C4 C3 -11.6(6) . . . . ?
Tb1 O7 C4 C5 167.0(3) . . . . ?
F12 C5 C4 O7 -65.4(5) . . . . ?
F11 C5 C4 O7 55.1(6) . . . . ?
F10 C5 C4 O7 173.9(4) . . . . ?
F12 C5 C4 C3 113.4(5) . . . . ?
F11 C5 C4 C3 -126.2(5) . . . . ?
F10 C5 C4 C3 -7.4(6) . . . . ?
O7 C4 C3 C2 -2.6(7) . . . . ?
C5 C4 C3 C2 178.9(4) . . . . ?
Tb1 O8 C2 C3 13.7(6) . . . . ?
Tb1 O8 C2 C1 -164.6(3) . . . . ?
C4 C3 C2 O8 1.8(7) . . . . ?
C4 C3 C2 C1 -179.9(4) . . . . ?
O8 C2 C1 F9 -159.9(4) . . . . ?
C3 C2 C1 F9 21.5(6) . . . . ?
O8 C2 C1 F8 -37.2(5) . . . . ?
C3 C2 C1 F8 144.2(4) . . . . ?
O8 C2 C1 F7 80.3(5) . . . . ?
C3 C2 C1 F7 -98.3(5) . . . . ?
Tb1 O5 C7 C8 -10.8(7) . . . . ?
Tb1 O5 C7 C6 166.4(3) . . . . ?
O5 C7 C8 C9 -0.4(8) . . . . ?
C6 C7 C8 C9 -177.5(4) . . . . ?
Tb1 O6 C9 C8 16.6(6) . . . . ?
Tb1 O6 C9 C10 -160.9(3) . . . . ?
C7 C8 C9 O6 -2.3(7) . . . . ?
C7 C8 C9 C10 175.1(4) . . . . ?
O6 C9 C10 F3 -36.6(5) . . . . ?
C8 C9 C10 F3 145.7(4) . . . . ?
O6 C9 C10 F1 -158.8(4) . . . . ?
C8 C9 C10 F1 23.5(6) . . . . ?
O6 C9 C10 F2 81.4(5) . . . . ?
C8 C9 C10 F2 -96.3(4) . . . . ?
C28 C23 C24 C25 2.8(6) . . . . ?
C22 C23 C24 C25 -175.0(4) . . . . ?
C23 C24 C25 C26 -1.5(7) . . . . ?
C24 C25 C26 C27 -1.1(6) . . . . ?
C24 C25 C26 C29 175.5(4) . . . . ?
C25 C26 C27 C28 2.4(6) . . . . ?
C29 C26 C27 C28 -174.1(4) . . . . ?
C26 C27 C28 C23 -1.1(6) . . . . ?
C24 C23 C28 C27 -1.5(6) . . . . ?
C22 C23 C28 C27 176.3(4) . . . . ?
O1 N31 C22 N34 -178.8(3) . . . . ?
C20 N31 C22 N34 -9.5(5) . . . . ?
O1 N31 C22 C23 1.6(7) . . . . ?
C20 N31 C22 C23 170.9(4) . . . . ?
O9 N34 C22 N31 176.4(4) . . . . ?
C17 N34 C22 N31 -10.7(5) . . . . ?
O9 N34 C22 C23 -4.0(7) . . . . ?
C17 N34 C22 C23 168.9(4) . . . . ?
C24 C23 C22 N31 147.8(4) . . . . ?
C28 C23 C22 N31 -30.0(7) . . . . ?
C24 C23 C22 N34 -31.7(6) . . . . ?
C28 C23 C22 N34 150.5(4) . . . . ?
O1 N31 C20 C19 -44.0(5) . . . . ?
C22 N31 C20 C19 146.0(4) . . . . ?
O1 N31 C20 C21 75.8(4) . . . . ?
C22 N31 C20 C21 -94.3(4) . . . . ?
O1 N31 C20 C17 -165.9(3) . . . . ?
C22 N31 C20 C17 24.0(4) . . . . ?
O9 N34 C17 C18 -40.3(5) . . . . ?
C22 N34 C17 C18 146.5(3) . . . . ?
