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

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

data_k11234
_database_code_depnum_ccdc_archive 'CCDC 1856921'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H11 F18 La N2 O6'
_chemical_formula_sum            'C25 H11 F18 La N2 O6'
_chemical_formula_weight         916.27

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'
O O 0.0106 0.0060 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.040(2)
_cell_length_b                   15.830(3)
_cell_length_c                   17.855(4)
_cell_angle_alpha                78.40(3)
_cell_angle_beta                 76.30(3)
_cell_angle_gamma                72.70(3)
_cell_volume                     3125.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    34028
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_F_000             1768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.517
_shelx_estimated_absorpt_T_min   0.694
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
__diffrn_source                  'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            33367
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.548
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11029
_reflns_number_gt                8087
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0589P)²+13.1714P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11029
_refine_ls_number_parameters     1075
_refine_ls_number_restraints     447
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1428
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.97310(3) 0.23637(3) 0.53504(2) 0.02935(13) Uani 1 1 d . U . . .
N1 N 1.0186(5) 0.3704(4) 0.5808(3) 0.0325(12) Uani 1 1 d . U . . .
C2 C 0.9675(6) 0.3907(5) 0.6525(4) 0.0368(16) Uani 1 1 d . U . . .
H2A H 0.906092 0.364364 0.681307 0.044 Uiso 1 1 calc R U . . .
C3 C 1.0008(7) 0.4485(5) 0.6860(4) 0.0406(17) Uani 1 1 d . U . . .
H3A H 0.962368 0.462092 0.736812 0.049 Uiso 1 1 calc R U . . .
C4 C 1.0895(7) 0.4858(5) 0.6451(4) 0.0481(19) Uani 1 1 d . U . . .
H4A H 1.114739 0.524867 0.667398 0.058 Uiso 1 1 calc R U . . .
C5 C 1.1430(7) 0.4658(5) 0.5699(5) 0.0465(18) Uani 1 1 d . U . . .
H5A H 1.204116 0.492142 0.540388 0.056 Uiso 1 1 calc R U . . .
C6 C 1.1069(6) 0.4080(4) 0.5388(4) 0.0341(15) Uani 1 1 d . U . . .
C7 C 1.1567(6) 0.3856(4) 0.4589(4) 0.0340(15) Uani 1 1 d . U . . .
C8 C 1.2507(7) 0.4146(6) 0.4110(4) 0.0480(19) Uani 1 1 d . U . . .
H8A H 1.286929 0.449673 0.429931 0.058 Uiso 1 1 calc R U . . .
C9 C 1.2923(7) 0.3937(6) 0.3375(5) 0.055(2) Uani 1 1 d . U . . .
H9A H 1.356873 0.414001 0.305151 0.066 Uiso 1 1 calc R U . . .
C10 C 1.2395(7) 0.3431(5) 0.3108(4) 0.0494(19) Uani 1 1 d . U . . .
H10A H 1.265344 0.328592 0.259265 0.059 Uiso 1 1 calc R U . . .
C11 C 1.1481(7) 0.3140(5) 0.3604(4) 0.0458(18) Uani 1 1 d . U . . .
H11A H 1.112498 0.277901 0.342119 0.055 Uiso 1 1 calc R U . . .
N12 N 1.1060(5) 0.3334(4) 0.4333(3) 0.0382(13) Uani 1 1 d . U . . .
O21 O 1.1792(4) 0.1784(3) 0.5559(3) 0.0415(11) Uani 1 1 d . U . . .
C22 C 1.2281(6) 0.1632(5) 0.6139(5) 0.0382(16) Uani 1 1 d . U . . .
C23 C 1.1757(7) 0.1505(5) 0.6917(5) 0.0439(17) Uani 1 1 d . U . . .
H23A H 1.223634 0.138124 0.729934 0.053 Uiso 1 1 calc R U . . .
C24 C 1.0569(6) 0.1551(4) 0.7158(4) 0.0358(15) Uani 1 1 d . U . . .
O25 O 0.9794(4) 0.1752(3) 0.6742(3) 0.0345(10) Uani 1 1 d . U . . .
C26 C 1.3586(7) 0.1606(6) 0.5910(5) 0.0515(19) Uani 1 1 d . U . . .
C27 C 1.0094(8) 0.1358(6) 0.8031(4) 0.0491(19) Uani 1 1 d . U . . .
F21 F 1.4184(4) 0.0972(4) 0.5485(4) 0.094(2) Uani 1 1 d . U . . .
F22 F 1.4118(5) 0.1441(5) 0.6519(4) 0.099(2) Uani 1 1 d . U . . .
F23 F 1.3761(5) 0.2356(4) 0.5524(4) 0.097(2) Uani 1 1 d . U . . .
F24 F 0.9263(6) 0.2059(5) 0.8285(3) 0.099(2) Uani 1 1 d . U . . .
F25 F 1.0897(5) 0.1170(5) 0.8466(3) 0.0897(19) Uani 1 1 d . U . . .
F26 F 0.9603(7) 0.0696(5) 0.8194(3) 0.100(2) Uani 1 1 d . U . . .
O31 O 0.8529(4) 0.1308(3) 0.5455(3) 0.0365(11) Uani 1 1 d . U . . .
C32 C 0.8320(6) 0.0935(4) 0.4962(4) 0.0346(15) Uani 1 1 d . U . . .
C33 C 0.9006(7) 0.0765(5) 0.4248(4) 0.0416(17) Uani 1 1 d . U . . .
H33A H 0.876280 0.045167 0.394209 0.050 Uiso 1 1 calc R U . . .
C34 C 1.0046(7) 0.1035(5) 0.3956(4) 0.0395(16) Uani 1 1 d . U . . .
O35 O 1.0521(4) 0.1432(3) 0.4282(3) 0.0423(12) Uani 1 1 d . U . . .
C36 C 0.7133(7) 0.0701(5) 0.5191(4) 0.0502(18) Uani 1 1 d D U . . .
C37 C 1.0694(8) 0.0858(5) 0.3121(5) 0.055(2) Uani 1 1 d D U . . .
F31A F 0.6337(11) 0.1434(8) 0.5028(13) 0.122(7) Uani 0.58 1 d D U P A 1
F32A F 0.695(3) 0.0268(17) 0.5876(9) 0.091(7) Uani 0.58 1 d D U P A 1
F33A F 0.7086(19) 0.0188(14) 0.4712(13) 0.082(6) Uani 0.58 1 d D U P A 1
F31B F 0.714(4) 0.005(2) 0.5762(16) 0.106(11) Uani 0.42 1 d D U P A 2
F32B F 0.667(3) 0.053(3) 0.4684(19) 0.127(14) Uani 0.42 1 d D U P A 2
F33B F 0.6320(16) 0.1292(14) 0.5605(14) 0.099(7) Uani 0.42 1 d D U P A 2
F34A F 1.1705(8) 0.1107(8) 0.2906(5) 0.079(3) Uani 0.71 1 d D U P B 1
F35A F 1.0997(10) 0.0018(5) 0.3067(6) 0.070(3) Uani 0.71 1 d D U P B 1
F36A F 1.0048(10) 0.1282(9) 0.2622(5) 0.093(3) Uani 0.71 1 d D U P B 1
F34B F 0.999(3) 0.059(3) 0.2797(14) 0.118(10) Uani 0.29 1 d D U P B 2
F35B F 1.074(5) 0.1597(15) 0.2680(14) 0.157(18) Uani 0.29 1 d D U P B 2
F36B F 1.158(3) 0.017(3) 0.308(2) 0.22(2) Uani 0.29 1 d D U P B 2
O41 O 0.7733(4) 0.3210(3) 0.5968(3) 0.0405(11) Uani 1 1 d . U . . .
C42 C 0.6740(7) 0.3463(5) 0.5770(5) 0.0430(16) Uani 1 1 d . U . . .
C43 C 0.6476(7) 0.3513(5) 0.5045(5) 0.0476(18) Uani 1 1 d . U . . .
H43A H 0.567119 0.368943 0.498724 0.057 Uiso 1 1 calc R U . . .
C44 C 0.7363(7) 0.3310(5) 0.4403(5) 0.0423(16) Uani 1 1 d . U . . .
O45 O 0.8471(4) 0.3089(3) 0.4364(3) 0.0406(11) Uani 1 1 d . U . . .
C46 C 0.5698(7) 0.3778(6) 0.6421(5) 0.0547(19) Uani 1 1 d . U . . .
C47 C 0.7013(8) 0.3397(5) 0.3616(5) 0.0513(19) Uani 1 1 d . U . . .
F41A F 0.4635(10) 0.4033(15) 0.6172(10) 0.096(5) Uani 0.55 1 d . U P C 1
F42A F 0.5616(19) 0.3206(13) 0.6987(13) 0.130(9) Uani 0.55 1 d . U P C 1
F43A F 0.5760(17) 0.4483(14) 0.6608(14) 0.101(6) Uani 0.55 1 d . U P C 1
F41B F 0.6043(19) 0.364(2) 0.7130(12) 0.107(7) Uani 0.45 1 d . U P C 2
F42B F 0.524(3) 0.4597(17) 0.6329(19) 0.155(13) Uani 0.45 1 d . U P C 2
F43B F 0.499(3) 0.329(3) 0.6593(19) 0.149(12) Uani 0.45 1 d . U P C 2
F44 F 0.7234(6) 0.4110(4) 0.3155(3) 0.0800(17) Uani 1 1 d . U . . .
F45 F 0.7552(6) 0.2690(4) 0.3273(4) 0.096(2) Uani 1 1 d . U . . .
F46 F 0.5854(5) 0.3489(4) 0.3673(4) 0.0890(18) Uani 1 1 d . U . . .
La2 La 0.52455(3) 0.73764(3) 0.98038(2) 0.02834(13) Uani 1 1 d . U . . .
N51 N 0.4453(5) 0.8404(4) 1.0915(3) 0.0332(12) Uani 1 1 d . U . . .
C52 C 0.3565(7) 0.8242(5) 1.1493(4) 0.0446(17) Uani 1 1 d . U . . .
H52A H 0.311637 0.787201 1.142150 0.054 Uiso 1 1 calc R U . . .
C53 C 0.3272(7) 0.8592(5) 1.2190(4) 0.0483(19) Uani 1 1 d . U . . .
H53A H 0.262947 0.847016 1.258226 0.058 Uiso 1 1 calc R U . . .
C54 C 0.3918(8) 0.9107(6) 1.2299(5) 0.053(2) Uani 1 1 d . U . . .
H54A H 0.374374 0.934906 1.277169 0.063 Uiso 1 1 calc R U . . .
C55 C 0.4827(7) 0.9277(5) 1.1719(4) 0.0447(18) Uani 1 1 d . U . . .
H55A H 0.528346 0.964128 1.179075 0.054 Uiso 1 1 calc R U . . .
C56 C 0.5092(6) 0.8923(4) 1.1027(4) 0.0333(15) Uani 1 1 d . U . . .
C57 C 0.6067(6) 0.9093(4) 1.0373(4) 0.0319(14) Uani 1 1 d . U . . .
C58 C 0.6773(7) 0.9633(5) 1.0384(5) 0.0440(18) Uani 1 1 d . U . . .
H58A H 0.665932 0.991685 1.082727 0.053 Uiso 1 1 calc R U . . .
C59 C 0.7646(6) 0.9761(5) 0.9747(5) 0.0442(18) Uani 1 1 d . U . . .
H59A H 0.813794 1.012866 0.975341 0.053 Uiso 1 1 calc R U . . .
C60 C 0.7800(6) 0.9366(5) 0.9118(4) 0.0376(16) Uani 1 1 d . U . . .
H60A H 0.839786 0.944831 0.867630 0.045 Uiso 1 1 calc R U . . .
C61 C 0.7067(6) 0.8837(4) 0.9131(4) 0.0331(15) Uani 1 1 d . U . . .
H61A H 0.716513 0.856370 0.868429 0.040 Uiso 1 1 calc R U . . .
N62 N 0.6224(5) 0.8691(3) 0.9743(3) 0.0291(11) Uani 1 1 d . U . . .
O71 O 0.4094(5) 0.6412(3) 1.0717(3) 0.0434(12) Uani 1 1 d . U . . .
C72 C 0.3434(7) 0.5981(5) 1.0629(4) 0.0416(16) Uani 1 1 d . U . . .
C73 C 0.3336(7) 0.5726(5) 0.9953(5) 0.0471(18) Uani 1 1 d . U . . .
H73A H 0.278060 0.539631 0.998122 0.057 Uiso 1 1 calc R U . . .
C74 C 0.4022(7) 0.5938(5) 0.9238(5) 0.0406(16) Uani 1 1 d . U . . .
O75 O 0.4824(4) 0.6343(3) 0.9105(3) 0.0354(11) Uani 1 1 d . U . . .
C76 C 0.2557(8) 0.5749(5) 1.1360(5) 0.053(2) Uani 1 1 d . U . . .
C77 C 0.3788(7) 0.5698(5) 0.8524(5) 0.0427(17) Uani 1 1 d . U . . .
F71 F 0.2630(7) 0.6074(5) 1.1967(4) 0.118(3) Uani 1 1 d . U . . .
F72 F 0.1467(5) 0.6018(6) 1.1271(4) 0.129(3) Uani 1 1 d . U . . .
F73 F 0.2766(6) 0.4887(4) 1.1585(3) 0.0903(19) Uani 1 1 d . U . . .
F74 F 0.4709(5) 0.5306(5) 0.8075(3) 0.100(2) Uani 1 1 d . U . . .
F75 F 0.3064(6) 0.5192(5) 0.8663(4) 0.110(2) Uani 1 1 d . U . . .
F76 F 0.3208(10) 0.6416(4) 0.8147(5) 0.163(4) Uani 1 1 d . U . . .
O81 O 0.7346(4) 0.6731(3) 0.9214(3) 0.0381(11) Uani 1 1 d . U . . .
C82 C 0.8319(6) 0.6544(4) 0.9430(4) 0.0368(15) Uani 1 1 d . U . . .
C83 C 0.8501(7) 0.6526(5) 1.0173(5) 0.0450(17) Uani 1 1 d . U . . .
H83A H 0.929007 0.641097 1.024891 0.054 Uiso 1 1 calc R U . . .
C84 C 0.7577(7) 0.6669(5) 1.0812(5) 0.0425(17) Uani 1 1 d . U . . .
O85 O 0.6499(4) 0.6831(3) 1.0809(3) 0.0388(11) Uani 1 1 d . U . . .
C86 C 0.9405(7) 0.6319(5) 0.8787(5) 0.0548(19) Uani 1 1 d D U . . .
C87 C 0.7865(8) 0.6646(6) 1.1597(5) 0.057(2) Uani 1 1 d . U . . .
F81A F 1.0387(9) 0.6109(16) 0.9048(11) 0.125(8) Uani 0.66 1 d D U P D 1
F82A F 0.9397(14) 0.5738(14) 0.8383(13) 0.134(8) Uani 0.66 1 d D U P D 1
F83A F 0.9424(17) 0.7042(9) 0.8293(9) 0.123(6) Uani 0.66 1 d D U P D 1
F81B F 0.924(2) 0.664(3) 0.8101(10) 0.117(12) Uani 0.34 1 d D U P D 2
F82B F 1.038(2) 0.647(3) 0.882(2) 0.126(14) Uani 0.34 1 d D U P D 2
F83B F 0.971(4) 0.5451(10) 0.8841(19) 0.129(14) Uani 0.34 1 d D U P D 2
F84 F 0.7259(7) 0.7387(5) 1.1895(4) 0.114(3) Uani 1 1 d . U . . .
F85 F 0.8977(6) 0.6606(6) 1.1582(4) 0.115(2) Uani 1 1 d . U . . .
F86 F 0.7580(8) 0.6004(5) 1.2097(4) 0.128(3) Uani 1 1 d . U . . .
O91 O 0.5066(5) 0.8232(3) 0.8493(3) 0.0438(12) Uani 1 1 d . U . . .
C92 C 0.4250(8) 0.8467(5) 0.8094(4) 0.0447(17) Uani 1 1 d . U . . .
C93 C 0.3048(8) 0.8501(5) 0.8371(5) 0.0493(18) Uani 1 1 d . U . . .
H93A H 0.253478 0.867347 0.800476 0.059 Uiso 1 1 calc R U . . .
C94 C 0.2565(7) 0.8296(5) 0.9154(5) 0.0431(17) Uani 1 1 d . U . . .
O95 O 0.3117(4) 0.8074(3) 0.9704(3) 0.0388(11) Uani 1 1 d . U . . .
C96 C 0.4645(7) 0.8738(5) 0.7243(5) 0.056(2) Uani 1 1 d D U . . .
C97 C 0.1256(7) 0.8378(5) 0.9373(5) 0.0492(19) Uani 1 1 d . U . . .
F91A F 0.533(3) 0.926(2) 0.7076(17) 0.149(11) Uani 0.58 1 d D U P E 1
F92A F 0.3774(15) 0.9077(16) 0.6868(10) 0.125(8) Uani 0.58 1 d D U P E 1
F93A F 0.519(2) 0.8050(14) 0.6900(15) 0.113(9) Uani 0.58 1 d D U P E 1
F91B F 0.470(3) 0.820(2) 0.6781(18) 0.103(11) Uani 0.42 1 d D U P E 2
F92B F 0.571(2) 0.883(3) 0.706(2) 0.142(16) Uani 0.42 1 d D U P E 2
F93B F 0.398(3) 0.9479(17) 0.6992(19) 0.185(17) Uani 0.42 1 d D U P E 2
F94 F 0.1039(5) 0.7654(4) 0.9857(4) 0.096(2) Uani 1 1 d . U . . .
F95 F 0.0680(4) 0.9068(4) 0.9752(4) 0.0844(18) Uani 1 1 d . U . . .
F96 F 0.0728(5) 0.8434(5) 0.8809(4) 0.098(2) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O21 2.466(5) . ?
La1 O31 2.470(4) . ?
La1 O45 2.478(5) . ?
La1 O35 2.480(5) . ?
La1 O25 2.490(5) . ?
La1 O41 2.493(5) . ?
La1 N1 2.659(5) . ?
La1 N12 2.680(6) . ?
N1 C2 1.340(9) . ?
N1 C6 1.366(9) . ?
C2 C3 1.382(10) . ?
C2 H2A 0.9500 . ?
C3 C4 1.361(11) . ?
C3 H3A 0.9500 . ?
C4 C5 1.400(11) . ?
C4 H4A 0.9500 . ?
C5 C6 1.375(10) . ?
C5 H5A 0.9500 . ?
C6 C7 1.480(10) . ?
C7 N12 1.359(9) . ?
C7 C8 1.383(10) . ?
C8 C9 1.360(11) . ?
C8 H8A 0.9500 . ?
C9 C10 1.369(12) . ?
C9 H9A 0.9500 . ?
C10 C11 1.373(10) . ?
C10 H10A 0.9500 . ?
C11 N12 1.342(9) . ?
C11 H11A 0.9500 . ?
O21 C22 1.258(8) . ?
C22 C23 1.384(11) . ?
C22 C26 1.518(10) . ?
C23 C24 1.377(10) . ?
C23 H23A 0.9500 . ?
C24 O25 1.257(8) . ?
C24 C27 1.531(10) . ?
C26 F23 1.296(9) . ?
C26 F21 1.311(10) . ?
C26 F22 1.334(10) . ?
C27 F26 1.302(9) . ?
C27 F25 1.311(9) . ?
C27 F24 1.329(10) . ?
O31 C32 1.261(8) . ?
C32 C33 1.374(10) . ?
C32 C36 1.525(10) . ?
C33 C34 1.393(10) . ?
C33 H33A 0.9500 . ?
C34 O35 1.258(8) . ?
C34 C37 1.548(11) . ?
C36 F32B 1.275(14) . ?
C36 F32A 1.279(12) . ?
C36 F31B 1.293(14) . ?
C36 F31A 1.298(11) . ?
C36 F33A 1.313(11) . ?
C36 F33B 1.330(13) . ?
C37 F36A 1.276(10) . ?
C37 F36B 1.276(15) . ?
C37 F35B 1.282(14) . ?
C37 F35A 1.286(9) . ?
C37 F34B 1.336(14) . ?
C37 F34A 1.337(9) . ?
O41 C42 1.253(9) . ?
C42 C43 1.387(11) . ?
C42 C46 1.532(11) . ?
C43 C44 1.387(11) . ?
C43 H43A 0.9500 . ?
C44 O45 1.263(9) . ?
C44 C47 1.530(11) . ?
C46 F42A 1.221(16) . ?
C46 F42B 1.24(2) . ?
C46 F43A 1.255(17) . ?
C46 F43B 1.26(2) . ?
C46 F41A 1.375(15) . ?
C46 F41B 1.38(2) . ?
C47 F45 1.305(10) . ?
C47 F44 1.312(9) . ?
C47 F46 1.340(10) . ?
La2 O71 2.470(5) . ?
La2 O75 2.471(4) . ?
La2 O85 2.475(5) . ?
La2 O91 2.480(5) . ?
La2 O81 2.486(5) . ?
La2 O95 2.504(5) . ?
La2 N51 2.640(6) . ?
La2 N62 2.653(5) . ?
N51 C52 1.344(9) . ?
N51 C56 1.351(9) . ?
C52 C53 1.390(11) . ?
C52 H52A 0.9500 . ?
C53 C54 1.350(11) . ?
C53 H53A 0.9500 . ?
C54 C55 1.366(11) . ?
C54 H54A 0.9500 . ?
C55 C56 1.388(10) . ?
C55 H55A 0.9500 . ?
C56 C57 1.492(10) . ?
C57 N62 1.350(8) . ?
C57 C58 1.378(10) . ?
C58 C59 1.381(10) . ?
C58 H58A 0.9500 . ?
C59 C60 1.341(10) . ?
C59 H59A 0.9500 . ?
C60 C61 1.379(9) . ?
C60 H60A 0.9500 . ?
C61 N62 1.338(8) . ?
C61 H61A 0.9500 . ?
O71 C72 1.244(8) . ?
C72 C73 1.388(11) . ?
C72 C76 1.529(11) . ?
C73 C74 1.385(11) . ?
C73 H73A 0.9500 . ?
C74 O75 1.264(8) . ?
C74 C77 1.509(10) . ?
C76 F72 1.291(10) . ?
C76 F73 1.308(9) . ?
C76 F71 1.320(10) . ?
C77 F74 1.275(9) . ?
C77 F76 1.294(9) . ?
C77 F75 1.301(9) . ?
O81 C82 1.253(8) . ?
C82 C83 1.388(10) . ?
C82 C86 1.527(11) . ?
C83 C84 1.395(11) . ?
C83 H83A 0.9500 . ?
C84 O85 1.247(8) . ?
C84 C87 1.513(11) . ?
C86 F81B 1.267(15) . ?
C86 F82A 1.280(11) . ?
C86 F82B 1.281(14) . ?
C86 F83A 1.299(12) . ?
C86 F81A 1.301(11) . ?
C86 F83B 1.303(14) . ?
C87 F86 1.283(11) . ?
C87 F85 1.315(10) . ?
C87 F84 1.322(11) . ?
O91 C92 1.272(9) . ?
C92 C93 1.403(11) . ?
C92 C96 1.496(11) . ?
C93 C94 1.394(11) . ?
C93 H93A 0.9500 . ?
C94 O95 1.251(8) . ?
C94 C97 1.503(11) . ?
C96 F93B 1.274(14) . ?
C96 F91B 1.276(14) . ?
C96 F91A 1.280(13) . ?
C96 F93A 1.282(13) . ?
C96 F92B 1.291(15) . ?
C96 F92A 1.299(12) . ?
C97 F96 1.289(9) . ?
C97 F95 1.325(9) . ?
C97 F94 1.343(10) . ?

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
O21 La1 O31 119.49(16) . . ?
O21 La1 O45 144.41(17) . . ?
O31 La1 O45 77.01(16) . . ?
O21 La1 O35 81.88(17) . . ?
O31 La1 O35 69.24(16) . . ?
O45 La1 O35 75.08(17) . . ?
O21 La1 O25 68.98(15) . . ?
O31 La1 O25 84.09(15) . . ?
O45 La1 O25 146.61(16) . . ?
O35 La1 O25 123.26(16) . . ?
O21 La1 O41 141.48(16) . . ?
O31 La1 O41 78.17(15) . . ?
O45 La1 O41 69.06(16) . . ?
O35 La1 O41 135.85(16) . . ?
O25 La1 O41 80.35(16) . . ?
O21 La1 N1 75.28(17) . . ?
O31 La1 N1 152.38(16) . . ?
O45 La1 N1 104.84(16) . . ?
O35 La1 N1 138.29(17) . . ?
O25 La1 N1 80.04(16) . . ?
O41 La1 N1 76.99(16) . . ?
O21 La1 N12 71.43(17) . . ?
O31 La1 N12 143.42(16) . . ?
O45 La1 N12 77.73(17) . . ?
O35 La1 N12 78.97(17) . . ?
O25 La1 N12 129.84(16) . . ?
O41 La1 N12 116.21(17) . . ?
N1 La1 N12 60.91(17) . . ?
C2 N1 C6 119.2(6) . . ?
C2 N1 La1 118.5(4) . . ?
C6 N1 La1 121.3(4) . . ?
N1 C2 C3 122.5(7) . . ?
N1 C2 H2A 118.8 . . ?
C3 C2 H2A 118.8 . . ?
C4 C3 C2 118.9(7) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C3 C4 C5 119.3(7) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C6 C5 C4 119.8(7) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
N1 C6 C5 120.3(7) . . ?
N1 C6 C7 116.7(6) . . ?
C5 C6 C7 123.0(6) . . ?
N12 C7 C8 120.0(7) . . ?
N12 C7 C6 116.8(6) . . ?
C8 C7 C6 123.3(6) . . ?
C9 C8 C7 121.3(8) . . ?
C9 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C8 C9 C10 118.9(7) . . ?
C8 C9 H9A 120.5 . . ?
C10 C9 H9A 120.5 . . ?
C9 C10 C11 118.2(7) . . ?
C9 C10 H10A 120.9 . . ?
C11 C10 H10A 120.9 . . ?
N12 C11 C10 123.8(7) . . ?
N12 C11 H11A 118.1 . . ?
C10 C11 H11A 118.1 . . ?
C11 N12 C7 117.8(6) . . ?
C11 N12 La1 119.7(5) . . ?
C7 N12 La1 120.3(4) . . ?
C22 O21 La1 134.6(5) . . ?
O21 C22 C23 127.4(7) . . ?
O21 C22 C26 112.5(7) . . ?
C23 C22 C26 120.1(7) . . ?
C24 C23 C22 122.5(7) . . ?
C24 C23 H23A 118.8 . . ?
C22 C23 H23A 118.8 . . ?
O25 C24 C23 127.6(7) . . ?
O25 C24 C27 114.2(6) . . ?
C23 C24 C27 118.2(7) . . ?
C24 O25 La1 134.8(4) . . ?
F23 C26 F21 108.0(8) . . ?
F23 C26 F22 105.7(7) . . ?
F21 C26 F22 105.2(7) . . ?
F23 C26 C22 112.4(7) . . ?
F21 C26 C22 111.8(7) . . ?
F22 C26 C22 113.2(7) . . ?
F26 C27 F25 107.2(7) . . ?
F26 C27 F24 106.3(8) . . ?
F25 C27 F24 105.7(7) . . ?
F26 C27 C24 111.8(6) . . ?
F25 C27 C24 114.2(7) . . ?
F24 C27 C24 111.1(7) . . ?
C32 O31 La1 133.1(4) . . ?
O31 C32 C33 127.4(7) . . ?
O31 C32 C36 114.2(6) . . ?
C33 C32 C36 118.3(6) . . ?
C32 C33 C34 122.5(7) . . ?
C32 C33 H33A 118.8 . . ?
C34 C33 H33A 118.8 . . ?
O35 C34 C33 127.8(7) . . ?
O35 C34 C37 114.8(7) . . ?
C33 C34 C37 117.4(6) . . ?
C34 O35 La1 132.5(5) . . ?
F32B C36 F31B 107(3) . . ?
F32A C36 F31A 117.3(17) . . ?
F32A C36 F33A 106.2(15) . . ?
F31A C36 F33A 102.9(14) . . ?
F32B C36 F33B 109.2(19) . . ?
F31B C36 F33B 94(2) . . ?
F32B C36 C32 121(2) . . ?
F32A C36 C32 114.0(13) . . ?
F31B C36 C32 111(2) . . ?
F31A C36 C32 106.3(9) . . ?
F33A C36 C32 109.3(11) . . ?
F33B C36 C32 111.4(11) . . ?
F36B C37 F35B 121(3) . . ?
F36A C37 F35A 109.4(9) . . ?
F36B C37 F34B 99(3) . . ?
F35B C37 F34B 100(2) . . ?
F36A C37 F34A 106.9(9) . . ?
F35A C37 F34A 105.1(9) . . ?
F36A C37 C34 111.1(8) . . ?
F36B C37 C34 115.6(19) . . ?
F35B C37 C34 110.2(14) . . ?
F35A C37 C34 111.2(8) . . ?
F34B C37 C34 108.2(13) . . ?
F34A C37 C34 112.8(7) . . ?
C42 O41 La1 133.3(5) . . ?
O41 C42 C43 128.6(7) . . ?
O41 C42 C46 114.6(7) . . ?
C43 C42 C46 116.8(7) . . ?
C42 C43 C44 121.3(7) . . ?
C42 C43 H43A 119.3 . . ?
C44 C43 H43A 119.3 . . ?
O45 C44 C43 128.2(7) . . ?
O45 C44 C47 113.0(7) . . ?
C43 C44 C47 118.7(7) . . ?
C44 O45 La1 132.4(5) . . ?
F42A C46 F43A 111.3(17) . . ?
F42B C46 F43B 116(2) . . ?
F42A C46 F41A 107.0(14) . . ?
F43A C46 F41A 103.2(12) . . ?
F42B C46 F41B 102.7(19) . . ?
F43B C46 F41B 98.8(18) . . ?
F42A C46 C42 113.0(11) . . ?
F42B C46 C42 113.8(15) . . ?
F43A C46 C42 110.1(11) . . ?
F43B C46 C42 112.1(13) . . ?
F41A C46 C42 111.7(9) . . ?
F41B C46 C42 112.1(11) . . ?
F45 C47 F44 109.7(8) . . ?
F45 C47 F46 105.3(7) . . ?
F44 C47 F46 105.6(7) . . ?
F45 C47 C44 111.8(6) . . ?
F44 C47 C44 111.0(6) . . ?
F46 C47 C44 113.1(8) . . ?
O71 La2 O75 69.55(16) . . ?
O71 La2 O85 80.75(16) . . ?
O75 La2 O85 121.87(16) . . ?
O71 La2 O91 133.25(16) . . ?
O75 La2 O91 75.93(15) . . ?
O85 La2 O91 145.62(16) . . ?
O71 La2 O81 120.11(17) . . ?
O75 La2 O81 84.31(15) . . ?
O85 La2 O81 68.92(16) . . ?
O91 La2 O81 85.68(17) . . ?
O71 La2 O95 73.37(17) . . ?
O75 La2 O95 77.36(15) . . ?
O85 La2 O95 139.43(16) . . ?
O91 La2 O95 69.01(17) . . ?
O81 La2 O95 151.59(16) . . ?
O71 La2 N51 83.46(17) . . ?
O75 La2 N51 146.67(16) . . ?
O85 La2 N51 70.00(16) . . ?
O91 La2 N51 112.64(17) . . ?
O81 La2 N51 127.30(16) . . ?
O95 La2 N51 76.39(16) . . ?
O71 La2 N62 142.16(16) . . ?
O75 La2 N62 148.29(16) . . ?
O85 La2 N62 75.46(16) . . ?
O91 La2 N62 76.81(16) . . ?
O81 La2 N62 77.77(16) . . ?
O95 La2 N62 107.36(16) . . ?
N51 La2 N62 60.98(17) . . ?
C52 N51 C56 117.9(6) . . ?
C52 N51 La2 118.8(5) . . ?
C56 N51 La2 121.2(4) . . ?
N51 C52 C53 123.1(7) . . ?
N51 C52 H52A 118.4 . . ?
C53 C52 H52A 118.4 . . ?
C54 C53 C52 118.6(7) . . ?
C54 C53 H53A 120.7 . . ?
C52 C53 H53A 120.7 . . ?
C53 C54 C55 119.2(7) . . ?
C53 C54 H54A 120.4 . . ?
C55 C54 H54A 120.4 . . ?
C54 C55 C56 120.8(8) . . ?
C54 C55 H55A 119.6 . . ?
C56 C55 H55A 119.6 . . ?
N51 C56 C55 120.4(7) . . ?
N51 C56 C57 116.5(6) . . ?
C55 C56 C57 123.1(7) . . ?
N62 C57 C58 120.3(6) . . ?
N62 C57 C56 115.9(6) . . ?
C58 C57 C56 123.7(6) . . ?
C59 C58 C57 119.7(7) . . ?
C59 C58 H58A 120.2 . . ?
C57 C58 H58A 120.2 . . ?
C60 C59 C58 120.2(7) . . ?
C60 C59 H59A 119.9 . . ?
C58 C59 H59A 119.9 . . ?
C59 C60 C61 118.1(7) . . ?
C59 C60 H60A 120.9 . . ?
C61 C60 H60A 120.9 . . ?
N62 C61 C60 123.2(6) . . ?
N62 C61 H61A 118.4 . . ?
C60 C61 H61A 118.4 . . ?
C61 N62 C57 118.5(6) . . ?
C61 N62 La2 118.8(4) . . ?
C57 N62 La2 121.3(4) . . ?
C72 O71 La2 133.1(5) . . ?
O71 C72 C73 129.1(7) . . ?
O71 C72 C76 115.3(7) . . ?
C73 C72 C76 115.6(7) . . ?
C74 C73 C72 122.0(7) . . ?
C74 C73 H73A 119.0 . . ?
C72 C73 H73A 119.0 . . ?
O75 C74 C73 126.9(7) . . ?
O75 C74 C77 114.7(7) . . ?
C73 C74 C77 118.4(7) . . ?
C74 O75 La2 133.5(5) . . ?
F72 C76 F73 106.1(7) . . ?
F72 C76 F71 107.9(8) . . ?
F73 C76 F71 104.3(8) . . ?
F72 C76 C72 113.5(8) . . ?
F73 C76 C72 112.0(7) . . ?
F71 C76 C72 112.5(7) . . ?
F74 C77 F76 110.6(8) . . ?
F74 C77 F75 105.4(7) . . ?
F76 C77 F75 101.4(8) . . ?
F74 C77 C74 114.9(7) . . ?
F76 C77 C74 108.6(6) . . ?
F75 C77 C74 115.1(7) . . ?
C82 O81 La2 135.0(5) . . ?
O81 C82 C83 127.3(7) . . ?
O81 C82 C86 114.6(6) . . ?
C83 C82 C86 118.1(6) . . ?
C82 C83 C84 122.9(7) . . ?
C82 C83 H83A 118.6 . . ?
C84 C83 H83A 118.6 . . ?
O85 C84 C83 126.4(7) . . ?
O85 C84 C87 114.6(7) . . ?
C83 C84 C87 119.0(7) . . ?
C84 O85 La2 135.5(5) . . ?
F81B C86 F82B 105(2) . . ?
F82A C86 F83A 105.0(13) . . ?
F82A C86 F81A 111.3(14) . . ?
F83A C86 F81A 105.2(14) . . ?
F81B C86 F83B 108(2) . . ?
F82B C86 F83B 101(3) . . ?
F81B C86 C82 115.2(14) . . ?
F82A C86 C82 115.1(9) . . ?
F82B C86 C82 120.1(16) . . ?
F83A C86 C82 107.6(9) . . ?
F81A C86 C82 111.9(10) . . ?
F83B C86 C82 105.4(16) . . ?
F86 C87 F85 108.5(8) . . ?
F86 C87 F84 105.8(9) . . ?
F85 C87 F84 104.1(8) . . ?
F86 C87 C84 112.3(7) . . ?
F85 C87 C84 114.7(8) . . ?
F84 C87 C84 110.7(7) . . ?
C92 O91 La2 133.6(5) . . ?
O91 C92 C93 126.9(7) . . ?
O91 C92 C96 114.9(7) . . ?
C93 C92 C96 118.2(7) . . ?
C94 C93 C92 123.6(7) . . ?
C94 C93 H93A 118.2 . . ?
C92 C93 H93A 118.2 . . ?
O95 C94 C93 125.8(7) . . ?
O95 C94 C97 116.1(7) . . ?
C93 C94 C97 118.1(7) . . ?
C94 O95 La2 134.0(5) . . ?
F93B C96 F91B 105(2) . . ?
F91A C96 F93A 107(2) . . ?
F93B C96 F92B 106(3) . . ?
F91B C96 F92B 101(2) . . ?
F91A C96 F92A 109.4(19) . . ?
F93A C96 F92A 99.9(14) . . ?
F93B C96 C92 111.8(16) . . ?
F91B C96 C92 117.4(17) . . ?
F91A C96 C92 115.1(15) . . ?
F93A C96 C92 110.7(15) . . ?
F92B C96 C92 114.1(19) . . ?
F92A C96 C92 113.4(11) . . ?
F96 C97 F95 107.6(7) . . ?
F96 C97 F94 103.9(7) . . ?
F95 C97 F94 105.8(8) . . ?
F96 C97 C94 116.0(8) . . ?
F95 C97 C94 112.1(6) . . ?
F94 C97 C94 110.7(6) . . ?

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
C6 N1 C2 C3 0.0(10) . . . . ?
La1 N1 C2 C3 168.8(5) . . . . ?
N1 C2 C3 C4 -0.6(11) . . . . ?
C2 C3 C4 C5 1.1(12) . . . . ?
C3 C4 C5 C6 -1.1(12) . . . . ?
C2 N1 C6 C5 0.1(10) . . . . ?
La1 N1 C6 C5 -168.5(5) . . . . ?
C2 N1 C6 C7 -177.8(6) . . . . ?
La1 N1 C6 C7 13.7(8) . . . . ?
C4 C5 C6 N1 0.4(11) . . . . ?
C4 C5 C6 C7 178.2(7) . . . . ?
N1 C6 C7 N12 3.2(9) . . . . ?
C5 C6 C7 N12 -174.6(7) . . . . ?
N1 C6 C7 C8 -176.4(7) . . . . ?
C5 C6 C7 C8 5.8(11) . . . . ?
N12 C7 C8 C9 1.7(12) . . . . ?
C6 C7 C8 C9 -178.8(7) . . . . ?
C7 C8 C9 C10 0.0(13) . . . . ?
C8 C9 C10 C11 -1.4(13) . . . . ?
C9 C10 C11 N12 1.2(13) . . . . ?
C10 C11 N12 C7 0.5(11) . . . . ?
C10 C11 N12 La1 -162.7(6) . . . . ?
C8 C7 N12 C11 -1.9(10) . . . . ?
C6 C7 N12 C11 178.6(6) . . . . ?
C8 C7 N12 La1 161.2(5) . . . . ?
C6 C7 N12 La1 -18.3(8) . . . . ?
La1 O21 C22 C23 20.8(11) . . . . ?
La1 O21 C22 C26 -158.5(5) . . . . ?
O21 C22 C23 C24 -1.4(12) . . . . ?
C26 C22 C23 C24 177.8(7) . . . . ?
C22 C23 C24 O25 -4.1(12) . . . . ?
C22 C23 C24 C27 177.3(7) . . . . ?
C23 C24 O25 La1 -9.5(11) . . . . ?
C27 C24 O25 La1 169.1(5) . . . . ?
O21 C22 C26 F23 60.6(10) . . . . ?
C23 C22 C26 F23 -118.7(9) . . . . ?
O21 C22 C26 F21 -61.0(9) . . . . ?
C23 C22 C26 F21 119.7(9) . . . . ?
O21 C22 C26 F22 -179.7(7) . . . . ?
C23 C22 C26 F22 1.0(11) . . . . ?
O25 C24 C27 F26 59.7(10) . . . . ?
C23 C24 C27 F26 -121.6(8) . . . . ?
O25 C24 C27 F25 -178.4(7) . . . . ?
C23 C24 C27 F25 0.4(11) . . . . ?
O25 C24 C27 F24 -58.9(9) . . . . ?
C23 C24 C27 F24 119.9(8) . . . . ?
La1 O31 C32 C33 24.2(11) . . . . ?
La1 O31 C32 C36 -152.4(5) . . . . ?
O31 C32 C33 C34 -3.0(12) . . . . ?
C36 C32 C33 C34 173.5(7) . . . . ?
C32 C33 C34 O35 2.1(12) . . . . ?
C32 C33 C34 C37 -176.1(7) . . . . ?
C33 C34 O35 La1 -22.0(11) . . . . ?
C37 C34 O35 La1 156.2(5) . . . . ?
O31 C32 C36 F32B 163(2) . . . . ?
C33 C32 C36 F32B -14(2) . . . . ?
O31 C32 C36 F32A -50.8(17) . . . . ?
C33 C32 C36 F32A 132.3(16) . . . . ?
O31 C32 C36 F31B -70(2) . . . . ?
C33 C32 C36 F31B 113(2) . . . . ?
O31 C32 C36 F31A 80.0(13) . . . . ?
C33 C32 C36 F31A -96.9(13) . . . . ?
O31 C32 C36 F33A -169.5(13) . . . . ?
C33 C32 C36 F33A 13.5(14) . . . . ?
O31 C32 C36 F33B 32.6(15) . . . . ?
C33 C32 C36 F33B -144.4(14) . . . . ?
O35 C34 C37 F36A -115.9(10) . . . . ?
C33 C34 C37 F36A 62.5(11) . . . . ?
O35 C34 C37 F36B 81(3) . . . . ?
C33 C34 C37 F36B -100(3) . . . . ?
O35 C34 C37 F35B -60(3) . . . . ?
C33 C34 C37 F35B 118(3) . . . . ?
O35 C34 C37 F35A 122.0(9) . . . . ?
C33 C34 C37 F35A -59.6(11) . . . . ?
O35 C34 C37 F34B -169(2) . . . . ?
C33 C34 C37 F34B 10(2) . . . . ?
O35 C34 C37 F34A 4.2(11) . . . . ?
C33 C34 C37 F34A -177.4(8) . . . . ?
La1 O41 C42 C43 -15.2(12) . . . . ?
La1 O41 C42 C46 166.5(5) . . . . ?
O41 C42 C43 C44 -3.4(12) . . . . ?
C46 C42 C43 C44 175.0(7) . . . . ?
C42 C43 C44 O45 -2.1(12) . . . . ?
C42 C43 C44 C47 -178.7(7) . . . . ?
C43 C44 O45 La1 25.9(11) . . . . ?
C47 C44 O45 La1 -157.4(5) . . . . ?
O41 C42 C46 F42A -58(2) . . . . ?
C43 C42 C46 F42A 123(2) . . . . ?
O41 C42 C46 F42B 110(3) . . . . ?
C43 C42 C46 F42B -69(3) . . . . ?
O41 C42 C46 F43A 67.0(16) . . . . ?
C43 C42 C46 F43A -111.6(15) . . . . ?
O41 C42 C46 F43B -116(3) . . . . ?
C43 C42 C46 F43B 65(3) . . . . ?
O41 C42 C46 F41A -179.0(13) . . . . ?
C43 C42 C46 F41A 2.4(15) . . . . ?
O41 C42 C46 F41B -6.2(18) . . . . ?
C43 C42 C46 F41B 175.3(16) . . . . ?
O45 C44 C47 F45 51.2(10) . . . . ?
C43 C44 C47 F45 -131.7(8) . . . . ?
O45 C44 C47 F44 -71.6(9) . . . . ?
C43 C44 C47 F44 105.4(9) . . . . ?
O45 C44 C47 F46 169.9(6) . . . . ?
C43 C44 C47 F46 -13.0(10) . . . . ?
C56 N51 C52 C53 0.7(11) . . . . ?
La2 N51 C52 C53 164.3(6) . . . . ?
N51 C52 C53 C54 -1.0(12) . . . . ?
C52 C53 C54 C55 0.7(12) . . . . ?
C53 C54 C55 C56 -0.3(12) . . . . ?
C52 N51 C56 C55 -0.2(10) . . . . ?
La2 N51 C56 C55 -163.4(5) . . . . ?
C52 N51 C56 C57 -179.7(6) . . . . ?
La2 N51 C56 C57 17.2(8) . . . . ?
C54 C55 C56 N51 0.0(11) . . . . ?
C54 C55 C56 C57 179.5(7) . . . . ?
N51 C56 C57 N62 -1.5(9) . . . . ?
C55 C56 C57 N62 179.1(6) . . . . ?
N51 C56 C57 C58 177.6(7) . . . . ?
C55 C56 C57 C58 -1.8(11) . . . . ?
N62 C57 C58 C59 -0.1(11) . . . . ?
C56 C57 C58 C59 -179.2(7) . . . . ?
C57 C58 C59 C60 0.5(12) . . . . ?
C58 C59 C60 C61 0.0(11) . . . . ?
C59 C60 C61 N62 -0.9(11) . . . . ?
C60 C61 N62 C57 1.3(10) . . . . ?
C60 C61 N62 La2 -165.8(5) . . . . ?
C58 C57 N62 C61 -0.7(9) . . . . ?
C56 C57 N62 C61 178.4(6) . . . . ?
C58 C57 N62 La2 166.1(5) . . . . ?
C56 C57 N62 La2 -14.8(7) . . . . ?
La2 O71 C72 C73 17.0(13) . . . . ?
La2 O71 C72 C76 -158.8(5) . . . . ?
O71 C72 C73 C74 0.2(13) . . . . ?
C76 C72 C73 C74 176.1(7) . . . . ?
C72 C73 C74 O75 2.7(13) . . . . ?
C72 C73 C74 C77 -175.2(7) . . . . ?
C73 C74 O75 La2 -23.0(11) . . . . ?
C77 C74 O75 La2 155.0(5) . . . . ?
O71 C72 C76 F72 124.6(9) . . . . ?
C73 C72 C76 F72 -51.8(10) . . . . ?
O71 C72 C76 F73 -115.3(8) . . . . ?
C73 C72 C76 F73 68.2(10) . . . . ?
O71 C72 C76 F71 1.7(11) . . . . ?
C73 C72 C76 F71 -174.7(8) . . . . ?
O75 C74 C77 F74 49.5(10) . . . . ?
C73 C74 C77 F74 -132.3(8) . . . . ?
O75 C74 C77 F76 -74.9(10) . . . . ?
C73 C74 C77 F76 103.3(10) . . . . ?
O75 C74 C77 F75 172.3(7) . . . . ?
C73 C74 C77 F75 -9.5(11) . . . . ?
La2 O81 C82 C83 11.0(11) . . . . ?
La2 O81 C82 C86 -168.7(4) . . . . ?
O81 C82 C83 C84 4.1(12) . . . . ?
C86 C82 C83 C84 -176.2(7) . . . . ?
C82 C83 C84 O85 -0.3(12) . . . . ?
C82 C83 C84 C87 -179.3(7) . . . . ?
C83 C84 O85 La2 -19.0(12) . . . . ?
C87 C84 O85 La2 160.1(5) . . . . ?
O81 C82 C86 F81B 24(2) . . . . ?
C83 C82 C86 F81B -156(2) . . . . ?
O81 C82 C86 F82A -50.1(17) . . . . ?
C83 C82 C86 F82A 130.2(15) . . . . ?
O81 C82 C86 F82B 151(3) . . . . ?
C83 C82 C86 F82B -28(3) . . . . ?
O81 C82 C86 F83A 66.6(12) . . . . ?
C83 C82 C86 F83A -113.1(12) . . . . ?
O81 C82 C86 F81A -178.3(13) . . . . ?
C83 C82 C86 F81A 1.9(15) . . . . ?
O81 C82 C86 F83B -95(2) . . . . ?
C83 C82 C86 F83B 85(2) . . . . ?
O85 C84 C87 F86 64.9(10) . . . . ?
C83 C84 C87 F86 -116.0(9) . . . . ?
O85 C84 C87 F85 -170.6(8) . . . . ?
C83 C84 C87 F85 8.6(12) . . . . ?
O85 C84 C87 F84 -53.1(10) . . . . ?
C83 C84 C87 F84 126.0(9) . . . . ?
La2 O91 C92 C93 18.3(12) . . . . ?
La2 O91 C92 C96 -162.3(5) . . . . ?
O91 C92 C93 C94 1.7(13) . . . . ?
C96 C92 C93 C94 -177.7(7) . . . . ?
C92 C93 C94 O95 1.3(13) . . . . ?
C92 C93 C94 C97 178.8(7) . . . . ?
C93 C94 O95 La2 -24.3(11) . . . . ?
C97 C94 O95 La2 158.1(5) . . . . ?
O91 C92 C96 F93B -131(2) . . . . ?
C93 C92 C96 F93B 48(3) . . . . ?
O91 C92 C96 F91B 107(2) . . . . ?
C93 C92 C96 F91B -73(2) . . . . ?
O91 C92 C96 F91A -45(2) . . . . ?
C93 C92 C96 F91A 135(2) . . . . ?
O91 C92 C96 F93A 76.7(16) . . . . ?
C93 C92 C96 F93A -103.8(16) . . . . ?
O91 C92 C96 F92B -10(2) . . . . ?
C93 C92 C96 F92B 169(2) . . . . ?
O91 C92 C96 F92A -171.9(14) . . . . ?
C93 C92 C96 F92A 7.5(16) . . . . ?
O95 C94 C97 F96 -167.0(7) . . . . ?
C93 C94 C97 F96 15.3(11) . . . . ?
O95 C94 C97 F95 68.9(9) . . . . ?
C93 C94 C97 F95 -108.8(9) . . . . ?
O95 C94 C97 F94 -48.9(9) . . . . ?
C93 C94 C97 F94 133.3(8) . . . . ?

_refine_diff_density_max         3.178
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.138


# start Validation Reply Form
_vrf_PLAT213_k11234              
;
PROBLEM: Atom F36B            has ADP max/min Ratio .....        5.6 prolat
RESPONSE: there are 5 disordered -CF3 groups which are modelled anisotropically as two PARTs.  F36b is at 0.29 occupancy and 
thus on the edge of what can be modelled successfully.
;
_vrf_PLAT094_k11234              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.09 Report
RESPONSE: This is typical of these complexes which show extensive disorder. 
;
_vrf_PLAT910_k11234              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: Presumably due to issues at the data collection stage
;
_vrf_PLAT971_k11234              
;
PROBLEM: Check Calcd Resid. Dens.  0.99A   From La1             3.21 eA-3  
RESPONSE: This is typical of these complexes which show extensive disorder.
;
# end Validation Reply Form

_chemical_properties_physical    Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_k11165
_database_code_depnum_ccdc_archive 'CCDC 1856922'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H11 Ce F18 N2 O6'
_chemical_formula_sum            'C25 H11 Ce F18 N2 O6'
_chemical_formula_weight         917.48

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'
O O 0.0106 0.0060 '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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.993(2)
_cell_length_b                   15.829(3)
_cell_length_c                   17.833(4)
_cell_angle_alpha                78.46(3)
_cell_angle_beta                 76.46(3)
_cell_angle_gamma                72.69(3)
_cell_volume                     3111.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11650
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_F_000             1772
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.614
_shelx_estimated_absorpt_T_min   0.760
_shelx_estimated_absorpt_T_max   0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            27817
_diffrn_reflns_av_unetI/netI     0.1194
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.565
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10936
_reflns_number_gt                6153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_structure_solution    'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1044P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difsum
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10936
_refine_ls_number_parameters     1042
_refine_ls_number_restraints     450
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.2038
_refine_ls_wR_factor_gt          0.1582
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.97327(5) 0.23732(3) 0.53406(3) 0.0322(2) Uani 1 1 d . U . . .
N1 N 1.0185(7) 0.3691(5) 0.5800(5) 0.0344(17) Uani 1 1 d . U . . .
C2 C 0.9671(9) 0.3899(6) 0.6516(6) 0.036(2) Uani 1 1 d . U . . .
H2A H 0.905901 0.363226 0.680324 0.043 Uiso 1 1 calc R U . . .
C3 C 0.9986(9) 0.4479(6) 0.6857(6) 0.040(2) Uani 1 1 d . U . . .
H3A H 0.959498 0.461401 0.736379 0.048 Uiso 1 1 calc R U . . .
C4 C 1.0879(11) 0.4859(6) 0.6446(6) 0.047(3) Uani 1 1 d . U . . .
H4A H 1.111811 0.525816 0.667030 0.056 Uiso 1 1 calc R U . . .
C5 C 1.1435(10) 0.4659(7) 0.5701(6) 0.047(3) Uani 1 1 d . U . . .
H5A H 1.205142 0.491888 0.540852 0.057 Uiso 1 1 calc R U . . .
C6 C 1.1063(9) 0.4071(6) 0.5398(6) 0.034(2) Uani 1 1 d . U . . .
C7 C 1.1574(8) 0.3837(6) 0.4594(6) 0.034(2) Uani 1 1 d . U . . .
C8 C 1.2512(10) 0.4156(7) 0.4122(6) 0.047(3) Uani 1 1 d . U . . .
H8A H 1.285588 0.452446 0.430586 0.056 Uiso 1 1 calc R U . . .
C9 C 1.2924(11) 0.3922(7) 0.3385(7) 0.056(3) Uani 1 1 d . U . . .
H9A H 1.358931 0.410485 0.306653 0.067 Uiso 1 1 calc R U . . .
C10 C 1.2393(10) 0.3435(7) 0.3108(6) 0.049(3) Uani 1 1 d . U . . .
H10A H 1.264948 0.329143 0.259196 0.058 Uiso 1 1 calc R U . . .
C11 C 1.1455(11) 0.3154(6) 0.3613(6) 0.049(3) Uani 1 1 d . U . . .
H11A H 1.107813 0.281257 0.342235 0.059 Uiso 1 1 calc R U . . .
N12 N 1.1049(8) 0.3326(5) 0.4335(5) 0.0388(18) Uani 1 1 d . U . . .
O21 O 1.1777(6) 0.1786(4) 0.5539(4) 0.0394(15) Uani 1 1 d . U . . .
C22 C 1.2281(9) 0.1628(6) 0.6119(6) 0.038(2) Uani 1 1 d . U . . .
C23 C 1.1764(9) 0.1511(6) 0.6903(6) 0.042(2) Uani 1 1 d . U . . .
H23A H 1.224711 0.139295 0.728418 0.051 Uiso 1 1 calc R U . . .
C24 C 1.0560(9) 0.1560(6) 0.7144(6) 0.036(2) Uani 1 1 d . U . . .
O25 O 0.9780(6) 0.1782(4) 0.6718(4) 0.0366(15) Uani 1 1 d . U . . .
C26 C 1.3573(10) 0.1587(7) 0.5898(7) 0.049(2) Uani 1 1 d . U . . .
C27 C 1.0082(11) 0.1359(7) 0.8010(6) 0.046(2) Uani 1 1 d . U . . .
F21 F 1.4182(6) 0.0975(5) 0.5463(6) 0.098(3) Uani 1 1 d . U . . .
F22 F 1.4131(7) 0.1424(6) 0.6503(5) 0.099(3) Uani 1 1 d . U . . .
F23 F 1.3771(7) 0.2343(5) 0.5508(5) 0.100(3) Uani 1 1 d . U . . .
F24 F 0.9267(8) 0.2059(5) 0.8263(4) 0.092(3) Uani 1 1 d . U . . .
F25 F 1.0901(7) 0.1172(6) 0.8454(4) 0.090(3) Uani 1 1 d . U . . .
F26 F 0.9600(9) 0.0706(5) 0.8170(4) 0.101(3) Uani 1 1 d . U . . .
O31 O 0.8523(6) 0.1341(4) 0.5444(4) 0.0359(15) Uani 1 1 d . U . . .
C32 C 0.8327(9) 0.0960(6) 0.4949(6) 0.035(2) Uani 1 1 d . U . . .
C33 C 0.9015(10) 0.0775(6) 0.4241(6) 0.040(2) Uani 1 1 d . U . . .
H33A H 0.877339 0.045339 0.393958 0.048 Uiso 1 1 calc R U . . .
C34 C 1.0042(10) 0.1042(6) 0.3954(6) 0.040(2) Uani 1 1 d . U . . .
O35 O 1.0518(6) 0.1463(4) 0.4279(4) 0.0383(15) Uani 1 1 d . U . . .
C36 C 0.7147(10) 0.0723(6) 0.5190(6) 0.051(2) Uani 1 1 d D U . . .
C37 C 1.0671(13) 0.0860(7) 0.3145(6) 0.058(3) Uani 1 1 d . U . . .
F31A F 0.629(2) 0.1351(15) 0.5534(18) 0.121(10) Uani 0.53 1 d D U P A 1
F32A F 0.7233(17) 0.0104(14) 0.5813(11) 0.065(6) Uani 0.53 1 d D U P A 1
F33A F 0.672(3) 0.049(2) 0.4677(15) 0.111(12) Uani 0.53 1 d D U P A 1
F31B F 0.714(3) 0.0167(18) 0.4727(16) 0.079(9) Uani 0.47 1 d D U P A 2
F32B F 0.632(2) 0.1454(14) 0.500(2) 0.133(14) Uani 0.47 1 d D U P A 2
F33B F 0.678(2) 0.033(3) 0.5876(13) 0.125(14) Uani 0.47 1 d D U P A 2
F34 F 1.1663(9) 0.1131(7) 0.2903(5) 0.128(4) Uani 1 1 d . U . . .
F35 F 1.1035(9) 0.0019(5) 0.3069(5) 0.108(3) Uani 1 1 d . U . . .
F36 F 1.0065(9) 0.1252(7) 0.2627(5) 0.146(4) Uani 1 1 d . U . . .
O41 O 0.7744(6) 0.3218(4) 0.5946(4) 0.0437(16) Uani 1 1 d . U . . .
C42 C 0.6744(10) 0.3460(6) 0.5762(6) 0.040(2) Uani 1 1 d . U . . .
C43 C 0.6504(11) 0.3501(7) 0.5017(7) 0.050(3) Uani 1 1 d . U . . .
H43A H 0.570056 0.367034 0.495000 0.060 Uiso 1 1 calc R U . . .
C44 C 0.7382(10) 0.3305(6) 0.4394(6) 0.041(2) Uani 1 1 d . U . . .
O45 O 0.8490(6) 0.3088(4) 0.4351(4) 0.0364(15) Uani 1 1 d . U . . .
C46 C 0.5705(10) 0.3778(6) 0.6402(7) 0.052(3) Uani 1 1 d D U . . .
C47 C 0.7038(11) 0.3388(6) 0.3606(7) 0.048(3) Uani 1 1 d . U . . .
F41A F 0.4655(9) 0.3846(14) 0.6242(10) 0.127(6) Uani 0.69 1 d D U P B 1
F42A F 0.5788(15) 0.3286(12) 0.7066(8) 0.141(7) Uani 0.69 1 d D U P B 1
F43A F 0.5647(11) 0.4568(7) 0.6508(8) 0.095(4) Uani 0.69 1 d D U P B 1
F41B F 0.607(3) 0.385(2) 0.7008(14) 0.088(9) Uiso 0.31 1 d D . P B 2
F42B F 0.486(2) 0.4401(18) 0.617(2) 0.102(10) Uiso 0.31 1 d D . P B 2
F43B F 0.524(3) 0.3123(15) 0.6702(15) 0.070(7) Uiso 0.31 1 d D . P B 2
F44 F 0.7259(7) 0.4108(5) 0.3139(4) 0.080(2) Uani 1 1 d . U . . .
F45 F 0.7592(8) 0.2701(4) 0.3247(5) 0.099(3) Uani 1 1 d . U . . .
F46 F 0.5880(7) 0.3486(5) 0.3648(5) 0.089(2) Uani 1 1 d . U . . .
Ce2 Ce 0.52368(5) 0.73856(3) 0.98104(3) 0.0315(2) Uani 1 1 d . U . . .
N51 N 0.4466(7) 0.8393(5) 1.0928(4) 0.0327(16) Uani 1 1 d . U . . .
C52 C 0.3587(10) 0.8239(7) 1.1503(6) 0.046(2) Uani 1 1 d . U . . .
H52A H 0.314724 0.785910 1.143445 0.055 Uiso 1 1 calc R U . . .
C53 C 0.3267(10) 0.8600(6) 1.2200(6) 0.043(2) Uani 1 1 d . U . . .
H53A H 0.261014 0.849685 1.258821 0.052 Uiso 1 1 calc R U . . .
C54 C 0.3941(10) 0.9103(7) 1.2292(6) 0.047(3) Uani 1 1 d . U . . .
H54A H 0.378948 0.933221 1.276921 0.056 Uiso 1 1 calc R U . . .
C55 C 0.4848(10) 0.9291(6) 1.1705(6) 0.042(2) Uani 1 1 d . U . . .
H55A H 0.529501 0.966649 1.177146 0.050 Uiso 1 1 calc R U . . .
C56 C 0.5105(9) 0.8933(5) 1.1023(5) 0.0295(19) Uani 1 1 d . U . . .
C57 C 0.6077(9) 0.9080(5) 1.0371(6) 0.031(2) Uani 1 1 d . U . . .
C58 C 0.6764(9) 0.9645(6) 1.0360(6) 0.043(3) Uani 1 1 d . U . . .
H58A H 0.661778 0.996204 1.078788 0.052 Uiso 1 1 calc R U . . .
C59 C 0.7662(10) 0.9753(7) 0.9736(7) 0.048(3) Uani 1 1 d . U . . .
H59A H 0.817860 1.010104 0.974842 0.057 Uiso 1 1 calc R U . . .
C60 C 0.7792(10) 0.9361(6) 0.9116(6) 0.043(2) Uani 1 1 d . U . . .
H60A H 0.838339 0.944529 0.867022 0.052 Uiso 1 1 calc R U . . .
C61 C 0.7060(9) 0.8831(5) 0.9128(5) 0.031(2) Uani 1 1 d . U . . .
H61A H 0.715077 0.856356 0.867756 0.037 Uiso 1 1 calc R U . . .
N62 N 0.6237(7) 0.8677(5) 0.9736(4) 0.0291(16) Uani 1 1 d . U . . .
O71 O 0.4084(6) 0.6451(4) 1.0721(4) 0.0387(16) Uani 1 1 d . U . . .
C72 C 0.3441(10) 0.5993(6) 1.0641(6) 0.041(2) Uani 1 1 d . U . . .
C73 C 0.3366(10) 0.5725(6) 0.9957(6) 0.048(3) Uani 1 1 d . U . . .
H73A H 0.284282 0.536810 0.998464 0.057 Uiso 1 1 calc R U . . .
C74 C 0.4027(9) 0.5962(6) 0.9247(6) 0.036(2) Uani 1 1 d . U . . .
O75 O 0.4823(6) 0.6367(4) 0.9114(4) 0.0356(15) Uani 1 1 d . U . . .
C76 C 0.2570(11) 0.5744(7) 1.1378(7) 0.050(3) Uani 1 1 d . U . . .
C77 C 0.3796(8) 0.5713(5) 0.8534(6) 0.045(2) Uani 1 1 d D U . . .
F71 F 0.2651(8) 0.6068(6) 1.1986(5) 0.104(3) Uani 1 1 d . U . . .
F72 F 0.1464(7) 0.6042(6) 1.1277(5) 0.116(3) Uani 1 1 d . U . . .
F73 F 0.2772(7) 0.4883(4) 1.1578(4) 0.082(2) Uani 1 1 d . U . . .
F74A F 0.4704(19) 0.536(2) 0.8045(17) 0.099(9) Uani 0.48 1 d D U P C 1
F75A F 0.296(2) 0.531(2) 0.8617(18) 0.093(10) Uani 0.48 1 d D U P C 1
F76A F 0.359(4) 0.6428(17) 0.801(2) 0.181(18) Uani 0.48 1 d D U P C 1
F74B F 0.303(2) 0.6366(13) 0.8209(14) 0.089(7) Uani 0.51 1 d D U P C 2
F75B F 0.475(2) 0.5233(18) 0.8151(19) 0.093(9) Uani 0.51 1 d D U P C 2
F76B F 0.321(3) 0.5099(18) 0.874(2) 0.101(10) Uani 0.51 1 d D U P C 2
O81 O 0.7316(6) 0.6749(4) 0.9218(4) 0.0369(15) Uani 1 1 d . U . . .
C82 C 0.8292(9) 0.6544(6) 0.9436(6) 0.038(2) Uani 1 1 d . U . . .
C83 C 0.8500(10) 0.6523(7) 1.0184(7) 0.049(3) Uani 1 1 d . U . . .
H83A H 0.929093 0.640605 1.026300 0.059 Uiso 1 1 calc R U . . .
C84 C 0.7574(10) 0.6668(6) 1.0799(6) 0.042(2) Uani 1 1 d . U . . .
O85 O 0.6476(6) 0.6835(4) 1.0808(4) 0.0389(15) Uani 1 1 d . U . . .
C86 C 0.9377(10) 0.6327(6) 0.8778(7) 0.056(3) Uani 1 1 d D U . . .
C87 C 0.7847(11) 0.6632(8) 1.1594(7) 0.057(3) Uani 1 1 d . U . . .
F81A F 1.038(2) 0.600(2) 0.901(3) 0.139(15) Uani 0.53 1 d D U P D 1
F82A F 0.934(3) 0.582(2) 0.8311(16) 0.119(11) Uani 0.53 1 d D U P D 1
F83A F 0.943(4) 0.7068(14) 0.8323(14) 0.114(11) Uani 0.53 1 d D U P D 1
F81B F 0.927(4) 0.679(2) 0.8107(14) 0.129(14) Uani 0.47 1 d D U P D 2
F82B F 1.035(2) 0.637(3) 0.894(3) 0.101(10) Uani 0.47 1 d D U P D 2
F83B F 0.951(4) 0.5491(13) 0.8736(17) 0.117(12) Uani 0.47 1 d D U P D 2
F84 F 0.7260(9) 0.7364(6) 1.1906(5) 0.113(3) Uani 1 1 d . U . . .
F85 F 0.8941(8) 0.6604(8) 1.1598(5) 0.125(3) Uani 1 1 d . U . . .
F86 F 0.7564(11) 0.6004(6) 1.2092(5) 0.140(4) Uani 1 1 d . U . . .
O91 O 0.5088(6) 0.8215(4) 0.8499(4) 0.0434(17) Uani 1 1 d . U . . .
C92 C 0.4250(10) 0.8460(6) 0.8102(6) 0.044(2) Uani 1 1 d . U . . .
C93 C 0.3047(11) 0.8487(7) 0.8377(7) 0.052(3) Uani 1 1 d . U . . .
H93A H 0.252967 0.864524 0.801192 0.062 Uiso 1 1 calc R U . . .
C94 C 0.2580(10) 0.8292(6) 0.9165(6) 0.042(2) Uani 1 1 d . U . . .
O95 O 0.3127(6) 0.8076(4) 0.9710(4) 0.0366(15) Uani 1 1 d . U . . .
C96 C 0.4661(9) 0.8727(6) 0.7243(7) 0.052(3) Uani 1 1 d D U . . .
C97 C 0.1255(10) 0.8400(7) 0.9375(8) 0.052(3) Uani 1 1 d . U . . .
F91A F 0.5509(15) 0.9125(12) 0.7096(6) 0.113(5) Uani 0.74 1 d D U P E 1
F92A F 0.3761(11) 0.9230(10) 0.6893(6) 0.115(4) Uani 0.74 1 d D U P E 1
F93A F 0.5067(14) 0.8047(7) 0.6866(6) 0.091(4) Uani 0.74 1 d D U P E 1
F91B F 0.429(4) 0.842(3) 0.6759(19) 0.090(12) Uiso 0.26 1 d D . P E 2
F92B F 0.5804(17) 0.859(3) 0.698(2) 0.100(14) Uiso 0.26 1 d D . P E 2
F93B F 0.436(4) 0.9589(11) 0.710(2) 0.084(10) Uiso 0.26 1 d D . P E 2
F94 F 0.1035(7) 0.7663(5) 0.9858(6) 0.103(3) Uani 1 1 d . U . . .
F95 F 0.0684(6) 0.9075(5) 0.9751(5) 0.090(3) Uani 1 1 d . U . . .
F96 F 0.0710(7) 0.8442(6) 0.8814(5) 0.101(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O21 2.433(6) . ?
Ce1 O31 2.444(6) . ?
Ce1 O35 2.449(6) . ?
Ce1 O25 2.455(6) . ?
Ce1 O45 2.458(6) . ?
Ce1 O41 2.473(7) . ?
Ce1 N1 2.624(7) . ?
Ce1 N12 2.644(8) . ?
N1 C2 1.342(12) . ?
N1 C6 1.354(12) . ?
C2 C3 1.375(12) . ?
C2 H2A 0.9500 . ?
C3 C4 1.373(14) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(15) . ?
C4 H4A 0.9500 . ?
C5 C6 1.384(13) . ?
C5 H5A 0.9500 . ?
C6 C7 1.496(14) . ?
C7 N12 1.361(11) . ?
C7 C8 1.397(13) . ?
C8 C9 1.374(15) . ?
C8 H8A 0.9500 . ?
C9 C10 1.356(15) . ?
C9 H9A 0.9500 . ?
C10 C11 1.392(15) . ?
C10 H10A 0.9500 . ?
C11 N12 1.319(12) . ?
C11 H11A 0.9500 . ?
O21 C22 1.263(11) . ?
C22 C23 1.390(14) . ?
C22 C26 1.492(14) . ?
C23 C24 1.390(14) . ?
C23 H23A 0.9500 . ?
C24 O25 1.267(11) . ?
C24 C27 1.521(14) . ?
C26 F21 1.298(13) . ?
C26 F23 1.315(12) . ?
C26 F22 1.343(13) . ?
C27 F26 1.282(11) . ?
C27 F24 1.319(13) . ?
C27 F25 1.333(12) . ?
O31 C32 1.262(10) . ?
C32 C33 1.370(14) . ?
C32 C36 1.515(14) . ?
C33 C34 1.374(14) . ?
C33 H33A 0.9500 . ?
C34 O35 1.281(11) . ?
C34 C37 1.503(15) . ?
C36 F33B 1.295(15) . ?
C36 F33A 1.302(14) . ?
C36 F31B 1.322(14) . ?
C36 F32B 1.325(14) . ?
C36 F32A 1.328(13) . ?
C36 F31A 1.328(14) . ?
C37 F36 1.259(14) . ?
C37 F35 1.295(12) . ?
C37 F34 1.333(14) . ?
O41 C42 1.246(11) . ?
C42 C43 1.408(14) . ?
C42 C46 1.517(16) . ?
C43 C44 1.355(15) . ?
C43 H43A 0.9500 . ?
C44 O45 1.257(12) . ?
C44 C47 1.526(14) . ?
C46 F42B 1.271(16) . ?
C46 F43A 1.280(11) . ?
C46 F43B 1.286(15) . ?
C46 F42A 1.287(12) . ?
C46 F41B 1.293(15) . ?
C46 F41A 1.325(11) . ?
C47 F45 1.298(13) . ?
C47 F44 1.326(11) . ?
C47 F46 1.338(13) . ?
Ce2 O71 2.437(6) . ?
Ce2 O75 2.441(6) . ?
Ce2 O85 2.445(6) . ?
Ce2 O81 2.459(7) . ?
Ce2 O91 2.459(6) . ?
Ce2 O95 2.473(6) . ?
Ce2 N51 2.626(8) . ?
Ce2 N62 2.630(7) . ?
N51 C52 1.330(12) . ?
N51 C56 1.363(11) . ?
C52 C53 1.397(14) . ?
C52 H52A 0.9500 . ?
C53 C54 1.345(14) . ?
C53 H53A 0.9500 . ?
C54 C55 1.380(15) . ?
C54 H54A 0.9500 . ?
C55 C56 1.375(13) . ?
C55 H55A 0.9500 . ?
C56 C57 1.478(13) . ?
C57 N62 1.356(11) . ?
C57 C58 1.380(12) . ?
C58 C59 1.379(15) . ?
C58 H58A 0.9500 . ?
C59 C60 1.329(14) . ?
C59 H59A 0.9500 . ?
C60 C61 1.378(12) . ?
C60 H60A 0.9500 . ?
C61 N62 1.321(12) . ?
C61 H61A 0.9500 . ?
O71 C72 1.252(11) . ?
C72 C73 1.397(14) . ?
C72 C76 1.540(15) . ?
C73 C74 1.374(14) . ?
C73 H73A 0.9500 . ?
C74 O75 1.255(11) . ?
C74 C77 1.511(14) . ?
C76 F73 1.301(11) . ?
C76 F72 1.311(13) . ?
C76 F71 1.323(13) . ?
C77 F74A 1.282(14) . ?
C77 F75B 1.296(14) . ?
C77 F74B 1.299(14) . ?
C77 F75A 1.304(14) . ?
C77 F76B 1.311(13) . ?
C77 F76A 1.315(14) . ?
O81 C82 1.250(11) . ?
C82 C83 1.406(14) . ?
C82 C86 1.539(15) . ?
C83 C84 1.366(15) . ?
C83 H83A 0.9500 . ?
C84 O85 1.260(12) . ?
C84 C87 1.516(15) . ?
C86 F82A 1.281(14) . ?
C86 F81B 1.284(16) . ?
C86 F81A 1.285(15) . ?
C86 F82B 1.293(15) . ?
C86 F83A 1.295(14) . ?
C86 F83B 1.299(15) . ?
C87 F86 1.264(13) . ?
C87 F85 1.301(14) . ?
C87 F84 1.317(14) . ?
O91 C92 1.286(12) . ?
C92 C93 1.401(15) . ?
C92 C96 1.511(15) . ?
C93 C94 1.395(15) . ?
C93 H93A 0.9500 . ?
C94 O95 1.235(11) . ?
C94 C97 1.509(15) . ?
C96 F91B 1.288(16) . ?
C96 F93B 1.291(15) . ?
C96 F93A 1.293(11) . ?
C96 F91A 1.299(11) . ?
C96 F92B 1.308(16) . ?
C96 F92A 1.340(11) . ?
C97 F96 1.298(12) . ?
C97 F95 1.303(13) . ?
C97 F94 1.359(13) . ?