O9 N34 C17 C16 80.5(4) . . . . ?
C22 N34 C17 C16 -92.7(4) . . . . ?
O9 N34 C17 C20 -162.2(4) . . . . ?
C22 N34 C17 C20 24.6(4) . . . . ?
N31 C20 C17 N34 -26.5(4) . . . . ?
C19 C20 C17 N34 -144.9(4) . . . . ?
C21 C20 C17 N34 86.3(4) . . . . ?
N31 C20 C17 C18 -145.0(4) . . . . ?
C19 C20 C17 C18 96.5(5) . . . . ?
C21 C20 C17 C18 -32.3(6) . . . . ?
N31 C20 C17 C16 86.2(4) . . . . ?
C19 C20 C17 C16 -32.3(5) . . . . ?
C21 C20 C17 C16 -161.1(4) . . . . ?
C30 O14 C29 O13 -6.1(6) . . . . ?
C30 O14 C29 C26 170.7(4) . . . . ?
C25 C26 C29 O13 5.5(7) . . . . ?
C27 C26 C29 O13 -177.9(4) . . . . ?
C25 C26 C29 O14 -171.2(4) . . . . ?
C27 C26 C29 O14 5.3(6) . . . . ?
C39 C38 C43 C42 -0.7(6) . . . . ?
C37 C38 C43 C42 178.8(3) . . . . ?
C38 C43 C42 C44 0.0(6) . . . . ?
C43 C42 C44 C40 1.2(6) . . . . ?
C43 C42 C44 C45 -179.1(4) . . . . ?
C42 C44 C40 C39 -1.7(6) . . . . ?
C45 C44 C40 C39 178.5(4) . . . . ?
C44 C40 C39 C38 1.0(6) . . . . ?
C43 C38 C39 C40 0.2(6) . . . . ?
C37 C38 C39 C40 -179.3(3) . . . . ?
O2 N52 C37 N55 -175.9(3) . . . . ?
C32 N52 C37 N55 -7.9(4) . . . . ?
O2 N52 C37 C38 4.3(6) . . . . ?
C32 N52 C37 C38 172.3(3) . . . . ?
O10 N55 C37 N52 174.3(3) . . . . ?
C35 N55 C37 N52 -10.0(4) . . . . ?
O10 N55 C37 C38 -6.0(6) . . . . ?
C35 N55 C37 C38 169.8(3) . . . . ?
C39 C38 C37 N52 -37.2(6) . . . . ?
C43 C38 C37 N52 143.2(4) . . . . ?
C39 C38 C37 N55 143.1(4) . . . . ?
C43 C38 C37 N55 -36.5(5) . . . . ?
O2 N52 C32 C31 -48.8(4) . . . . ?
C37 N52 C32 C31 142.3(3) . . . . ?
O2 N52 C32 C33 71.3(4) . . . . ?
C37 N52 C32 C33 -97.6(4) . . . . ?
O2 N52 C32 C35 -170.2(3) . . . . ?
C37 N52 C32 C35 20.9(4) . . . . ?
O10 N55 C35 C34 -41.0(5) . . . . ?
C37 N55 C35 C34 143.1(3) . . . . ?
O10 N55 C35 C36 78.8(4) . . . . ?
C37 N55 C35 C36 -97.1(4) . . . . ?
O10 N55 C35 C32 -162.0(3) . . . . ?
C37 N55 C35 C32 22.1(4) . . . . ?
C31 C32 C35 N55 -141.1(3) . . . . ?
N52 C32 C35 N55 -23.5(3) . . . . ?
C33 C32 C35 N55 88.4(4) . . . . ?
C31 C32 C35 C34 101.7(4) . . . . ?
N52 C32 C35 C34 -140.7(3) . . . . ?
C33 C32 C35 C34 -28.8(5) . . . . ?
C31 C32 C35 C36 -27.4(5) . . . . ?
N52 C32 C35 C36 90.2(4) . . . . ?
C33 C32 C35 C36 -157.9(4) . . . . ?
C46 O12 C45 O11 -1.7(7) . . . . ?
C46 O12 C45 C44 177.2(4) . . . . ?