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
O21 Ce1 O31 119.5(2) . . ?
O21 Ce1 O35 81.2(2) . . ?
O31 Ce1 O35 70.0(2) . . ?
O21 Ce1 O25 69.7(2) . . ?
O31 Ce1 O25 84.19(19) . . ?
O35 Ce1 O25 124.1(2) . . ?
O21 Ce1 O45 143.7(2) . . ?
O31 Ce1 O45 76.7(2) . . ?
O35 Ce1 O45 74.4(2) . . ?
O25 Ce1 O45 146.6(2) . . ?
O21 Ce1 O41 142.3(2) . . ?
O31 Ce1 O41 77.7(2) . . ?
O35 Ce1 O41 135.8(2) . . ?
O25 Ce1 O41 80.1(2) . . ?
O45 Ce1 O41 69.3(2) . . ?
O21 Ce1 N1 75.8(2) . . ?
O31 Ce1 N1 151.9(2) . . ?
O35 Ce1 N1 138.1(2) . . ?
O25 Ce1 N1 79.5(2) . . ?
O45 Ce1 N1 105.3(2) . . ?
O41 Ce1 N1 77.0(2) . . ?
O21 Ce1 N12 71.5(2) . . ?
O31 Ce1 N12 143.4(2) . . ?
O35 Ce1 N12 78.4(2) . . ?
O25 Ce1 N12 130.1(2) . . ?
O45 Ce1 N12 77.4(2) . . ?
O41 Ce1 N12 116.1(2) . . ?
N1 Ce1 N12 61.3(2) . . ?
C2 N1 C6 117.8(8) . . ?
C2 N1 Ce1 118.9(6) . . ?
C6 N1 Ce1 122.4(6) . . ?
N1 C2 C3 123.4(9) . . ?
N1 C2 H2A 118.3 . . ?
C3 C2 H2A 118.3 . . ?
C4 C3 C2 118.4(10) . . ?
C4 C3 H3A 120.8 . . ?
C2 C3 H3A 120.8 . . ?
C3 C4 C5 119.9(9) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C6 C5 C4 118.1(9) . . ?
C6 C5 H5A 120.9 . . ?
C4 C5 H5A 120.9 . . ?
N1 C6 C5 122.4(9) . . ?
N1 C6 C7 115.3(8) . . ?
C5 C6 C7 122.2(9) . . ?
N12 C7 C8 121.7(10) . . ?
N12 C7 C6 116.5(8) . . ?
C8 C7 C6 121.7(9) . . ?
C9 C8 C7 118.4(10) . . ?
C9 C8 H8A 120.8 . . ?
C7 C8 H8A 120.8 . . ?
C10 C9 C8 120.8(11) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C9 C10 C11 117.0(10) . . ?
C9 C10 H10A 121.5 . . ?
C11 C10 H10A 121.5 . . ?
N12 C11 C10 125.0(10) . . ?
N12 C11 H11A 117.5 . . ?
C10 C11 H11A 117.5 . . ?
C11 N12 C7 117.0(9) . . ?
C11 N12 Ce1 120.8(6) . . ?
C7 N12 Ce1 120.1(6) . . ?
C22 O21 Ce1 134.7(7) . . ?
O21 C22 C23 127.6(10) . . ?
O21 C22 C26 113.2(10) . . ?
C23 C22 C26 119.2(9) . . ?
C24 C23 C22 121.8(9) . . ?
C24 C23 H23A 119.1 . . ?
C22 C23 H23A 119.1 . . ?
O25 C24 C23 127.0(9) . . ?
O25 C24 C27 114.5(9) . . ?
C23 C24 C27 118.5(9) . . ?
C24 O25 Ce1 135.4(6) . . ?
F21 C26 F23 105.9(10) . . ?
F21 C26 F22 105.0(9) . . ?
F23 C26 F22 104.3(9) . . ?
F21 C26 C22 113.6(10) . . ?
F23 C26 C22 112.5(9) . . ?
F22 C26 C22 114.5(10) . . ?
F26 C27 F24 107.1(11) . . ?
F26 C27 F25 107.4(9) . . ?
F24 C27 F25 104.8(9) . . ?
F26 C27 C24 112.6(9) . . ?
F24 C27 C24 110.6(8) . . ?
F25 C27 C24 113.8(10) . . ?
C32 O31 Ce1 132.8(6) . . ?
O31 C32 C33 128.4(9) . . ?
O31 C32 C36 112.9(9) . . ?
C33 C32 C36 118.7(8) . . ?
C32 C33 C34 122.0(9) . . ?
C32 C33 H33A 119.0 . . ?
C34 C33 H33A 119.0 . . ?
O35 C34 C33 128.0(10) . . ?
O35 C34 C37 115.0(10) . . ?
C33 C34 C37 117.0(9) . . ?
C34 O35 Ce1 132.5(7) . . ?
F33B C36 F31B 103(3) . . ?
F33B C36 F32B 110(2) . . ?
F31B C36 F32B 104(2) . . ?
F33A C36 F32A 111(2) . . ?
F33A C36 F31A 107(2) . . ?
F32A C36 F31A 97.2(18) . . ?
F33B C36 C32 123.7(16) . . ?
F33A C36 C32 119.4(16) . . ?
F31B C36 C32 107.8(14) . . ?
F32B C36 C32 106.9(15) . . ?
F32A C36 C32 106.6(11) . . ?
F31A C36 C32 112.6(16) . . ?
F36 C37 F35 107.6(11) . . ?
F36 C37 F34 103.4(11) . . ?
F35 C37 F34 102.9(12) . . ?
F36 C37 C34 113.7(12) . . ?
F35 C37 C34 114.1(9) . . ?
F34 C37 C34 114.0(10) . . ?
C42 O41 Ce1 134.1(7) . . ?
O41 C42 C43 126.3(11) . . ?
O41 C42 C46 115.7(9) . . ?
C43 C42 C46 118.0(10) . . ?
C44 C43 C42 122.1(11) . . ?
C44 C43 H43A 118.9 . . ?
C42 C43 H43A 118.9 . . ?
O45 C44 C43 129.2(10) . . ?
O45 C44 C47 112.3(10) . . ?
C43 C44 C47 118.5(10) . . ?
C44 O45 Ce1 131.7(7) . . ?
F42B C46 F43B 105(2) . . ?
F43A C46 F42A 106.0(15) . . ?
F42B C46 F41B 119(2) . . ?
F43B C46 F41B 98.0(18) . . ?
F43A C46 F41A 104.4(12) . . ?
F42A C46 F41A 108.4(14) . . ?
F42B C46 C42 114.4(19) . . ?
F43A C46 C42 110.8(9) . . ?
F43B C46 C42 107.8(15) . . ?
F42A C46 C42 113.0(10) . . ?
F41B C46 C42 110.9(17) . . ?
F41A C46 C42 113.8(10) . . ?
F45 C47 F44 107.8(11) . . ?
F45 C47 F46 105.8(9) . . ?
F44 C47 F46 104.6(8) . . ?
F45 C47 C44 113.0(8) . . ?
F44 C47 C44 111.2(8) . . ?
F46 C47 C44 113.8(11) . . ?
O71 Ce2 O75 70.4(2) . . ?
O71 Ce2 O85 80.3(2) . . ?
O75 Ce2 O85 121.6(2) . . ?
O71 Ce2 O81 120.9(2) . . ?
O75 Ce2 O81 83.9(2) . . ?
O85 Ce2 O81 69.5(2) . . ?
O71 Ce2 O91 133.8(2) . . ?
O75 Ce2 O91 75.3(2) . . ?
O85 Ce2 O91 145.5(2) . . ?
O81 Ce2 O91 84.3(2) . . ?
O71 Ce2 O95 73.0(2) . . ?
O75 Ce2 O95 77.5(2) . . ?
O85 Ce2 O95 139.3(2) . . ?
O81 Ce2 O95 151.1(2) . . ?
O91 Ce2 O95 69.9(2) . . ?
O71 Ce2 N51 82.5(2) . . ?
O75 Ce2 N51 147.1(2) . . ?
O85 Ce2 N51 69.5(2) . . ?
O81 Ce2 N51 127.2(2) . . ?
O91 Ce2 N51 114.2(2) . . ?
O95 Ce2 N51 77.0(2) . . ?
O71 Ce2 N62 142.2(2) . . ?
O75 Ce2 N62 147.4(2) . . ?
O85 Ce2 N62 75.9(2) . . ?
O81 Ce2 N62 77.0(2) . . ?
O91 Ce2 N62 76.6(2) . . ?
O95 Ce2 N62 107.9(2) . . ?
N51 Ce2 N62 61.9(2) . . ?
C52 N51 C56 118.2(9) . . ?
C52 N51 Ce2 119.4(6) . . ?
C56 N51 Ce2 120.9(6) . . ?
N51 C52 C53 124.3(10) . . ?
N51 C52 H52A 117.9 . . ?
C53 C52 H52A 117.9 . . ?
C54 C53 C52 116.3(10) . . ?
C54 C53 H53A 121.9 . . ?
C52 C53 H53A 121.9 . . ?
C53 C54 C55 121.2(10) . . ?
C53 C54 H54A 119.4 . . ?
C55 C54 H54A 119.4 . . ?
C56 C55 C54 119.8(10) . . ?
C56 C55 H55A 120.1 . . ?
C54 C55 H55A 120.1 . . ?
N51 C56 C55 120.1(9) . . ?
N51 C56 C57 116.2(8) . . ?
C55 C56 C57 123.6(9) . . ?
N62 C57 C58 119.2(9) . . ?
N62 C57 C56 117.3(8) . . ?
C58 C57 C56 123.3(9) . . ?
C59 C58 C57 120.7(10) . . ?
C59 C58 H58A 119.7 . . ?
C57 C58 H58A 119.7 . . ?
C60 C59 C58 118.8(9) . . ?
C60 C59 H59A 120.6 . . ?
C58 C59 H59A 120.6 . . ?
C59 C60 C61 119.2(10) . . ?
C59 C60 H60A 120.4 . . ?
C61 C60 H60A 120.4 . . ?
N62 C61 C60 123.0(9) . . ?
N62 C61 H61A 118.5 . . ?
C60 C61 H61A 118.5 . . ?
C61 N62 C57 118.8(7) . . ?
C61 N62 Ce2 119.8(6) . . ?
C57 N62 Ce2 120.3(6) . . ?
C72 O71 Ce2 133.6(6) . . ?
O71 C72 C73 128.1(10) . . ?
O71 C72 C76 115.8(9) . . ?
C73 C72 C76 116.0(9) . . ?
C74 C73 C72 122.1(9) . . ?
C74 C73 H73A 119.0 . . ?
C72 C73 H73A 119.0 . . ?
O75 C74 C73 127.4(10) . . ?
O75 C74 C77 114.7(8) . . ?
C73 C74 C77 117.9(8) . . ?
C74 O75 Ce2 133.2(6) . . ?
F73 C76 F72 106.9(9) . . ?
F73 C76 F71 106.3(10) . . ?
F72 C76 F71 107.7(11) . . ?
F73 C76 C72 112.0(10) . . ?
F72 C76 C72 111.7(10) . . ?
F71 C76 C72 112.0(9) . . ?
F75B C77 F74B 124(2) . . ?
F74A C77 F75A 110(2) . . ?
F75B C77 F76B 97(2) . . ?
F74B C77 F76B 100.7(18) . . ?
F74A C77 F76A 89(3) . . ?
F75A C77 F76A 108(2) . . ?
F74A C77 C74 117.3(17) . . ?
F75B C77 C74 111.9(16) . . ?
F74B C77 C74 110.8(14) . . ?
F75A C77 C74 118.7(16) . . ?
F76B C77 C74 110.1(16) . . ?
F76A C77 C74 109.4(16) . . ?
C82 O81 Ce2 135.0(6) . . ?
O81 C82 C83 128.1(10) . . ?
O81 C82 C86 113.9(9) . . ?
C83 C82 C86 117.9(10) . . ?
C84 C83 C82 120.6(10) . . ?
C84 C83 H83A 119.7 . . ?
C82 C83 H83A 119.7 . . ?
O85 C84 C83 128.8(10) . . ?
O85 C84 C87 112.7(10) . . ?
C83 C84 C87 118.5(10) . . ?
C84 O85 Ce2 134.3(7) . . ?
F82A C86 F81A 107(2) . . ?
F81B C86 F82B 108(3) . . ?
F82A C86 F83A 102.7(19) . . ?
F81A C86 F83A 107(2) . . ?
F81B C86 F83B 109(2) . . ?
F82B C86 F83B 106(2) . . ?
F82A C86 C82 116.8(17) . . ?
F81B C86 C82 116(2) . . ?
F81A C86 C82 115(2) . . ?
F82B C86 C82 113(2) . . ?
F83A C86 C82 107.4(18) . . ?
F83B C86 C82 103.8(17) . . ?
F86 C87 F85 108.3(10) . . ?
F86 C87 F84 104.7(12) . . ?
F85 C87 F84 101.6(11) . . ?
F86 C87 C84 113.8(10) . . ?
F85 C87 C84 115.1(11) . . ?
F84 C87 C84 112.1(9) . . ?
C92 O91 Ce2 132.7(6) . . ?
O91 C92 C93 127.5(10) . . ?
O91 C92 C96 113.8(10) . . ?
C93 C92 C96 118.7(9) . . ?
C94 C93 C92 122.6(10) . . ?
C94 C93 H93A 118.7 . . ?
C92 C93 H93A 118.7 . . ?
O95 C94 C93 126.8(11) . . ?
O95 C94 C97 116.7(10) . . ?
C93 C94 C97 116.3(10) . . ?
C94 O95 Ce2 133.9(7) . . ?
F91B C96 F93B 108(2) . . ?
F93A C96 F91A 105.9(13) . . ?
F91B C96 F92B 104(3) . . ?
F93B C96 F92B 98(2) . . ?
F93A C96 F92A 102.5(11) . . ?
F91A C96 F92A 110.1(12) . . ?
F91B C96 C92 118(2) . . ?
F93B C96 C92 108.2(18) . . ?
F93A C96 C92 112.2(9) . . ?
F91A C96 C92 113.4(9) . . ?
F92B C96 C92 118(2) . . ?
F92A C96 C92 112.1(10) . . ?
F96 C97 F95 108.0(10) . . ?
F96 C97 F94 102.1(9) . . ?
F95 C97 F94 105.9(11) . . ?
F96 C97 C94 117.2(11) . . ?
F95 C97 C94 113.2(9) . . ?
F94 C97 C94 109.3(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 C3 0.5(14) . . . . ?
Ce1 N1 C2 C3 169.6(7) . . . . ?
N1 C2 C3 C4 -0.6(15) . . . . ?
C2 C3 C4 C5 0.6(15) . . . . ?
C3 C4 C5 C6 -0.3(16) . . . . ?
C2 N1 C6 C5 -0.2(14) . . . . ?
Ce1 N1 C6 C5 -169.0(7) . . . . ?
C2 N1 C6 C7 -178.1(8) . . . . ?
Ce1 N1 C6 C7 13.1(11) . . . . ?
C4 C5 C6 N1 0.1(15) . . . . ?
C4 C5 C6 C7 177.9(9) . . . . ?
N1 C6 C7 N12 4.6(12) . . . . ?
C5 C6 C7 N12 -173.4(9) . . . . ?
N1 C6 C7 C8 -177.8(9) . . . . ?
C5 C6 C7 C8 4.2(15) . . . . ?
N12 C7 C8 C9 -1.6(16) . . . . ?
C6 C7 C8 C9 -179.1(9) . . . . ?
C7 C8 C9 C10 3.5(16) . . . . ?
C8 C9 C10 C11 -2.7(16) . . . . ?
C9 C10 C11 N12 0.0(17) . . . . ?
C10 C11 N12 C7 1.8(15) . . . . ?
C10 C11 N12 Ce1 -161.6(8) . . . . ?
C8 C7 N12 C11 -0.9(14) . . . . ?
C6 C7 N12 C11 176.7(8) . . . . ?
C8 C7 N12 Ce1 162.6(7) . . . . ?
C6 C7 N12 Ce1 -19.8(11) . . . . ?
Ce1 O21 C22 C23 20.2(14) . . . . ?
Ce1 O21 C22 C26 -158.8(7) . . . . ?
O21 C22 C23 C24 -0.2(16) . . . . ?
C26 C22 C23 C24 178.7(9) . . . . ?
C22 C23 C24 O25 -6.2(16) . . . . ?
C22 C23 C24 C27 175.8(9) . . . . ?
C23 C24 O25 Ce1 -7.1(15) . . . . ?
C27 C24 O25 Ce1 171.0(6) . . . . ?
O21 C22 C26 F21 -59.5(12) . . . . ?
C23 C22 C26 F21 121.5(11) . . . . ?
O21 C22 C26 F23 60.9(13) . . . . ?
C23 C22 C26 F23 -118.1(11) . . . . ?
O21 C22 C26 F22 179.8(9) . . . . ?
C23 C22 C26 F22 0.8(14) . . . . ?
O25 C24 C27 F26 60.8(13) . . . . ?
C23 C24 C27 F26 -120.9(11) . . . . ?
O25 C24 C27 F24 -59.0(11) . . . . ?
C23 C24 C27 F24 119.3(11) . . . . ?
O25 C24 C27 F25 -176.7(8) . . . . ?
C23 C24 C27 F25 1.6(14) . . . . ?
Ce1 O31 C32 C33 23.3(15) . . . . ?
Ce1 O31 C32 C36 -154.3(6) . . . . ?
O31 C32 C33 C34 -3.4(16) . . . . ?
C36 C32 C33 C34 174.1(9) . . . . ?
C32 C33 C34 O35 1.5(17) . . . . ?
C32 C33 C34 C37 -175.7(9) . . . . ?
C33 C34 O35 Ce1 -19.5(15) . . . . ?
C37 C34 O35 Ce1 157.7(7) . . . . ?
O31 C32 C36 F33B -47(3) . . . . ?
C33 C32 C36 F33B 135(3) . . . . ?
O31 C32 C36 F33A 166.5(19) . . . . ?
C33 C32 C36 F33A -11(2) . . . . ?
O31 C32 C36 F31B -166.7(16) . . . . ?
C33 C32 C36 F31B 15.5(19) . . . . ?
O31 C32 C36 F32B 82(2) . . . . ?
C33 C32 C36 F32B -96(2) . . . . ?
O31 C32 C36 F32A -66.4(16) . . . . ?
C33 C32 C36 F32A 115.8(16) . . . . ?
O31 C32 C36 F31A 39.0(19) . . . . ?
C33 C32 C36 F31A -138.8(17) . . . . ?
O35 C34 C37 F36 -115.4(12) . . . . ?
C33 C34 C37 F36 62.1(14) . . . . ?
O35 C34 C37 F35 120.6(12) . . . . ?
C33 C34 C37 F35 -61.8(15) . . . . ?
O35 C34 C37 F34 2.8(15) . . . . ?
C33 C34 C37 F34 -179.7(11) . . . . ?
Ce1 O41 C42 C43 -17.0(15) . . . . ?
Ce1 O41 C42 C46 165.9(6) . . . . ?
O41 C42 C43 C44 -2.9(16) . . . . ?
C46 C42 C43 C44 174.2(9) . . . . ?
C42 C43 C44 O45 -1.6(17) . . . . ?
C42 C43 C44 C47 -178.6(8) . . . . ?
C43 C44 O45 Ce1 25.3(15) . . . . ?
C47 C44 O45 Ce1 -157.6(6) . . . . ?
O41 C42 C46 F42B 146(2) . . . . ?
C43 C42 C46 F42B -31(2) . . . . ?
O41 C42 C46 F43A 76.5(13) . . . . ?
C43 C42 C46 F43A -100.8(12) . . . . ?
O41 C42 C46 F43B -98.0(17) . . . . ?
C43 C42 C46 F43B 84.7(17) . . . . ?
O41 C42 C46 F42A -42.2(18) . . . . ?
C43 C42 C46 F42A 140.5(16) . . . . ?
O41 C42 C46 F41B 8.3(19) . . . . ?
C43 C42 C46 F41B -169.1(17) . . . . ?
O41 C42 C46 F41A -166.3(13) . . . . ?
C43 C42 C46 F41A 16.4(16) . . . . ?
O45 C44 C47 F45 49.7(12) . . . . ?
C43 C44 C47 F45 -132.9(11) . . . . ?
O45 C44 C47 F44 -71.7(11) . . . . ?
C43 C44 C47 F44 105.7(12) . . . . ?
O45 C44 C47 F46 170.5(8) . . . . ?
C43 C44 C47 F46 -12.1(13) . . . . ?
C56 N51 C52 C53 0.4(15) . . . . ?
Ce2 N51 C52 C53 166.4(8) . . . . ?
N51 C52 C53 C54 -2.9(16) . . . . ?
C52 C53 C54 C55 3.9(16) . . . . ?
C53 C54 C55 C56 -2.5(16) . . . . ?
C52 N51 C56 C55 1.2(13) . . . . ?
Ce2 N51 C56 C55 -164.6(7) . . . . ?
C52 N51 C56 C57 179.6(8) . . . . ?
Ce2 N51 C56 C57 13.8(10) . . . . ?
C54 C55 C56 N51 -0.1(15) . . . . ?
C54 C55 C56 C57 -178.5(9) . . . . ?
N51 C56 C57 N62 0.9(12) . . . . ?
C55 C56 C57 N62 179.3(8) . . . . ?
N51 C56 C57 C58 176.6(9) . . . . ?
C55 C56 C57 C58 -5.0(15) . . . . ?
N62 C57 C58 C59 -4.5(15) . . . . ?
C56 C57 C58 C59 179.8(9) . . . . ?
C57 C58 C59 C60 5.4(17) . . . . ?
C58 C59 C60 C61 -2.6(16) . . . . ?
C59 C60 C61 N62 -1.2(15) . . . . ?
C60 C61 N62 C57 2.1(14) . . . . ?
C60 C61 N62 Ce2 -166.2(7) . . . . ?
C58 C57 N62 C61 0.8(13) . . . . ?
C56 C57 N62 C61 176.7(8) . . . . ?
C58 C57 N62 Ce2 169.0(7) . . . . ?
C56 C57 N62 Ce2 -15.1(10) . . . . ?
Ce2 O71 C72 C73 14.5(16) . . . . ?
Ce2 O71 C72 C76 -161.5(6) . . . . ?
O71 C72 C73 C74 -1.0(18) . . . . ?
C76 C72 C73 C74 175.0(10) . . . . ?
C72 C73 C74 O75 6.0(17) . . . . ?
C72 C73 C74 C77 -174.3(9) . . . . ?
C73 C74 O75 Ce2 -24.5(15) . . . . ?
C77 C74 O75 Ce2 155.8(6) . . . . ?
O71 C72 C76 F73 -119.0(11) . . . . ?
C73 C72 C76 F73 64.5(13) . . . . ?
O71 C72 C76 F72 121.1(11) . . . . ?
C73 C72 C76 F72 -55.3(13) . . . . ?
O71 C72 C76 F71 0.2(14) . . . . ?
C73 C72 C76 F71 -176.2(10) . . . . ?
O75 C74 C77 F74A 46(2) . . . . ?
C73 C74 C77 F74A -134(2) . . . . ?
O75 C74 C77 F75B 56.5(19) . . . . ?
C73 C74 C77 F75B -123.2(18) . . . . ?
O75 C74 C77 F74B -86.4(17) . . . . ?
C73 C74 C77 F74B 93.9(18) . . . . ?
O75 C74 C77 F75A -178(2) . . . . ?
C73 C74 C77 F75A 2(2) . . . . ?
O75 C74 C77 F76B 163.0(18) . . . . ?
C73 C74 C77 F76B -17(2) . . . . ?
O75 C74 C77 F76A -53(2) . . . . ?
C73 C74 C77 F76A 127(2) . . . . ?
Ce2 O81 C82 C83 8.5(14) . . . . ?
Ce2 O81 C82 C86 -169.1(5) . . . . ?
O81 C82 C83 C84 5.6(16) . . . . ?
C86 C82 C83 C84 -176.9(9) . . . . ?
C82 C83 C84 O85 -0.4(17) . . . . ?
C82 C83 C84 C87 179.7(9) . . . . ?
C83 C84 O85 Ce2 -19.0(15) . . . . ?
C87 C84 O85 Ce2 161.0(7) . . . . ?
O81 C82 C86 F82A -45(2) . . . . ?
C83 C82 C86 F82A 137(2) . . . . ?
O81 C82 C86 F81B 35(2) . . . . ?
C83 C82 C86 F81B -142(2) . . . . ?
O81 C82 C86 F81A -171(2) . . . . ?
C83 C82 C86 F81A 11(2) . . . . ?
O81 C82 C86 F82B 161(2) . . . . ?
C83 C82 C86 F82B -16(2) . . . . ?
O81 C82 C86 F83A 69.8(19) . . . . ?
C83 C82 C86 F83A -108(2) . . . . ?
O81 C82 C86 F83B -84(2) . . . . ?
C83 C82 C86 F83B 98(2) . . . . ?
O85 C84 C87 F86 64.5(14) . . . . ?
C83 C84 C87 F86 -115.5(13) . . . . ?
O85 C84 C87 F85 -169.6(10) . . . . ?
C83 C84 C87 F85 10.4(16) . . . . ?
O85 C84 C87 F84 -54.1(13) . . . . ?
C83 C84 C87 F84 125.8(12) . . . . ?
Ce2 O91 C92 C93 15.3(16) . . . . ?
Ce2 O91 C92 C96 -163.6(6) . . . . ?
O91 C92 C93 C94 4.1(18) . . . . ?
C96 C92 C93 C94 -176.9(9) . . . . ?
C92 C93 C94 O95 0.0(17) . . . . ?
C92 C93 C94 C97 176.7(10) . . . . ?
C93 C94 O95 Ce2 -23.8(15) . . . . ?
C97 C94 O95 Ce2 159.4(6) . . . . ?
O91 C92 C96 F91B 134(2) . . . . ?
C93 C92 C96 F91B -45(3) . . . . ?
O91 C92 C96 F93B -103(2) . . . . ?
C93 C92 C96 F93B 78(2) . . . . ?
O91 C92 C96 F93A 84.8(13) . . . . ?
C93 C92 C96 F93A -94.2(14) . . . . ?
O91 C92 C96 F91A -35.1(16) . . . . ?
C93 C92 C96 F91A 145.8(14) . . . . ?
O91 C92 C96 F92B 8(2) . . . . ?
C93 C92 C96 F92B -172(2) . . . . ?
O91 C92 C96 F92A -160.5(11) . . . . ?
C93 C92 C96 F92A 20.4(15) . . . . ?
O95 C94 C97 F96 -166.1(9) . . . . ?
C93 C94 C97 F96 16.9(14) . . . . ?
O95 C94 C97 F95 67.2(13) . . . . ?
C93 C94 C97 F95 -109.9(12) . . . . ?
O95 C94 C97 F94 -50.6(13) . . . . ?
C93 C94 C97 F94 132.3(10) . . . . ?

_refine_diff_density_max         2.548
_refine_diff_density_min         -1.792
_refine_diff_density_rms         0.176


# start Validation Reply Form
_vrf_PLAT213_k11165              
;
PROBLEM: Atom F41A            has ADP max/min Ratio .....        5.1 prolat
RESPONSE: There are 5 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully.
;
_vrf_PLAT973_k11165              
;
PROBLEM: Check Calcd Positive Resid. Density on       Ce2       2.92 eA-3  
RESPONSE: Due to weak data and a relatively large crystal
;
_vrf_PLAT910_k11165              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: Yes, some peaks were omitted as they had negative values for Fobs.
;
# end Validation Reply Form

_exptl_crystal_recrystallization_method Sublimation
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_k11163
_database_code_depnum_ccdc_archive 'CCDC 1856929'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H19 Ce F18 N4 O6'
_chemical_formula_sum            'C35 H19 Ce F18 N4 O6'
_chemical_formula_weight         1073.66

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   21.819(4)
_cell_length_b                   11.828(2)
_cell_length_c                   18.116(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.98(3)
_cell_angle_gamma                90
_cell_volume                     4089.9(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    23613
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_F_000             2100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    1.244
_shelx_estimated_absorpt_T_min   0.605
_shelx_estimated_absorpt_T_max   0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            20806
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.570
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3617
_reflns_number_gt                2959
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_structure_solution    'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+32.7423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00018(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3617
_refine_ls_number_parameters     372
_refine_ls_number_restraints     190
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce Ce 0.500000 0.80698(3) 0.750000 0.03061(15) Uani 1 2 d S TU P A .
N1 N 0.5220(2) 0.8534(3) 0.9094(3) 0.0394(10) Uani 1 1 d . U . . .
C2 C 0.5882(3) 0.8643(4) 0.9726(3) 0.0430(13) Uani 1 1 d . U . . .
H2A H 0.624723 0.868513 0.958461 0.052 Uiso 1 1 calc R U . . .
C3 C 0.6062(3) 0.8697(4) 1.0572(4) 0.0480(14) Uani 1 1 d . U . . .
H3A H 0.653603 0.878218 1.099831 0.058 Uiso 1 1 calc R U . . .
C4 C 0.5527(4) 0.8622(5) 1.0775(4) 0.0572(15) Uani 1 1 d . U . . .
H4A H 0.562931 0.864178 1.134723 0.069 Uiso 1 1 calc R U . . .
C5 C 0.4850(3) 0.8518(5) 1.0140(4) 0.0528(14) Uani 1 1 d . U . . .
H5A H 0.447866 0.847212 1.027088 0.063 Uiso 1 1 calc R U . . .
C6 C 0.4705(3) 0.8481(4) 0.9305(3) 0.0388(12) Uani 1 1 d . U . . .
C7 C 0.3975(3) 0.8442(4) 0.8588(4) 0.0405(12) Uani 1 1 d . U . . .
C8 C 0.3389(3) 0.8442(6) 0.8712(4) 0.0654(18) Uani 1 1 d . U . . .
H8A H 0.344858 0.841486 0.926701 0.079 Uiso 1 1 calc R U . . .
C9 C 0.2728(3) 0.8482(6) 0.8026(5) 0.071(2) Uani 1 1 d . U . . .
H9A H 0.232773 0.848478 0.810363 0.085 Uiso 1 1 calc R U . . .
C10 C 0.2652(3) 0.8517(5) 0.7236(5) 0.0606(17) Uani 1 1 d . U . . .
H10A H 0.220117 0.855200 0.675169 0.073 Uiso 1 1 calc R U . . .
C11 C 0.3252(3) 0.8501(5) 0.7162(4) 0.0535(15) Uani 1 1 d . U . . .
H11A H 0.319979 0.851921 0.660981 0.064 Uiso 1 1 calc R U . . .
N12 N 0.3903(2) 0.8462(4) 0.7815(3) 0.0413(10) Uani 1 1 d . U . . .
O21 O 0.53178(17) 0.6381(3) 0.6910(2) 0.0383(8) Uani 1 1 d . U . . .
C22A C 0.5024(3) 0.5560(5) 0.6456(4) 0.0399(15) Uani 0.77 1 d . U P A 1
C23A C 0.4311(4) 0.5340(6) 0.6040(5) 0.057(2) Uani 0.77 1 d . U P A 1
H23A H 0.414729 0.465311 0.573374 0.069 Uiso 0.77 1 calc R U P A 1
C24A C 0.3837(5) 0.6076(9) 0.6054(6) 0.046(2) Uani 0.77 1 d . U P A 1
C22B C 0.5641(12) 0.559(2) 0.7150(16) 0.046(5) Uani 0.23 1 d . U P A 3
C23B C 0.6111(11) 0.5337(19) 0.7996(16) 0.045(5) Uani 0.23 1 d . U P A 3
H23B H 0.631387 0.460447 0.813610 0.054 Uiso 0.23 1 calc R U P A 3
C24B C 0.6296(16) 0.616(3) 0.866(2) 0.041(7) Uani 0.23 1 d . U P A 3
O25 O 0.39400(16) 0.7049(3) 0.6415(2) 0.0386(8) Uani 1 1 d . U . . .
C26 C 0.5520(4) 0.4703(5) 0.6396(4) 0.0674(17) Uani 1 1 d D U . . .
C27 C 0.3084(3) 0.5732(5) 0.5558(5) 0.0740(19) Uani 1 1 d D U . . .
F21A F 0.5237(6) 0.4038(8) 0.5704(8) 0.106(4) Uani 0.48 1 d D U P A 1
F22A F 0.5810(11) 0.3818(10) 0.6862(8) 0.131(6) Uani 0.48 1 d D U P A 1
F23A F 0.5855(13) 0.5226(17) 0.6068(15) 0.111(6) Uani 0.48 1 d D U P A 1
F21B F 0.5938(8) 0.4301(11) 0.7129(7) 0.123(5) Uani 0.52 1 d D U P A 2
F23B F 0.5026(9) 0.408(2) 0.5969(14) 0.274(13) Uani 0.52 1 d D U P A 2
F22B F 0.6007(12) 0.510(2) 0.6267(18) 0.141(8) Uani 0.52 1 d D U P A 2
F24A F 0.3025(14) 0.623(2) 0.4905(10) 0.241(13) Uani 0.44 1 d D U P A 1
F25A F 0.2921(6) 0.4712(10) 0.5650(13) 0.110(7) Uani 0.44 1 d D U P A 1
F26A F 0.2630(10) 0.6374(16) 0.563(2) 0.208(12) Uani 0.44 1 d D U P A 1
F24B F 0.2771(8) 0.563(2) 0.5984(11) 0.202(9) Uani 0.56 1 d D U P A 2
F25B F 0.2699(5) 0.629(2) 0.4941(11) 0.164(7) Uani 0.56 1 d D U P A 2
F26B F 0.3029(7) 0.4820(12) 0.5120(13) 0.190(8) Uani 0.56 1 d D U P A 2
O31 O 0.43052(17) 0.9857(3) 0.6864(2) 0.0387(8) Uani 1 1 d . U . . .
C32 C 0.4387(3) 1.0899(4) 0.6963(3) 0.0362(11) Uani 1 1 d . U . . .
C33 C 0.500000 1.1478(6) 0.750000 0.0458(19) Uani 1 2 d S TU P . .
H33A H 0.500001 1.228128 0.750000 0.069 Uiso 1 2 calc R U P . .
C34 C 0.3724(3) 1.1586(5) 0.6435(4) 0.0510(14) Uani 1 1 d . U . . .
F31 F 0.3291(2) 1.1499(5) 0.6733(3) 0.124(2) Uani 1 1 d . U . . .
F32 F 0.3838(2) 1.2662(3) 0.6381(3) 0.121(2) Uani 1 1 d . U . . .
F33 F 0.33837(18) 1.1217(3) 0.5649(2) 0.0737(11) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce O25 2.503(3) . ?
Ce O25 2.503(3) 2_656 ?
Ce O21 2.517(3) . ?
Ce O21 2.517(3) 2_656 ?
Ce O31 2.530(3) 2_656 ?
Ce O31 2.530(3) . ?
Ce N1 2.744(4) 2_656 ?
Ce N1 2.744(4) . ?
Ce N12 2.755(4) 2_656 ?
Ce N12 2.755(4) . ?
N1 C2 1.345(7) . ?
N1 C6 1.352(6) . ?
C2 C3 1.387(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.385(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.369(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.387(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.491(7) . ?
C7 N12 1.332(7) . ?
C7 C8 1.401(7) . ?
C8 C9 1.375(9) . ?
C8 H8A 0.9500 . ?
C9 C10 1.359(9) . ?
C9 H9A 0.9500 . ?
C10 C11 1.380(7) . ?
C10 H10A 0.9500 . ?
C11 N12 1.339(7) . ?
C11 H11A 0.9500 . ?
O21 C22B 1.13(2) . ?
O21 C22A 1.233(7) . ?
C22A C23A 1.386(10) . ?
C22A C26 1.524(9) . ?
C23A C24A 1.363(12) . ?
C23A H23A 0.9500 . ?
C24A O25 1.289(11) . ?
C24A C27 1.497(11) . ?
C22B C23B 1.40(3) . ?
C22B C26 1.64(2) . ?
C23B C24B 1.45(4) . ?
C23B H23B 0.9500 . ?
C24B O25 1.15(4) 2_656 ?
C24B C27 1.49(3) 2_656 ?
C26 F23B 1.221(11) . ?
C26 F22B 1.281(12) . ?
C26 F21B 1.285(10) . ?
C26 F23A 1.300(12) . ?
C26 F22A 1.302(11) . ?
C26 F21A 1.350(10) . ?
C27 F25B 1.218(11) . ?
C27 F24B 1.258(11) . ?
C27 F24A 1.269(13) . ?
C27 F25A 1.291(10) . ?
C27 F26A 1.299(13) . ?
C27 F26B 1.311(11) . ?
O31 C32 1.246(6) . ?
C32 C33 1.394(6) . ?
C32 C34 1.525(7) . ?
C33 H33A 0.9500 . ?
C34 F31 1.300(7) . ?
C34 F32 1.309(7) . ?
C34 F33 1.321(7) . ?

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
O25 Ce O25 122.32(16) . 2_656 ?
O25 Ce O21 67.89(11) . . ?
O25 Ce O21 67.09(11) 2_656 . ?
O25 Ce O21 67.09(11) . 2_656 ?
O25 Ce O21 67.89(11) 2_656 2_656 ?
O21 Ce O21 74.94(16) . 2_656 ?
O25 Ce O31 151.93(11) . 2_656 ?
O25 Ce O31 85.62(11) 2_656 2_656 ?
O21 Ce O31 128.96(11) . 2_656 ?
O21 Ce O31 134.22(11) 2_656 2_656 ?
O25 Ce O31 85.62(11) . . ?
O25 Ce O31 151.93(11) 2_656 . ?
O21 Ce O31 134.22(11) . . ?
O21 Ce O31 128.96(11) 2_656 . ?
O31 Ce O31 66.66(15) 2_656 . ?
O25 Ce N1 69.28(12) . 2_656 ?
O25 Ce N1 123.16(11) 2_656 2_656 ?
O21 Ce N1 69.84(12) . 2_656 ?
O21 Ce N1 131.49(12) 2_656 2_656 ?
O31 Ce N1 94.16(12) 2_656 2_656 ?
O31 Ce N1 65.97(11) . 2_656 ?
O25 Ce N1 123.16(12) . . ?
O25 Ce N1 69.28(12) 2_656 . ?
O21 Ce N1 131.48(12) . . ?
O21 Ce N1 69.84(12) 2_656 . ?
O31 Ce N1 65.97(11) 2_656 . ?
O31 Ce N1 94.16(12) . . ?
N1 Ce N1 156.90(17) 2_656 . ?
O25 Ce N12 118.92(12) . 2_656 ?
O25 Ce N12 71.27(12) 2_656 2_656 ?
O21 Ce N12 66.41(12) . 2_656 ?
O21 Ce N12 131.88(12) 2_656 2_656 ?
O31 Ce N12 64.18(12) 2_656 2_656 ?
O31 Ce N12 98.86(12) . 2_656 ?
N1 Ce N12 58.34(13) 2_656 2_656 ?
N1 Ce N12 117.22(13) . 2_656 ?
O25 Ce N12 71.27(12) . . ?
O25 Ce N12 118.93(12) 2_656 . ?
O21 Ce N12 131.88(12) . . ?
O21 Ce N12 66.41(12) 2_656 . ?
O31 Ce N12 98.86(12) 2_656 . ?
O31 Ce N12 64.18(11) . . ?
N1 Ce N12 117.22(13) 2_656 . ?
N1 Ce N12 58.34(13) . . ?
N12 Ce N12 160.60(18) 2_656 . ?
C2 N1 C6 117.4(5) . . ?
C2 N1 Ce 118.9(3) . . ?
C6 N1 Ce 122.8(3) . . ?
N1 C2 C3 123.9(5) . . ?
N1 C2 H2A 118.0 . . ?
C3 C2 H2A 118.0 . . ?
C4 C3 C2 117.7(6) . . ?
C4 C3 H3A 121.1 . . ?
C2 C3 H3A 121.1 . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
N1 C6 C5 121.7(5) . . ?
N1 C6 C7 116.0(5) . . ?
C5 C6 C7 122.2(5) . . ?
N12 C7 C8 121.1(5) . . ?
N12 C7 C6 116.6(4) . . ?
C8 C7 C6 122.2(5) . . ?
C9 C8 C7 119.6(6) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C10 C9 C8 119.5(6) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C9 C10 C11 117.7(6) . . ?
C9 C10 H10A 121.2 . . ?
C11 C10 H10A 121.2 . . ?
N12 C11 C10 124.4(6) . . ?
N12 C11 H11A 117.8 . . ?
C10 C11 H11A 117.8 . . ?
C7 N12 C11 117.7(5) . . ?
C7 N12 Ce 122.9(3) . . ?
C11 N12 Ce 118.6(4) . . ?
C22B O21 Ce 138.2(13) . . ?
C22A O21 Ce 138.4(4) . . ?
O21 C22A C23A 126.4(6) . . ?
O21 C22A C26 114.5(6) . . ?
C23A C22A C26 119.0(6) . . ?
C24A C23A C22A 122.2(7) . . ?
C24A C23A H23A 118.9 . . ?
C22A C23A H23A 118.9 . . ?
O25 C24A C23A 129.3(8) . . ?
O25 C24A C27 114.7(8) . . ?
C23A C24A C27 115.9(8) . . ?
O21 C22B C23B 126(2) . . ?
O21 C22B C26 113.1(19) . . ?
C23B C22B C26 120.9(19) . . ?
C22B C23B C24B 122(2) . . ?
C22B C23B H23B 119.0 . . ?
C24B C23B H23B 119.0 . . ?
O25 C24B C23B 126(3) 2_656 . ?
O25 C24B C27 125(3) 2_656 2_656 ?
C24B O25 Ce 136.6(16) 2_656 . ?
C24A O25 Ce 134.2(5) . . ?
F23B C26 F22B 131.4(19) . . ?
F23B C26 F21B 113.5(16) . . ?
F22B C26 F21B 95.1(16) . . ?
F23A C26 F22A 118.4(17) . . ?
F23A C26 F21A 87.7(10) . . ?
F22A C26 F21A 89.6(9) . . ?
F23A C26 C22A 107.0(12) . . ?
F22A C26 C22A 128.8(10) . . ?
F21A C26 C22A 115.7(7) . . ?
F25B C27 F24B 106.1(13) . . ?
F24A C27 F25A 129.8(17) . . ?
F24A C27 F26A 95(2) . . ?
F25A C27 F26A 105.3(13) . . ?
F25B C27 F26B 94.0(16) . . ?
F24B C27 F26B 112.1(13) . . ?
F24A C27 C24B 111.2(18) . 2_656 ?
F25A C27 C24B 112.0(16) . 2_656 ?
F26A C27 C24B 95.5(17) . 2_656 ?
F24A C27 C24A 91.2(13) . . ?
F25A C27 C24A 117.9(8) . . ?
F26A C27 C24A 116.7(12) . . ?
C32 O31 Ce 138.5(3) . . ?
O31 C32 C33 127.5(5) . . ?
O31 C32 C34 114.2(5) . . ?
C33 C32 C34 118.3(5) . . ?
C32 C33 C32 121.1(7) . 2_656 ?
C32 C33 H33A 119.4 . . ?
C32 C33 H33A 119.4 2_656 . ?
F31 C34 F32 108.0(5) . . ?
F31 C34 F33 106.2(6) . . ?
F32 C34 F33 105.6(5) . . ?
F31 C34 C32 110.9(5) . . ?
F32 C34 C32 114.1(5) . . ?
F33 C34 C32 111.6(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
C6 N1 C2 C3 0.4(7) . . . . ?
Ce N1 C2 C3 -169.3(4) . . . . ?
N1 C2 C3 C4 0.7(8) . . . . ?
C2 C3 C4 C5 -1.1(8) . . . . ?
C3 C4 C5 C6 0.5(9) . . . . ?
C2 N1 C6 C5 -1.0(7) . . . . ?
Ce N1 C6 C5 168.2(4) . . . . ?
C2 N1 C6 C7 175.9(4) . . . . ?
Ce N1 C6 C7 -14.9(6) . . . . ?
C4 C5 C6 N1 0.6(8) . . . . ?
C4 C5 C6 C7 -176.1(5) . . . . ?
N1 C6 C7 N12 0.1(6) . . . . ?
C5 C6 C7 N12 177.0(5) . . . . ?
N1 C6 C7 C8 -176.8(5) . . . . ?
C5 C6 C7 C8 0.1(8) . . . . ?
N12 C7 C8 C9 -1.1(9) . . . . ?
C6 C7 C8 C9 175.6(5) . . . . ?
C7 C8 C9 C10 0.2(10) . . . . ?
C8 C9 C10 C11 0.6(10) . . . . ?
C9 C10 C11 N12 -0.5(10) . . . . ?
C8 C7 N12 C11 1.1(8) . . . . ?
C6 C7 N12 C11 -175.8(5) . . . . ?
C8 C7 N12 Ce -168.4(4) . . . . ?
C6 C7 N12 Ce 14.7(6) . . . . ?
C10 C11 N12 C7 -0.3(8) . . . . ?
C10 C11 N12 Ce 169.6(5) . . . . ?
Ce O21 C22A C23A 4.5(11) . . . . ?
Ce O21 C22A C26 -172.9(4) . . . . ?
O21 C22A C23A C24A 3.8(13) . . . . ?
C26 C22A C23A C24A -178.9(7) . . . . ?
C22A C23A C24A O25 0.9(15) . . . . ?
C22A C23A C24A C27 178.7(7) . . . . ?
Ce O21 C22B C23B -10(4) . . . . ?
Ce O21 C22B C26 170.0(4) . . . . ?
O21 C22B C23B C24B -8(4) . . . . ?
C26 C22B C23B C24B 172(2) . . . . ?
C22B C23B C24B O25 4(4) . . . 2_656 ?
C22B C23B C24B C27 -167.2(19) . . . 2_656 ?
C23A C24A O25 Ce -13.6(13) . . . . ?
C27 C24A O25 Ce 168.7(4) . . . . ?
O21 C22A C26 F23A -61.4(13) . . . . ?
C23A C22A C26 F23A 121.0(13) . . . . ?
O21 C22A C26 F22A 90.8(14) . . . . ?
C23A C22A C26 F22A -86.8(14) . . . . ?
O21 C22A C26 F21A -157.1(9) . . . . ?
C23A C22A C26 F21A 25.3(11) . . . . ?
O25 C24A C27 F24A 87.9(17) . . . . ?
C23A C24A C27 F24A -90.1(17) . . . . ?
O25 C24A C27 F25A -134.7(14) . . . . ?
C23A C24A C27 F25A 47.2(17) . . . . ?
O25 C24A C27 F26A -8(2) . . . . ?
C23A C24A C27 F26A 174(2) . . . . ?
Ce O31 C32 C33 5.6(8) . . . . ?
Ce O31 C32 C34 -173.2(3) . . . . ?
O31 C32 C33 C32 -2.7(4) . . . 2_656 ?
C34 C32 C33 C32 176.1(5) . . . 2_656 ?
O31 C32 C34 F31 73.1(7) . . . . ?
C33 C32 C34 F31 -105.8(6) . . . . ?
O31 C32 C34 F32 -164.7(5) . . . . ?
C33 C32 C34 F32 16.4(7) . . . . ?
O31 C32 C34 F33 -45.1(7) . . . . ?
C33 C32 C34 F33 136.0(5) . . . . ?

_refine_diff_density_max         1.490
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.112


# start Validation Reply Form
_vrf_PLAT213_k11163              
;
PROBLEM: Atom F25B            has ADP max/min Ratio .....        5.3 prolat
RESPONSE: There are 2 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully.
;
# end Validation Reply Form

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methylene chloride/hexanes'
####################################################################### 
# 
# 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_k10268
_database_code_depnum_ccdc_archive 'CCDC 1856925'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H11 F18 N2 O6 Pr'
_chemical_formula_sum            'C25 H11 F18 N2 O6 Pr'
_chemical_formula_weight         918.27

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'
O O 0.0106 0.0060 '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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9492(3)
_cell_length_b                   15.8540(5)
_cell_length_c                   17.8253(5)
_cell_angle_alpha                78.5449(14)
_cell_angle_beta                 76.6137(16)
_cell_angle_gamma                72.7269(15)
_cell_volume                     3106.17(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    20498
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.720
_shelx_estimated_absorpt_T_min   0.747
_shelx_estimated_absorpt_T_max   0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            33787
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.564
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10948
_reflns_number_gt                7640
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0565P)²+7.6897P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10948
_refine_ls_number_parameters     1045
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1313
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.97323(3) 0.23917(2) 0.53267(2) 0.02789(12) Uani 1 1 d . U . . .
N1 N 1.0185(4) 0.3693(3) 0.5798(3) 0.0305(11) Uani 1 1 d . U . . .
C2 C 0.9666(5) 0.3896(4) 0.6517(4) 0.0318(14) Uani 1 1 d . U . . .
H2A H 0.904287 0.363693 0.679917 0.038 Uiso 1 1 calc R U . . .
C3 C 1.0007(6) 0.4469(4) 0.6862(4) 0.0345(15) Uani 1 1 d . U . . .
H3A H 0.962480 0.459876 0.737148 0.041 Uiso 1 1 calc R U . . .
C4 C 1.0899(7) 0.4843(5) 0.6458(4) 0.0454(18) Uani 1 1 d . U . . .
H4A H 1.115874 0.522956 0.668306 0.055 Uiso 1 1 calc R U . . .
C5 C 1.1421(6) 0.4646(5) 0.5708(4) 0.0416(17) Uani 1 1 d . U . . .
H5A H 1.203151 0.491140 0.541322 0.050 Uiso 1 1 calc R U . . .
C6 C 1.1059(6) 0.4072(4) 0.5393(4) 0.0327(14) Uani 1 1 d . U . . .
C7 C 1.1568(5) 0.3845(4) 0.4588(4) 0.0301(14) Uani 1 1 d . U . . .
C8 C 1.2509(6) 0.4144(5) 0.4116(4) 0.0424(17) Uani 1 1 d . U . . .
H8A H 1.286505 0.450221 0.430495 0.051 Uiso 1 1 calc R U . . .
C9 C 1.2928(6) 0.3926(5) 0.3378(4) 0.0511(19) Uani 1 1 d . U . . .
H9A H 1.359443 0.410991 0.306061 0.061 Uiso 1 1 calc R U . . .
C10 C 1.2375(6) 0.3441(5) 0.3104(4) 0.0452(18) Uani 1 1 d . U . . .
H10A H 1.262931 0.329971 0.258691 0.054 Uiso 1 1 calc R U . . .
C11 C 1.1445(6) 0.3163(5) 0.3592(4) 0.0419(17) Uani 1 1 d . U . . .
H11A H 1.106166 0.282821 0.339779 0.050 Uiso 1 1 calc R U . . .
N12 N 1.1043(5) 0.3337(3) 0.4331(3) 0.0323(12) Uani 1 1 d . U . . .
O21 O 1.1772(4) 0.1799(3) 0.5515(3) 0.0371(11) Uani 1 1 d . U . . .
C22 C 1.2275(6) 0.1638(4) 0.6087(4) 0.0380(16) Uani 1 1 d . U . . .
C23 C 1.1771(6) 0.1505(5) 0.6872(4) 0.0393(16) Uani 1 1 d . U . . .
H23A H 1.226273 0.137364 0.725178 0.047 Uiso 1 1 calc R U . . .
C24 C 1.0575(6) 0.1560(4) 0.7111(4) 0.0341(14) Uani 1 1 d . U . . .
O25 O 0.9786(4) 0.1777(3) 0.6695(2) 0.0324(10) Uani 1 1 d . U . . .
C26 C 1.3601(6) 0.1583(5) 0.5861(5) 0.0462(18) Uani 1 1 d . U . . .
C27 C 1.0101(7) 0.1352(5) 0.7982(4) 0.0460(17) Uani 1 1 d . U . . .
F21 F 1.4186(4) 0.0974(4) 0.5433(4) 0.104(2) Uani 1 1 d . U . . .
F22 F 1.4142(4) 0.1422(5) 0.6468(4) 0.103(2) Uani 1 1 d . U . . .
F23 F 1.3784(4) 0.2344(4) 0.5485(4) 0.095(2) Uani 1 1 d . U . . .
F24 F 0.9261(5) 0.2054(4) 0.8240(3) 0.0906(18) Uani 1 1 d . U . . .
F25 F 1.0911(4) 0.1176(4) 0.8421(3) 0.0820(17) Uani 1 1 d . U . . .
F26 F 0.9602(6) 0.0705(4) 0.8143(3) 0.0929(19) Uani 1 1 d . U . . .
O31 O 0.8540(4) 0.1349(3) 0.5448(2) 0.0346(10) Uani 1 1 d . U . . .
C32 C 0.8350(6) 0.0964(4) 0.4953(4) 0.0325(14) Uani 1 1 d . U . . .
C33 C 0.9048(6) 0.0773(5) 0.4239(4) 0.0411(17) Uani 1 1 d . U . . .
H33A H 0.881814 0.044219 0.393842 0.049 Uiso 1 1 calc R U . . .
C34 C 1.0080(6) 0.1060(4) 0.3955(4) 0.0354(15) Uani 1 1 d . U . . .
O35 O 1.0537(4) 0.1474(3) 0.4280(2) 0.0369(10) Uani 1 1 d . U . . .
C36 C 0.7171(6) 0.0715(4) 0.5179(4) 0.0436(16) Uani 1 1 d D U . . .
C37 C 1.0729(7) 0.0864(5) 0.3133(4) 0.0486(18) Uani 1 1 d . U . . .
F31A F 0.6322(12) 0.1363(10) 0.5516(11) 0.109(7) Uani 0.55 1 d D U P A 1
F32A F 0.7204(19) 0.0079(12) 0.5774(9) 0.076(6) Uani 0.55 1 d D U P A 1
F33A F 0.677(2) 0.0463(19) 0.4670(14) 0.113(10) Uani 0.55 1 d D U P A 1
F31B F 0.715(2) 0.0176(18) 0.4707(17) 0.071(6) Uani 0.45 1 d D U P A 2
F32B F 0.6356(15) 0.1436(10) 0.4960(13) 0.106(8) Uani 0.45 1 d D U P A 2
F33B F 0.690(2) 0.0346(16) 0.5887(8) 0.080(7) Uani 0.45 1 d D U P A 2
F34 F 1.1717(5) 0.1134(4) 0.2907(3) 0.104(2) Uani 1 1 d . U . . .
F35 F 1.1067(5) 0.0016(3) 0.3076(3) 0.0918(18) Uani 1 1 d . U . . .
F36 F 1.0074(6) 0.1265(5) 0.2628(3) 0.137(3) Uani 1 1 d . U . . .
O41 O 0.7754(4) 0.3225(3) 0.5937(3) 0.0387(11) Uani 1 1 d . U . . .
C42 C 0.6753(6) 0.3470(4) 0.5743(4) 0.0376(15) Uani 1 1 d . U . . .
C43 C 0.6515(6) 0.3496(5) 0.5008(4) 0.0425(16) Uani 1 1 d . U . . .
H43A H 0.570744 0.364846 0.494507 0.051 Uiso 1 1 calc R U . . .
C44 C 0.7400(6) 0.3309(4) 0.4371(4) 0.0373(15) Uani 1 1 d . U . . .
O45 O 0.8501(4) 0.3083(3) 0.4342(2) 0.0359(10) Uani 1 1 d . U . . .
C46 C 0.5695(6) 0.3782(5) 0.6383(5) 0.0484(17) Uani 1 1 d D U . . .
C47 C 0.7048(7) 0.3399(5) 0.3583(5) 0.0483(18) Uani 1 1 d . U . . .
F41A F 0.4652(8) 0.4031(13) 0.6152(8) 0.093(4) Uani 0.6 1 d D U P B 1
F42A F 0.5629(16) 0.3194(10) 0.6975(10) 0.127(8) Uani 0.6 1 d D U P B 1
F43A F 0.5774(13) 0.4490(9) 0.6585(11) 0.093(5) Uani 0.6 1 d D U P B 1
F41B F 0.5999(18) 0.3635(18) 0.7070(9) 0.089(6) Uani 0.4 1 d D U P B 2
F42B F 0.527(3) 0.4620(10) 0.6291(18) 0.130(12) Uani 0.4 1 d D U P B 2
F43B F 0.491(3) 0.335(2) 0.6508(19) 0.147(12) Uani 0.4 1 d D U P B 2
F44 F 0.7247(5) 0.4123(3) 0.3129(3) 0.0772(15) Uani 1 1 d . U . . .
F45 F 0.7599(6) 0.2693(4) 0.3239(3) 0.095(2) Uani 1 1 d . U . . .
F46 F 0.5896(5) 0.3483(4) 0.3629(3) 0.0841(16) Uani 1 1 d . U . . .
Pr2 Pr 0.52277(3) 0.73996(2) 0.98138(2) 0.02712(12) Uani 1 1 d . U . . .
N51 N 0.4462(4) 0.8399(3) 1.0923(3) 0.0308(11) Uani 1 1 d . U . . .
C52 C 0.3565(6) 0.8240(5) 1.1500(4) 0.0389(16) Uani 1 1 d . U . . .
H52A H 0.310615 0.787480 1.142738 0.047 Uiso 1 1 calc R U . . .
C53 C 0.3283(6) 0.8591(5) 1.2199(4) 0.0421(17) Uani 1 1 d . U . . .
H53A H 0.264161 0.847302 1.259482 0.051 Uiso 1 1 calc R U . . .
C54 C 0.3950(6) 0.9104(5) 1.2298(4) 0.0463(18) Uani 1 1 d . U . . .
H54A H 0.379101 0.934196 1.277264 0.056 Uiso 1 1 calc R U . . .
C55 C 0.4858(6) 0.9279(5) 1.1708(4) 0.0412(17) Uani 1 1 d . U . . .
H55A H 0.532040 0.964572 1.177307 0.049 Uiso 1 1 calc R U . . .
C56 C 0.5099(5) 0.8926(4) 1.1025(3) 0.0280(13) Uani 1 1 d . U . . .
C57 C 0.6067(5) 0.9087(4) 1.0368(4) 0.0304(14) Uani 1 1 d . U . . .
C58 C 0.6773(6) 0.9638(4) 1.0372(4) 0.0411(17) Uani 1 1 d . U . . .
H58A H 0.665457 0.993060 1.081158 0.049 Uiso 1 1 calc R U . . .
C59 C 0.7656(6) 0.9763(5) 0.9730(4) 0.0429(17) Uani 1 1 d . U . . .
H59A H 0.815712 1.012769 0.973341 0.052 Uiso 1 1 calc R U . . .
C60 C 0.7794(6) 0.9359(4) 0.9102(4) 0.0348(15) Uani 1 1 d . U . . .
H60A H 0.838790 0.943973 0.865661 0.042 Uiso 1 1 calc R U . . .
C61 C 0.7056(5) 0.8827(4) 0.9118(4) 0.0322(15) Uani 1 1 d . U . . .
H61A H 0.714342 0.855540 0.867116 0.039 Uiso 1 1 calc R U . . .
N62 N 0.6225(4) 0.8678(3) 0.9735(3) 0.0285(11) Uani 1 1 d . U . . .
O71 O 0.4105(4) 0.6458(3) 1.0725(2) 0.0386(11) Uani 1 1 d . U . . .
C72 C 0.3448(6) 0.6012(5) 1.0646(4) 0.0380(15) Uani 1 1 d . U . . .
C73 C 0.3365(6) 0.5736(5) 0.9970(4) 0.0439(17) Uani 1 1 d . U . . .
H73A H 0.283143 0.538544 0.999735 0.053 Uiso 1 1 calc R U . . .
C74 C 0.4046(6) 0.5962(4) 0.9261(4) 0.0340(14) Uani 1 1 d . U . . .
O75 O 0.4833(4) 0.6376(3) 0.9121(2) 0.0314(10) Uani 1 1 d . U . . .
C76 C 0.2575(7) 0.5774(5) 1.1367(5) 0.0492(18) Uani 1 1 d . U . . .
C77 C 0.3831(6) 0.5701(5) 0.8542(4) 0.0410(16) Uani 1 1 d . U . . .
F71 F 0.2666(5) 0.6080(4) 1.1995(3) 0.0935(19) Uani 1 1 d . U . . .
F72 F 0.1465(4) 0.6072(4) 1.1284(3) 0.099(2) Uani 1 1 d . U . . .
F73 F 0.2767(4) 0.4900(3) 1.1573(3) 0.0752(15) Uani 1 1 d . U . . .
F74 F 0.4751(5) 0.5315(4) 0.8094(3) 0.0914(19) Uani 1 1 d . U . . .
F75 F 0.3095(5) 0.5197(4) 0.8687(3) 0.104(2) Uani 1 1 d . U . . .
F76 F 0.3239(8) 0.6423(4) 0.8148(4) 0.151(3) Uani 1 1 d . U . . .
O81 O 0.7288(4) 0.6753(3) 0.9222(3) 0.0348(10) Uani 1 1 d . U . . .
C82 C 0.8278(6) 0.6546(4) 0.9443(4) 0.0355(15) Uani 1 1 d . U . . .
C83 C 0.8470(6) 0.6526(5) 1.0176(4) 0.0432(17) Uani 1 1 d . U . . .
H83A H 0.926619 0.640988 1.025212 0.052 Uiso 1 1 calc R U . . .
C84 C 0.7551(6) 0.6670(4) 1.0809(4) 0.0383(15) Uani 1 1 d . U . . .
O85 O 0.6454(4) 0.6839(3) 1.0808(2) 0.0346(10) Uani 1 1 d . U . . .
C86 C 0.9358(6) 0.6328(5) 0.8786(5) 0.0529(18) Uani 1 1 d D U . . .
C87 C 0.7830(7) 0.6622(6) 1.1607(5) 0.056(2) Uani 1 1 d . U . . .
F81A F 1.0361(16) 0.605(2) 0.904(2) 0.124(11) Uani 0.55 1 d D U P C 1
F82A F 0.930(2) 0.5751(18) 0.8396(19) 0.117(9) Uani 0.55 1 d D U P C 1
F83A F 0.942(2) 0.7050(13) 0.8306(12) 0.115(8) Uani 0.55 1 d D U P C 1
F81B F 0.922(3) 0.6829(18) 0.8130(12) 0.121(11) Uani 0.45 1 d D U P C 2
F82B F 1.0370(19) 0.634(2) 0.893(2) 0.079(6) Uani 0.45 1 d D U P C 2
F83B F 0.954(3) 0.5514(16) 0.867(2) 0.141(15) Uani 0.45 1 d D U P C 2
F84 F 0.7247(6) 0.7356(5) 1.1909(4) 0.120(2) Uani 1 1 d . U . . .
F85 F 0.8936(5) 0.6587(6) 1.1604(3) 0.126(3) Uani 1 1 d . U . . .
F86 F 0.7540(8) 0.6005(5) 1.2106(4) 0.137(3) Uani 1 1 d . U . . .
O91 O 0.5071(4) 0.8230(3) 0.8511(3) 0.0398(11) Uani 1 1 d . U . . .
C92 C 0.4250(7) 0.8457(4) 0.8120(4) 0.0400(15) Uani 1 1 d . U . . .
C93 C 0.3049(7) 0.8489(5) 0.8381(4) 0.0487(18) Uani 1 1 d . U . . .
H93A H 0.253216 0.865115 0.801364 0.058 Uiso 1 1 calc R U . . .
C94 C 0.2585(6) 0.8289(5) 0.9167(4) 0.0391(16) Uani 1 1 d . U . . .
O95 O 0.3129(4) 0.8081(3) 0.9718(3) 0.0348(10) Uani 1 1 d . U . . .
C96 C 0.4663(6) 0.8723(5) 0.7248(4) 0.0471(17) Uani 1 1 d D U . . .
C97 C 0.1260(6) 0.8386(5) 0.9379(5) 0.0467(17) Uani 1 1 d . U . . .
F91A F 0.5438(19) 0.9170(17) 0.7110(14) 0.115(8) Uani 0.6 1 d D U P D 1
F92A F 0.3775(11) 0.9132(13) 0.6877(7) 0.105(5) Uani 0.6 1 d D U P D 1
F93A F 0.5144(19) 0.8023(10) 0.6917(11) 0.089(5) Uani 0.6 1 d D U P D 1
F91B F 0.456(3) 0.825(2) 0.6783(17) 0.123(12) Uani 0.4 1 d D U P D 2
F92B F 0.5776(16) 0.872(2) 0.704(2) 0.124(12) Uani 0.4 1 d D U P D 2
F93B F 0.413(3) 0.9543(11) 0.7070(15) 0.152(13) Uani 0.4 1 d D U P D 2
F94 F 0.1023(5) 0.7663(4) 0.9875(4) 0.103(2) Uani 1 1 d . U . . .
F95 F 0.0685(4) 0.9065(4) 0.9762(4) 0.0917(19) Uani 1 1 d . U . . .
F96 F 0.0710(4) 0.8436(5) 0.8825(3) 0.0967(19) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O21 2.415(4) . ?
Pr1 O31 2.433(4) . ?
Pr1 O45 2.433(4) . ?
Pr1 O35 2.437(4) . ?
Pr1 O25 2.448(4) . ?
Pr1 O41 2.458(4) . ?
Pr1 N1 2.611(5) . ?
Pr1 N12 2.626(5) . ?
N1 C2 1.344(8) . ?
N1 C6 1.351(8) . ?
C2 C3 1.389(9) . ?
C2 H2A 0.9500 . ?
C3 C4 1.362(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.391(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.371(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.493(9) . ?
C7 N12 1.353(8) . ?
C7 C8 1.385(9) . ?
C8 C9 1.369(10) . ?
C8 H8A 0.9500 . ?
C9 C10 1.367(11) . ?
C9 H9A 0.9500 . ?
C10 C11 1.369(9) . ?
C10 H10A 0.9500 . ?
C11 N12 1.348(8) . ?
C11 H11A 0.9500 . ?
O21 C22 1.248(8) . ?
C22 C23 1.390(9) . ?
C22 C26 1.523(9) . ?
C23 C24 1.374(9) . ?
C23 H23A 0.9500 . ?
C24 O25 1.260(7) . ?
C24 C27 1.530(9) . ?
C26 F21 1.283(9) . ?
C26 F23 1.312(9) . ?
C26 F22 1.330(9) . ?
C27 F26 1.288(8) . ?
C27 F25 1.316(8) . ?
C27 F24 1.335(9) . ?
O31 C32 1.263(7) . ?
C32 C33 1.385(9) . ?
C32 C36 1.520(9) . ?
C33 C34 1.392(9) . ?
C33 H33A 0.9500 . ?
C34 O35 1.254(8) . ?
C34 C37 1.536(9) . ?
C36 F33A 1.291(13) . ?
C36 F33B 1.292(13) . ?
C36 F32A 1.308(11) . ?
C36 F31B 1.319(12) . ?
C36 F32B 1.321(12) . ?
C36 F31A 1.338(11) . ?
C37 F36 1.277(9) . ?
C37 F35 1.302(8) . ?
C37 F34 1.323(9) . ?
O41 C42 1.251(8) . ?
C42 C43 1.394(10) . ?
C42 C46 1.526(10) . ?
C43 C44 1.374(10) . ?
C43 H43A 0.9500 . ?
C44 O45 1.248(8) . ?
C44 C47 1.526(10) . ?
C46 F42A 1.265(11) . ?
C46 F42B 1.266(13) . ?
C46 F43B 1.274(12) . ?
C46 F43A 1.280(11) . ?
C46 F41B 1.315(13) . ?
C46 F41A 1.326(10) . ?
C47 F45 1.308(9) . ?
C47 F44 1.316(9) . ?
C47 F46 1.327(9) . ?
Pr2 O71 2.425(4) . ?
Pr2 O85 2.425(4) . ?
Pr2 O75 2.429(4) . ?
Pr2 O81 2.440(4) . ?
Pr2 O95 2.450(4) . ?
Pr2 O91 2.450(4) . ?
Pr2 N62 2.607(5) . ?
Pr2 N51 2.608(5) . ?
N51 C56 1.346(8) . ?
N51 C52 1.349(8) . ?
C52 C53 1.395(9) . ?
C52 H52A 0.9500 . ?
C53 C54 1.355(10) . ?
C53 H53A 0.9500 . ?
C54 C55 1.377(10) . ?
C54 H54A 0.9500 . ?
C55 C56 1.376(9) . ?
C55 H55A 0.9500 . ?
C56 C57 1.484(9) . ?
C57 N62 1.359(8) . ?
C57 C58 1.386(9) . ?
C58 C59 1.391(9) . ?
C58 H58A 0.9500 . ?
C59 C60 1.352(9) . ?
C59 H59A 0.9500 . ?
C60 C61 1.382(8) . ?
C60 H60A 0.9500 . ?
C61 N62 1.333(8) . ?
C61 H61A 0.9500 . ?
O71 C72 1.248(8) . ?
C72 C73 1.394(10) . ?
C72 C76 1.518(10) . ?
C73 C74 1.380(9) . ?
C73 H73A 0.9500 . ?
C74 O75 1.253(7) . ?
C74 C77 1.519(9) . ?
C76 F72 1.302(9) . ?
C76 F73 1.325(8) . ?
C76 F71 1.342(9) . ?
C77 F74 1.268(8) . ?
C77 F75 1.307(8) . ?
C77 F76 1.316(9) . ?
O81 C82 1.264(8) . ?
C82 C83 1.371(10) . ?
C82 C86 1.534(10) . ?
C83 C84 1.381(10) . ?
C83 H83A 0.9500 . ?
C84 O85 1.258(7) . ?
C84 C87 1.518(10) . ?
C86 F82A 1.282(13) . ?
C86 F81B 1.292(14) . ?
C86 F83B 1.296(14) . ?
C86 F83A 1.296(13) . ?
C86 F81A 1.301(13) . ?
C86 F82B 1.301(13) . ?
C87 F86 1.258(10) . ?
C87 F85 1.304(9) . ?
C87 F84 1.313(10) . ?
O91 C92 1.258(8) . ?
C92 C93 1.392(10) . ?
C92 C96 1.531(10) . ?
C93 C94 1.393(10) . ?
C93 H93A 0.9500 . ?
C94 O95 1.239(8) . ?
C94 C97 1.508(9) . ?
C96 F91B 1.266(14) . ?
C96 F93A 1.277(11) . ?
C96 F91A 1.279(12) . ?
C96 F93B 1.278(13) . ?
C96 F92B 1.293(14) . ?
C96 F92A 1.315(10) . ?
C97 F96 1.285(9) . ?
C97 F95 1.315(9) . ?
C97 F94 1.360(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O21 Pr1 O31 118.28(15) . . ?
O21 Pr1 O45 143.22(15) . . ?
O31 Pr1 O45 77.39(15) . . ?
O21 Pr1 O35 79.84(15) . . ?
O31 Pr1 O35 70.40(14) . . ?
O45 Pr1 O35 74.76(15) . . ?
O21 Pr1 O25 69.94(14) . . ?
O31 Pr1 O25 82.42(14) . . ?
O45 Pr1 O25 146.75(14) . . ?
O35 Pr1 O25 122.48(15) . . ?
O21 Pr1 O41 142.47(15) . . ?
O31 Pr1 O41 78.01(14) . . ?
O45 Pr1 O41 70.11(15) . . ?
O35 Pr1 O41 136.81(15) . . ?
O25 Pr1 O41 80.09(15) . . ?
O21 Pr1 N1 76.24(16) . . ?
O31 Pr1 N1 151.33(14) . . ?
O45 Pr1 N1 106.24(16) . . ?
O35 Pr1 N1 138.26(15) . . ?
O25 Pr1 N1 80.02(15) . . ?
O41 Pr1 N1 76.78(15) . . ?
O21 Pr1 N12 71.49(16) . . ?
O31 Pr1 N12 144.22(15) . . ?
O45 Pr1 N12 77.67(15) . . ?
O35 Pr1 N12 78.55(15) . . ?
O25 Pr1 N12 130.61(15) . . ?
O41 Pr1 N12 116.36(16) . . ?
N1 Pr1 N12 61.65(16) . . ?
C2 N1 C6 118.6(5) . . ?
C2 N1 Pr1 118.8(4) . . ?
C6 N1 Pr1 121.7(4) . . ?
N1 C2 C3 122.5(6) . . ?
N1 C2 H2A 118.8 . . ?
C3 C2 H2A 118.8 . . ?
C4 C3 C2 118.9(6) . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C3 C4 C5 118.6(6) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
C6 C5 C4 120.4(6) . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
N1 C6 C5 120.9(6) . . ?
N1 C6 C7 115.9(5) . . ?
C5 C6 C7 123.1(6) . . ?
N12 C7 C8 121.0(6) . . ?
N12 C7 C6 116.3(5) . . ?
C8 C7 C6 122.7(6) . . ?
C9 C8 C7 120.3(7) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 119.1(7) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
C9 C10 C11 118.4(7) . . ?
C9 C10 H10A 120.8 . . ?
C11 C10 H10A 120.8 . . ?
N12 C11 C10 123.8(7) . . ?
N12 C11 H11A 118.1 . . ?
C10 C11 H11A 118.1 . . ?
C11 N12 C7 117.3(5) . . ?
C11 N12 Pr1 120.4(4) . . ?
C7 N12 Pr1 120.3(4) . . ?
C22 O21 Pr1 134.4(4) . . ?
O21 C22 C23 127.9(6) . . ?
O21 C22 C26 113.2(6) . . ?
C23 C22 C26 118.9(6) . . ?
C24 C23 C22 121.4(6) . . ?
C24 C23 H23A 119.3 . . ?
C22 C23 H23A 119.3 . . ?
O25 C24 C23 127.8(6) . . ?
O25 C24 C27 114.0(6) . . ?
C23 C24 C27 118.2(6) . . ?
C24 O25 Pr1 134.4(4) . . ?
F21 C26 F23 107.8(7) . . ?
F21 C26 F22 106.1(7) . . ?
F23 C26 F22 104.2(7) . . ?
F21 C26 C22 113.3(6) . . ?
F23 C26 C22 111.2(6) . . ?
F22 C26 C22 113.6(6) . . ?
F26 C27 F25 108.3(7) . . ?
F26 C27 F24 105.6(7) . . ?
F25 C27 F24 104.9(6) . . ?
F26 C27 C24 112.8(6) . . ?
F25 C27 C24 114.1(6) . . ?
F24 C27 C24 110.6(6) . . ?
C32 O31 Pr1 132.0(4) . . ?
O31 C32 C33 128.7(6) . . ?
O31 C32 C36 113.8(6) . . ?
C33 C32 C36 117.5(6) . . ?
C32 C33 C34 120.9(6) . . ?
C32 C33 H33A 119.6 . . ?
C34 C33 H33A 119.6 . . ?
O35 C34 C33 128.3(6) . . ?
O35 C34 C37 115.7(6) . . ?
C33 C34 C37 116.0(6) . . ?
C34 O35 Pr1 132.8(4) . . ?
F33A C36 F32A 106.1(17) . . ?
F33B C36 F31B 108.0(18) . . ?
F33B C36 F32B 114.5(15) . . ?
F31B C36 F32B 100.6(16) . . ?
F33A C36 F31A 109.7(14) . . ?
F32A C36 F31A 98.9(12) . . ?
F33A C36 C32 119.9(14) . . ?
F33B C36 C32 117.1(13) . . ?
F32A C36 C32 110.0(11) . . ?
F31B C36 C32 109.2(14) . . ?
F32B C36 C32 106.1(10) . . ?
F31A C36 C32 110.1(9) . . ?
F36 C37 F35 108.5(7) . . ?
F36 C37 F34 106.1(7) . . ?
F35 C37 F34 104.9(7) . . ?
F36 C37 C34 111.2(7) . . ?
F35 C37 C34 112.8(6) . . ?
F34 C37 C34 112.9(6) . . ?
C42 O41 Pr1 133.2(4) . . ?
O41 C42 C43 126.8(6) . . ?
O41 C42 C46 115.7(6) . . ?
C43 C42 C46 117.5(6) . . ?
C44 C43 C42 122.7(6) . . ?
C44 C43 H43A 118.6 . . ?
C42 C43 H43A 118.6 . . ?
O45 C44 C43 127.9(6) . . ?
O45 C44 C47 113.4(6) . . ?
C43 C44 C47 118.7(6) . . ?
C44 O45 Pr1 132.7(4) . . ?
F42B C46 F43B 114(2) . . ?
F42A C46 F43A 109.5(14) . . ?
F42B C46 F41B 101.9(17) . . ?
F43B C46 F41B 101.8(17) . . ?
F42A C46 F41A 107.6(11) . . ?
F43A C46 F41A 103.7(10) . . ?
F42A C46 C42 112.6(9) . . ?
F42B C46 C42 112.4(15) . . ?
F43B C46 C42 113.3(11) . . ?
F43A C46 C42 109.4(9) . . ?
F41B C46 C42 112.5(10) . . ?
F41A C46 C42 113.6(8) . . ?
F45 C47 F44 110.6(7) . . ?
F45 C47 F46 105.0(6) . . ?
F44 C47 F46 104.7(6) . . ?
F45 C47 C44 111.5(6) . . ?
F44 C47 C44 111.1(6) . . ?
F46 C47 C44 113.6(7) . . ?
O71 Pr2 O85 78.92(15) . . ?
O71 Pr2 O75 70.63(14) . . ?
O85 Pr2 O75 120.45(15) . . ?
O71 Pr2 O81 119.73(15) . . ?
O85 Pr2 O81 69.93(14) . . ?
O75 Pr2 O81 82.59(14) . . ?
O71 Pr2 O95 73.72(15) . . ?
O85 Pr2 O95 139.00(14) . . ?
O75 Pr2 O95 78.10(14) . . ?
O81 Pr2 O95 150.91(15) . . ?
O71 Pr2 O91 134.45(15) . . ?
O85 Pr2 O91 146.07(14) . . ?
O75 Pr2 O91 75.78(14) . . ?
O81 Pr2 O91 84.44(15) . . ?
O95 Pr2 O91 69.91(14) . . ?
O71 Pr2 N62 142.32(15) . . ?
O85 Pr2 N62 76.81(15) . . ?
O75 Pr2 N62 147.03(14) . . ?
O81 Pr2 N62 77.66(15) . . ?
O95 Pr2 N62 107.96(15) . . ?
O91 Pr2 N62 76.25(15) . . ?
O71 Pr2 N51 82.61(15) . . ?
O85 Pr2 N51 69.74(15) . . ?
O75 Pr2 N51 147.49(14) . . ?
O81 Pr2 N51 127.90(15) . . ?
O95 Pr2 N51 76.88(15) . . ?
O91 Pr2 N51 113.91(16) . . ?
N62 Pr2 N51 62.11(15) . . ?
C56 N51 C52 118.5(6) . . ?
C56 N51 Pr2 121.1(4) . . ?
C52 N51 Pr2 118.8(4) . . ?
N51 C52 C53 122.5(7) . . ?
N51 C52 H52A 118.7 . . ?
C53 C52 H52A 118.7 . . ?
C54 C53 C52 118.2(6) . . ?
C54 C53 H53A 120.9 . . ?
C52 C53 H53A 120.9 . . ?
C53 C54 C55 119.6(7) . . ?
C53 C54 H54A 120.2 . . ?
C55 C54 H54A 120.2 . . ?
C54 C55 C56 120.3(7) . . ?
C54 C55 H55A 119.9 . . ?
C56 C55 H55A 119.9 . . ?
N51 C56 C55 120.9(6) . . ?
N51 C56 C57 116.2(5) . . ?
C55 C56 C57 122.9(6) . . ?
N62 C57 C58 120.1(6) . . ?
N62 C57 C56 116.7(5) . . ?
C58 C57 C56 123.1(6) . . ?
C57 C58 C59 119.8(6) . . ?
C57 C58 H58A 120.1 . . ?
C59 C58 H58A 120.1 . . ?
C60 C59 C58 119.4(6) . . ?
C60 C59 H59A 120.3 . . ?
C58 C59 H59A 120.3 . . ?
C59 C60 C61 118.8(6) . . ?
C59 C60 H60A 120.6 . . ?
C61 C60 H60A 120.6 . . ?
N62 C61 C60 122.9(6) . . ?
N62 C61 H61A 118.6 . . ?
C60 C61 H61A 118.6 . . ?
C61 N62 C57 119.0(5) . . ?
C61 N62 Pr2 119.5(4) . . ?
C57 N62 Pr2 120.5(4) . . ?
C72 O71 Pr2 133.2(4) . . ?
O71 C72 C73 128.5(6) . . ?
O71 C72 C76 116.4(6) . . ?
C73 C72 C76 115.0(6) . . ?
C74 C73 C72 121.1(6) . . ?
C74 C73 H73A 119.4 . . ?
C72 C73 H73A 119.4 . . ?
O75 C74 C73 128.2(6) . . ?
O75 C74 C77 113.9(6) . . ?
C73 C74 C77 117.9(6) . . ?
C74 O75 Pr2 132.8(4) . . ?
F72 C76 F73 106.2(6) . . ?
F72 C76 F71 107.1(7) . . ?
F73 C76 F71 104.8(7) . . ?
F72 C76 C72 113.5(7) . . ?
F73 C76 C72 112.1(6) . . ?
F71 C76 C72 112.5(6) . . ?
F74 C77 F75 106.2(6) . . ?
F74 C77 F76 109.6(7) . . ?
F75 C77 F76 101.2(7) . . ?
F74 C77 C74 116.1(6) . . ?
F75 C77 C74 114.5(6) . . ?
F76 C77 C74 108.2(6) . . ?
C82 O81 Pr2 134.4(4) . . ?
O81 C82 C83 127.5(6) . . ?
O81 C82 C86 113.7(6) . . ?
C83 C82 C86 118.8(6) . . ?
C82 C83 C84 122.6(6) . . ?
C82 C83 H83A 118.7 . . ?
C84 C83 H83A 118.7 . . ?
O85 C84 C83 126.8(7) . . ?
O85 C84 C87 113.4(6) . . ?
C83 C84 C87 119.8(6) . . ?
C84 O85 Pr2 134.6(4) . . ?
F81B C86 F83B 107(2) . . ?
F82A C86 F83A 107.7(17) . . ?
F82A C86 F81A 109(2) . . ?
F83A C86 F81A 105.7(17) . . ?
F81B C86 F82B 107.5(19) . . ?
F83B C86 F82B 104(2) . . ?
F82A C86 C82 112.9(12) . . ?
F81B C86 C82 113.5(15) . . ?
F83B C86 C82 109.1(18) . . ?
F83A C86 C82 109.1(13) . . ?
F81A C86 C82 112.4(16) . . ?
F82B C86 C82 115.6(18) . . ?
F86 C87 F85 108.6(7) . . ?
F86 C87 F84 104.8(8) . . ?
F85 C87 F84 102.2(8) . . ?
F86 C87 C84 114.8(7) . . ?
F85 C87 C84 114.5(7) . . ?
F84 C87 C84 110.9(6) . . ?
C92 O91 Pr2 132.5(4) . . ?
O91 C92 C93 128.3(7) . . ?
O91 C92 C96 114.1(6) . . ?
C93 C92 C96 117.7(6) . . ?
C94 C93 C92 121.7(7) . . ?
C94 C93 H93A 119.1 . . ?
C92 C93 H93A 119.1 . . ?
O95 C94 C93 127.2(7) . . ?
O95 C94 C97 116.1(6) . . ?
C93 C94 C97 116.6(6) . . ?
C94 O95 Pr2 133.2(4) . . ?
F93A C96 F91A 107.1(14) . . ?
F91B C96 F93B 110.7(19) . . ?
F91B C96 F92B 102(2) . . ?
F93B C96 F92B 103(2) . . ?
F93A C96 F92A 102.2(11) . . ?
F91A C96 F92A 111.3(15) . . ?
F91B C96 C92 117.6(18) . . ?
F93A C96 C92 109.7(11) . . ?
F91A C96 C92 112.7(13) . . ?
F93B C96 C92 108.0(13) . . ?
F92B C96 C92 115.2(19) . . ?
F92A C96 C92 113.1(8) . . ?
F96 C97 F95 107.5(6) . . ?
F96 C97 F94 102.9(6) . . ?
F95 C97 F94 104.3(7) . . ?
F96 C97 C94 117.5(7) . . ?
F95 C97 C94 112.7(6) . . ?
F94 C97 C94 110.7(6) . . ?