C42 C44 C45 O11 -178.0(4) . . . . ?
C40 C44 C45 O11 1.8(7) . . . . ?
C42 C44 C45 O12 3.1(6) . . . . ?
C40 C44 C45 O12 -177.1(3) . . . . ?
Tb1 O3 C14 C13 0.9(6) . . . . ?
Tb1 O3 C14 C15 -179.9(2) . . . . ?
F14 C15 C14 O3 -71.0(5) . . . . ?
F13 C15 C14 O3 168.0(3) . . . . ?
F15 C15 C14 O3 48.8(5) . . . . ?
F14 C15 C14 C13 108.3(4) . . . . ?
F13 C15 C14 C13 -12.8(5) . . . . ?
F15 C15 C14 C13 -131.9(4) . . . . ?
O3 C14 C13 C12 -0.8(6) . . . . ?
C15 C14 C13 C12 -179.9(3) . . . . ?
Tb1 O4 C12 C13 -7.4(6) . . . . ?
Tb1 O4 C12 C11 170.4(2) . . . . ?
C14 C13 C12 O4 4.1(6) . . . . ?
C14 C13 C12 C11 -173.5(3) . . . . ?
O4 C12 C11 F18 50.7(5) . . . . ?
C13 C12 C11 F18 -131.3(4) . . . . ?
O4 C12 C11 F17 -69.3(4) . . . . ?
C13 C12 C11 F17 108.7(4) . . . . ?
O4 C12 C11 F16 171.4(3) . . . . ?
C13 C12 C11 F16 -10.6(5) . . . . ?
O5 C7 C6 F5A 32.5(16) . . . . ?
C8 C7 C6 F5A -149.9(15) . . . . ?
O5 C7 C6 F4B -176(3) . . . . ?
C8 C7 C6 F4B 1(3) . . . . ?
O5 C7 C6 F6A -99.9(13) . . . . ?
C8 C7 C6 F6A 77.7(14) . . . . ?
O5 C7 C6 F5B 53.9(12) . . . . ?
C8 C7 C6 F5B -128.5(11) . . . . ?
O5 C7 C6 F6B -55(2) . . . . ?
C8 C7 C6 F6B 123(2) . . . . ?
O5 C7 C6 F4A 148.0(7) . . . . ?
C8 C7 C6 F4A -34.4(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.102
####################################################################### 
# 
# 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_p131225c
_database_code_depnum_ccdc_archive 'CCDC 1025972'
_audit_update_record             
;
2014-09-24 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H41 Dy F18 N4 O14'
_chemical_formula_weight         1366.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.9453(10)
_cell_length_b                   10.4449(6)
_cell_length_c                   21.5316(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.426(3)
_cell_angle_gamma                90.00
_cell_volume                     5380.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2716
_exptl_absorpt_coefficient_mu    1.517
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9526
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4750
_reflns_number_gt                4273
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0251P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4750
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0825
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.0000 0.33517(2) 0.2500 0.01506(9) Uani 1 2 d S . .
F2 F 0.11854(10) 0.6990(3) 0.17077(12) 0.0512(8) Uani 1 1 d . . .
F9 F -0.14634(11) 0.0306(3) 0.14696(12) 0.0607(9) Uani 1 1 d . . .
F3 F 0.05274(11) 0.6671(3) 0.10270(11) 0.0520(8) Uani 1 1 d . . .
F7 F -0.06669(12) -0.0570(3) 0.14581(15) 0.0747(11) Uani 1 1 d . . .
F8 F -0.12579(14) -0.1223(3) 0.20925(13) 0.0675(9) Uani 1 1 d . . .
F6 F 0.06854(12) 0.1003(4) 0.06332(11) 0.0666(10) Uani 1 1 d . . .
F5 F 0.15271(12) 0.0768(3) 0.09729(12) 0.0690(10) Uani 1 1 d . . .
F4 F 0.12168(11) 0.2625(3) 0.07460(11) 0.0534(8) Uani 1 1 d . . .
F1 F 0.05191(13) 0.8340(3) 0.15985(14) 0.0631(9) Uani 1 1 d . . .