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
C6 N1 C2 C3 -1.0(9) . . . . ?
Pr1 N1 C2 C3 168.8(5) . . . . ?
N1 C2 C3 C4 0.1(10) . . . . ?
C2 C3 C4 C5 1.0(11) . . . . ?
C3 C4 C5 C6 -1.4(11) . . . . ?
C2 N1 C6 C5 0.6(10) . . . . ?
Pr1 N1 C6 C5 -168.9(5) . . . . ?
C2 N1 C6 C7 -177.9(6) . . . . ?
Pr1 N1 C6 C7 12.6(8) . . . . ?
C4 C5 C6 N1 0.6(11) . . . . ?
C4 C5 C6 C7 179.0(6) . . . . ?
N1 C6 C7 N12 4.6(9) . . . . ?
C5 C6 C7 N12 -173.8(6) . . . . ?
N1 C6 C7 C8 -176.7(6) . . . . ?
C5 C6 C7 C8 4.9(11) . . . . ?
N12 C7 C8 C9 -0.3(11) . . . . ?
C6 C7 C8 C9 -179.0(7) . . . . ?
C7 C8 C9 C10 2.6(11) . . . . ?
C8 C9 C10 C11 -2.3(11) . . . . ?
C9 C10 C11 N12 -0.3(11) . . . . ?
C10 C11 N12 C7 2.6(10) . . . . ?
C10 C11 N12 Pr1 -161.4(6) . . . . ?
C8 C7 N12 C11 -2.2(9) . . . . ?
C6 C7 N12 C11 176.5(6) . . . . ?
C8 C7 N12 Pr1 161.8(5) . . . . ?
C6 C7 N12 Pr1 -19.5(7) . . . . ?
Pr1 O21 C22 C23 21.2(11) . . . . ?
Pr1 O21 C22 C26 -159.2(5) . . . . ?
O21 C22 C23 C24 -1.4(11) . . . . ?
C26 C22 C23 C24 179.1(7) . . . . ?
C22 C23 C24 O25 -4.5(11) . . . . ?
C22 C23 C24 C27 176.5(6) . . . . ?
C23 C24 O25 Pr1 -9.1(11) . . . . ?
C27 C24 O25 Pr1 169.9(4) . . . . ?
O21 C22 C26 F21 -59.5(9) . . . . ?
C23 C22 C26 F21 120.0(8) . . . . ?
O21 C22 C26 F23 62.1(9) . . . . ?
C23 C22 C26 F23 -118.3(8) . . . . ?
O21 C22 C26 F22 179.2(7) . . . . ?
C23 C22 C26 F22 -1.2(10) . . . . ?
O25 C24 C27 F26 59.7(9) . . . . ?
C23 C24 C27 F26 -121.2(8) . . . . ?
O25 C24 C27 F25 -176.3(6) . . . . ?
C23 C24 C27 F25 2.8(10) . . . . ?
O25 C24 C27 F24 -58.4(8) . . . . ?
C23 C24 C27 F24 120.7(7) . . . . ?
Pr1 O31 C32 C33 24.0(10) . . . . ?
Pr1 O31 C32 C36 -153.7(4) . . . . ?
O31 C32 C33 C34 -4.1(11) . . . . ?
C36 C32 C33 C34 173.5(6) . . . . ?
C32 C33 C34 O35 2.6(12) . . . . ?
C32 C33 C34 C37 -175.9(7) . . . . ?
C33 C34 O35 Pr1 -21.3(11) . . . . ?
C37 C34 O35 Pr1 157.3(5) . . . . ?
O31 C32 C36 F33A 167.8(16) . . . . ?
C33 C32 C36 F33A -10.1(18) . . . . ?
O31 C32 C36 F33B -45.3(15) . . . . ?
C33 C32 C36 F33B 136.8(15) . . . . ?
O31 C32 C36 F32A -68.8(12) . . . . ?
C33 C32 C36 F32A 113.2(12) . . . . ?
O31 C32 C36 F31B -168.4(16) . . . . ?
C33 C32 C36 F31B 13.6(17) . . . . ?
O31 C32 C36 F32B 83.9(13) . . . . ?
C33 C32 C36 F32B -94.0(13) . . . . ?
O31 C32 C36 F31A 39.1(12) . . . . ?
C33 C32 C36 F31A -138.8(11) . . . . ?
O35 C34 C37 F36 -116.2(8) . . . . ?
C33 C34 C37 F36 62.5(9) . . . . ?
O35 C34 C37 F35 121.6(7) . . . . ?
C33 C34 C37 F35 -59.7(9) . . . . ?
O35 C34 C37 F34 2.9(10) . . . . ?
C33 C34 C37 F34 -178.4(7) . . . . ?
Pr1 O41 C42 C43 -15.1(10) . . . . ?
Pr1 O41 C42 C46 165.9(4) . . . . ?
O41 C42 C43 C44 -5.1(11) . . . . ?
C46 C42 C43 C44 173.9(6) . . . . ?
C42 C43 C44 O45 1.3(12) . . . . ?
C42 C43 C44 C47 -177.1(6) . . . . ?
C43 C44 O45 Pr1 22.7(10) . . . . ?
C47 C44 O45 Pr1 -158.8(4) . . . . ?
O41 C42 C46 F42A -57.1(16) . . . . ?
C43 C42 C46 F42A 123.7(15) . . . . ?
O41 C42 C46 F42B 106.3(19) . . . . ?
C43 C42 C46 F42B -73(2) . . . . ?
O41 C42 C46 F43B -123(2) . . . . ?
C43 C42 C46 F43B 58(3) . . . . ?
O41 C42 C46 F43A 64.9(12) . . . . ?
C43 C42 C46 F43A -114.3(12) . . . . ?
O41 C42 C46 F41B -8.1(16) . . . . ?
C43 C42 C46 F41B 172.7(15) . . . . ?
O41 C42 C46 F41A -179.8(11) . . . . ?
C43 C42 C46 F41A 1.1(13) . . . . ?
O45 C44 C47 F45 50.3(9) . . . . ?
C43 C44 C47 F45 -131.0(8) . . . . ?
O45 C44 C47 F44 -73.6(8) . . . . ?
C43 C44 C47 F44 105.1(8) . . . . ?
O45 C44 C47 F46 168.7(6) . . . . ?
C43 C44 C47 F46 -12.6(9) . . . . ?
C56 N51 C52 C53 -0.8(10) . . . . ?
Pr2 N51 C52 C53 164.8(5) . . . . ?
N51 C52 C53 C54 -0.6(11) . . . . ?
C52 C53 C54 C55 1.4(11) . . . . ?
C53 C54 C55 C56 -0.9(11) . . . . ?
C52 N51 C56 C55 1.4(9) . . . . ?
Pr2 N51 C56 C55 -163.9(5) . . . . ?
C52 N51 C56 C57 -179.3(5) . . . . ?
Pr2 N51 C56 C57 15.4(7) . . . . ?
C54 C55 C56 N51 -0.6(10) . . . . ?
C54 C55 C56 C57 -179.8(6) . . . . ?
N51 C56 C57 N62 -0.9(8) . . . . ?
C55 C56 C57 N62 178.4(6) . . . . ?
N51 C56 C57 C58 177.7(6) . . . . ?
C55 C56 C57 C58 -3.0(10) . . . . ?
N62 C57 C58 C59 -0.9(10) . . . . ?
C56 C57 C58 C59 -179.4(6) . . . . ?
C57 C58 C59 C60 1.6(11) . . . . ?
C58 C59 C60 C61 -0.5(11) . . . . ?
C59 C60 C61 N62 -1.4(10) . . . . ?
C60 C61 N62 C57 2.1(9) . . . . ?
C60 C61 N62 Pr2 -166.4(5) . . . . ?
C58 C57 N62 C61 -1.0(9) . . . . ?
C56 C57 N62 C61 177.7(5) . . . . ?
C58 C57 N62 Pr2 167.5(5) . . . . ?
C56 C57 N62 Pr2 -13.9(7) . . . . ?
Pr2 O71 C72 C73 17.3(11) . . . . ?
Pr2 O71 C72 C76 -159.3(5) . . . . ?
O71 C72 C73 C74 -1.3(12) . . . . ?
C76 C72 C73 C74 175.4(6) . . . . ?
C72 C73 C74 O75 4.0(12) . . . . ?
C72 C73 C74 C77 -175.1(7) . . . . ?
C73 C74 O75 Pr2 -22.5(10) . . . . ?
C77 C74 O75 Pr2 156.6(4) . . . . ?
O71 C72 C76 F72 120.9(8) . . . . ?
C73 C72 C76 F72 -56.1(9) . . . . ?
O71 C72 C76 F73 -118.7(7) . . . . ?
C73 C72 C76 F73 64.2(9) . . . . ?
O71 C72 C76 F71 -0.9(10) . . . . ?
C73 C72 C76 F71 -178.0(7) . . . . ?
O75 C74 C77 F74 49.5(9) . . . . ?
C73 C74 C77 F74 -131.3(7) . . . . ?
O75 C74 C77 F75 173.9(6) . . . . ?
C73 C74 C77 F75 -7.0(10) . . . . ?
O75 C74 C77 F76 -74.1(8) . . . . ?
C73 C74 C77 F76 105.1(8) . . . . ?
Pr2 O81 C82 C83 9.3(11) . . . . ?
Pr2 O81 C82 C86 -168.4(4) . . . . ?
O81 C82 C83 C84 5.7(12) . . . . ?
C86 C82 C83 C84 -176.7(6) . . . . ?
C82 C83 C84 O85 -0.6(12) . . . . ?
C82 C83 C84 C87 178.9(7) . . . . ?
C83 C84 O85 Pr2 -19.6(11) . . . . ?
C87 C84 O85 Pr2 160.8(5) . . . . ?
O81 C82 C86 F82A -51(2) . . . . ?
C83 C82 C86 F82A 131(2) . . . . ?
O81 C82 C86 F81B 37.7(18) . . . . ?
C83 C82 C86 F81B -140.3(17) . . . . ?
O81 C82 C86 F83B -81(2) . . . . ?
C83 C82 C86 F83B 101(2) . . . . ?
O81 C82 C86 F83A 68.2(14) . . . . ?
C83 C82 C86 F83A -109.8(14) . . . . ?
O81 C82 C86 F81A -174.9(15) . . . . ?
C83 C82 C86 F81A 7.2(17) . . . . ?
O81 C82 C86 F82B 162.5(17) . . . . ?
C83 C82 C86 F82B -15.5(19) . . . . ?
O85 C84 C87 F86 63.6(10) . . . . ?
C83 C84 C87 F86 -116.0(9) . . . . ?
O85 C84 C87 F85 -169.8(7) . . . . ?
C83 C84 C87 F85 10.6(11) . . . . ?
O85 C84 C87 F84 -54.9(10) . . . . ?
C83 C84 C87 F84 125.5(8) . . . . ?
Pr2 O91 C92 C93 17.1(11) . . . . ?
Pr2 O91 C92 C96 -162.6(4) . . . . ?
O91 C92 C93 C94 2.6(12) . . . . ?
C96 C92 C93 C94 -177.7(7) . . . . ?
C92 C93 C94 O95 1.1(12) . . . . ?
C92 C93 C94 C97 177.5(7) . . . . ?
C93 C94 O95 Pr2 -24.8(11) . . . . ?
C97 C94 O95 Pr2 158.8(5) . . . . ?
O91 C92 C96 F91B 117(2) . . . . ?
C93 C92 C96 F91B -63(2) . . . . ?
O91 C92 C96 F93A 80.1(12) . . . . ?
C93 C92 C96 F93A -99.6(12) . . . . ?
O91 C92 C96 F91A -39.1(16) . . . . ?
C93 C92 C96 F91A 141.1(15) . . . . ?
O91 C92 C96 F93B -117(2) . . . . ?
C93 C92 C96 F93B 63(2) . . . . ?
O91 C92 C96 F92B -3(2) . . . . ?
C93 C92 C96 F92B 177.2(19) . . . . ?
O91 C92 C96 F92A -166.5(12) . . . . ?
C93 C92 C96 F92A 13.8(14) . . . . ?
O95 C94 C97 F96 -167.2(7) . . . . ?
C93 C94 C97 F96 16.0(10) . . . . ?
O95 C94 C97 F95 66.9(9) . . . . ?
C93 C94 C97 F95 -109.9(8) . . . . ?
O95 C94 C97 F94 -49.5(9) . . . . ?
C93 C94 C97 F94 133.7(7) . . . . ?

_refine_diff_density_max         1.907
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.131


# start Validation Reply Form
_vrf_PLAT910_k10268              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: Presumably due to issues at the data collection stage 
;
# end Validation Reply Form

_chemical_properties_physical    Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_two
_database_code_depnum_ccdc_archive 'CCDC 1856933'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H19 F18 N4 Nd O6'
_chemical_formula_sum            'C35 H19 F18 N4 Nd O6'
_chemical_formula_weight         1077.78

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   21.7670(2)
_cell_length_b                   11.76298(8)
_cell_length_c                   18.04081(18)
_cell_angle_alpha                90
_cell_angle_beta                 118.8228(13)
_cell_angle_gamma                90
_cell_volume                     4047.00(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    40465
_cell_measurement_theta_min      3.3022
_cell_measurement_theta_max      32.7120

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             2108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.415
_shelx_estimated_absorpt_T_min   0.601
_shelx_estimated_absorpt_T_max   0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3693
_diffrn_reflns_number            35909
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.309
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3573
_reflns_number_gt                3488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+11.5700P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3573
_refine_ls_number_parameters     374
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0579
_refine_ls_wR_factor_gt          0.0573
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd Nd 0.500000 0.80660(2) 0.750000 0.02637(7) Uani 1 2 d S TU P A .
N1 N 0.52250(11) 0.85257(18) 0.90939(13) 0.0339(5) Uani 1 1 d . U . . .
C2 C 0.58821(15) 0.8645(2) 0.97195(17) 0.0389(6) Uani 1 1 d . U . . .
H2A H 0.624687 0.869550 0.957444 0.047 Uiso 1 1 calc R U . . .
C3 C 0.60630(17) 0.8700(2) 1.05669(18) 0.0456(7) Uani 1 1 d . U . . .
H3A H 0.653730 0.878702 1.099342 0.055 Uiso 1 1 calc R U . . .
C4 C 0.55293(19) 0.8623(3) 1.07682(19) 0.0540(8) Uani 1 1 d . U . . .
H4A H 0.563110 0.864737 1.134269 0.065 Uiso 1 1 calc R U . . .
C5 C 0.48538(18) 0.8512(3) 1.01381(19) 0.0494(7) Uani 1 1 d . U . . .
H5A H 0.448351 0.846164 1.027346 0.059 Uiso 1 1 calc R U . . .
C6 C 0.47062(15) 0.8473(2) 0.92988(17) 0.0366(6) Uani 1 1 d . U . . .
C7 C 0.39789(15) 0.8429(2) 0.85842(18) 0.0386(6) Uani 1 1 d . U . . .
C8 C 0.33956(18) 0.8422(3) 0.8711(2) 0.0599(9) Uani 1 1 d . U . . .
H8A H 0.345513 0.838751 0.926813 0.072 Uiso 1 1 calc R U . . .
C9 C 0.27320(18) 0.8465(3) 0.8023(3) 0.0662(10) Uani 1 1 d . U . . .
H9A H 0.233119 0.845876 0.810284 0.079 Uiso 1 1 calc R U . . .
C10 C 0.26556(16) 0.8515(3) 0.7229(2) 0.0561(8) Uani 1 1 d . U . . .
H10A H 0.220407 0.855860 0.674609 0.067 Uiso 1 1 calc R U . . .
C11 C 0.32538(14) 0.8503(3) 0.7148(2) 0.0479(7) Uani 1 1 d . U . . .
H11A H 0.320184 0.852926 0.659469 0.058 Uiso 1 1 calc R U . . .
N12 N 0.39045(11) 0.8454(2) 0.78057(15) 0.0383(5) Uani 1 1 d . U . . .
O21 O 0.53166(9) 0.63965(15) 0.69123(11) 0.0351(4) Uani 1 1 d . U . . .
C22A C 0.5030(2) 0.5568(3) 0.6472(2) 0.0392(8) Uani 0.74 1 d . U P A 1
C23A C 0.4315(2) 0.5349(3) 0.6051(3) 0.0538(11) Uani 0.74 1 d . U P A 1
H23A H 0.414881 0.466197 0.574005 0.065 Uiso 0.74 1 calc R U P A 1
C24A C 0.3842(3) 0.6101(5) 0.6073(3) 0.0429(12) Uani 0.74 1 d . U P A 1
C22B C 0.5636(5) 0.5579(8) 0.7162(6) 0.0334(19) Uani 0.26 1 d . U P A 3
C23B C 0.6115(5) 0.5329(9) 0.7997(7) 0.041(2) Uani 0.26 1 d . U P A 3
H23B H 0.633640 0.460521 0.813550 0.050 Uiso 0.26 1 calc R U P A 3
C24B C 0.6276(6) 0.6139(12) 0.8642(9) 0.033(3) Uani 0.26 1 d . U P A 3
O25 O 0.39480(9) 0.70724(15) 0.64250(11) 0.0357(4) Uani 1 1 d . U . . .
C26 C 0.55286(19) 0.4704(3) 0.6414(2) 0.0616(9) Uani 1 1 d D U . . .
C27 C 0.30893(19) 0.5760(3) 0.5562(2) 0.0727(11) Uani 1 1 d D U . . .
F21A F 0.5215(3) 0.4010(4) 0.5712(3) 0.1048(19) Uani 0.57 1 d D U P A 1
F22A F 0.5830(6) 0.3842(6) 0.6885(5) 0.134(3) Uani 0.57 1 d D U P A 1
F23A F 0.5992(5) 0.5198(9) 0.6250(8) 0.105(3) Uani 0.57 1 d D U P A 1
F21B F 0.5952(6) 0.4327(8) 0.7149(5) 0.113(4) Uani 0.43 1 d D U P A 2
F23B F 0.4980(6) 0.4191(14) 0.6053(8) 0.228(7) Uani 0.43 1 d D U P A 2
F22B F 0.5800(9) 0.5085(16) 0.6007(10) 0.134(6) Uani 0.43 1 d D U P A 2
F24A F 0.3027(9) 0.6229(13) 0.4864(5) 0.253(7) Uani 0.54 1 d D U P A 1
F25A F 0.2936(3) 0.4704(5) 0.5617(7) 0.121(3) Uani 0.54 1 d D U P A 1
F26A F 0.2603(4) 0.6323(9) 0.5599(12) 0.208(6) Uani 0.54 1 d D U P A 1
F24B F 0.2818(4) 0.5633(18) 0.6057(5) 0.173(6) Uani 0.46 1 d D U P A 2
F25B F 0.2710(3) 0.6338(10) 0.5000(6) 0.132(4) Uani 0.46 1 d D U P A 2
F26B F 0.3053(5) 0.4850(9) 0.5102(8) 0.155(4) Uani 0.46 1 d D U P A 2
O31 O 0.43083(9) 0.98342(15) 0.68649(11) 0.0353(4) Uani 1 1 d . U . . .
C32 C 0.43908(14) 1.0879(2) 0.69629(15) 0.0337(5) Uani 1 1 d . U . . .
C33 C 0.500000 1.1461(3) 0.750000 0.0398(8) Uani 1 2 d S TU P . .
H33A H 0.499999 1.226872 0.750000 0.060 Uiso 1 2 calc R U P . .
C34 C 0.37230(17) 1.1567(3) 0.64287(19) 0.0472(7) Uani 1 1 d . U . . .
F31 F 0.32936(15) 1.1489(3) 0.67388(18) 0.1156(12) Uani 1 1 d . U . . .
F32 F 0.38378(14) 1.26458(18) 0.63693(18) 0.1104(11) Uani 1 1 d . U . . .
F33 F 0.33841(10) 1.11897(18) 0.56454(12) 0.0663(5) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd O25 2.4675(17) . ?
Nd O25 2.4675(17) 2_656 ?
Nd O21 2.4820(17) . ?
Nd O21 2.4820(17) 2_656 ?
Nd O31 2.4985(17) 2_656 ?
Nd O31 2.4985(17) . ?
Nd N1 2.728(2) . ?
Nd N1 2.728(2) 2_656 ?
Nd N12 2.732(2) 2_656 ?
Nd N12 2.733(2) . ?
N1 C2 1.335(3) . ?
N1 C6 1.348(3) . ?
C2 C3 1.384(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.364(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.389(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.484(4) . ?
C7 N12 1.334(4) . ?
C7 C8 1.395(4) . ?
C8 C9 1.378(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.361(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.379(4) . ?
C10 H10A 0.9500 . ?
C11 N12 1.340(4) . ?
C11 H11A 0.9500 . ?
O21 C22B 1.143(10) . ?
O21 C22A 1.221(4) . ?
C22A C23A 1.388(6) . ?
C22A C26 1.527(5) . ?
C23A C24A 1.372(7) . ?
C23A H23A 0.9500 . ?
C24A O25 1.273(6) . ?
C24A C27 1.497(6) . ?
C22B C23B 1.390(14) . ?
C22B C26 1.621(10) . ?
C23B C24B 1.412(18) . ?
C23B H23B 0.9500 . ?
C24B O25 1.183(15) 2_656 ?
C24B C27 1.503(14) 2_656 ?
C26 F23B 1.211(8) . ?
C26 F22A 1.282(7) . ?
C26 F21B 1.275(8) . ?
C26 F22B 1.228(11) . ?
C26 F23A 1.316(8) . ?
C26 F21A 1.380(5) . ?
C27 F25B 1.167(7) . ?
C27 F24B 1.297(8) . ?
C27 F26A 1.278(9) . ?
C27 F25A 1.303(6) . ?
C27 F24A 1.320(9) . ?
C27 F26B 1.333(8) . ?
O31 C32 1.242(3) . ?
C32 C33 1.389(3) . ?
C32 C34 1.532(4) . ?
C33 H33A 0.9500 . ?
C34 F31 1.304(4) . ?
C34 F32 1.308(4) . ?
C34 F33 1.316(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
O25 Nd O25 123.46(8) . 2_656 ?
O25 Nd O21 68.47(6) . . ?
O25 Nd O21 67.50(6) 2_656 . ?
O25 Nd O21 67.50(6) . 2_656 ?
O25 Nd O21 68.47(6) 2_656 2_656 ?
O21 Nd O21 75.40(8) . 2_656 ?
O25 Nd O31 151.70(6) . 2_656 ?
O25 Nd O31 84.73(6) 2_656 2_656 ?
O21 Nd O31 128.65(6) . 2_656 ?
O21 Nd O31 133.85(6) 2_656 2_656 ?
O25 Nd O31 84.73(6) . . ?
O25 Nd O31 151.70(6) 2_656 . ?
O21 Nd O31 133.85(6) . . ?
O21 Nd O31 128.65(6) 2_656 . ?
O31 Nd O31 67.29(8) 2_656 . ?
O25 Nd N1 123.32(6) . . ?
O25 Nd N1 68.81(6) 2_656 . ?
O21 Nd N1 131.40(6) . . ?
O21 Nd N1 69.65(6) 2_656 . ?
O31 Nd N1 65.75(6) 2_656 . ?
O31 Nd N1 94.63(6) . . ?
O25 Nd N1 68.81(6) . 2_656 ?
O25 Nd N1 123.32(6) 2_656 2_656 ?
O21 Nd N1 69.65(6) . 2_656 ?
O21 Nd N1 131.40(6) 2_656 2_656 ?
O31 Nd N1 94.63(6) 2_656 2_656 ?
O31 Nd N1 65.75(6) . 2_656 ?
N1 Nd N1 157.14(9) . 2_656 ?
O25 Nd N12 119.34(6) . 2_656 ?
O25 Nd N12 70.63(7) 2_656 2_656 ?
O21 Nd N12 66.24(6) . 2_656 ?
O21 Nd N12 131.88(6) 2_656 2_656 ?
O31 Nd N12 64.01(6) 2_656 2_656 ?
O31 Nd N12 99.19(7) . 2_656 ?
N1 Nd N12 116.67(7) . 2_656 ?
N1 Nd N12 58.99(7) 2_656 2_656 ?
O25 Nd N12 70.63(7) . . ?
O25 Nd N12 119.34(6) 2_656 . ?
O21 Nd N12 131.88(7) . . ?
O21 Nd N12 66.24(6) 2_656 . ?
O31 Nd N12 99.19(6) 2_656 . ?
O31 Nd N12 64.01(6) . . ?
N1 Nd N12 58.99(7) . . ?
N1 Nd N12 116.67(7) 2_656 . ?
N12 Nd N12 160.75(10) 2_656 . ?
C2 N1 C6 118.1(2) . . ?
C2 N1 Nd 119.11(16) . . ?
C6 N1 Nd 122.10(17) . . ?
N1 C2 C3 123.8(3) . . ?
N1 C2 H2A 118.1 . . ?
C3 C2 H2A 118.1 . . ?
C4 C3 C2 117.5(3) . . ?
C4 C3 H3A 121.3 . . ?
C2 C3 H3A 121.3 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
N1 C6 C5 120.9(3) . . ?
N1 C6 C7 116.6(2) . . ?
C5 C6 C7 122.5(2) . . ?
N12 C7 C8 121.0(3) . . ?
N12 C7 C6 116.8(2) . . ?
C8 C7 C6 122.1(3) . . ?
C9 C8 C7 119.6(3) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C10 C9 C8 119.5(3) . . ?
C10 C9 H9A 120.3 . . ?
C8 C9 H9A 120.3 . . ?
C9 C10 C11 117.9(3) . . ?
C9 C10 H10A 121.0 . . ?
C11 C10 H10A 121.0 . . ?
N12 C11 C10 123.8(3) . . ?
N12 C11 H11A 118.1 . . ?
C10 C11 H11A 118.1 . . ?
C7 N12 C11 118.2(2) . . ?
C7 N12 Nd 122.26(17) . . ?
C11 N12 Nd 118.77(18) . . ?
C22B O21 Nd 137.6(5) . . ?
C22A O21 Nd 138.5(2) . . ?
O21 C22A C23A 126.3(4) . . ?
O21 C22A C26 114.7(3) . . ?
C23A C22A C26 119.0(3) . . ?
C24A C23A C22A 121.5(4) . . ?
C24A C23A H23A 119.2 . . ?
C22A C23A H23A 119.2 . . ?
O25 C24A C23A 129.5(4) . . ?
O25 C24A C27 115.4(4) . . ?
C23A C24A C27 115.0(4) . . ?
O21 C22B C23B 126.9(9) . . ?
O21 C22B C26 113.0(7) . . ?
C23B C22B C26 119.9(8) . . ?
C22B C23B C24B 120.6(10) . . ?
C22B C23B H23B 119.7 . . ?
C24B C23B H23B 119.7 . . ?
O25 C24B C23B 128.0(12) 2_656 . ?
O25 C24B C27 121.1(11) 2_656 2_656 ?
C24B O25 Nd 134.4(7) 2_656 . ?
C24A O25 Nd 133.9(3) . . ?
F23B C26 F21B 114.6(11) . . ?
F23B C26 F22B 119.6(11) . . ?
F21B C26 F22B 115.7(11) . . ?
F22A C26 F23A 107.2(8) . . ?
F22A C26 F21A 90.5(5) . . ?
F23A C26 F21A 98.5(6) . . ?
F22A C26 C22A 129.4(6) . . ?
F23A C26 C22A 111.7(6) . . ?
F21A C26 C22A 113.8(3) . . ?
F25B C27 F24B 107.3(8) . . ?
F26A C27 F25A 103.9(7) . . ?
F26A C27 F24A 97.3(10) . . ?
F25A C27 F24A 124.0(9) . . ?
F25B C27 F26B 97.1(9) . . ?
F24B C27 F26B 115.2(9) . . ?
F26A C27 C24A 121.2(6) . . ?
F25A C27 C24A 116.9(4) . . ?
F24A C27 C24A 93.1(7) . . ?
F26A C27 C24B 101.5(9) . 2_656 ?
F25A C27 C24B 111.2(7) . 2_656 ?
F24A C27 C24B 114.3(9) . 2_656 ?
C24A C27 C24B 26.2(4) . 2_656 ?
C32 O31 Nd 138.11(17) . . ?
O31 C32 C33 127.7(3) . . ?
O31 C32 C34 113.9(2) . . ?
C33 C32 C34 118.4(3) . . ?
C32 C33 C32 120.9(3) 2_656 . ?
C32 C33 H33A 119.6 2_656 . ?
C32 C33 H33A 119.6 . . ?
F31 C34 F32 108.0(3) . . ?
F31 C34 F33 106.9(3) . . ?
F32 C34 F33 105.6(3) . . ?
F31 C34 C32 110.6(2) . . ?
F32 C34 C32 113.8(3) . . ?
F33 C34 C32 111.6(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
C6 N1 C2 C3 1.1(4) . . . . ?
Nd N1 C2 C3 -169.4(2) . . . . ?
N1 C2 C3 C4 0.1(4) . . . . ?
C2 C3 C4 C5 -0.8(5) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C2 N1 C6 C5 -1.7(4) . . . . ?
Nd N1 C6 C5 168.5(2) . . . . ?
C2 N1 C6 C7 175.5(2) . . . . ?
Nd N1 C6 C7 -14.3(3) . . . . ?
C4 C5 C6 N1 1.0(4) . . . . ?
C4 C5 C6 C7 -175.9(3) . . . . ?
N1 C6 C7 N12 -0.6(4) . . . . ?
C5 C6 C7 N12 176.5(3) . . . . ?
N1 C6 C7 C8 -177.2(3) . . . . ?
C5 C6 C7 C8 -0.1(4) . . . . ?
N12 C7 C8 C9 -1.3(5) . . . . ?
C6 C7 C8 C9 175.2(3) . . . . ?
C7 C8 C9 C10 -0.1(6) . . . . ?
C8 C9 C10 C11 1.1(6) . . . . ?
C9 C10 C11 N12 -0.7(5) . . . . ?
C8 C7 N12 C11 1.7(4) . . . . ?
C6 C7 N12 C11 -175.0(3) . . . . ?
C8 C7 N12 Nd -168.1(2) . . . . ?
C6 C7 N12 Nd 15.2(3) . . . . ?
C10 C11 N12 C7 -0.7(5) . . . . ?
C10 C11 N12 Nd 169.5(3) . . . . ?
Nd O21 C22A C23A 7.0(6) . . . . ?
Nd O21 C22A C26 -171.7(2) . . . . ?
O21 C22A C23A C24A 2.1(7) . . . . ?
C26 C22A C23A C24A -179.2(4) . . . . ?
C22A C23A C24A O25 2.3(8) . . . . ?
C22A C23A C24A C27 178.0(4) . . . . ?
Nd O21 C22B C23B -14.8(15) . . . . ?
Nd O21 C22B C26 169.8(2) . . . . ?
O21 C22B C23B C24B -2.7(17) . . . . ?
C26 C22B C23B C24B 172.4(9) . . . . ?
C22B C23B C24B O25 -0.6(19) . . . 2_656 ?
C22B C23B C24B C27 -167.8(9) . . . 2_656 ?
C23A C24A O25 Nd -15.1(7) . . . . ?
C27 C24A O25 Nd 169.2(2) . . . . ?
O21 C22A C26 F22A 89.8(7) . . . . ?
C23A C22A C26 F22A -89.1(7) . . . . ?
O21 C22A C26 F23A -47.8(7) . . . . ?
C23A C22A C26 F23A 133.4(7) . . . . ?
O21 C22A C26 F21A -158.2(4) . . . . ?
C23A C22A C26 F21A 23.0(6) . . . . ?
O25 C24A C27 F26A -11.2(12) . . . . ?
C23A C24A C27 F26A 172.5(11) . . . . ?
O25 C24A C27 F25A -139.7(8) . . . . ?
C23A C24A C27 F25A 44.0(9) . . . . ?
O25 C24A C27 F24A 89.3(9) . . . . ?
C23A C24A C27 F24A -87.0(9) . . . . ?
Nd O31 C32 C33 5.4(4) . . . . ?
Nd O31 C32 C34 -173.24(17) . . . . ?
O31 C32 C33 C32 -2.57(19) . . . 2_656 ?
C34 C32 C33 C32 176.0(2) . . . 2_656 ?
O31 C32 C34 F31 74.0(3) . . . . ?
C33 C32 C34 F31 -104.7(3) . . . . ?
O31 C32 C34 F32 -164.2(3) . . . . ?
C33 C32 C34 F32 17.0(4) . . . . ?
O31 C32 C34 F33 -44.8(3) . . . . ?
C33 C32 C34 F33 136.5(2) . . . . ?

_refine_diff_density_max         0.566
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.058


# start Validation Reply Form
_vrf_PLAT213_two                 
;
PROBLEM: Atom F25B            has ADP max/min Ratio .....       20.6 prolat
RESPONSE: There are 2 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully
;
# end Validation Reply Form

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene/hexanes'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_new1
_database_code_depnum_ccdc_archive 'CCDC 1856926'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H11 F18 N2 Nd O6'
_chemical_formula_sum            'C25 H11 F18 N2 Nd O6'
_chemical_formula_weight         921.60

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9200(3)
_cell_length_b                   15.8414(3)
_cell_length_c                   17.8065(4)
_cell_angle_alpha                78.642(2)
_cell_angle_beta                 76.711(2)
_cell_angle_gamma                72.859(2)
_cell_volume                     3096.69(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    43657
_cell_measurement_theta_min      3.3414
_cell_measurement_theta_max      30.4392

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_F_000             1780
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    1.828
_shelx_estimated_absorpt_T_min   0.407
_shelx_estimated_absorpt_T_max   0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4067
_exptl_absorpt_correction_T_max  0.6100
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3693
_diffrn_reflns_number            49263
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.348
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10914
_reflns_number_gt                10583
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0779P)²+21.6863P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10914
_refine_ls_number_parameters     1099
_refine_ls_number_restraints     504
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.97336(3) 0.24069(2) 0.03144(2) 0.02234(11) Uani 1 1 d . U . . .
N1 N 1.0171(4) 0.3685(3) 0.0798(3) 0.0268(10) Uani 1 1 d . U . . .
C2 C 0.9671(6) 0.3882(4) 0.1517(4) 0.0309(13) Uani 1 1 d . U . . .
H2A H 0.905555 0.361507 0.180324 0.037 Uiso 1 1 calc R U . . .
C3 C 1.0001(6) 0.4453(5) 0.1864(4) 0.0359(14) Uani 1 1 d . U . . .
H3A H 0.961826 0.457823 0.237530 0.043 Uiso 1 1 calc R U . . .
C4 C 1.0891(7) 0.4837(5) 0.1459(4) 0.0447(17) Uani 1 1 d . U . . .
H4A H 1.114370 0.523014 0.168354 0.054 Uiso 1 1 calc R U . . .
C5 C 1.1422(7) 0.4638(5) 0.0705(4) 0.0410(15) Uani 1 1 d . U . . .
H5A H 1.203570 0.490256 0.041176 0.049 Uiso 1 1 calc R U . . .
C6 C 1.1062(5) 0.4068(4) 0.0389(4) 0.0286(12) Uani 1 1 d . U . . .
C7 C 1.1554(6) 0.3857(4) -0.0416(4) 0.0292(12) Uani 1 1 d . U . . .
C8 C 1.2513(6) 0.4147(5) -0.0875(4) 0.0438(16) Uani 1 1 d . U . . .
H8A H 1.289013 0.448102 -0.067259 0.053 Uiso 1 1 calc R U . . .
C9 C 1.2915(7) 0.3951(5) -0.1620(4) 0.0467(17) Uani 1 1 d . U . . .
H9A H 1.356619 0.415484 -0.193882 0.056 Uiso 1 1 calc R U . . .
C10 C 1.2373(7) 0.3458(5) -0.1905(4) 0.0456(17) Uani 1 1 d . U . . .
H10A H 1.262680 0.332146 -0.242410 0.055 Uiso 1 1 calc R U . . .
C11 C 1.1445(7) 0.3169(5) -0.1408(4) 0.0397(15) Uani 1 1 d . U . . .
H11A H 1.107502 0.282092 -0.159999 0.048 Uiso 1 1 calc R U . . .
N12 N 1.1029(5) 0.3345(4) -0.0673(3) 0.0320(11) Uani 1 1 d . U . . .
O21 O 0.9773(4) 0.1784(3) 0.1674(2) 0.0293(9) Uani 1 1 d . U . . .
C22 C 1.0567(6) 0.1565(4) 0.2093(4) 0.0324(13) Uani 1 1 d . U . . .
C23 C 1.1764(6) 0.1511(5) 0.1855(4) 0.0407(15) Uani 1 1 d . U . . .
H23A H 1.225549 0.137910 0.223645 0.049 Uiso 1 1 calc R U . . .
C24 C 1.2277(6) 0.1646(4) 0.1069(4) 0.0356(14) Uani 1 1 d . U . . .
O25 O 1.1773(4) 0.1816(3) 0.0499(3) 0.0357(10) Uani 1 1 d . U . . .
C26 C 1.0095(7) 0.1363(5) 0.2963(4) 0.0437(16) Uani 1 1 d . U . . .
C27 C 1.3614(6) 0.1590(5) 0.0848(5) 0.0456(17) Uani 1 1 d . U . . .
F21 F 0.9588(7) 0.0711(5) 0.3121(3) 0.094(2) Uani 1 1 d . U . . .
F22 F 1.0914(5) 0.1175(5) 0.3398(3) 0.0835(19) Uani 1 1 d . U . . .
F23 F 0.9247(6) 0.2062(5) 0.3219(3) 0.0869(19) Uani 1 1 d . U . . .
F24 F 1.4139(5) 0.1429(6) 0.1457(4) 0.103(2) Uani 1 1 d . U . . .
F25 F 1.3791(5) 0.2340(4) 0.0471(5) 0.090(2) Uani 1 1 d . U . . .
F26 F 1.4185(5) 0.0962(5) 0.0426(5) 0.104(3) Uani 1 1 d . U . . .
O31 O 0.7767(4) 0.3225(3) 0.0927(3) 0.0340(10) Uani 1 1 d . U . . .
C32 C 0.6764(6) 0.3465(4) 0.0733(4) 0.0347(13) Uani 1 1 d . U . . .
C33 C 0.6510(6) 0.3499(5) -0.0002(5) 0.0420(15) Uani 1 1 d . U . . .
H33A H 0.570036 0.365408 -0.006393 0.050 Uiso 1 1 calc R U . . .
C34 C 0.7404(6) 0.3314(4) -0.0642(4) 0.0361(14) Uani 1 1 d . U . . .
O35 O 0.8516(4) 0.3096(3) -0.0665(3) 0.0343(10) Uani 1 1 d . U . . .
C36 C 0.5704(6) 0.3778(5) 0.1371(4) 0.0463(16) Uani 1 1 d D U . . .
C37 C 0.7051(7) 0.3406(5) -0.1431(5) 0.0431(16) Uani 1 1 d . U . . .
F31A F 0.5778(13) 0.3288(10) 0.2037(7) 0.100(5) Uani 0.59 1 d D U P A 1
F32A F 0.5678(14) 0.4569(8) 0.1500(10) 0.088(4) Uani 0.59 1 d D U P A 1
F33A F 0.4665(9) 0.3858(15) 0.1218(11) 0.104(6) Uani 0.59 1 d D U P A 1
F31B F 0.487(3) 0.441(2) 0.1124(17) 0.199(18) Uani 0.41 1 d D U P A 2
F32B F 0.519(2) 0.3147(13) 0.1657(14) 0.098(6) Uani 0.41 1 d D U P A 2
F33B F 0.601(2) 0.393(3) 0.1965(15) 0.153(12) Uani 0.41 1 d D U P A 2
F34 F 0.5895(5) 0.3486(5) -0.1380(4) 0.0836(18) Uani 1 1 d . U . . .
F35 F 0.7253(6) 0.4122(4) -0.1879(3) 0.0805(18) Uani 1 1 d . U . . .
F36 F 0.7597(7) 0.2699(4) -0.1768(4) 0.092(2) Uani 1 1 d . U . . .
O41 O 0.8545(4) 0.1372(3) 0.0437(2) 0.0303(9) Uani 1 1 d . U . . .
C42 C 0.8361(6) 0.0975(4) -0.0048(4) 0.0299(12) Uani 1 1 d . U . . .
C43 C 0.9053(6) 0.0786(5) -0.0752(4) 0.0377(14) Uani 1 1 d . U . . .
H43A H 0.881758 0.045821 -0.105400 0.045 Uiso 1 1 calc R U . . .
C44 C 1.0097(6) 0.1065(4) -0.1039(4) 0.0329(13) Uani 1 1 d . U . . .
O45 O 1.0546(4) 0.1486(3) -0.0720(3) 0.0358(10) Uani 1 1 d . U . . .
C46 C 0.7165(6) 0.0725(4) 0.0182(4) 0.0431(15) Uani 1 1 d D U . . .
C47 C 1.0744(8) 0.0866(5) -0.1863(4) 0.0464(17) Uani 1 1 d . U . . .
F41A F 0.7057(16) 0.0245(9) 0.0852(5) 0.080(4) Uani 0.7 1 d D U P B 1
F42A F 0.7048(11) 0.0243(8) -0.0298(7) 0.079(3) Uani 0.7 1 d D U P B 1
F43A F 0.6315(8) 0.1449(6) 0.0162(14) 0.134(7) Uani 0.7 1 d D U P B 1
F41B F 0.653(3) 0.084(4) -0.0332(13) 0.152(18) Uani 0.3 1 d D U P B 2
F42B F 0.6416(18) 0.119(2) 0.0709(16) 0.090(9) Uani 0.3 1 d D U P B 2
F43B F 0.723(4) 0.001(2) 0.067(2) 0.129(16) Uani 0.3 1 d D U P B 2
F44 F 1.1723(6) 0.1143(5) -0.2090(3) 0.096(2) Uani 1 1 d . U . . .
F45 F 1.0078(7) 0.1248(6) -0.2373(3) 0.125(3) Uani 1 1 d . U . . .
F46 F 1.1081(6) 0.0012(4) -0.1910(3) 0.0862(19) Uani 1 1 d . U . . .
Nd2 Nd 0.47782(2) 0.25868(2) 0.51839(2) 0.02141(11) Uani 1 1 d . U . . .
N51 N 0.5555(4) 0.1594(3) 0.4080(3) 0.0293(10) Uani 1 1 d . U . . .
C52 C 0.6439(6) 0.1756(5) 0.3504(4) 0.0391(15) Uani 1 1 d . U . . .
H52A H 0.689667 0.212479 0.357471 0.047 Uiso 1 1 calc R U . . .
C53 C 0.6713(6) 0.1410(5) 0.2815(4) 0.0424(16) Uani 1 1 d . U . . .
H53A H 0.735809 0.152815 0.242158 0.051 Uiso 1 1 calc R U . . .
C54 C 0.6042(7) 0.0894(5) 0.2704(4) 0.0455(17) Uani 1 1 d . U . . .
H54A H 0.620595 0.065529 0.222894 0.055 Uiso 1 1 calc R U . . .
C55 C 0.5129(6) 0.0725(5) 0.3290(4) 0.0389(15) Uani 1 1 d . U . . .
H55A H 0.465457 0.036554 0.322550 0.047 Uiso 1 1 calc R U . . .
C56 C 0.4905(5) 0.1085(4) 0.3975(4) 0.0280(12) Uani 1 1 d . U . . .
C57 C 0.3921(5) 0.0915(4) 0.4642(3) 0.0251(11) Uani 1 1 d . U . . .
C58 C 0.3220(6) 0.0359(5) 0.4632(4) 0.0386(15) Uani 1 1 d . U . . .
H58A H 0.333657 0.006951 0.419041 0.046 Uiso 1 1 calc R U . . .
C59 C 0.2345(6) 0.0231(5) 0.5276(5) 0.0417(16) Uani 1 1 d . U . . .
H59A H 0.184956 -0.014035 0.527337 0.050 Uiso 1 1 calc R U . . .
C60 C 0.2199(6) 0.0636(4) 0.5906(4) 0.0343(14) Uani 1 1 d . U . . .
H60A H 0.160438 0.055454 0.635153 0.041 Uiso 1 1 calc R U . . .
C61 C 0.2941(6) 0.1174(4) 0.5885(4) 0.0304(13) Uani 1 1 d . U . . .
H61A H 0.285410 0.144753 0.633121 0.036 Uiso 1 1 calc R U . . .
N62 N 0.3777(4) 0.1327(3) 0.5263(3) 0.0242(10) Uani 1 1 d . U . . .
O71 O 0.6877(4) 0.1918(3) 0.5276(3) 0.0327(9) Uani 1 1 d . U . . .
C72 C 0.7417(6) 0.1707(4) 0.5832(4) 0.0359(14) Uani 1 1 d . U . . .
C73 C 0.6943(7) 0.1511(5) 0.6611(4) 0.0429(16) Uani 1 1 d . U . . .
H73A H 0.745696 0.134873 0.698155 0.052 Uiso 1 1 calc R U . . .
C74 C 0.5741(7) 0.1543(4) 0.6871(4) 0.0378(14) Uani 1 1 d . U . . .
O75 O 0.4915(4) 0.1771(3) 0.6476(3) 0.0338(10) Uani 1 1 d . U . . .
C76 C 0.8753(6) 0.1614(5) 0.5609(5) 0.0431(16) Uani 1 1 d . U . . .
C77 C 0.5326(7) 0.1278(4) 0.7744(4) 0.0464(16) Uani 1 1 d D U . . .
F71 F 0.9292(5) 0.1568(6) 0.6171(4) 0.095(2) Uani 1 1 d . U . . .
F72 F 0.9316(4) 0.0925(4) 0.5242(5) 0.097(2) Uani 1 1 d . U . . .
F73 F 0.8976(5) 0.2330(5) 0.5121(5) 0.099(2) Uani 1 1 d . U . . .
F74A F 0.480(2) 0.1982(10) 0.8060(10) 0.103(7) Uani 0.58 1 d D U P C 1
F75A F 0.459(2) 0.080(2) 0.7883(16) 0.132(10) Uani 0.58 1 d D U P C 1
F76A F 0.6211(13) 0.0908(16) 0.8114(9) 0.115(7) Uani 0.58 1 d D U P C 1
F74B F 0.593(3) 0.0495(14) 0.7951(18) 0.159(15) Uani 0.42 1 d D U P C 2
F75B F 0.537(3) 0.1777(19) 0.8204(14) 0.115(10) Uani 0.42 1 d D U P C 2
F76B F 0.4229(18) 0.124(2) 0.793(2) 0.112(11) Uani 0.42 1 d D U P C 2
O81 O 0.5895(4) 0.3521(3) 0.4279(3) 0.0366(10) Uani 1 1 d . U . . .
C82 C 0.6551(6) 0.3976(4) 0.4352(4) 0.0344(13) Uani 1 1 d . U . . .
C83 C 0.6637(6) 0.4241(5) 0.5032(4) 0.0407(15) Uani 1 1 d . U . . .
H83A H 0.718553 0.457985 0.500772 0.049 Uiso 1 1 calc R U . . .
C84 C 0.5952(6) 0.4025(4) 0.5736(4) 0.0319(13) Uani 1 1 d . U . . .
O85 O 0.5164(4) 0.3608(3) 0.5868(2) 0.0303(9) Uani 1 1 d . U . . .
C86 C 0.7418(7) 0.4218(5) 0.3612(5) 0.0465(17) Uani 1 1 d . U . . .
C87 C 0.6186(6) 0.4285(4) 0.6460(4) 0.0394(14) Uani 1 1 d D U . . .
F81 F 0.7226(5) 0.5087(3) 0.3425(3) 0.0756(16) Uani 1 1 d . U . . .
F82 F 0.7312(6) 0.3913(4) 0.3006(3) 0.0870(19) Uani 1 1 d . U . . .
F83 F 0.8532(4) 0.3912(5) 0.3713(4) 0.097(2) Uani 1 1 d . U . . .
F84A F 0.5263(17) 0.460(2) 0.6960(16) 0.092(8) Uani 0.62 1 d D U P D 1
F85A F 0.6929(15) 0.3597(10) 0.6779(10) 0.099(5) Uani 0.62 1 d D U P D 1
F86A F 0.6825(15) 0.4866(10) 0.6264(9) 0.072(4) Uani 0.62 1 d D U P D 1
F84B F 0.707(3) 0.459(3) 0.6463(19) 0.124(13) Uani 0.38 1 d D U P D 2
F85B F 0.523(2) 0.481(3) 0.679(2) 0.072(9) Uani 0.38 1 d D U P D 2
F86B F 0.623(4) 0.3613(14) 0.7029(15) 0.147(14) Uani 0.38 1 d D U P D 2
O91 O 0.3561(4) 0.3153(3) 0.4190(3) 0.0334(10) Uani 1 1 d . U . . .
C92 C 0.2467(6) 0.3328(4) 0.4189(4) 0.0358(14) Uani 1 1 d . U . . .
C93 C 0.1533(6) 0.3479(5) 0.4826(5) 0.0441(16) Uani 1 1 d . U . . .
H93A H 0.073253 0.361012 0.474995 0.053 Uiso 1 1 calc R U . . .
C94 C 0.1749(6) 0.3442(4) 0.5567(4) 0.0345(13) Uani 1 1 d . U . . .
O95 O 0.2736(4) 0.3245(3) 0.5773(3) 0.0322(9) Uani 1 1 d . U . . .
C96 C 0.2165(6) 0.3379(5) 0.3393(5) 0.0525(18) Uani 1 1 d D U . . .
C97 C 0.0662(6) 0.3664(5) 0.6212(5) 0.0478(17) Uani 1 1 d D U . . .
F91A F 0.1068(9) 0.3360(10) 0.3419(8) 0.092(4) Uani 0.72 1 d D U P E 1
F92A F 0.2815(15) 0.2674(10) 0.3069(13) 0.106(6) Uani 0.72 1 d D U P E 1
F93A F 0.237(2) 0.4075(11) 0.2934(11) 0.123(8) Uani 0.72 1 d D U P E 1
F91B F 0.277(5) 0.381(3) 0.283(2) 0.089(11) Uani 0.28 1 d D U P E 2
F92B F 0.112(2) 0.390(4) 0.332(2) 0.18(2) Uani 0.28 1 d D U P E 2
F93B F 0.245(6) 0.261(2) 0.317(4) 0.17(2) Uani 0.28 1 d D U P E 2
F94A F 0.0595(18) 0.4416(10) 0.6428(11) 0.132(8) Uani 0.71 1 d D U P F 1
F95A F -0.0358(11) 0.3731(11) 0.6027(12) 0.089(4) Uani 0.71 1 d D U P F 1
F96A F 0.0768(13) 0.3048(11) 0.6813(7) 0.119(6) Uani 0.71 1 d D U P F 1
F94B F 0.041(3) 0.2945(14) 0.662(2) 0.127(16) Uani 0.29 1 d D U P F 2
F95B F 0.080(4) 0.408(3) 0.6724(19) 0.083(10) Uani 0.29 1 d D U P F 2
F96B F -0.031(3) 0.415(3) 0.598(3) 0.139(18) Uani 0.29 1 d D U P F 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
Nd1 O25 2.408(4) . ?
Nd1 O35 2.412(4) . ?
Nd1 O41 2.415(4) . ?
Nd1 O45 2.421(4) . ?
Nd1 O21 2.434(4) . ?
Nd1 O31 2.440(4) . ?
Nd1 N1 2.575(5) . ?
Nd1 N12 2.600(5) . ?
N1 C2 1.338(8) . ?
N1 C6 1.369(8) . ?
C2 C3 1.377(9) . ?
C2 H2A 0.9500 . ?
C3 C4 1.368(10) . ?
C3 H3A 0.9500 . ?
C4 C5 1.400(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.362(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.482(9) . ?
C7 N12 1.356(8) . ?
C7 C8 1.384(9) . ?
C8 C9 1.366(11) . ?
C8 H8A 0.9500 . ?
C9 C10 1.376(12) . ?
C9 H9A 0.9500 . ?
C10 C11 1.380(10) . ?
C10 H10A 0.9500 . ?
C11 N12 1.342(8) . ?
C11 H11A 0.9500 . ?
O21 C22 1.266(8) . ?
C22 C23 1.374(10) . ?
C22 C26 1.527(9) . ?
C23 C24 1.395(10) . ?
C23 H23A 0.9500 . ?
C24 O25 1.242(8) . ?
C24 C27 1.532(9) . ?
C26 F21 1.300(9) . ?
C26 F22 1.314(9) . ?
C26 F23 1.335(10) . ?
C27 F25 1.294(9) . ?
C27 F26 1.296(10) . ?
C27 F24 1.319(10) . ?
O31 C32 1.251(8) . ?
C32 C33 1.398(10) . ?
C32 C36 1.525(10) . ?
C33 C34 1.382(11) . ?
C33 H33A 0.9500 . ?
C34 O35 1.261(8) . ?
C34 C37 1.524(9) . ?
C36 F31B 1.276(13) . ?
C36 F33B 1.279(13) . ?
C36 F32B 1.286(12) . ?
C36 F31A 1.289(10) . ?
C36 F33A 1.294(10) . ?
C36 F32A 1.308(10) . ?
C37 F36 1.301(9) . ?
C37 F35 1.303(9) . ?
C37 F34 1.330(9) . ?
O41 C42 1.254(7) . ?
C42 C43 1.367(10) . ?
C42 C46 1.534(9) . ?
C43 C44 1.396(10) . ?
C43 H43A 0.9500 . ?
C44 O45 1.246(8) . ?
C44 C47 1.539(9) . ?
C46 F41B 1.268(14) . ?
C46 F43B 1.274(15) . ?
C46 F41A 1.284(10) . ?
C46 F43A 1.288(9) . ?
C46 F42A 1.307(9) . ?
C46 F42B 1.314(14) . ?
C47 F45 1.286(10) . ?
C47 F46 1.306(9) . ?
C47 F44 1.317(10) . ?
Nd2 O85 2.405(4) . ?
Nd2 O81 2.407(4) . ?
Nd2 O91 2.415(4) . ?
Nd2 O75 2.423(4) . ?
Nd2 O95 2.424(4) . ?
Nd2 O71 2.442(4) . ?
Nd2 N62 2.578(5) . ?
Nd2 N51 2.592(5) . ?
N51 C56 1.335(8) . ?
N51 C52 1.336(8) . ?
C52 C53 1.375(10) . ?
C52 H52A 0.9500 . ?
C53 C54 1.367(11) . ?
C53 H53A 0.9500 . ?
C54 C55 1.373(11) . ?
C54 H54A 0.9500 . ?
C55 C56 1.386(9) . ?
C55 H55A 0.9500 . ?
C56 C57 1.509(9) . ?
C57 N62 1.344(8) . ?
C57 C58 1.387(9) . ?
C58 C59 1.387(10) . ?
C58 H58A 0.9500 . ?
C59 C60 1.353(10) . ?
C59 H59A 0.9500 . ?
C60 C61 1.388(9) . ?
C60 H60A 0.9500 . ?
C61 N62 1.344(8) . ?
C61 H61A 0.9500 . ?
O71 C72 1.242(8) . ?
C72 C73 1.384(11) . ?
C72 C76 1.519(10) . ?
C73 C74 1.389(11) . ?
C73 H73A 0.9500 . ?
C74 O75 1.266(8) . ?
C74 C77 1.532(10) . ?
C76 F71 1.288(9) . ?
C76 F72 1.309(9) . ?
C76 F73 1.341(10) . ?
C77 F75B 1.266(13) . ?
C77 F74B 1.270(13) . ?
C77 F74A 1.276(11) . ?
C77 F75A 1.279(13) . ?
C77 F76B 1.292(14) . ?
C77 F76A 1.301(11) . ?
O81 C82 1.250(8) . ?
C82 C83 1.391(10) . ?
C82 C86 1.536(10) . ?
C83 C84 1.372(10) . ?
C83 H83A 0.9500 . ?
C84 O85 1.256(8) . ?
C84 C87 1.533(9) . ?
C86 F82 1.310(10) . ?
C86 F83 1.314(10) . ?
C86 F81 1.315(9) . ?
C87 F84B 1.285(14) . ?
C87 F84A 1.285(13) . ?
C87 F85B 1.292(14) . ?
C87 F86A 1.309(10) . ?
C87 F85A 1.310(11) . ?
C87 F86B 1.315(13) . ?
O91 C92 1.251(8) . ?
C92 C93 1.397(11) . ?
C92 C96 1.522(10) . ?
C93 C94 1.389(10) . ?
C93 H93A 0.9500 . ?
C94 O95 1.246(8) . ?
C94 C97 1.525(10) . ?
C96 F93A 1.285(12) . ?
C96 F93B 1.287(16) . ?
C96 F92B 1.298(15) . ?
C96 F91B 1.297(15) . ?
C96 F91A 1.307(10) . ?
C96 F92A 1.310(11) . ?
C97 F95B 1.290(15) . ?
C97 F94B 1.297(15) . ?
C97 F96B 1.299(15) . ?
C97 F94A 1.299(11) . ?
C97 F96A 1.300(11) . ?
C97 F95A 1.301(10) . ?

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
O25 Nd1 O35 142.87(16) . . ?
O25 Nd1 O41 118.25(16) . . ?
O35 Nd1 O41 77.76(15) . . ?
O25 Nd1 O45 79.20(16) . . ?
O35 Nd1 O45 75.31(16) . . ?
O41 Nd1 O45 70.62(15) . . ?
O25 Nd1 O21 70.48(15) . . ?
O35 Nd1 O21 146.54(15) . . ?
O41 Nd1 O21 81.58(14) . . ?
O45 Nd1 O21 121.67(15) . . ?
O25 Nd1 O31 142.52(15) . . ?
O35 Nd1 O31 70.45(15) . . ?
O41 Nd1 O31 77.69(15) . . ?
O45 Nd1 O31 137.27(15) . . ?
O21 Nd1 O31 79.66(15) . . ?
O25 Nd1 N1 76.44(16) . . ?
O35 Nd1 N1 106.41(16) . . ?
O41 Nd1 N1 150.54(15) . . ?
O45 Nd1 N1 138.84(15) . . ?
O21 Nd1 N1 80.01(15) . . ?
O31 Nd1 N1 76.53(15) . . ?
O25 Nd1 N12 71.57(17) . . ?
O35 Nd1 N12 77.22(17) . . ?
O41 Nd1 N12 144.24(15) . . ?
O45 Nd1 N12 78.58(16) . . ?
O21 Nd1 N12 131.46(15) . . ?
O31 Nd1 N12 116.63(16) . . ?
N1 Nd1 N12 62.47(16) . . ?
C2 N1 C6 118.2(5) . . ?
C2 N1 Nd1 119.9(4) . . ?
C6 N1 Nd1 121.0(4) . . ?
N1 C2 C3 123.3(6) . . ?
N1 C2 H2A 118.3 . . ?
C3 C2 H2A 118.3 . . ?
C4 C3 C2 118.7(6) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C3 C4 C5 118.5(7) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
C6 C5 C4 120.4(7) . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
C5 C6 N1 120.8(6) . . ?
C5 C6 C7 123.0(6) . . ?
N1 C6 C7 116.2(5) . . ?
N12 C7 C8 121.6(6) . . ?
N12 C7 C6 116.1(5) . . ?
C8 C7 C6 122.3(6) . . ?
C9 C8 C7 119.9(7) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 119.7(7) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
C9 C10 C11 117.3(7) . . ?
C9 C10 H10A 121.4 . . ?
C11 C10 H10A 121.4 . . ?
N12 C11 C10 124.7(7) . . ?
N12 C11 H11A 117.7 . . ?
C10 C11 H11A 117.7 . . ?
C11 N12 C7 116.7(6) . . ?
C11 N12 Nd1 120.9(4) . . ?
C7 N12 Nd1 120.2(4) . . ?
C22 O21 Nd1 133.9(4) . . ?
O21 C22 C23 127.7(6) . . ?
O21 C22 C26 114.1(6) . . ?
C23 C22 C26 118.1(6) . . ?
C22 C23 C24 121.8(6) . . ?
C22 C23 H23A 119.1 . . ?
C24 C23 H23A 119.1 . . ?
O25 C24 C23 127.6(6) . . ?
O25 C24 C27 113.6(6) . . ?
C23 C24 C27 118.8(6) . . ?
C24 O25 Nd1 134.5(4) . . ?
F21 C26 F22 107.9(7) . . ?
F21 C26 F23 105.2(7) . . ?
F22 C26 F23 106.3(7) . . ?
F21 C26 C22 112.2(6) . . ?
F22 C26 C22 113.9(6) . . ?
F23 C26 C22 110.8(6) . . ?
F25 C27 F26 108.9(8) . . ?
F25 C27 F24 105.4(7) . . ?
F26 C27 F24 106.4(7) . . ?
F25 C27 C24 110.8(6) . . ?
F26 C27 C24 111.7(6) . . ?
F24 C27 C24 113.3(7) . . ?
C32 O31 Nd1 132.9(4) . . ?
O31 C32 C33 127.5(6) . . ?
O31 C32 C36 115.8(6) . . ?
C33 C32 C36 116.7(6) . . ?
C34 C33 C32 121.8(6) . . ?
C34 C33 H33A 119.1 . . ?
C32 C33 H33A 119.1 . . ?
O35 C34 C33 127.5(6) . . ?
O35 C34 C37 114.0(7) . . ?
C33 C34 C37 118.5(6) . . ?
C34 O35 Nd1 132.7(4) . . ?
F31B C36 F33B 113(2) . . ?
F31B C36 F32B 103(2) . . ?
F33B C36 F32B 103.0(19) . . ?
F31A C36 F33A 108.0(13) . . ?
F31A C36 F32A 104.1(12) . . ?
F33A C36 F32A 105.3(12) . . ?
F31B C36 C32 113.7(14) . . ?
F33B C36 C32 113.3(11) . . ?
F32B C36 C32 109.6(10) . . ?
F31A C36 C32 113.2(7) . . ?
F33A C36 C32 115.4(9) . . ?
F32A C36 C32 109.8(7) . . ?
F36 C37 F35 111.0(8) . . ?
F36 C37 F34 104.9(7) . . ?
F35 C37 F34 105.2(6) . . ?
F36 C37 C34 111.0(6) . . ?
F35 C37 C34 111.2(6) . . ?
F34 C37 C34 113.2(7) . . ?
C42 O41 Nd1 132.4(4) . . ?
O41 C42 C43 128.3(6) . . ?
O41 C42 C46 113.7(6) . . ?
C43 C42 C46 117.9(6) . . ?
C42 C43 C44 121.5(6) . . ?
C42 C43 H43A 119.2 . . ?
C44 C43 H43A 119.2 . . ?
O45 C44 C43 127.8(6) . . ?
O45 C44 C47 115.9(6) . . ?
C43 C44 C47 116.2(6) . . ?
C44 O45 Nd1 132.7(4) . . ?
F41B C46 F43B 117(3) . . ?
F41A C46 F43A 111.4(13) . . ?
F41A C46 F42A 104.7(9) . . ?
F43A C46 F42A 107.6(11) . . ?
F41B C46 F42B 102(2) . . ?
F43B C46 F42B 91(3) . . ?
F41B C46 C42 119.2(14) . . ?
F43B C46 C42 112(2) . . ?
F41A C46 C42 112.5(9) . . ?
F43A C46 C42 108.4(7) . . ?
F42A C46 C42 112.3(7) . . ?
F42B C46 C42 111.9(13) . . ?
F45 C47 F46 107.7(8) . . ?
F45 C47 F44 106.7(8) . . ?
F46 C47 F44 105.7(7) . . ?
F45 C47 C44 111.7(7) . . ?
F46 C47 C44 112.2(6) . . ?
F44 C47 C44 112.5(6) . . ?
O85 Nd2 O81 70.60(15) . . ?
O85 Nd2 O91 119.81(15) . . ?
O81 Nd2 O91 78.48(15) . . ?
O85 Nd2 O75 76.08(15) . . ?
O81 Nd2 O75 134.88(15) . . ?
O91 Nd2 O75 145.99(15) . . ?
O85 Nd2 O95 81.73(14) . . ?
O81 Nd2 O95 119.16(16) . . ?
O91 Nd2 O95 70.18(15) . . ?
O75 Nd2 O95 84.10(16) . . ?
O85 Nd2 O71 78.22(15) . . ?
O81 Nd2 O71 73.40(16) . . ?
O91 Nd2 O71 138.68(15) . . ?
O75 Nd2 O71 70.67(15) . . ?
O95 Nd2 O71 150.82(15) . . ?
O85 Nd2 N62 146.99(15) . . ?
O81 Nd2 N62 142.37(15) . . ?
O91 Nd2 N62 77.08(15) . . ?
O75 Nd2 N62 76.09(15) . . ?
O95 Nd2 N62 78.10(15) . . ?
O71 Nd2 N62 108.55(15) . . ?
O85 Nd2 N51 147.15(15) . . ?
O81 Nd2 N51 82.27(16) . . ?
O91 Nd2 N51 70.17(16) . . ?
O75 Nd2 N51 114.10(16) . . ?
O95 Nd2 N51 128.93(15) . . ?
O71 Nd2 N51 76.50(15) . . ?
N62 Nd2 N51 62.70(16) . . ?
C56 N51 C52 118.5(6) . . ?
C56 N51 Nd2 120.1(4) . . ?
C52 N51 Nd2 119.2(4) . . ?
N51 C52 C53 122.6(7) . . ?
N51 C52 H52A 118.7 . . ?
C53 C52 H52A 118.7 . . ?
C54 C53 C52 119.0(7) . . ?
C54 C53 H53A 120.5 . . ?
C52 C53 H53A 120.5 . . ?
C53 C54 C55 118.9(7) . . ?
C53 C54 H54A 120.5 . . ?
C55 C54 H54A 120.5 . . ?
C54 C55 C56 119.4(7) . . ?
C54 C55 H55A 120.3 . . ?
C56 C55 H55A 120.3 . . ?
N51 C56 C55 121.5(6) . . ?
N51 C56 C57 116.7(5) . . ?
C55 C56 C57 121.8(6) . . ?
N62 C57 C58 121.4(6) . . ?
N62 C57 C56 115.6(5) . . ?
C58 C57 C56 122.9(6) . . ?
C57 C58 C59 119.1(6) . . ?
C57 C58 H58A 120.4 . . ?
C59 C58 H58A 120.4 . . ?
C60 C59 C58 119.9(6) . . ?
C60 C59 H59A 120.0 . . ?
C58 C59 H59A 120.0 . . ?
C59 C60 C61 118.1(6) . . ?
C59 C60 H60A 120.9 . . ?
C61 C60 H60A 120.9 . . ?
N62 C61 C60 123.2(6) . . ?
N62 C61 H61A 118.4 . . ?
C60 C61 H61A 118.4 . . ?
C57 N62 C61 118.1(5) . . ?
C57 N62 Nd2 121.2(4) . . ?
C61 N62 Nd2 119.8(4) . . ?
C72 O71 Nd2 132.7(4) . . ?
O71 C72 C73 127.0(7) . . ?
O71 C72 C76 115.0(6) . . ?
C73 C72 C76 117.9(6) . . ?
C72 C73 C74 122.3(6) . . ?
C72 C73 H73A 118.9 . . ?
C74 C73 H73A 118.9 . . ?
O75 C74 C73 128.3(6) . . ?
O75 C74 C77 114.0(6) . . ?
C73 C74 C77 117.7(6) . . ?
C74 O75 Nd2 132.1(4) . . ?
F71 C76 F72 107.7(7) . . ?
F71 C76 F73 103.5(7) . . ?
F72 C76 F73 106.0(8) . . ?
F71 C76 C72 116.1(7) . . ?
F72 C76 C72 112.2(6) . . ?
F73 C76 C72 110.6(6) . . ?
F75B C77 F74B 108(2) . . ?
F74A C77 F75A 107.5(18) . . ?
F75B C77 F76B 103(2) . . ?
F74B C77 F76B 105(2) . . ?
F74A C77 F76A 102.9(13) . . ?
F75A C77 F76A 111.1(18) . . ?
F75B C77 C74 117.4(14) . . ?
F74B C77 C74 109.1(15) . . ?
F74A C77 C74 109.1(10) . . ?
F75A C77 C74 112.9(14) . . ?
F76B C77 C74 114.2(19) . . ?
F76A C77 C74 112.8(10) . . ?
C82 O81 Nd2 133.8(4) . . ?
O81 C82 C83 127.6(6) . . ?
O81 C82 C86 115.9(6) . . ?
C83 C82 C86 116.4(6) . . ?
C84 C83 C82 121.8(6) . . ?
C84 C83 H83A 119.1 . . ?
C82 C83 H83A 119.1 . . ?
O85 C84 C83 127.5(6) . . ?
O85 C84 C87 114.9(6) . . ?
C83 C84 C87 117.6(6) . . ?
C84 O85 Nd2 133.3(4) . . ?
F82 C86 F83 108.6(7) . . ?
F82 C86 F81 106.6(7) . . ?
F83 C86 F81 106.5(7) . . ?
F82 C86 C82 112.5(6) . . ?
F83 C86 C82 111.2(7) . . ?
F81 C86 C82 111.2(6) . . ?
F84B C87 F85B 108(3) . . ?
F84A C87 F86A 107.6(18) . . ?
F84A C87 F85A 111.7(16) . . ?
F86A C87 F85A 100.9(12) . . ?
F84B C87 F86B 105(2) . . ?
F85B C87 F86B 96(3) . . ?
F84B C87 C84 124.0(16) . . ?
F84A C87 C84 116.6(15) . . ?
F85B C87 C84 109.9(18) . . ?
F86A C87 C84 111.0(8) . . ?
F85A C87 C84 107.9(9) . . ?
F86B C87 C84 110.3(12) . . ?
C92 O91 Nd2 134.5(4) . . ?
O91 C92 C93 127.1(6) . . ?
O91 C92 C96 114.2(6) . . ?
C93 C92 C96 118.6(6) . . ?
C94 C93 C92 121.4(6) . . ?
C94 C93 H93A 119.3 . . ?
C92 C93 H93A 119.3 . . ?
O95 C94 C93 127.5(6) . . ?
O95 C94 C97 115.4(6) . . ?
C93 C94 C97 117.1(6) . . ?
C94 O95 Nd2 134.9(4) . . ?
F93B C96 F92B 117(4) . . ?
F93B C96 F91B 102(4) . . ?
F92B C96 F91B 97(3) . . ?
F93A C96 F91A 109.0(13) . . ?
F93A C96 F92A 108.1(14) . . ?
F91A C96 F92A 103.8(11) . . ?
F93A C96 C92 111.5(12) . . ?
F93B C96 C92 112(3) . . ?
F92B C96 C92 113(2) . . ?
F91B C96 C92 114(3) . . ?
F91A C96 C92 113.9(9) . . ?
F92A C96 C92 110.1(10) . . ?
F95B C97 F94B 104(2) . . ?
F95B C97 F96B 105(3) . . ?
F94B C97 F96B 106(3) . . ?
F94A C97 F96A 108.1(13) . . ?
F94A C97 F95A 107.2(12) . . ?
F96A C97 F95A 106.5(11) . . ?
F95B C97 C94 115(2) . . ?
F94B C97 C94 111.3(16) . . ?
F96B C97 C94 115(3) . . ?
F94A C97 C94 109.6(10) . . ?
F96A C97 C94 109.9(8) . . ?
F95A C97 C94 115.3(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 C3 0.3(9) . . . . ?
Nd1 N1 C2 C3 169.3(5) . . . . ?
N1 C2 C3 C4 -0.4(10) . . . . ?
C2 C3 C4 C5 0.5(11) . . . . ?
C3 C4 C5 C6 -0.6(11) . . . . ?
C4 C5 C6 N1 0.6(10) . . . . ?
C4 C5 C6 C7 177.6(7) . . . . ?
C2 N1 C6 C5 -0.4(9) . . . . ?
Nd1 N1 C6 C5 -169.2(5) . . . . ?
C2 N1 C6 C7 -177.6(5) . . . . ?
Nd1 N1 C6 C7 13.5(7) . . . . ?
C5 C6 C7 N12 -174.0(6) . . . . ?
N1 C6 C7 N12 3.1(8) . . . . ?
C5 C6 C7 C8 7.5(10) . . . . ?
N1 C6 C7 C8 -175.3(6) . . . . ?
N12 C7 C8 C9 3.1(11) . . . . ?
C6 C7 C8 C9 -178.5(7) . . . . ?
C7 C8 C9 C10 -0.8(12) . . . . ?
C8 C9 C10 C11 -1.1(12) . . . . ?
C9 C10 C11 N12 0.9(12) . . . . ?
C10 C11 N12 C7 1.3(10) . . . . ?
C10 C11 N12 Nd1 -162.1(6) . . . . ?
C8 C7 N12 C11 -3.3(9) . . . . ?
C6 C7 N12 C11 178.3(6) . . . . ?
C8 C7 N12 Nd1 160.3(5) . . . . ?
C6 C7 N12 Nd1 -18.2(7) . . . . ?
Nd1 O21 C22 C23 -9.5(10) . . . . ?
Nd1 O21 C22 C26 168.9(4) . . . . ?
O21 C22 C23 C24 -4.6(12) . . . . ?
C26 C22 C23 C24 177.1(7) . . . . ?
C22 C23 C24 O25 -0.6(12) . . . . ?
C22 C23 C24 C27 179.0(7) . . . . ?
C23 C24 O25 Nd1 20.1(11) . . . . ?
C27 C24 O25 Nd1 -159.5(5) . . . . ?
O21 C22 C26 F21 59.9(9) . . . . ?
C23 C22 C26 F21 -121.5(8) . . . . ?
O21 C22 C26 F22 -177.1(7) . . . . ?
C23 C22 C26 F22 1.4(10) . . . . ?
O21 C22 C26 F23 -57.4(8) . . . . ?
C23 C22 C26 F23 121.2(8) . . . . ?
O25 C24 C27 F25 60.4(9) . . . . ?
C23 C24 C27 F25 -119.3(8) . . . . ?
O25 C24 C27 F26 -61.2(9) . . . . ?
C23 C24 C27 F26 119.1(9) . . . . ?
O25 C24 C27 F24 178.6(7) . . . . ?
C23 C24 C27 F24 -1.1(10) . . . . ?
Nd1 O31 C32 C33 -15.5(11) . . . . ?
Nd1 O31 C32 C36 166.2(4) . . . . ?
O31 C32 C33 C34 -4.5(12) . . . . ?
C36 C32 C33 C34 173.8(6) . . . . ?
C32 C33 C34 O35 0.2(12) . . . . ?
C32 C33 C34 C37 -177.3(6) . . . . ?
C33 C34 O35 Nd1 24.1(10) . . . . ?
C37 C34 O35 Nd1 -158.2(4) . . . . ?
O31 C32 C36 F31B 145(3) . . . . ?
C33 C32 C36 F31B -33(3) . . . . ?
O31 C32 C36 F33B 14(2) . . . . ?
C33 C32 C36 F33B -164(2) . . . . ?
O31 C32 C36 F32B -100.3(17) . . . . ?
C33 C32 C36 F32B 81.3(17) . . . . ?
O31 C32 C36 F31A -41.9(15) . . . . ?
C33 C32 C36 F31A 139.7(13) . . . . ?
O31 C32 C36 F33A -167.1(13) . . . . ?
C33 C32 C36 F33A 14.5(15) . . . . ?
O31 C32 C36 F32A 74.0(12) . . . . ?
C33 C32 C36 F32A -104.4(12) . . . . ?
O35 C34 C37 F36 51.6(9) . . . . ?
C33 C34 C37 F36 -130.5(8) . . . . ?
O35 C34 C37 F35 -72.5(8) . . . . ?
C33 C34 C37 F35 105.3(8) . . . . ?
O35 C34 C37 F34 169.3(6) . . . . ?
C33 C34 C37 F34 -12.9(9) . . . . ?
Nd1 O41 C42 C43 22.5(10) . . . . ?
Nd1 O41 C42 C46 -154.0(4) . . . . ?
O41 C42 C43 C44 -2.4(11) . . . . ?
C46 C42 C43 C44 174.0(6) . . . . ?
C42 C43 C44 O45 1.1(11) . . . . ?
C42 C43 C44 C47 -175.8(6) . . . . ?
C43 C44 O45 Nd1 -20.0(11) . . . . ?
C47 C44 O45 Nd1 157.0(5) . . . . ?
O41 C42 C46 F41B 137(3) . . . . ?
C43 C42 C46 F41B -40(3) . . . . ?
O41 C42 C46 F43B -81(3) . . . . ?
C43 C42 C46 F43B 102(3) . . . . ?
O41 C42 C46 F41A -56.5(10) . . . . ?
C43 C42 C46 F41A 126.6(10) . . . . ?
O41 C42 C46 F43A 67.1(14) . . . . ?
C43 C42 C46 F43A -109.8(13) . . . . ?
O41 C42 C46 F42A -174.2(8) . . . . ?
C43 C42 C46 F42A 8.9(10) . . . . ?
O41 C42 C46 F42B 19.0(19) . . . . ?
C43 C42 C46 F42B -158.0(18) . . . . ?
O45 C44 C47 F45 -116.9(9) . . . . ?
C43 C44 C47 F45 60.4(10) . . . . ?
O45 C44 C47 F46 122.1(8) . . . . ?
C43 C44 C47 F46 -60.6(9) . . . . ?
O45 C44 C47 F44 3.0(10) . . . . ?
C43 C44 C47 F44 -179.6(7) . . . . ?
C56 N51 C52 C53 -0.8(10) . . . . ?
Nd2 N51 C52 C53 -164.4(5) . . . . ?
N51 C52 C53 C54 1.3(11) . . . . ?
C52 C53 C54 C55 -1.0(11) . . . . ?
C53 C54 C55 C56 0.3(11) . . . . ?
C52 N51 C56 C55 0.1(9) . . . . ?
Nd2 N51 C56 C55 163.5(5) . . . . ?
C52 N51 C56 C57 179.6(5) . . . . ?
Nd2 N51 C56 C57 -16.9(7) . . . . ?
C54 C55 C56 N51 0.2(10) . . . . ?
C54 C55 C56 C57 -179.4(6) . . . . ?
N51 C56 C57 N62 2.5(8) . . . . ?
C55 C56 C57 N62 -178.0(6) . . . . ?
N51 C56 C57 C58 -176.3(6) . . . . ?
C55 C56 C57 C58 3.3(9) . . . . ?
N62 C57 C58 C59 0.4(10) . . . . ?
C56 C57 C58 C59 179.1(6) . . . . ?
C57 C58 C59 C60 -1.0(11) . . . . ?
C58 C59 C60 C61 0.1(11) . . . . ?
C59 C60 C61 N62 1.5(10) . . . . ?
C58 C57 N62 C61 1.1(8) . . . . ?
C56 C57 N62 C61 -177.7(5) . . . . ?
C58 C57 N62 Nd2 -167.9(5) . . . . ?
C56 C57 N62 Nd2 13.4(6) . . . . ?
C60 C61 N62 C57 -2.1(9) . . . . ?
C60 C61 N62 Nd2 167.0(5) . . . . ?
Nd2 O71 C72 C73 23.9(11) . . . . ?
Nd2 O71 C72 C76 -159.4(4) . . . . ?
O71 C72 C73 C74 -0.9(12) . . . . ?
C76 C72 C73 C74 -177.6(7) . . . . ?
C72 C73 C74 O75 -2.6(12) . . . . ?
C72 C73 C74 C77 177.7(6) . . . . ?
C73 C74 O75 Nd2 -17.0(11) . . . . ?
C77 C74 O75 Nd2 162.8(4) . . . . ?
O71 C72 C76 F71 167.0(7) . . . . ?
C73 C72 C76 F71 -16.0(10) . . . . ?
O71 C72 C76 F72 -68.7(9) . . . . ?
C73 C72 C76 F72 108.4(8) . . . . ?
O71 C72 C76 F73 49.5(9) . . . . ?
C73 C72 C76 F73 -133.5(8) . . . . ?
O75 C74 C77 F75B -113(2) . . . . ?
C73 C74 C77 F75B 66(2) . . . . ?
O75 C74 C77 F74B 124(2) . . . . ?
C73 C74 C77 F74B -57(2) . . . . ?
O75 C74 C77 F74A -77.2(13) . . . . ?
C73 C74 C77 F74A 102.6(13) . . . . ?
O75 C74 C77 F75A 42.2(19) . . . . ?
C73 C74 C77 F75A -138.0(19) . . . . ?
O75 C74 C77 F76B 7(2) . . . . ?
C73 C74 C77 F76B -173.2(19) . . . . ?
O75 C74 C77 F76A 169.2(14) . . . . ?
C73 C74 C77 F76A -11.0(15) . . . . ?
Nd2 O81 C82 C83 -15.7(11) . . . . ?
Nd2 O81 C82 C86 160.1(5) . . . . ?
O81 C82 C83 C84 -1.0(12) . . . . ?
C86 C82 C83 C84 -176.7(6) . . . . ?
C82 C83 C84 O85 -2.4(11) . . . . ?
C82 C83 C84 C87 175.3(6) . . . . ?
C83 C84 O85 Nd2 22.3(10) . . . . ?
C87 C84 O85 Nd2 -155.4(4) . . . . ?
O81 C82 C86 F82 1.1(10) . . . . ?
C83 C82 C86 F82 177.4(7) . . . . ?
O81 C82 C86 F83 -121.0(8) . . . . ?
C83 C82 C86 F83 55.3(9) . . . . ?
O81 C82 C86 F81 120.5(7) . . . . ?
C83 C82 C86 F81 -63.2(9) . . . . ?
O85 C84 C87 F84B 169(2) . . . . ?
C83 C84 C87 F84B -9(3) . . . . ?
O85 C84 C87 F84A -43.3(19) . . . . ?
C83 C84 C87 F84A 138.8(19) . . . . ?
O85 C84 C87 F85B -61(3) . . . . ?
C83 C84 C87 F85B 121(3) . . . . ?
O85 C84 C87 F86A -166.9(10) . . . . ?
C83 C84 C87 F86A 15.2(12) . . . . ?
O85 C84 C87 F85A 83.3(12) . . . . ?
C83 C84 C87 F85A -94.6(12) . . . . ?
O85 C84 C87 F86B 44(2) . . . . ?
C83 C84 C87 F86B -134(2) . . . . ?
Nd2 O91 C92 C93 19.5(11) . . . . ?
Nd2 O91 C92 C96 -160.7(5) . . . . ?
O91 C92 C93 C94 -0.3(12) . . . . ?
C96 C92 C93 C94 179.9(7) . . . . ?
C92 C93 C94 O95 -3.2(12) . . . . ?
C92 C93 C94 C97 177.0(7) . . . . ?
C93 C94 O95 Nd2 -12.6(11) . . . . ?
C97 C94 O95 Nd2 167.3(4) . . . . ?
O91 C92 C96 F93A -70.8(14) . . . . ?
C93 C92 C96 F93A 109.1(14) . . . . ?
O91 C92 C96 F93B 71(4) . . . . ?
C93 C92 C96 F93B -109(4) . . . . ?
O91 C92 C96 F92B -153(3) . . . . ?
C93 C92 C96 F92B 27(3) . . . . ?
O91 C92 C96 F91B -44(3) . . . . ?
C93 C92 C96 F91B 136(3) . . . . ?
O91 C92 C96 F91A 165.3(9) . . . . ?
C93 C92 C96 F91A -14.8(12) . . . . ?
O91 C92 C96 F92A 49.3(13) . . . . ?
C93 C92 C96 F92A -130.9(12) . . . . ?
O95 C94 C97 F95B 36(2) . . . . ?
C93 C94 C97 F95B -144(2) . . . . ?
O95 C94 C97 F94B -82(2) . . . . ?
C93 C94 C97 F94B 98(2) . . . . ?
O95 C94 C97 F96B 158(3) . . . . ?
C93 C94 C97 F96B -22(3) . . . . ?
O95 C94 C97 F94A 69.3(13) . . . . ?
C93 C94 C97 F94A -110.8(12) . . . . ?
O95 C94 C97 F96A -49.4(12) . . . . ?
C93 C94 C97 F96A 130.5(11) . . . . ?
O95 C94 C97 F95A -169.7(10) . . . . ?
C93 C94 C97 F95A 10.2(12) . . . . ?