O7 O 0.26346(10) 0.3723(3) 0.08551(12) 0.0333(7) Uani 1 1 d . . .
O4 O -0.04972(11) 0.1592(3) 0.20836(11) 0.0258(7) Uani 1 1 d . . .
O6 O 0.29899(13) 0.1845(3) 0.11845(14) 0.0467(9) Uani 1 1 d . . .
O3 O 0.05506(9) 0.2616(3) 0.17181(10) 0.0221(6) Uani 1 1 d . . .
O2 O 0.03778(9) 0.5141(3) 0.20123(10) 0.0221(6) Uani 1 1 d . . .
O1 O 0.06975(9) 0.4141(3) 0.31695(10) 0.0231(6) Uani 1 1 d . . .
O5 O 0.23659(11) 0.3218(4) 0.42320(13) 0.0499(11) Uani 1 1 d . . .
N1 N 0.10616(11) 0.3868(3) 0.36182(13) 0.0204(7) Uani 1 1 d . . .
N2 N 0.18484(12) 0.3445(4) 0.41205(14) 0.0319(10) Uani 1 1 d . . .
C5 C 0.08744(15) 0.1679(4) 0.16613(17) 0.0231(9) Uani 1 1 d . . .
C23 C 0.03677(15) 0.3417(5) 0.43997(18) 0.0354(12) Uani 1 1 d . . .
H23A H 0.0073 0.3800 0.4148 0.053 Uiso 1 1 calc R . .
H23B H 0.0285 0.3495 0.4830 0.053 Uiso 1 1 calc R . .
H23C H 0.0400 0.2528 0.4294 0.053 Uiso 1 1 calc R . .
C8 C -0.10576(16) -0.0185(4) 0.18299(18) 0.0316(10) Uani 1 1 d . . .
C7 C -0.08379(15) 0.0829(4) 0.23000(17) 0.0253(9) Uani 1 1 d . . .
C19 C 0.16930(16) 0.4326(5) 0.51620(17) 0.0361(11) Uani 1 1 d . . .
H19A H 0.2019 0.3908 0.5341 0.054 Uiso 1 1 calc R . .
H19B H 0.1423 0.4438 0.5475 0.054 Uiso 1 1 calc R . .
H19C H 0.1796 0.5147 0.5002 0.054 Uiso 1 1 calc R . .
C6 C 0.10509(15) 0.0792(4) 0.21076(17) 0.0285(10) Uani 1 1 d . . .
H6 H 0.1312 0.0172 0.2011 0.034 Uiso 1 1 calc R . .
C16 C 0.27027(15) 0.2774(5) 0.12617(18) 0.0308(10) Uani 1 1 d . . .
C17 C 0.29814(16) 0.3662(5) 0.03176(18) 0.0418(13) Uani 1 1 d . . .
H17A H 0.2868 0.4318 0.0027 0.063 Uiso 1 1 calc R . .
H17B H 0.2939 0.2839 0.0123 0.063 Uiso 1 1 calc R . .
H17C H 0.3366 0.3789 0.0448 0.063 Uiso 1 1 calc R . .
C3 C 0.06377(16) 0.7106(5) 0.16004(18) 0.0309(10) Uani 1 1 d . . .
C4 C 0.10822(17) 0.1505(5) 0.10007(19) 0.0335(11) Uani 1 1 d . . .
C2 C 0.03137(15) 0.6314(4) 0.20719(16) 0.0230(9) Uani 1 1 d . . .
C1 C 0.0000 0.6987(6) 0.2500 0.0286(14) Uani 1 2 d S . .
H1 H 0.0000 0.7878 0.2500 0.034 Uiso 1 2 calc SR . .
C10 C 0.18705(14) 0.3384(4) 0.29587(16) 0.0233(9) Uani 1 1 d . . .
C15 C 0.17159(14) 0.4124(4) 0.24374(16) 0.0223(9) Uani 1 1 d . . .
H15 H 0.1434 0.4733 0.2460 0.027 Uiso 1 1 calc R . .
C14 C 0.19873(14) 0.3941(4) 0.18839(16) 0.0248(9) Uani 1 1 d . . .
H14 H 0.1896 0.4452 0.1541 0.030 Uiso 1 1 calc R . .
C13 C 0.23938(15) 0.2998(4) 0.18432(17) 0.0277(10) Uani 1 1 d . . .
C12 C 0.25339(16) 0.2249(5) 0.23611(18) 0.0344(11) Uani 1 1 d . . .
H12 H 0.2800 0.1605 0.2332 0.041 Uiso 1 1 calc R . .
C11 C 0.22832(15) 0.2450(5) 0.29178(18) 0.0335(11) Uani 1 1 d . . .
H11 H 0.2389 0.1965 0.3265 0.040 Uiso 1 1 calc R . .
C9 C 0.15927(14) 0.3567(4) 0.35486(16) 0.0222(9) Uani 1 1 d . . .
C21 C 0.09155(14) 0.4093(4) 0.42845(16) 0.0245(9) Uani 1 1 d . . .
C18 C 0.14406(15) 0.3509(4) 0.46350(16) 0.0262(10) Uani 1 1 d . . .
C22 C 0.08537(16) 0.5527(5) 0.43593(18) 0.0353(11) Uani 1 1 d . . .
H22A H 0.1201 0.5938 0.4276 0.053 Uiso 1 1 calc R . .
H22B H 0.0755 0.5717 0.4777 0.053 Uiso 1 1 calc R . .
H22C H 0.0566 0.5835 0.4073 0.053 Uiso 1 1 calc R . .
C20 C 0.13715(17) 0.2142(5) 0.48560(18) 0.0370(11) Uani 1 1 d . . .
H20A H 0.1238 0.1618 0.4515 0.056 Uiso 1 1 calc R . .
H20B H 0.1107 0.2121 0.5179 0.056 Uiso 1 1 calc R . .
H20C H 0.1725 0.1821 0.5014 0.056 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.312(2) 2 ?
Dy1 O1 2.312(2) . ?
Dy1 O3 2.313(2) 2 ?
Dy1 O3 2.313(2) . ?
Dy1 O2 2.344(3) 2 ?
Dy1 O2 2.344(3) . ?
Dy1 O4 2.347(3) . ?
Dy1 O4 2.347(3) 2 ?
F2 C3 1.328(4) . ?
F9 C8 1.321(5) . ?
F3 C3 1.332(5) . ?
F7 C8 1.319(4) . ?
F8 C8 1.322(5) . ?
F6 C4 1.319(5) . ?
F5 C4 1.318(5) . ?
F4 C4 1.337(5) . ?
F1 C3 1.319(5) . ?
O7 C16 1.328(5) . ?
O7 C17 1.454(4) . ?
O4 C7 1.245(4) . ?
O6 C16 1.205(5) . ?
O3 C5 1.258(4) . ?
O2 C2 1.243(5) . ?
O1 N1 1.305(3) . ?
O5 N2 1.274(4) . ?
N1 C9 1.324(4) . ?
N1 C21 1.509(4) . ?
N2 C9 1.358(5) . ?
N2 C18 1.509(4) . ?
C5 C6 1.387(5) . ?
C5 C4 1.537(5) . ?
C23 C21 1.519(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C8 C7 1.542(6) . ?
C7 C6 1.394(5) 2 ?
C19 C18 1.524(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C6 C7 1.394(5) 2 ?
C6 H6 0.9300 . ?
C16 C13 1.499(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C3 C2 1.544(5) . ?
C2 C1 1.402(5) . ?
C1 C2 1.402(5) 2 ?
C1 H1 0.9300 . ?
C10 C11 1.394(5) . ?
C10 C15 1.399(5) . ?
C10 C9 1.471(5) . ?
C15 C14 1.395(5) . ?
C15 H15 0.9300 . ?
C14 C13 1.390(6) . ?
C14 H14 0.9300 . ?
C13 C12 1.391(6) . ?
C12 C11 1.379(5) . ?
C12 H12 0.9300 . ?
C11 H11 0.9300 . ?
C21 C22 1.514(6) . ?
C21 C18 1.563(5) . ?
C18 C20 1.516(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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 O1 138.21(14) 2 . ?