_refine_diff_density_max         4.253
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.161


# start Validation Reply Form
_vrf_PLAT213_new1                
;
PROBLEM: Atom F86B            has ADP max/min Ratio .....        6.6 prolat
RESPONSE: There are 6 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully.
;
_vrf_PLAT971_new1                
;
PROBLEM: Check Calcd Resid. Dens.  0.85A   From Nd2             4.37 eA-3  
RESPONSE: Due to a relatively large crystal, the absorption correction has left some unaccounted for electron density.
;
_vrf_PLAT910_new1                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         25 Note  
RESPONSE: Presumably due to issues at the data collection stage.
;
# end Validation Reply Form

_chemical_properties_physical    Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_k11208
_database_code_depnum_ccdc_archive 'CCDC 1858639'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H19 F18 N4 O6 Pr'
_chemical_formula_sum            'C35 H19 F18 N4 O6 Pr'
_chemical_formula_weight         1074.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   21.786(4)
_cell_length_b                   11.792(2)
_cell_length_c                   18.081(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.89(3)
_cell_angle_gamma                90
_cell_volume                     4066.9(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7953
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_F_000             2104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.329
_shelx_estimated_absorpt_T_min   0.741
_shelx_estimated_absorpt_T_max   0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            16383
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.573
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_full        25.024
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3594
_reflns_number_gt                2988
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_structure_solution    'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²+27.3342P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00072(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3594
_refine_ls_number_parameters     375
_refine_ls_number_restraints     525
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.0976
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr Pr 0.500000 0.80687(3) 0.750000 0.03331(17) Uani 1 2 d S TU P A .
N1 N 0.5225(2) 0.8524(4) 0.9096(3) 0.0390(10) Uani 1 1 d . U . . .
C2 C 0.5883(3) 0.8641(4) 0.9723(3) 0.0423(12) Uani 1 1 d . U . . .
H2A H 0.624832 0.869064 0.958005 0.051 Uiso 1 1 calc R U . . .
C3 C 0.6061(3) 0.8693(5) 1.0569(3) 0.0490(14) Uani 1 1 d . U . . .
H3A H 0.653573 0.877695 1.099558 0.059 Uiso 1 1 calc R U . . .
C4 C 0.5529(4) 0.8621(5) 1.0775(4) 0.0563(15) Uani 1 1 d . U . . .
H4A H 0.563162 0.864350 1.134831 0.068 Uiso 1 1 calc R U . . .
C5 C 0.4849(3) 0.8515(5) 1.0137(4) 0.0532(14) Uani 1 1 d . U . . .
H5A H 0.447720 0.846437 1.026797 0.064 Uiso 1 1 calc R U . . .
C6 C 0.4706(3) 0.8483(4) 0.9300(3) 0.0404(12) Uani 1 1 d . U . . .
C7 C 0.3979(3) 0.8441(4) 0.8590(4) 0.0423(12) Uani 1 1 d . U . . .
C8 C 0.3392(3) 0.8432(6) 0.8711(4) 0.0627(17) Uani 1 1 d . U . . .
H8A H 0.344862 0.840168 0.926591 0.075 Uiso 1 1 calc R U . . .
C9 C 0.2729(3) 0.8469(6) 0.8020(5) 0.0686(19) Uani 1 1 d . U . . .
H9A H 0.232711 0.845702 0.809571 0.082 Uiso 1 1 calc R U . . .
C10 C 0.2654(3) 0.8521(5) 0.7232(4) 0.0583(16) Uani 1 1 d . U . . .
H10A H 0.220311 0.856782 0.674858 0.070 Uiso 1 1 calc R U . . .
C11 C 0.3249(3) 0.8505(5) 0.7152(4) 0.0529(15) Uani 1 1 d . U . . .
H11A H 0.319662 0.852774 0.659918 0.064 Uiso 1 1 calc R U . . .
N12 N 0.3901(2) 0.8458(4) 0.7807(3) 0.0437(10) Uani 1 1 d . U . . .
O21 O 0.53166(18) 0.6391(3) 0.6911(2) 0.0386(8) Uani 1 1 d . U . . .
C22A C 0.5028(4) 0.5571(6) 0.6467(4) 0.0414(16) Uani 0.75 1 d . U P A 1
C23A C 0.4314(4) 0.5340(7) 0.6045(5) 0.056(2) Uani 0.75 1 d . U P A 1
H23A H 0.415229 0.465257 0.573721 0.067 Uiso 0.75 1 calc R U P A 1
C24A C 0.3838(5) 0.6085(8) 0.6063(5) 0.043(2) Uani 0.75 1 d . U P A 1
C22B C 0.5633(11) 0.5608(19) 0.7160(14) 0.040(4) Uani 0.25 1 d . U P A 3
C23B C 0.6111(12) 0.5319(19) 0.8000(15) 0.048(5) Uani 0.25 1 d . U P A 3
H23B H 0.630519 0.457866 0.813541 0.058 Uiso 0.25 1 calc R U P A 3
C24B C 0.6297(13) 0.615(2) 0.8638(17) 0.039(6) Uani 0.25 1 d . U P A 3
O25 O 0.39438(17) 0.7057(3) 0.6422(2) 0.0385(8) Uani 1 1 d . U . . .
C26 C 0.5528(4) 0.4707(5) 0.6399(4) 0.0649(17) Uani 1 1 d D U . . .
C27 C 0.3090(3) 0.5747(5) 0.5564(4) 0.0741(19) Uani 1 1 d D U . . .
F21A F 0.5231(5) 0.4030(8) 0.5703(6) 0.104(3) Uani 0.55 1 d D U P A 1
F22A F 0.5826(10) 0.3828(9) 0.6876(7) 0.132(5) Uani 0.55 1 d D U P A 1
F23A F 0.6005(7) 0.5228(13) 0.6286(10) 0.091(4) Uani 0.55 1 d D U P A 1
F21B F 0.5932(8) 0.4310(12) 0.7140(7) 0.107(5) Uani 0.45 1 d D U P A 2
F23B F 0.4975(9) 0.416(2) 0.6013(13) 0.211(9) Uani 0.45 1 d D U P A 2
F22B F 0.5813(13) 0.508(2) 0.5982(13) 0.129(7) Uani 0.45 1 d D U P A 2
F24A F 0.2807(7) 0.566(2) 0.6047(8) 0.172(7) Uani 0.51 1 d D U P A 1
F25A F 0.2696(5) 0.6370(15) 0.4990(10) 0.127(6) Uani 0.51 1 d D U P A 1
F26A F 0.3043(9) 0.4842(13) 0.5126(14) 0.180(8) Uani 0.51 1 d D U P A 1
F24B F 0.3017(14) 0.617(2) 0.4863(10) 0.212(9) Uani 0.49 1 d D U P A 2
F25B F 0.2932(6) 0.4700(10) 0.5637(13) 0.133(7) Uani 0.49 1 d D U P A 2
F26B F 0.2603(7) 0.6344(15) 0.5588(17) 0.169(7) Uani 0.49 1 d D U P A 2
O31 O 0.43072(17) 0.9845(3) 0.6863(2) 0.0387(8) Uani 1 1 d . U . . .
C32 C 0.4391(3) 1.0888(5) 0.6965(3) 0.0383(11) Uani 1 1 d . U . . .
C33 C 0.500000 1.1466(7) 0.750000 0.0452(18) Uani 1 2 d S TU P . .
H33A H 0.500001 1.227173 0.749999 0.068 Uiso 1 2 calc R U P . .
C34 C 0.3727(3) 1.1570(5) 0.6433(4) 0.0513(14) Uani 1 1 d . U . . .
F31 F 0.3291(3) 1.1498(5) 0.6738(3) 0.120(2) Uani 1 1 d . U . . .
F32 F 0.3836(2) 1.2655(3) 0.6374(3) 0.1142(19) Uani 1 1 d . U . . .
F33 F 0.33837(18) 1.1206(3) 0.5648(2) 0.0712(11) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr O25 2.487(3) . ?
Pr O25 2.487(3) 2_656 ?
Pr O21 2.497(3) . ?
Pr O21 2.497(3) 2_656 ?
Pr O31 2.512(3) 2_656 ?
Pr O31 2.512(3) . ?
Pr N1 2.737(4) . ?
Pr N1 2.737(4) 2_656 ?
Pr N12 2.746(4) . ?
Pr N12 2.746(4) 2_656 ?
N1 C2 1.337(7) . ?
N1 C6 1.347(7) . ?
C2 C3 1.387(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.379(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.375(9) . ?
C4 H4A 0.9500 . ?
C5 C6 1.391(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.481(8) . ?
C7 N12 1.341(7) . ?
C7 C8 1.399(8) . ?
C8 C9 1.381(9) . ?
C8 H8A 0.9500 . ?
C9 C10 1.355(9) . ?
C9 H9A 0.9500 . ?
C10 C11 1.372(8) . ?
C10 H10A 0.9500 . ?
C11 N12 1.340(7) . ?
C11 H11A 0.9500 . ?
O21 C22B 1.11(2) . ?
O21 C22A 1.219(8) . ?
C22A C23A 1.389(10) . ?
C22A C26 1.539(9) . ?
C23A C24A 1.373(13) . ?
C23A H23A 0.9500 . ?
C24A O25 1.281(11) . ?
C24A C27 1.485(11) . ?
C22B C23B 1.41(3) . ?
C22B C26 1.66(2) . ?
C23B C24B 1.41(4) . ?
C23B H23B 0.9500 . ?
C24B O25 1.18(3) 2_656 ?
C24B C27 1.49(3) 2_656 ?
C26 F23B 1.241(12) . ?
C26 F22B 1.265(13) . ?
C26 F21B 1.284(11) . ?
C26 F22A 1.303(10) . ?
C26 F23A 1.306(11) . ?
C26 F21A 1.361(9) . ?
C27 F25A 1.222(11) . ?
C27 F24A 1.295(11) . ?
C27 F24B 1.299(12) . ?
C27 F26A 1.304(12) . ?
C27 F26B 1.291(12) . ?
C27 F25B 1.306(10) . ?
O31 C32 1.244(6) . ?
C32 C33 1.387(7) . ?
C32 C34 1.523(8) . ?
C33 H33A 0.9500 . ?
C34 F31 1.311(7) . ?
C34 F32 1.314(7) . ?
C34 F33 1.316(7) . ?

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
O25 Pr O25 122.64(16) . 2_656 ?
O25 Pr O21 68.10(11) . . ?
O25 Pr O21 67.20(11) 2_656 . ?
O25 Pr O21 67.20(11) . 2_656 ?
O25 Pr O21 68.11(11) 2_656 2_656 ?
O21 Pr O21 75.21(17) . 2_656 ?
O25 Pr O31 151.99(11) . 2_656 ?
O25 Pr O31 85.26(11) 2_656 2_656 ?
O21 Pr O31 128.86(11) . 2_656 ?
O21 Pr O31 133.91(11) 2_656 2_656 ?
O25 Pr O31 85.26(11) . . ?
O25 Pr O31 151.99(11) 2_656 . ?
O21 Pr O31 133.91(11) . . ?
O21 Pr O31 128.86(11) 2_656 . ?
O31 Pr O31 67.04(16) 2_656 . ?
O25 Pr N1 123.17(12) . . ?
O25 Pr N1 68.98(12) 2_656 . ?
O21 Pr N1 131.29(12) . . ?
O21 Pr N1 69.59(12) 2_656 . ?
O31 Pr N1 65.87(12) 2_656 . ?
O31 Pr N1 94.67(12) . . ?
O25 Pr N1 68.98(12) . 2_656 ?
O25 Pr N1 123.17(12) 2_656 2_656 ?
O21 Pr N1 69.59(12) . 2_656 ?
O21 Pr N1 131.29(12) 2_656 2_656 ?
O31 Pr N1 94.67(12) 2_656 2_656 ?
O31 Pr N1 65.87(12) . 2_656 ?
N1 Pr N1 157.35(18) . 2_656 ?
O25 Pr N12 70.83(13) . . ?
O25 Pr N12 119.26(13) 2_656 . ?
O21 Pr N12 131.80(13) . . ?
O21 Pr N12 66.31(12) 2_656 . ?
O31 Pr N12 99.06(12) 2_656 . ?
O31 Pr N12 64.14(12) . . ?
N1 Pr N12 58.88(13) . . ?
N1 Pr N12 116.82(13) 2_656 . ?
O25 Pr N12 119.26(13) . 2_656 ?
O25 Pr N12 70.83(13) 2_656 2_656 ?
O21 Pr N12 66.31(12) . 2_656 ?
O21 Pr N12 131.80(12) 2_656 2_656 ?
O31 Pr N12 64.14(12) 2_656 2_656 ?
O31 Pr N12 99.06(13) . 2_656 ?
N1 Pr N12 116.82(13) . 2_656 ?
N1 Pr N12 58.88(13) 2_656 2_656 ?
N12 Pr N12 160.76(19) . 2_656 ?
C2 N1 C6 118.0(5) . . ?
C2 N1 Pr 119.1(3) . . ?
C6 N1 Pr 122.3(3) . . ?
N1 C2 C3 123.6(5) . . ?
N1 C2 H2A 118.2 . . ?
C3 C2 H2A 118.2 . . ?
C4 C3 C2 118.1(6) . . ?
C4 C3 H3A 121.0 . . ?
C2 C3 H3A 121.0 . . ?
C5 C4 C3 119.0(5) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C4 C5 C6 120.0(6) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
N1 C6 C5 121.3(5) . . ?
N1 C6 C7 116.9(5) . . ?
C5 C6 C7 121.8(5) . . ?
N12 C7 C8 120.4(5) . . ?
N12 C7 C6 116.8(5) . . ?
C8 C7 C6 122.8(5) . . ?
C9 C8 C7 119.6(6) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
C9 C10 C11 118.0(6) . . ?
C9 C10 H10A 121.0 . . ?
C11 C10 H10A 121.0 . . ?
N12 C11 C10 124.0(6) . . ?
N12 C11 H11A 118.0 . . ?
C10 C11 H11A 118.0 . . ?
C11 N12 C7 118.3(5) . . ?
C11 N12 Pr 118.8(4) . . ?
C7 N12 Pr 122.2(3) . . ?
C22B O21 Pr 137.0(11) . . ?
C22A O21 Pr 138.5(4) . . ?
O21 C22A C23A 126.9(7) . . ?
O21 C22A C26 114.7(6) . . ?
C23A C22A C26 118.3(6) . . ?
C24A C23A C22A 121.4(7) . . ?
C24A C23A H23A 119.3 . . ?
C22A C23A H23A 119.3 . . ?
O25 C24A C23A 129.1(8) . . ?
O25 C24A C27 115.1(8) . . ?
C23A C24A C27 115.7(8) . . ?
O21 C22B C23B 129(2) . . ?
O21 C22B C26 112.6(16) . . ?
C23B C22B C26 118.2(17) . . ?
C22B C23B C24B 119(2) . . ?
C22B C23B H23B 120.4 . . ?
C24B C23B H23B 120.4 . . ?
O25 C24B C23B 128(2) 2_656 . ?
O25 C24B C27 122(2) 2_656 2_656 ?
C24B O25 Pr 135.4(13) 2_656 . ?
C24A O25 Pr 134.3(5) . . ?
F23B C26 F22B 117.9(15) . . ?
F23B C26 F21B 112.8(16) . . ?
F22B C26 F21B 117.5(17) . . ?
F22A C26 F23A 107.3(13) . . ?
F22A C26 F21A 90.4(8) . . ?
F23A C26 F21A 100.9(9) . . ?
F22A C26 C22A 128.2(10) . . ?
F23A C26 C22A 110.4(9) . . ?
F21A C26 C22A 115.1(6) . . ?
F25A C27 F24A 104.7(13) . . ?
F25A C27 F26A 99.1(15) . . ?
F24A C27 F26A 114.9(14) . . ?
F24B C27 F26B 96.2(15) . . ?
F24B C27 F25B 123.3(16) . . ?
F26B C27 F25B 104.6(12) . . ?
F25A C27 C24B 124.5(15) . 2_656 ?
F24A C27 C24B 82.4(13) . 2_656 ?
F26A C27 C24B 128.1(14) . 2_656 ?
F25A C27 C24A 118.0(8) . . ?
F24A C27 C24A 110.6(8) . . ?
F26A C27 C24A 109.3(10) . . ?
C32 O31 Pr 138.1(3) . . ?
O31 C32 C33 127.7(5) . . ?
O31 C32 C34 113.8(5) . . ?
C33 C32 C34 118.5(5) . . ?
C32 C33 C32 121.1(7) . 2_656 ?
C32 C33 H33A 119.4 . . ?
C32 C33 H33A 119.4 2_656 . ?
F31 C34 F32 107.1(6) . . ?
F31 C34 F33 106.4(6) . . ?
F32 C34 F33 105.1(5) . . ?
F31 C34 C32 111.1(5) . . ?
F32 C34 C32 114.3(5) . . ?
F33 C34 C32 112.3(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
C6 N1 C2 C3 1.6(8) . . . . ?
Pr N1 C2 C3 -169.5(4) . . . . ?
N1 C2 C3 C4 0.0(8) . . . . ?
C2 C3 C4 C5 -0.8(8) . . . . ?
C3 C4 C5 C6 0.0(9) . . . . ?
C2 N1 C6 C5 -2.5(8) . . . . ?
Pr N1 C6 C5 168.3(4) . . . . ?
C2 N1 C6 C7 175.5(5) . . . . ?
Pr N1 C6 C7 -13.7(6) . . . . ?
C4 C5 C6 N1 1.7(9) . . . . ?
C4 C5 C6 C7 -176.2(5) . . . . ?
N1 C6 C7 N12 -0.6(7) . . . . ?
C5 C6 C7 N12 177.4(5) . . . . ?
N1 C6 C7 C8 -177.9(5) . . . . ?
C5 C6 C7 C8 0.1(8) . . . . ?
N12 C7 C8 C9 -1.5(9) . . . . ?
C6 C7 C8 C9 175.7(6) . . . . ?
C7 C8 C9 C10 -0.5(11) . . . . ?
C8 C9 C10 C11 1.8(10) . . . . ?
C9 C10 C11 N12 -1.1(10) . . . . ?
C10 C11 N12 C7 -0.9(9) . . . . ?
C10 C11 N12 Pr 169.7(5) . . . . ?
C8 C7 N12 C11 2.2(8) . . . . ?
C6 C7 N12 C11 -175.2(5) . . . . ?
C8 C7 N12 Pr -168.1(4) . . . . ?
C6 C7 N12 Pr 14.5(6) . . . . ?
Pr O21 C22A C23A 5.9(12) . . . . ?
Pr O21 C22A C26 -172.8(4) . . . . ?
O21 C22A C23A C24A 2.8(13) . . . . ?
C26 C22A C23A C24A -178.5(7) . . . . ?
C22A C23A C24A O25 1.6(14) . . . . ?
C22A C23A C24A C27 178.3(7) . . . . ?
Pr O21 C22B C23B -12(3) . . . . ?
Pr O21 C22B C26 170.6(4) . . . . ?
O21 C22B C23B C24B -8(4) . . . . ?
C26 C22B C23B C24B 169.3(18) . . . . ?
C22B C23B C24B O25 7(4) . . . 2_656 ?
C22B C23B C24B C27 -168.3(18) . . . 2_656 ?
C23A C24A O25 Pr -14.1(13) . . . . ?
C27 C24A O25 Pr 169.1(4) . . . . ?
O21 C22A C26 F22A 90.3(12) . . . . ?
C23A C22A C26 F22A -88.5(13) . . . . ?
O21 C22A C26 F23A -44.0(11) . . . . ?
C23A C22A C26 F23A 137.2(10) . . . . ?
O21 C22A C26 F21A -157.4(8) . . . . ?
C23A C22A C26 F21A 23.7(11) . . . . ?
O25 C24A C27 F25A 57.9(16) . . . . ?
C23A C24A C27 F25A -119.3(15) . . . . ?
O25 C24A C27 F24A -62.6(16) . . . . ?
C23A C24A C27 F24A 120.2(16) . . . . ?
O25 C24A C27 F26A 170.0(13) . . . . ?
C23A C24A C27 F26A -7.2(15) . . . . ?
Pr O31 C32 C33 5.9(8) . . . . ?
Pr O31 C32 C34 -173.1(3) . . . . ?
O31 C32 C33 C32 -2.9(4) . . . 2_656 ?
C34 C32 C33 C32 176.1(5) . . . 2_656 ?
O31 C32 C34 F31 74.2(7) . . . . ?
C33 C32 C34 F31 -104.9(6) . . . . ?
O31 C32 C34 F32 -164.4(5) . . . . ?
C33 C32 C34 F32 16.5(7) . . . . ?
O31 C32 C34 F33 -44.8(7) . . . . ?
C33 C32 C34 F33 136.1(5) . . . . ?

_refine_diff_density_max         2.533
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.108


# start Validation Reply Form
_vrf_PLAT213_k11208              
;
PROBLEM: Atom F21B            has ADP max/min Ratio .....        5.4 prolat
RESPONSE: There are 2 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully.
;
# end Validation Reply Form

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methylene chloride/hexanes'
####################################################################### 
# 
# 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_k11211
_database_code_depnum_ccdc_archive 'CCDC 1856932'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H19 F18 N4 O6 Sm'
_chemical_formula_sum            'C35 H19 F18 N4 O6 Sm'
_chemical_formula_weight         1083.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   21.775(4)
_cell_length_b                   11.724(2)
_cell_length_c                   18.017(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.73(3)
_cell_angle_gamma                90
_cell_volume                     4033.3(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14869
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_F_000             2116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.588
_shelx_estimated_absorpt_T_min   0.630
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            23131
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.578
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_full        25.023
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3564
_reflns_number_gt                3215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_structure_solution    'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²+35.7264P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00079(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3564
_refine_ls_number_parameters     336
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1186
_refine_ls_wR_factor_gt          0.1138
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
PR Sm 0.500000 0.80620(3) 0.750000 0.02754(17) Uani 1 2 d S TU P A .
N1 N 0.5227(2) 0.8520(4) 0.9088(3) 0.0332(9) Uani 1 1 d . U . . .
C2 C 0.5886(3) 0.8643(5) 0.9712(3) 0.0383(12) Uani 1 1 d . U . . .
H2A H 0.625074 0.868956 0.956664 0.046 Uiso 1 1 calc R U . . .
C3 C 0.6064(4) 0.8706(5) 1.0564(4) 0.0448(14) Uani 1 1 d . U . . .
H3A H 0.653619 0.880436 1.099055 0.054 Uiso 1 1 calc R U . . .
C4 C 0.5532(4) 0.8621(6) 1.0767(4) 0.0518(16) Uani 1 1 d . U . . .
H4A H 0.563394 0.864528 1.134183 0.062 Uiso 1 1 calc R U . . .
C5 C 0.4854(4) 0.8500(5) 1.0134(4) 0.0486(14) Uani 1 1 d . U . . .
H5A H 0.448454 0.843957 1.027070 0.058 Uiso 1 1 calc R U . . .
C6 C 0.4708(3) 0.8465(5) 0.9297(4) 0.0379(12) Uani 1 1 d . U . . .
C7 C 0.3982(3) 0.8415(5) 0.8579(4) 0.0389(12) Uani 1 1 d . U . . .
C8 C 0.3400(4) 0.8406(7) 0.8710(5) 0.0591(18) Uani 1 1 d . U . . .
H8A H 0.346005 0.837115 0.926808 0.071 Uiso 1 1 calc R U . . .
C9 C 0.2734(4) 0.8448(7) 0.8021(5) 0.0649(19) Uani 1 1 d . U . . .
H9A H 0.233423 0.843770 0.810176 0.078 Uiso 1 1 calc R U . . .
C10 C 0.2658(3) 0.8505(6) 0.7229(5) 0.0537(16) Uani 1 1 d . U . . .
H10A H 0.220632 0.854554 0.674697 0.064 Uiso 1 1 calc R U . . .
C11 C 0.3255(3) 0.8501(6) 0.7145(4) 0.0466(14) Uani 1 1 d . U . . .
H11A H 0.320192 0.853685 0.659061 0.056 Uiso 1 1 calc R U . . .
N12 N 0.3907(2) 0.8449(4) 0.7802(3) 0.0375(10) Uani 1 1 d . U . . .
O21 O 0.53110(19) 0.6408(3) 0.6917(2) 0.0345(8) Uani 1 1 d . U . . .
C22A C 0.5031(4) 0.5580(7) 0.6471(5) 0.0366(16) Uani 0.7 1 d . U P A 1
C23A C 0.4317(5) 0.5343(7) 0.6064(6) 0.051(2) Uani 0.7 1 d . U P A 1
H23A H 0.415648 0.464001 0.577130 0.062 Uiso 0.7 1 calc R U P A 1
C24A C 0.3842(6) 0.6093(10) 0.6072(7) 0.041(2) Uani 0.7 1 d . U P A 1
C22B C 0.5625(10) 0.5584(17) 0.7138(12) 0.039(4) Uani 0.3 1 d . U P A 3
C23B C 0.6104(10) 0.5300(17) 0.8011(13) 0.043(4) Uani 0.3 1 d . U P A 3
H23B H 0.631205 0.456584 0.816543 0.052 Uiso 0.3 1 calc R U P A 3
C24B C 0.6257(12) 0.620(2) 0.8651(16) 0.034(5) Uani 0.3 1 d . U P A 3
O25 O 0.39548(18) 0.7078(3) 0.6433(2) 0.0332(8) Uani 1 1 d . U . . .
C26 C 0.5535(4) 0.4713(5) 0.6412(4) 0.0600(17) Uani 1 1 d D U . . .
C27 C 0.3101(4) 0.5761(5) 0.5572(4) 0.072(2) Uani 1 1 d D U . . .
F21A F 0.5240(5) 0.4045(8) 0.5716(6) 0.097(2) Uani 0.52 1 d D U P A 1
F22A F 0.5840(7) 0.3817(8) 0.6869(6) 0.095(2) Uani 0.52 1 d D U P A 1
F23A F 0.6019(8) 0.5210(17) 0.6287(10) 0.133(4) Uani 0.52 1 d D U P A 1
F21B F 0.5924(6) 0.4299(10) 0.7145(6) 0.097(2) Uani 0.48 1 d D U P A 2
F22B F 0.5839(7) 0.5145(11) 0.6038(8) 0.095(2) Uani 0.48 1 d D U P A 2
F23B F 0.4960(6) 0.4244(15) 0.6004(9) 0.133(4) Uani 0.48 1 d D U P A 2
F24A F 0.2913(10) 0.6158(18) 0.4847(7) 0.182(6) Uani 0.55 1 d D U P A 1
F25A F 0.2934(4) 0.4690(8) 0.5537(9) 0.104(3) Uani 0.55 1 d D U P A 1
F26A F 0.2650(7) 0.6243(13) 0.5794(14) 0.149(4) Uani 0.55 1 d D U P A 1
F24B F 0.2873(10) 0.527(3) 0.6050(10) 0.182(6) Uani 0.45 1 d D U P A 2
F25B F 0.2664(5) 0.6433(10) 0.5091(12) 0.104(3) Uani 0.45 1 d D U P A 2
F26B F 0.3110(8) 0.4837(14) 0.5137(14) 0.149(4) Uani 0.45 1 d D U P A 2
O31 O 0.43115(19) 0.9809(3) 0.6865(2) 0.0335(8) Uani 1 1 d . U . . .
C32 C 0.4391(3) 1.0855(5) 0.6963(3) 0.0322(11) Uani 1 1 d . U . . .
C33 C 0.500000 1.1463(7) 0.750000 0.0402(18) Uani 1 2 d S TU P . .
H33A H 0.500000 1.227326 0.749999 0.060 Uiso 1 2 calc R U P . .
C34 C 0.3724(4) 1.1547(5) 0.6428(4) 0.0462(14) Uani 1 1 d . U . . .
F31 F 0.3294(3) 1.1474(6) 0.6741(4) 0.110(2) Uani 1 1 d D U . . .
F32 F 0.3835(3) 1.2634(4) 0.6365(4) 0.103(2) Uani 1 1 d D U . . .
F33 F 0.3382(2) 1.1162(4) 0.5648(2) 0.0637(11) Uani 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
PR O25 2.449(4) 2_656 ?
PR O25 2.449(4) . ?
PR O21 2.451(4) 2_656 ?
PR O21 2.451(4) . ?
PR O31 2.471(4) 2_656 ?
PR O31 2.471(4) . ?
PR N1 2.713(4) . ?
PR N1 2.713(4) 2_656 ?
PR N12 2.722(5) 2_656 ?
PR N12 2.722(5) . ?
N1 C2 1.339(7) . ?
N1 C6 1.353(7) . ?
C2 C3 1.393(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.375(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.372(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.385(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.487(9) . ?
C7 N12 1.331(7) . ?
C7 C8 1.396(8) . ?
C8 C9 1.383(11) . ?
C8 H8A 0.9500 . ?
C9 C10 1.355(11) . ?
C9 H9A 0.9500 . ?
C10 C11 1.380(9) . ?
C10 H10A 0.9500 . ?
C11 N12 1.344(8) . ?
C11 H11A 0.9500 . ?
O21 C22B 1.14(2) . ?
O21 C22A 1.219(8) . ?
C22A C23A 1.391(12) . ?
C22A C26 1.536(11) . ?
C23A C24A 1.363(16) . ?
C23A H23A 0.9500 . ?
C24A O25 1.290(13) . ?
C24A C27 1.474(14) . ?
C22B C23B 1.45(3) . ?
C22B C26 1.60(2) . ?
C23B C24B 1.48(3) . ?
C23B H23B 0.9500 . ?
C24B O25 1.11(3) 2_656 ?
C24B C27 1.52(2) 2_656 ?
C26 F23B 1.234(10) . ?
C26 F22B 1.257(11) . ?
C26 F21B 1.274(10) . ?
C26 F22A 1.303(10) . ?
C26 F23A 1.316(12) . ?
C26 F21A 1.351(9) . ?
C27 F25B 1.218(10) . ?
C27 F24A 1.256(11) . ?
C27 F25A 1.300(10) . ?
C27 F24B 1.316(13) . ?
C27 F26A 1.348(11) . ?
C27 F26B 1.344(12) . ?
O31 C32 1.239(6) . ?
C32 C33 1.404(7) . ?
C32 C34 1.533(8) . ?
C33 H33A 0.9500 . ?
C34 F31 1.308(8) . ?
C34 F32 1.312(8) . ?
C34 F33 1.315(7) . ?

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
O25 PR O25 123.82(17) 2_656 . ?
O25 PR O21 68.59(12) 2_656 2_656 ?
O25 PR O21 67.66(12) . 2_656 ?
O25 PR O21 67.66(12) 2_656 . ?
O25 PR O21 68.59(12) . . ?
O21 PR O21 75.40(18) 2_656 . ?
O25 PR O31 84.20(12) 2_656 2_656 ?
O25 PR O31 151.87(12) . 2_656 ?
O21 PR O31 133.54(12) 2_656 2_656 ?
O21 PR O31 128.56(12) . 2_656 ?
O25 PR O31 151.87(12) 2_656 . ?
O25 PR O31 84.20(12) . . ?
O21 PR O31 128.56(12) 2_656 . ?
O21 PR O31 133.54(12) . . ?
O31 PR O31 67.97(17) 2_656 . ?
O25 PR N1 68.64(13) 2_656 . ?
O25 PR N1 123.40(13) . . ?
O21 PR N1 69.65(13) 2_656 . ?
O21 PR N1 131.36(13) . . ?
O31 PR N1 65.50(12) 2_656 . ?
O31 PR N1 94.97(13) . . ?
O25 PR N1 123.40(13) 2_656 2_656 ?
O25 PR N1 68.64(13) . 2_656 ?
O21 PR N1 131.36(13) 2_656 2_656 ?
O21 PR N1 69.65(13) . 2_656 ?
O31 PR N1 94.97(13) 2_656 2_656 ?
O31 PR N1 65.50(12) . 2_656 ?
N1 PR N1 157.19(19) . 2_656 ?
O25 PR N12 70.34(14) 2_656 2_656 ?
O25 PR N12 119.57(13) . 2_656 ?
O21 PR N12 131.75(13) 2_656 2_656 ?
O21 PR N12 66.30(13) . 2_656 ?
O31 PR N12 63.89(13) 2_656 2_656 ?
O31 PR N12 99.40(14) . 2_656 ?
N1 PR N12 116.36(14) . 2_656 ?
N1 PR N12 59.33(14) 2_656 2_656 ?
O25 PR N12 119.57(13) 2_656 . ?
O25 PR N12 70.34(14) . . ?
O21 PR N12 66.30(13) 2_656 . ?
O21 PR N12 131.75(14) . . ?
O31 PR N12 99.40(14) 2_656 . ?
O31 PR N12 63.89(13) . . ?
N1 PR N12 59.33(14) . . ?
N1 PR N12 116.36(14) 2_656 . ?
N12 PR N12 160.8(2) 2_656 . ?
C2 N1 C6 118.2(5) . . ?
C2 N1 PR 119.1(3) . . ?
C6 N1 PR 122.0(4) . . ?
N1 C2 C3 123.3(6) . . ?
N1 C2 H2A 118.3 . . ?
C3 C2 H2A 118.3 . . ?
C4 C3 C2 117.8(6) . . ?
C4 C3 H3A 121.1 . . ?
C2 C3 H3A 121.1 . . ?
C5 C4 C3 119.6(6) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 120.0(6) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
N1 C6 C5 121.1(6) . . ?
N1 C6 C7 116.2(5) . . ?
C5 C6 C7 122.6(5) . . ?
N12 C7 C8 121.1(6) . . ?
N12 C7 C6 117.0(5) . . ?
C8 C7 C6 121.7(6) . . ?
C9 C8 C7 119.5(7) . . ?
C9 C8 H8A 120.3 . . ?
C7 C8 H8A 120.3 . . ?
C10 C9 C8 119.5(6) . . ?
C10 C9 H9A 120.3 . . ?
C8 C9 H9A 120.3 . . ?
C9 C10 C11 118.0(7) . . ?
C9 C10 H10A 121.0 . . ?
C11 C10 H10A 121.0 . . ?
N12 C11 C10 123.8(6) . . ?
N12 C11 H11A 118.1 . . ?
C10 C11 H11A 118.1 . . ?
C7 N12 C11 118.1(5) . . ?
C7 N12 PR 122.0(4) . . ?
C11 N12 PR 119.2(4) . . ?
C22B O21 PR 139.8(10) . . ?
C22A O21 PR 139.3(5) . . ?
O21 C22A C23A 125.7(8) . . ?
O21 C22A C26 115.1(7) . . ?
C23A C22A C26 119.0(7) . . ?
C24A C23A C22A 121.8(9) . . ?
C24A C23A H23A 119.1 . . ?
C22A C23A H23A 119.1 . . ?
O25 C24A C23A 128.5(10) . . ?
O25 C24A C27 115.5(9) . . ?
C23A C24A C27 116.0(10) . . ?
O21 C22B C23B 125.0(17) . . ?
O21 C22B C26 116.0(15) . . ?
C23B C22B C26 118.9(15) . . ?
C22B C23B C24B 117.3(18) . . ?
C22B C23B H23B 121.4 . . ?
C24B C23B H23B 121.4 . . ?
O25 C24B C23B 129(2) 2_656 . ?
O25 C24B C27 125(2) 2_656 2_656 ?
C24B O25 PR 135.5(13) 2_656 . ?
C24A O25 PR 134.2(6) . . ?
F23B C26 F22B 120.3(11) . . ?
F23B C26 F21B 115.3(12) . . ?
F22B C26 F21B 116.8(10) . . ?
F22A C26 F23A 105.0(11) . . ?
F22A C26 F21A 89.4(7) . . ?
F23A C26 F21A 99.1(11) . . ?
F22A C26 C22A 130.9(8) . . ?
F23A C26 C22A 112.1(10) . . ?
F21A C26 C22A 114.3(6) . . ?
F24A C27 F25A 111.3(12) . . ?
F25B C27 F24B 109.9(12) . . ?
F24A C27 F26A 103.5(12) . . ?
F25A C27 F26A 101.2(10) . . ?
F25B C27 F26B 109.3(12) . . ?
F24B C27 F26B 98.3(13) . . ?
F24A C27 C24A 104.5(11) . . ?
F25A C27 C24A 118.9(7) . . ?
F26A C27 C24A 116.6(9) . . ?
F24A C27 C24B 121.9(15) . 2_656 ?
F25A C27 C24B 119.0(12) . 2_656 ?
F26A C27 C24B 93.7(12) . 2_656 ?
C24A C27 C24B 24.8(8) . 2_656 ?
C32 O31 PR 138.0(3) . . ?
O31 C32 C33 128.4(5) . . ?
O31 C32 C34 114.2(5) . . ?
C33 C32 C34 117.4(5) . . ?
C32 C33 C32 119.0(7) 2_656 . ?
C32 C33 H33A 120.5 2_656 . ?
C32 C33 H33A 120.5 . . ?
F31 C34 F32 107.5(6) . . ?
F31 C34 F33 106.5(6) . . ?
F32 C34 F33 105.9(5) . . ?
F31 C34 C32 110.6(5) . . ?
F32 C34 C32 114.3(6) . . ?
F33 C34 C32 111.6(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
C6 N1 C2 C3 0.7(8) . . . . ?
PR N1 C2 C3 -169.9(4) . . . . ?
N1 C2 C3 C4 0.9(9) . . . . ?
C2 C3 C4 C5 -1.2(9) . . . . ?
C3 C4 C5 C6 0.0(10) . . . . ?
C2 N1 C6 C5 -2.0(8) . . . . ?
PR N1 C6 C5 168.4(4) . . . . ?
C2 N1 C6 C7 175.6(5) . . . . ?
PR N1 C6 C7 -14.1(6) . . . . ?
C4 C5 C6 N1 1.7(9) . . . . ?
C4 C5 C6 C7 -175.7(6) . . . . ?
N1 C6 C7 N12 -1.2(7) . . . . ?
C5 C6 C7 N12 176.3(6) . . . . ?
N1 C6 C7 C8 -177.2(6) . . . . ?
C5 C6 C7 C8 0.3(9) . . . . ?
N12 C7 C8 C9 -0.8(11) . . . . ?
C6 C7 C8 C9 175.0(6) . . . . ?
C7 C8 C9 C10 -0.4(12) . . . . ?
C8 C9 C10 C11 0.9(12) . . . . ?
C9 C10 C11 N12 -0.3(11) . . . . ?
C8 C7 N12 C11 1.4(9) . . . . ?
C6 C7 N12 C11 -174.6(5) . . . . ?
C8 C7 N12 PR -168.1(5) . . . . ?
C6 C7 N12 PR 15.9(7) . . . . ?
C10 C11 N12 C7 -0.9(10) . . . . ?
C10 C11 N12 PR 168.9(5) . . . . ?
PR O21 C22A C23A 4.3(13) . . . . ?
PR O21 C22A C26 -172.2(4) . . . . ?
O21 C22A C23A C24A 5.6(15) . . . . ?
C26 C22A C23A C24A -178.1(9) . . . . ?
C22A C23A C24A O25 -0.4(17) . . . . ?
C22A C23A C24A C27 176.5(8) . . . . ?
PR O21 C22B C23B -11(3) . . . . ?
PR O21 C22B C26 170.6(5) . . . . ?
O21 C22B C23B C24B -7(3) . . . . ?
C26 C22B C23B C24B 170.7(16) . . . . ?
C22B C23B C24B O25 2(3) . . . 2_656 ?
C22B C23B C24B C27 -165.3(16) . . . 2_656 ?
C23A C24A O25 PR -14.0(15) . . . . ?
C27 C24A O25 PR 169.0(5) . . . . ?
O21 C22A C26 F22A 90.5(12) . . . . ?
C23A C22A C26 F22A -86.2(12) . . . . ?
O21 C22A C26 F23A -45.6(12) . . . . ?
C23A C22A C26 F23A 137.7(11) . . . . ?
O21 C22A C26 F21A -157.4(8) . . . . ?
C23A C22A C26 F21A 25.9(12) . . . . ?
O25 C24A C27 F24A 88.3(14) . . . . ?
C23A C24A C27 F24A -89.1(14) . . . . ?
O25 C24A C27 F25A -147.0(11) . . . . ?
C23A C24A C27 F25A 35.7(15) . . . . ?
O25 C24A C27 F26A -25.3(15) . . . . ?
C23A C24A C27 F26A 157.3(13) . . . . ?
PR O31 C32 C33 6.0(8) . . . . ?
PR O31 C32 C34 -173.1(3) . . . . ?
O31 C32 C33 C32 -2.9(4) . . . 2_656 ?
C34 C32 C33 C32 176.2(5) . . . 2_656 ?
O31 C32 C34 F31 74.5(7) . . . . ?
C33 C32 C34 F31 -104.6(6) . . . . ?
O31 C32 C34 F32 -164.0(5) . . . . ?
C33 C32 C34 F32 16.8(7) . . . . ?
O31 C32 C34 F33 -43.9(7) . . . . ?
C33 C32 C34 F33 137.0(5) . . . . ?