O1 Dy1 O3 98.82(8) 2 2 ?
O1 Dy1 O3 94.80(8) . 2 ?
O1 Dy1 O3 94.80(8) 2 . ?
O1 Dy1 O3 98.82(8) . . ?
O3 Dy1 O3 141.18(14) 2 . ?
O1 Dy1 O2 73.30(9) 2 2 ?
O1 Dy1 O2 73.66(9) . 2 ?
O3 Dy1 O2 72.31(9) 2 2 ?
O3 Dy1 O2 146.49(9) . 2 ?
O1 Dy1 O2 73.66(9) 2 . ?
O1 Dy1 O2 73.30(9) . . ?
O3 Dy1 O2 146.49(9) 2 . ?
O3 Dy1 O2 72.31(9) . . ?
O2 Dy1 O2 74.27(12) 2 . ?
O1 Dy1 O4 72.52(9) 2 . ?
O1 Dy1 O4 149.20(10) . . ?
O3 Dy1 O4 73.87(9) 2 . ?
O3 Dy1 O4 75.95(9) . . ?
O2 Dy1 O4 126.60(8) 2 . ?
O2 Dy1 O4 130.72(8) . . ?
O1 Dy1 O4 149.20(10) 2 2 ?
O1 Dy1 O4 72.52(9) . 2 ?
O3 Dy1 O4 75.95(9) 2 2 ?
O3 Dy1 O4 73.87(9) . 2 ?
O2 Dy1 O4 130.72(8) 2 2 ?
O2 Dy1 O4 126.60(8) . 2 ?
O4 Dy1 O4 76.92(13) . 2 ?
C16 O7 C17 115.7(4) . . ?
C7 O4 Dy1 133.5(2) . . ?
C5 O3 Dy1 134.6(2) . . ?
C2 O2 Dy1 133.5(2) . . ?
N1 O1 Dy1 145.7(2) . . ?
O1 N1 C9 125.6(3) . . ?
O1 N1 C21 119.7(3) . . ?
C9 N1 C21 114.0(3) . . ?
O5 N2 C9 125.9(3) . . ?
O5 N2 C18 121.6(3) . . ?
C9 N2 C18 112.4(3) . . ?
O3 C5 C6 128.5(3) . . ?
O3 C5 C4 114.0(3) . . ?
C6 C5 C4 117.4(4) . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
F7 C8 F9 106.5(4) . . ?
F7 C8 F8 106.8(4) . . ?
F9 C8 F8 107.4(3) . . ?
F7 C8 C7 112.1(3) . . ?
F9 C8 C7 109.9(4) . . ?
F8 C8 C7 113.7(3) . . ?
O4 C7 C6 129.1(4) . 2 ?
O4 C7 C8 113.9(3) . . ?
C6 C7 C8 117.0(4) 2 . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C6 C7 120.2(4) . 2 ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 2 . ?
O6 C16 O7 124.4(4) . . ?
O6 C16 C13 123.0(4) . . ?
O7 C16 C13 112.5(4) . . ?
O7 C17 H17A 109.5 . . ?
O7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O7 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
F1 C3 F2 107.5(4) . . ?
F1 C3 F3 107.2(4) . . ?
F2 C3 F3 106.6(3) . . ?
F1 C3 C2 114.3(4) . . ?
F2 C3 C2 110.9(3) . . ?
F3 C3 C2 110.0(3) . . ?
F5 C4 F6 107.7(4) . . ?
F5 C4 F4 106.4(3) . . ?
F6 C4 F4 106.4(4) . . ?
F5 C4 C5 113.9(3) . . ?
F6 C4 C5 110.4(3) . . ?
F4 C4 C5 111.7(4) . . ?
O2 C2 C1 129.4(4) . . ?
O2 C2 C3 113.1(3) . . ?
C1 C2 C3 117.5(4) . . ?
C2 C1 C2 119.8(6) . 2 ?
C2 C1 H1 120.1 . . ?
C2 C1 H1 120.1 2 . ?
C11 C10 C15 120.0(3) . . ?
C11 C10 C9 119.6(3) . . ?
C15 C10 C9 120.4(3) . . ?
C14 C15 C10 119.5(4) . . ?
C14 C15 H15 120.2 . . ?
C10 C15 H15 120.2 . . ?
C13 C14 C15 120.3(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C13 C12 119.6(3) . . ?
C14 C13 C16 122.3(4) . . ?
C12 C13 C16 118.1(4) . . ?
C11 C12 C13 120.8(4) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C11 C10 119.8(4) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
N1 C9 N2 108.5(3) . . ?
N1 C9 C10 126.9(3) . . ?
N2 C9 C10 124.6(3) . . ?
N1 C21 C22 106.4(3) . . ?
N1 C21 C23 108.6(3) . . ?
C22 C21 C23 110.7(3) . . ?
N1 C21 C18 100.6(3) . . ?
C22 C21 C18 114.5(3) . . ?
C23 C21 C18 115.0(4) . . ?
N2 C18 C20 105.7(3) . . ?
N2 C18 C19 108.8(3) . . ?
C20 C18 C19 109.8(3) . . ?
N2 C18 C21 101.3(3) . . ?
C20 C18 C21 115.0(3) . . ?
C19 C18 C21 115.2(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Dy1 O4 C7 -106.9(4) 2 . . . ?
O1 Dy1 O4 C7 69.8(4) . . . . ?
O3 Dy1 O4 C7 -1.9(3) 2 . . . ?
O3 Dy1 O4 C7 153.4(4) . . . . ?
O2 Dy1 O4 C7 -54.4(4) 2 . . . ?
O2 Dy1 O4 C7 -155.6(3) . . . . ?
O4 Dy1 O4 C7 77.0(3) 2 . . . ?
O1 Dy1 O3 C5 -146.3(3) 2 . . . ?
O1 Dy1 O3 C5 73.3(3) . . . . ?
O3 Dy1 O3 C5 -35.8(3) 2 . . . ?
O2 Dy1 O3 C5 147.0(3) 2 . . . ?
O2 Dy1 O3 C5 142.6(3) . . . . ?
O4 Dy1 O3 C5 -75.7(3) . . . . ?
O4 Dy1 O3 C5 4.5(3) 2 . . . ?
O1 Dy1 O2 C2 74.8(3) 2 . . . ?
O1 Dy1 O2 C2 -79.3(3) . . . . ?
O3 Dy1 O2 C2 -6.4(4) 2 . . . ?
O3 Dy1 O2 C2 175.4(3) . . . . ?
O2 Dy1 O2 C2 -2.0(3) 2 . . . ?
O4 Dy1 O2 C2 123.1(3) . . . . ?
O4 Dy1 O2 C2 -131.4(3) 2 . . . ?
O1 Dy1 O1 N1 167.0(4) 2 . . . ?
O3 Dy1 O1 N1 58.1(4) 2 . . . ?
O3 Dy1 O1 N1 -85.5(4) . . . . ?
O2 Dy1 O1 N1 128.1(4) 2 . . . ?
O2 Dy1 O1 N1 -153.9(4) . . . . ?
O4 Dy1 O1 N1 -8.1(4) . . . . ?
O4 Dy1 O1 N1 -15.6(3) 2 . . . ?
Dy1 O1 N1 C9 94.5(5) . . . . ?
Dy1 O1 N1 C21 -95.7(4) . . . . ?
Dy1 O3 C5 C6 -6.8(6) . . . . ?
Dy1 O3 C5 C4 171.7(2) . . . . ?
Dy1 O4 C7 C6 1.3(6) . . . 2 ?
Dy1 O4 C7 C8 179.6(2) . . . . ?
F7 C8 C7 O4 36.9(5) . . . . ?
F9 C8 C7 O4 -81.4(4) . . . . ?
F8 C8 C7 O4 158.2(4) . . . . ?
F7 C8 C7 C6 -144.5(4) . . . 2 ?
F9 C8 C7 C6 97.2(4) . . . 2 ?
F8 C8 C7 C6 -23.2(5) . . . 2 ?
O3 C5 C6 C7 4.2(7) . . . 2 ?
C4 C5 C6 C7 -174.2(4) . . . 2 ?
C17 O7 C16 O6 -6.5(6) . . . . ?
C17 O7 C16 C13 171.9(3) . . . . ?
O3 C5 C4 F5 162.6(4) . . . . ?
C6 C5 C4 F5 -18.8(6) . . . . ?
O3 C5 C4 F6 -76.1(5) . . . . ?
C6 C5 C4 F6 102.5(4) . . . . ?
O3 C5 C4 F4 42.0(5) . . . . ?
C6 C5 C4 F4 -139.4(4) . . . . ?
Dy1 O2 C2 C1 4.3(6) . . . . ?
Dy1 O2 C2 C3 -176.3(2) . . . . ?
F1 C3 C2 O2 171.5(3) . . . . ?
F2 C3 C2 O2 -66.8(5) . . . . ?
F3 C3 C2 O2 50.8(5) . . . . ?
F1 C3 C2 C1 -9.0(5) . . . . ?
F2 C3 C2 C1 112.7(4) . . . . ?
F3 C3 C2 C1 -129.7(3) . . . . ?
O2 C2 C1 C2 -2.2(3) . . . 2 ?
C3 C2 C1 C2 178.4(4) . . . 2 ?
C11 C10 C15 C14 -1.6(6) . . . . ?
C9 C10 C15 C14 179.6(4) . . . . ?
C10 C15 C14 C13 2.4(6) . . . . ?
C15 C14 C13 C12 -0.9(6) . . . . ?
C15 C14 C13 C16 -179.2(4) . . . . ?
O6 C16 C13 C14 -168.0(4) . . . . ?
O7 C16 C13 C14 13.6(6) . . . . ?
O6 C16 C13 C12 13.6(6) . . . . ?
O7 C16 C13 C12 -164.8(4) . . . . ?
C14 C13 C12 C11 -1.4(7) . . . . ?
C16 C13 C12 C11 176.9(4) . . . . ?
C13 C12 C11 C10 2.2(7) . . . . ?
C15 C10 C11 C12 -0.7(6) . . . . ?
C9 C10 C11 C12 178.1(4) . . . . ?
O1 N1 C9 N2 175.3(4) . . . . ?
C21 N1 C9 N2 5.0(5) . . . . ?
O1 N1 C9 C10 -5.0(7) . . . . ?
C21 N1 C9 C10 -175.3(4) . . . . ?
O5 N2 C9 N1 -176.7(4) . . . . ?
C18 N2 C9 N1 7.7(5) . . . . ?
O5 N2 C9 C10 3.6(7) . . . . ?
C18 N2 C9 C10 -172.1(4) . . . . ?
C11 C10 C9 N1 -144.1(4) . . . . ?
C15 C10 C9 N1 34.7(6) . . . . ?
C11 C10 C9 N2 35.6(6) . . . . ?
C15 C10 C9 N2 -145.6(4) . . . . ?
O1 N1 C21 C22 -65.7(4) . . . . ?
C9 N1 C21 C22 105.2(4) . . . . ?
O1 N1 C21 C23 53.5(5) . . . . ?
C9 N1 C21 C23 -135.5(4) . . . . ?
O1 N1 C21 C18 174.6(3) . . . . ?
C9 N1 C21 C18 -14.5(5) . . . . ?
O5 N2 C18 C20 -71.6(5) . . . . ?
C9 N2 C18 C20 104.3(4) . . . . ?
O5 N2 C18 C19 46.3(5) . . . . ?
C9 N2 C18 C19 -137.8(4) . . . . ?
O5 N2 C18 C21 168.1(4) . . . . ?
C9 N2 C18 C21 -16.0(5) . . . . ?
N1 C21 C18 N2 16.6(4) . . . . ?
C22 C21 C18 N2 -97.1(4) . . . . ?
C23 C21 C18 N2 133.0(4) . . . . ?
N1 C21 C18 C20 -96.9(4) . . . . ?
C22 C21 C18 C20 149.4(3) . . . . ?
C23 C21 C18 C20 19.6(5) . . . . ?
N1 C21 C18 C19 133.8(3) . . . . ?
C22 C21 C18 C19 20.2(5) . . . . ?
C23 C21 C18 C19 -109.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.110