_refine_diff_density_max         2.203
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.122


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: anhydrous toluene/hexane'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_eh110
_database_code_depnum_ccdc_archive 'CCDC 1856928'
_audit_update_record             
;
2018-10-07 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H11 F18 N2 O6 Sm'
_chemical_formula_sum            'C25 H11 F18 N2 O6 Sm'
_chemical_formula_weight         927.71

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.8612(19)
_cell_length_b                   15.851(3)
_cell_length_c                   17.880(3)
_cell_angle_alpha                78.721(3)
_cell_angle_beta                 76.813(4)
_cell_angle_gamma                72.850(3)
_cell_volume                     3097.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5258
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.05

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_F_000             1788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.047
_shelx_estimated_absorpt_T_min   0.644
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_T_max  0.9045
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30731
_diffrn_reflns_av_unetI/netI     0.1192
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.350
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             10844
_reflns_number_gt                6504
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10.2'
_computing_publication_material  'Microsoft Office 2013'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0495P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10844
_refine_ls_number_parameters     1042
_refine_ls_number_restraints     516
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.97877(4) 0.25709(3) 0.01791(2) 0.02421(15) Uani 1 1 d . U . . .
N1 N 0.8780(6) 0.1340(5) 0.0270(4) 0.0241(16) Uani 1 1 d . U . . .
C2 C 0.7942(8) 0.1178(6) 0.0892(5) 0.034(2) Uani 1 1 d . U . . .
H2A H 0.784496 0.145828 0.133461 0.041 Uiso 1 1 calc R U . . .
C3 C 0.7203(8) 0.0615(6) 0.0920(5) 0.031(2) Uani 1 1 d . U . . .
H3A H 0.662905 0.051034 0.136963 0.037 Uiso 1 1 calc R U . . .
C4 C 0.7344(9) 0.0226(7) 0.0276(6) 0.045(3) Uani 1 1 d . U . . .
H4A H 0.683029 -0.012707 0.025926 0.054 Uiso 1 1 calc R U . . .
C5 C 0.8231(9) 0.0346(6) -0.0346(5) 0.036(2) Uani 1 1 d . U . . .
H5A H 0.837959 0.003036 -0.077370 0.044 Uiso 1 1 calc R U . . .
C6 C 0.8912(8) 0.0926(6) -0.0355(5) 0.0234(19) Uani 1 1 d . U . . .
C7 C 0.9901(9) 0.1092(6) -0.1013(5) 0.028(2) Uani 1 1 d . U . . .
C8 C 1.0113(10) 0.0738(7) -0.1699(5) 0.044(3) Uani 1 1 d . U . . .
H8A H 0.963826 0.037414 -0.175756 0.052 Uiso 1 1 calc R U . . .
C9 C 1.1001(11) 0.0915(7) -0.2286(6) 0.051(3) Uani 1 1 d . U . . .
H9A H 1.112000 0.069793 -0.276495 0.062 Uiso 1 1 calc R U . . .
C10 C 1.1712(9) 0.1395(7) -0.2194(5) 0.041(3) Uani 1 1 d . U . . .
H10A H 1.237338 0.148338 -0.258609 0.049 Uiso 1 1 calc R U . . .
C11 C 1.1442(9) 0.1765(7) -0.1492(6) 0.047(3) Uani 1 1 d . U . . .
H11A H 1.190612 0.213533 -0.143074 0.056 Uiso 1 1 calc R U . . .
N12 N 1.0553(6) 0.1609(5) -0.0910(4) 0.0260(16) Uani 1 1 d . U . . .
O21 O 0.8576(6) 0.3148(4) -0.0796(3) 0.0328(15) Uani 1 1 d . U . . .
C22 C 0.7483(9) 0.3330(6) -0.0802(6) 0.035(2) Uani 1 1 d . U . . .
C23 C 0.6548(10) 0.3489(7) -0.0172(6) 0.046(3) Uani 1 1 d . U . . .
H23A H 0.574349 0.363278 -0.025031 0.056 Uiso 1 1 calc R U . . .
C24 C 0.6765(9) 0.3442(6) 0.0560(6) 0.034(2) Uani 1 1 d . U . . .
O25 O 0.7761(6) 0.3229(4) 0.0773(3) 0.0331(15) Uani 1 1 d . U . . .
C26 C 0.7179(8) 0.3379(7) -0.1603(7) 0.054(3) Uani 1 1 d D U . . .
C27 C 0.5687(9) 0.3663(7) 0.1218(6) 0.051(3) Uani 1 1 d D U . . .
F21A F 0.7389(14) 0.4091(8) -0.2069(6) 0.091(4) Uani 0.7 1 d D U P A 1
F22A F 0.6055(8) 0.3386(9) -0.1590(5) 0.073(3) Uani 0.7 1 d D U P A 1
F23A F 0.7809(11) 0.2654(7) -0.1931(6) 0.078(3) Uani 0.7 1 d D U P A 1
F21B F 0.708(4) 0.2616(17) -0.169(2) 0.147(18) Uiso 0.3 1 d D . P A 2
F22B F 0.799(2) 0.3633(19) -0.2162(15) 0.079(10) Uiso 0.3 1 d D . P A 2
F23B F 0.620(2) 0.4039(18) -0.1678(19) 0.109(11) Uiso 0.3 1 d D . P A 2
F24 F 0.5700(8) 0.3008(7) 0.1787(5) 0.128(4) Uani 1 1 d D U . . .
F25 F 0.4658(6) 0.3808(7) 0.1021(5) 0.118(3) Uani 1 1 d D U . . .
F26 F 0.5686(7) 0.4294(7) 0.1545(6) 0.137(4) Uani 1 1 d D U . . .
O31 O 1.1862(5) 0.1911(4) 0.0273(3) 0.0296(14) Uani 1 1 d . U . . .
C32 C 1.2405(9) 0.1704(6) 0.0822(6) 0.036(2) Uani 1 1 d . U . . .
C33 C 1.1937(10) 0.1517(7) 0.1609(5) 0.043(3) Uani 1 1 d . U . . .
H33A H 1.245277 0.136091 0.197807 0.052 Uiso 1 1 calc R U . . .
C34 C 1.0720(10) 0.1556(7) 0.1860(5) 0.037(2) Uani 1 1 d . U . . .
O35 O 0.9907(6) 0.1771(4) 0.1461(3) 0.0307(15) Uani 1 1 d . U . . .
C36 C 1.3753(10) 0.1617(6) 0.0610(6) 0.047(3) Uani 1 1 d D U . . .
C37 C 1.0308(9) 0.1286(6) 0.2729(6) 0.048(3) Uani 1 1 d D U . . .
F31 F 1.3983(6) 0.2321(6) 0.0130(5) 0.108(3) Uani 1 1 d D U . . .
F32 F 1.4324(6) 0.0923(6) 0.0250(6) 0.108(3) Uani 1 1 d D U . . .
F33 F 1.4297(6) 0.1574(7) 0.1172(4) 0.104(3) Uani 1 1 d D U . . .
F34A F 1.112(2) 0.118(3) 0.3144(17) 0.098(11) Uani 0.39 1 d D U P B 1
F35A F 0.997(4) 0.0560(17) 0.2876(16) 0.114(14) Uani 0.39 1 d D U P B 1
F36A F 0.941(3) 0.1908(19) 0.3001(15) 0.111(12) Uani 0.39 1 d D U P B 1
F34B F 0.9293(16) 0.1097(16) 0.2876(9) 0.099(7) Uani 0.61 1 d D U P B 2
F35B F 1.013(2) 0.1923(11) 0.3138(8) 0.079(5) Uani 0.61 1 d D U P B 2
F36B F 1.1087(18) 0.0622(15) 0.3020(12) 0.141(11) Uani 0.61 1 d D U P B 2
O41 O 1.0152(6) 0.3593(4) 0.0868(3) 0.0344(16) Uani 1 1 d . U . . .
C42 C 1.0940(9) 0.4015(6) 0.0723(6) 0.033(2) Uani 1 1 d . U . . .
C43 C 1.1609(9) 0.4241(7) 0.0021(6) 0.042(3) Uani 1 1 d . U . . .
H43A H 1.213219 0.460452 -0.000948 0.050 Uiso 1 1 calc R U . . .
C44 C 1.1542(9) 0.3960(6) -0.0633(6) 0.034(2) Uani 1 1 d . U . . .
O45 O 1.0900(6) 0.3500(4) -0.0736(3) 0.0353(16) Uani 1 1 d . U . . .
C46 C 1.1145(8) 0.4277(6) 0.1448(5) 0.038(2) Uani 1 1 d D U . . .
C47 C 1.2402(11) 0.4197(7) -0.1369(7) 0.050(3) Uani 1 1 d . U . . .
F41A F 1.1717(15) 0.3552(5) 0.1851(7) 0.121(5) Uani 0.8 1 d D U P C 1
F42A F 1.0200(7) 0.4694(7) 0.1888(4) 0.064(2) Uani 0.8 1 d D U P C 1
F43A F 1.1882(9) 0.4805(7) 0.1290(5) 0.077(3) Uani 0.8 1 d D U P C 1
F41B F 1.080(6) 0.5133(13) 0.152(4) 0.25(4) Uiso 0.2 1 d D . P C 2
F42B F 1.2240(17) 0.400(3) 0.159(2) 0.086(14) Uiso 0.2 1 d D . P C 2
F43B F 1.052(3) 0.394(3) 0.2097(15) 0.075(11) Uiso 0.2 1 d D . P C 2
F44 F 1.3527(6) 0.3885(6) -0.1293(4) 0.097(3) Uani 1 1 d D U . . .
F45 F 1.2227(7) 0.5065(4) -0.1565(4) 0.080(2) Uani 1 1 d D U . . .
F46 F 1.2284(7) 0.3903(5) -0.2000(4) 0.089(3) Uani 1 1 d D U . . .
Sm2 Sm 0.47387(4) 0.24271(3) 0.52938(2) 0.02480(15) Uani 1 1 d . U . . .
N51 N 0.6006(7) 0.3362(5) 0.4329(4) 0.0325(18) Uani 1 1 d . U . . .
C52 C 0.6447(9) 0.3173(7) 0.3579(5) 0.043(3) Uani 1 1 d . U . . .
H52A H 0.611186 0.280148 0.338584 0.051 Uiso 1 1 calc R U . . .
C53 C 0.7367(10) 0.3506(7) 0.3092(5) 0.044(3) Uani 1 1 d . U . . .
H53A H 0.760012 0.341467 0.256324 0.053 Uiso 1 1 calc R U . . .
C54 C 0.7907(10) 0.3954(8) 0.3388(6) 0.050(3) Uani 1 1 d . U . . .
H54A H 0.858029 0.413797 0.307746 0.060 Uiso 1 1 calc R U . . .
C55 C 0.7525(9) 0.4154(7) 0.4118(6) 0.046(3) Uani 1 1 d . U . . .
H55A H 0.790313 0.449279 0.431512 0.056 Uiso 1 1 calc R U . . .
C56 C 0.6558(8) 0.3852(6) 0.4580(5) 0.029(2) Uani 1 1 d . U . . .
C57 C 0.6066(9) 0.4067(6) 0.5391(5) 0.030(2) Uani 1 1 d . U . . .
C58 C 0.6422(9) 0.4634(7) 0.5719(5) 0.039(2) Uani 1 1 d . U . . .
H58A H 0.703904 0.489961 0.543205 0.046 Uiso 1 1 calc R U . . .
C59 C 0.5896(10) 0.4826(7) 0.6462(5) 0.042(3) Uani 1 1 d . U . . .
H59A H 0.615472 0.521329 0.668970 0.051 Uiso 1 1 calc R U . . .
C60 C 0.5003(9) 0.4450(6) 0.6861(5) 0.035(2) Uani 1 1 d . U . . .
H60A H 0.461552 0.458197 0.736729 0.043 Uiso 1 1 calc R U . . .
C61 C 0.4661(9) 0.3862(6) 0.6514(5) 0.034(2) Uani 1 1 d . U . . .
H61A H 0.404355 0.359471 0.679677 0.040 Uiso 1 1 calc R U . . .
N62 N 0.5174(6) 0.3669(5) 0.5800(4) 0.0250(16) Uani 1 1 d . U . . .
O71 O 0.5551(6) 0.1508(4) 0.4267(3) 0.0363(16) Uani 1 1 d . U . . .
C72 C 0.5104(10) 0.1079(7) 0.3959(5) 0.036(2) Uani 1 1 d . U . . .
C73 C 0.4077(9) 0.0797(7) 0.4242(5) 0.040(3) Uani 1 1 d . U . . .
H73A H 0.384220 0.045816 0.395018 0.048 Uiso 1 1 calc R U . . .
C74 C 0.3380(9) 0.1007(7) 0.4954(6) 0.035(2) Uani 1 1 d . U . . .
O75 O 0.3563(6) 0.1403(4) 0.5420(3) 0.0318(15) Uani 1 1 d . U . . .
C76 C 0.5769(12) 0.0871(8) 0.3145(6) 0.054(3) Uani 1 1 d . U . . .
C77 C 0.2210(10) 0.0738(6) 0.5180(5) 0.047(2) Uani 1 1 d D U . . .
F71 F 0.5098(8) 0.1234(6) 0.2628(4) 0.114(3) Uani 1 1 d . U . . .
F72 F 0.6737(8) 0.1167(6) 0.2900(4) 0.096(3) Uani 1 1 d . U . . .
F73 F 0.6107(7) 0.0006(5) 0.3092(4) 0.086(3) Uani 1 1 d . U . . .
F74A F 0.209(3) 0.0187(17) 0.4766(14) 0.089(8) Uani 0.54 1 d D U P D 1
F75A F 0.205(4) 0.033(2) 0.5889(14) 0.096(11) Uani 0.54 1 d D U P D 1
F76A F 0.133(2) 0.1453(13) 0.504(2) 0.139(12) Uani 0.54 1 d D U P D 1
F74B F 0.136(2) 0.132(2) 0.558(2) 0.152(16) Uani 0.46 1 d D U P D 2
F75B F 0.179(4) 0.055(3) 0.4647(12) 0.145(17) Uani 0.46 1 d D U P D 2
F76B F 0.223(4) 0.008(2) 0.5740(17) 0.078(11) Uani 0.46 1 d D U P D 2
O81 O 0.2781(6) 0.3224(4) 0.5901(3) 0.0345(15) Uani 1 1 d . U . . .
C82 C 0.1786(9) 0.3454(6) 0.5707(6) 0.032(2) Uani 1 1 d . U . . .
C83 C 0.1509(10) 0.3497(7) 0.4977(6) 0.042(2) Uani 1 1 d . U . . .
H83A H 0.069677 0.363747 0.491503 0.050 Uiso 1 1 calc R U . . .
C84 C 0.2436(10) 0.3331(7) 0.4342(6) 0.039(2) Uani 1 1 d . U . . .
O85 O 0.3541(6) 0.3108(4) 0.4319(3) 0.0366(16) Uani 1 1 d . U . . .
C86 C 0.0719(9) 0.3751(6) 0.6350(6) 0.043(2) Uani 1 1 d D U . . .
C87 C 0.2073(11) 0.3410(8) 0.3547(6) 0.045(3) Uani 1 1 d . U . . .
F81A F 0.084(3) 0.427(3) 0.6778(19) 0.150(15) Uani 0.53 1 d D U P E 1
F82A F -0.0259(16) 0.421(2) 0.6098(13) 0.112(10) Uani 0.53 1 d D U P E 1
F83A F 0.044(3) 0.3086(16) 0.682(2) 0.145(15) Uani 0.53 1 d D U P E 1
F81B F -0.0277(18) 0.363(2) 0.6291(18) 0.108(11) Uani 0.47 1 d D U P E 2
F82B F 0.090(3) 0.335(3) 0.7039(12) 0.111(13) Uani 0.47 1 d D U P E 2
F83B F 0.060(3) 0.4580(12) 0.6392(17) 0.092(11) Uani 0.47 1 d D U P E 2
F84 F 0.2617(8) 0.2704(5) 0.3212(4) 0.101(3) Uani 1 1 d . U . . .
F85 F 0.2310(8) 0.4098(5) 0.3097(4) 0.094(3) Uani 1 1 d . U . . .
F86 F 0.0913(7) 0.3498(6) 0.3598(4) 0.088(2) Uani 1 1 d . U . . .
O91 O 0.4772(6) 0.1799(4) 0.6637(3) 0.0299(14) Uani 1 1 d . U . . .
C92 C 0.5563(9) 0.1575(6) 0.7053(5) 0.035(2) Uani 1 1 d . U . . .
C93 C 0.6782(9) 0.1508(7) 0.6812(6) 0.040(3) Uani 1 1 d . U . . .
H93A H 0.728449 0.136711 0.718776 0.048 Uiso 1 1 calc R U . . .
C94 C 0.7272(9) 0.1642(7) 0.6038(6) 0.036(2) Uani 1 1 d . U . . .
O95 O 0.6761(6) 0.1827(4) 0.5464(4) 0.0341(15) Uani 1 1 d . U . . .
C96 C 0.5109(11) 0.1357(8) 0.7918(6) 0.048(3) Uani 1 1 d . U . . .
C97 C 0.8638(10) 0.1585(8) 0.5799(7) 0.046(3) Uani 1 1 d . U . . .
F91 F 0.4632(8) 0.0688(6) 0.8066(4) 0.103(3) Uani 1 1 d D U . . .
F92 F 0.4261(8) 0.2038(5) 0.8183(4) 0.095(3) Uani 1 1 d D U . . .
F93 F 0.5930(7) 0.1178(6) 0.8348(4) 0.090(3) Uani 1 1 d D U . . .
F94 F 0.9158(7) 0.1423(7) 0.6416(5) 0.117(3) Uani 1 1 d . U . . .
F95 F 0.9190(6) 0.0970(6) 0.5388(6) 0.120(4) Uani 1 1 d . U . . .
F96 F 0.8815(6) 0.2330(5) 0.5443(5) 0.098(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O21 2.385(6) . ?
Sm1 O41 2.401(6) . ?
Sm1 O31 2.404(6) . ?
Sm1 O35 2.405(6) . ?
Sm1 O25 2.405(6) . ?
Sm1 O45 2.409(5) . ?
Sm1 N1 2.534(7) . ?
Sm1 N12 2.545(7) . ?
N1 C2 1.351(10) . ?
N1 C6 1.361(11) . ?
C2 C3 1.412(13) . ?
C2 H2A 0.9500 . ?
C3 C4 1.364(13) . ?
C3 H3A 0.9500 . ?
C4 C5 1.372(12) . ?
C4 H4A 0.9500 . ?
C5 C6 1.387(12) . ?
C5 H5A 0.9500 . ?
C6 C7 1.503(12) . ?
C7 N12 1.343(12) . ?
C7 C8 1.388(12) . ?
C8 C9 1.358(13) . ?
C8 H8A 0.9500 . ?
C9 C10 1.345(15) . ?
C9 H9A 0.9500 . ?
C10 C11 1.421(14) . ?
C10 H10A 0.9500 . ?
C11 N12 1.345(10) . ?
C11 H11A 0.9500 . ?
O21 C22 1.243(11) . ?
C22 C23 1.392(13) . ?
C22 C26 1.538(15) . ?
C23 C24 1.375(14) . ?
C23 H23A 0.9500 . ?
C24 O25 1.255(11) . ?
C24 C27 1.533(14) . ?
C26 F21B 1.292(15) . ?
C26 F22B 1.308(15) . ?
C26 F21A 1.316(11) . ?
C26 F22A 1.324(11) . ?
C26 F23B 1.327(15) . ?
C26 F23A 1.334(11) . ?
C27 F26 1.254(10) . ?
C27 F25 1.290(10) . ?
C27 F24 1.303(10) . ?
O31 C32 1.235(11) . ?
C32 C33 1.397(13) . ?
C32 C36 1.528(14) . ?
C33 C34 1.397(14) . ?
C33 H33A 0.9500 . ?
C34 O35 1.258(11) . ?
C34 C37 1.534(13) . ?
C36 F33 1.294(10) . ?
C36 F32 1.312(10) . ?
C36 F31 1.324(10) . ?
C37 F34B 1.283(12) . ?
C37 F35A 1.287(13) . ?
C37 F36B 1.290(12) . ?
C37 F36A 1.294(14) . ?
C37 F34A 1.300(13) . ?
C37 F35B 1.300(12) . ?
O41 C42 1.256(11) . ?
C42 C43 1.369(12) . ?
C42 C46 1.525(13) . ?
C43 C44 1.357(13) . ?
C43 H43A 0.9500 . ?
C44 O45 1.261(11) . ?
C44 C47 1.527(12) . ?
C46 F42A 1.294(9) . ?
C46 F42B 1.312(16) . ?
C46 F41A 1.318(10) . ?
C46 F41B 1.319(16) . ?
C46 F43A 1.331(10) . ?
C46 F43B 1.338(15) . ?
C47 F44 1.308(13) . ?
C47 F45 1.317(12) . ?
C47 F46 1.353(13) . ?
Sm2 O95 2.371(7) . ?
Sm2 O75 2.383(6) . ?
Sm2 O85 2.389(7) . ?
Sm2 O81 2.414(6) . ?
Sm2 O71 2.415(6) . ?
Sm2 O91 2.417(5) . ?
Sm2 N62 2.544(7) . ?
Sm2 N51 2.562(7) . ?
N51 C56 1.344(12) . ?
N51 C52 1.381(11) . ?
C52 C53 1.398(13) . ?
C52 H52A 0.9500 . ?
C53 C54 1.328(15) . ?
C53 H53A 0.9500 . ?
C54 C55 1.348(14) . ?
C54 H54A 0.9500 . ?
C55 C56 1.401(12) . ?
C55 H55A 0.9500 . ?
C56 C57 1.499(12) . ?
C57 C58 1.369(13) . ?
C57 N62 1.382(11) . ?
C58 C59 1.385(12) . ?
C58 H58A 0.9500 . ?
C59 C60 1.358(13) . ?
C59 H59A 0.9500 . ?
C60 C61 1.408(13) . ?
C60 H60A 0.9500 . ?
C61 N62 1.334(11) . ?
C61 H61A 0.9500 . ?
O71 C72 1.241(11) . ?
C72 C73 1.374(13) . ?
C72 C76 1.537(13) . ?
C73 C74 1.393(12) . ?
C73 H73A 0.9500 . ?
C74 O75 1.225(11) . ?
C74 C77 1.516(14) . ?
C76 F71 1.294(14) . ?
C76 F72 1.318(14) . ?
C76 F73 1.326(12) . ?
C77 F75B 1.295(15) . ?
C77 F76B 1.291(15) . ?
C77 F75A 1.304(15) . ?
C77 F74A 1.307(13) . ?
C77 F76A 1.321(14) . ?
C77 F74B 1.330(15) . ?
O81 C82 1.236(11) . ?
C82 C83 1.402(13) . ?
C82 C86 1.531(13) . ?
C83 C84 1.394(13) . ?
C83 H83A 0.9500 . ?
C84 O85 1.246(12) . ?
C84 C87 1.550(14) . ?
C86 F81A 1.282(15) . ?
C86 F81B 1.284(14) . ?
C86 F83A 1.288(14) . ?
C86 F83B 1.295(14) . ?
C86 F82A 1.302(14) . ?
C86 F82B 1.304(15) . ?
C87 F85 1.285(11) . ?
C87 F84 1.298(12) . ?
C87 F86 1.324(13) . ?
O91 C92 1.257(11) . ?
C92 C93 1.389(13) . ?
C92 C96 1.523(13) . ?
C93 C94 1.375(13) . ?
C93 H93A 0.9500 . ?
C94 O95 1.252(11) . ?
C94 C97 1.559(13) . ?
C96 F91 1.300(13) . ?
C96 F93 1.309(13) . ?
C96 F92 1.321(13) . ?
C97 F95 1.266(13) . ?
C97 F96 1.278(12) . ?
C97 F94 1.330(13) . ?

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
O21 Sm1 O41 118.9(2) . . ?
O21 Sm1 O31 139.0(2) . . ?
O41 Sm1 O31 78.7(2) . . ?
O21 Sm1 O35 145.9(2) . . ?
O41 Sm1 O35 75.7(2) . . ?
O31 Sm1 O35 71.1(2) . . ?
O21 Sm1 O25 70.6(2) . . ?
O41 Sm1 O25 80.4(2) . . ?
O31 Sm1 O25 150.0(2) . . ?
O35 Sm1 O25 83.1(2) . . ?
O21 Sm1 O45 77.4(2) . . ?
O41 Sm1 O45 71.9(2) . . ?
O31 Sm1 O45 73.9(2) . . ?
O35 Sm1 O45 135.9(2) . . ?
O25 Sm1 O45 119.2(2) . . ?
O21 Sm1 N1 77.9(2) . . ?
O41 Sm1 N1 145.8(2) . . ?
O31 Sm1 N1 108.9(2) . . ?
O35 Sm1 N1 75.7(2) . . ?
O25 Sm1 N1 77.9(2) . . ?
O45 Sm1 N1 142.2(2) . . ?
O21 Sm1 N12 70.4(2) . . ?
O41 Sm1 N12 147.6(2) . . ?
O31 Sm1 N12 76.7(2) . . ?
O35 Sm1 N12 115.0(2) . . ?
O25 Sm1 N12 129.7(2) . . ?
O45 Sm1 N12 81.2(2) . . ?
N1 Sm1 N12 63.8(2) . . ?
C2 N1 C6 117.3(8) . . ?
C2 N1 Sm1 121.0(6) . . ?
C6 N1 Sm1 120.9(5) . . ?
N1 C2 C3 123.6(9) . . ?
N1 C2 H2A 118.2 . . ?
C3 C2 H2A 118.2 . . ?
C4 C3 C2 117.5(8) . . ?
C4 C3 H3A 121.3 . . ?
C2 C3 H3A 121.3 . . ?
C3 C4 C5 119.8(9) . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 C6 120.4(9) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
N1 C6 C5 121.2(8) . . ?
N1 C6 C7 115.0(8) . . ?
C5 C6 C7 123.6(8) . . ?
N12 C7 C8 121.8(8) . . ?
N12 C7 C6 116.8(8) . . ?
C8 C7 C6 121.4(9) . . ?
C9 C8 C7 119.7(10) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C10 C9 C8 120.4(10) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
C9 C10 C11 117.9(9) . . ?
C9 C10 H10A 121.1 . . ?
C11 C10 H10A 121.1 . . ?
N12 C11 C10 122.3(10) . . ?
N12 C11 H11A 118.9 . . ?
C10 C11 H11A 118.9 . . ?
C7 N12 C11 117.7(8) . . ?
C7 N12 Sm1 120.0(5) . . ?
C11 N12 Sm1 120.4(7) . . ?
C22 O21 Sm1 134.8(6) . . ?
O21 C22 C23 126.9(10) . . ?
O21 C22 C26 114.4(9) . . ?
C23 C22 C26 118.7(10) . . ?
C24 C23 C22 121.4(10) . . ?
C24 C23 H23A 119.3 . . ?
C22 C23 H23A 119.3 . . ?
O25 C24 C23 127.9(10) . . ?
O25 C24 C27 113.8(9) . . ?
C23 C24 C27 118.3(9) . . ?
C24 O25 Sm1 134.1(6) . . ?
F21B C26 F22B 110(2) . . ?
F21A C26 F22A 107.5(10) . . ?
F21B C26 F23B 113(2) . . ?
F22B C26 F23B 102.8(17) . . ?
F21A C26 F23A 109.1(11) . . ?
F22A C26 F23A 102.9(11) . . ?
F21B C26 C22 110(2) . . ?
F22B C26 C22 111.4(17) . . ?
F21A C26 C22 111.3(10) . . ?
F22A C26 C22 114.6(9) . . ?
F23B C26 C22 108.6(18) . . ?
F23A C26 C22 111.0(9) . . ?
F26 C27 F25 109.6(10) . . ?
F26 C27 F24 102.6(11) . . ?
F25 C27 F24 104.1(10) . . ?
F26 C27 C24 113.4(9) . . ?
F25 C27 C24 114.4(9) . . ?
F24 C27 C24 111.8(9) . . ?
C32 O31 Sm1 132.8(6) . . ?
O31 C32 C33 127.7(10) . . ?
O31 C32 C36 115.8(9) . . ?
C33 C32 C36 116.5(9) . . ?
C34 C33 C32 120.9(10) . . ?
C34 C33 H33A 119.6 . . ?
C32 C33 H33A 119.6 . . ?
O35 C34 C33 128.2(9) . . ?
O35 C34 C37 114.9(9) . . ?
C33 C34 C37 116.9(9) . . ?
C34 O35 Sm1 132.1(6) . . ?
F33 C36 F32 107.3(10) . . ?
F33 C36 F31 103.1(9) . . ?
F32 C36 F31 106.2(9) . . ?
F33 C36 C32 116.8(9) . . ?
F32 C36 C32 111.6(9) . . ?
F31 C36 C32 111.1(8) . . ?
F34B C37 F36B 109.0(14) . . ?
F35A C37 F36A 107.6(18) . . ?
F35A C37 F34A 107.2(16) . . ?
F36A C37 F34A 105.3(16) . . ?
F34B C37 F35B 103.9(13) . . ?
F36B C37 F35B 105.8(14) . . ?
F34B C37 C34 112.4(11) . . ?
F35A C37 C34 112.9(15) . . ?
F36B C37 C34 112.2(13) . . ?
F36A C37 C34 109.8(15) . . ?
F34A C37 C34 113.7(16) . . ?
F35B C37 C34 112.9(10) . . ?
C42 O41 Sm1 132.0(6) . . ?
O41 C42 C43 128.3(10) . . ?
O41 C42 C46 112.8(8) . . ?
C43 C42 C46 118.9(9) . . ?
C44 C43 C42 121.5(9) . . ?
C44 C43 H43A 119.2 . . ?
C42 C43 H43A 119.2 . . ?
O45 C44 C43 130.4(8) . . ?
O45 C44 C47 113.0(9) . . ?
C43 C44 C47 116.5(9) . . ?
C44 O45 Sm1 130.7(6) . . ?
F42A C46 F41A 110.2(10) . . ?
F42B C46 F41B 105(2) . . ?
F42A C46 F43A 104.6(8) . . ?
F41A C46 F43A 103.9(10) . . ?
F42B C46 F43B 102.0(19) . . ?
F41B C46 F43B 101(2) . . ?
F42A C46 C42 116.3(8) . . ?
F42B C46 C42 117(2) . . ?
F41A C46 C42 108.2(8) . . ?
F41B C46 C42 117(3) . . ?
F43A C46 C42 113.0(8) . . ?
F43B C46 C42 112.2(18) . . ?
F44 C47 F45 106.1(10) . . ?
F44 C47 F46 107.2(10) . . ?
F45 C47 F46 104.7(9) . . ?
F44 C47 C44 112.5(10) . . ?
F45 C47 C44 112.2(9) . . ?
F46 C47 C44 113.6(9) . . ?
O95 Sm2 O75 117.4(2) . . ?
O95 Sm2 O85 142.0(2) . . ?
O75 Sm2 O85 78.3(2) . . ?
O95 Sm2 O81 143.3(2) . . ?
O75 Sm2 O81 77.2(2) . . ?
O85 Sm2 O81 71.1(2) . . ?
O95 Sm2 O71 78.4(2) . . ?
O75 Sm2 O71 70.7(2) . . ?
O85 Sm2 O71 75.0(2) . . ?
O81 Sm2 O71 137.1(2) . . ?
O95 Sm2 O91 71.0(2) . . ?
O75 Sm2 O91 80.8(2) . . ?
O85 Sm2 O91 146.8(2) . . ?
O81 Sm2 O91 79.4(2) . . ?
O71 Sm2 O91 121.3(2) . . ?
O95 Sm2 N62 76.9(2) . . ?
O75 Sm2 N62 149.6(2) . . ?
O85 Sm2 N62 107.5(2) . . ?
O81 Sm2 N62 76.8(2) . . ?
O71 Sm2 N62 139.6(2) . . ?
O91 Sm2 N62 79.3(2) . . ?
O95 Sm2 N51 72.1(2) . . ?
O75 Sm2 N51 144.6(2) . . ?
O85 Sm2 N51 76.6(2) . . ?
O81 Sm2 N51 116.6(2) . . ?
O71 Sm2 N51 79.0(2) . . ?
O91 Sm2 N51 132.0(2) . . ?
N62 Sm2 N51 63.2(2) . . ?
C56 N51 C52 115.8(8) . . ?
C56 N51 Sm2 120.6(5) . . ?
C52 N51 Sm2 120.5(6) . . ?
N51 C52 C53 122.5(10) . . ?
N51 C52 H52A 118.7 . . ?
C53 C52 H52A 118.7 . . ?
C54 C53 C52 118.3(9) . . ?
C54 C53 H53A 120.8 . . ?
C52 C53 H53A 120.8 . . ?
C53 C54 C55 121.7(10) . . ?
C53 C54 H54A 119.2 . . ?
C55 C54 H54A 119.2 . . ?
C54 C55 C56 118.7(11) . . ?
C54 C55 H55A 120.7 . . ?
C56 C55 H55A 120.7 . . ?
N51 C56 C55 122.7(9) . . ?
N51 C56 C57 115.6(8) . . ?
C55 C56 C57 121.7(10) . . ?
C58 C57 N62 120.4(8) . . ?
C58 C57 C56 124.1(9) . . ?
N62 C57 C56 115.5(8) . . ?
C57 C58 C59 121.0(9) . . ?
C57 C58 H58A 119.5 . . ?
C59 C58 H58A 119.5 . . ?
C60 C59 C58 118.8(9) . . ?
C60 C59 H59A 120.6 . . ?
C58 C59 H59A 120.6 . . ?
C59 C60 C61 119.1(8) . . ?
C59 C60 H60A 120.4 . . ?
C61 C60 H60A 120.4 . . ?
N62 C61 C60 122.2(9) . . ?
N62 C61 H61A 118.9 . . ?
C60 C61 H61A 118.9 . . ?
C61 N62 C57 118.5(8) . . ?
C61 N62 Sm2 120.2(6) . . ?
C57 N62 Sm2 120.7(5) . . ?
C72 O71 Sm2 132.6(6) . . ?
O71 C72 C73 128.4(9) . . ?
O71 C72 C76 115.0(9) . . ?
C73 C72 C76 116.6(10) . . ?
C72 C73 C74 120.2(9) . . ?
C72 C73 H73A 119.9 . . ?
C74 C73 H73A 119.9 . . ?
O75 C74 C73 129.0(9) . . ?
O75 C74 C77 114.9(8) . . ?
C73 C74 C77 116.1(9) . . ?
C74 O75 Sm2 132.9(6) . . ?
F71 C76 F72 105.4(10) . . ?
F71 C76 F73 105.6(10) . . ?
F72 C76 F73 106.8(10) . . ?
F71 C76 C72 111.6(10) . . ?
F72 C76 C72 113.9(10) . . ?
F73 C76 C72 112.9(9) . . ?
F75B C77 F76B 107(2) . . ?
F75A C77 F74A 104(2) . . ?
F75A C77 F76A 113(2) . . ?
F74A C77 F76A 102(2) . . ?
F75B C77 F74B 110(3) . . ?
F76B C77 F74B 95(2) . . ?
F75B C77 C74 118.6(16) . . ?
F76B C77 C74 113(2) . . ?
F75A C77 C74 113(2) . . ?
F74A C77 C74 115.9(15) . . ?
F76A C77 C74 108.1(15) . . ?
F74B C77 C74 111.4(18) . . ?
C82 O81 Sm2 132.5(6) . . ?
O81 C82 C83 128.8(9) . . ?
O81 C82 C86 115.2(9) . . ?
C83 C82 C86 116.0(9) . . ?
C84 C83 C82 119.4(10) . . ?
C84 C83 H83A 120.3 . . ?
C82 C83 H83A 120.3 . . ?
O85 C84 C83 129.1(10) . . ?
O85 C84 C87 113.9(10) . . ?
C83 C84 C87 117.0(10) . . ?
C84 O85 Sm2 132.3(6) . . ?
F81A C86 F83A 106(2) . . ?
F81B C86 F83B 111(2) . . ?
F81A C86 F82A 102(2) . . ?
F83A C86 F82A 106.0(18) . . ?
F81B C86 F82B 104.8(19) . . ?
F83B C86 F82B 103(2) . . ?
F81A C86 C82 116.1(16) . . ?
F81B C86 C82 115.8(15) . . ?
F83A C86 C82 112.1(16) . . ?
F83B C86 C82 108.0(13) . . ?
F82A C86 C82 113.9(13) . . ?
F82B C86 C82 113.0(15) . . ?
F85 C87 F84 109.3(10) . . ?
F85 C87 F86 106.4(10) . . ?
F84 C87 F86 105.3(10) . . ?
F85 C87 C84 110.4(9) . . ?
F84 C87 C84 111.7(10) . . ?
F86 C87 C84 113.3(10) . . ?
C92 O91 Sm2 134.0(6) . . ?
O91 C92 C93 127.3(9) . . ?
O91 C92 C96 115.1(9) . . ?
C93 C92 C96 117.6(10) . . ?
C94 C93 C92 121.0(10) . . ?
C94 C93 H93A 119.5 . . ?
C92 C93 H93A 119.5 . . ?
O95 C94 C93 128.7(10) . . ?
O95 C94 C97 112.3(9) . . ?
C93 C94 C97 119.0(10) . . ?
C94 O95 Sm2 134.0(6) . . ?
F91 C96 F93 107.7(10) . . ?
F91 C96 F92 106.2(10) . . ?
F93 C96 F92 105.5(10) . . ?
F91 C96 C92 111.8(9) . . ?
F93 C96 C92 114.3(10) . . ?
F92 C96 C92 110.8(9) . . ?
F95 C97 F96 110.1(11) . . ?
F95 C97 F94 107.1(11) . . ?
F96 C97 F94 104.6(10) . . ?
F95 C97 C94 112.0(9) . . ?
F96 C97 C94 111.2(9) . . ?
F94 C97 C94 111.6(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 C3 -0.6(14) . . . . ?
Sm1 N1 C2 C3 168.6(7) . . . . ?
N1 C2 C3 C4 -0.7(15) . . . . ?
C2 C3 C4 C5 4.0(15) . . . . ?
C3 C4 C5 C6 -6.0(16) . . . . ?
C2 N1 C6 C5 -1.4(13) . . . . ?
Sm1 N1 C6 C5 -170.6(7) . . . . ?
C2 N1 C6 C7 -176.8(8) . . . . ?
Sm1 N1 C6 C7 14.0(10) . . . . ?
C4 C5 C6 N1 4.7(15) . . . . ?
C4 C5 C6 C7 179.8(9) . . . . ?
N1 C6 C7 N12 1.2(12) . . . . ?
C5 C6 C7 N12 -174.1(9) . . . . ?
N1 C6 C7 C8 -177.7(9) . . . . ?
C5 C6 C7 C8 7.0(15) . . . . ?
N12 C7 C8 C9 0.0(16) . . . . ?
C6 C7 C8 C9 178.8(10) . . . . ?
C7 C8 C9 C10 3.1(18) . . . . ?
C8 C9 C10 C11 -4.9(17) . . . . ?
C9 C10 C11 N12 3.8(16) . . . . ?
C8 C7 N12 C11 -1.1(14) . . . . ?
C6 C7 N12 C11 180.0(8) . . . . ?
C8 C7 N12 Sm1 163.3(7) . . . . ?
C6 C7 N12 Sm1 -15.6(11) . . . . ?
C10 C11 N12 C7 -0.8(15) . . . . ?
C10 C11 N12 Sm1 -165.1(8) . . . . ?
Sm1 O21 C22 C23 20.4(15) . . . . ?
Sm1 O21 C22 C26 -159.8(6) . . . . ?
O21 C22 C23 C24 -1.1(17) . . . . ?
C26 C22 C23 C24 179.1(9) . . . . ?
C22 C23 C24 O25 -3.0(17) . . . . ?
C22 C23 C24 C27 177.6(9) . . . . ?
C23 C24 O25 Sm1 -11.7(15) . . . . ?
C27 C24 O25 Sm1 167.8(6) . . . . ?
O21 C22 C26 F21B 93(2) . . . . ?
C23 C22 C26 F21B -87(2) . . . . ?
O21 C22 C26 F22B -29.7(18) . . . . ?
C23 C22 C26 F22B 150.1(16) . . . . ?
O21 C22 C26 F21A -71.2(13) . . . . ?
C23 C22 C26 F21A 108.6(13) . . . . ?
O21 C22 C26 F22A 166.6(10) . . . . ?
C23 C22 C26 F22A -13.6(14) . . . . ?
O21 C22 C26 F23B -142.2(18) . . . . ?
C23 C22 C26 F23B 37.6(19) . . . . ?
O21 C22 C26 F23A 50.6(12) . . . . ?
C23 C22 C26 F23A -129.6(11) . . . . ?
O25 C24 C27 F26 59.1(13) . . . . ?
C23 C24 C27 F26 -121.4(12) . . . . ?
O25 C24 C27 F25 -174.3(10) . . . . ?
C23 C24 C27 F25 5.2(14) . . . . ?
O25 C24 C27 F24 -56.3(12) . . . . ?
C23 C24 C27 F24 123.2(11) . . . . ?
Sm1 O31 C32 C33 23.4(15) . . . . ?
Sm1 O31 C32 C36 -158.6(6) . . . . ?
O31 C32 C33 C34 -0.4(17) . . . . ?
C36 C32 C33 C34 -178.4(9) . . . . ?
C32 C33 C34 O35 -2.1(17) . . . . ?
C32 C33 C34 C37 176.6(9) . . . . ?
C33 C34 O35 Sm1 -18.2(16) . . . . ?
C37 C34 O35 Sm1 163.1(6) . . . . ?
O31 C32 C36 F33 166.9(9) . . . . ?
C33 C32 C36 F33 -14.8(14) . . . . ?
O31 C32 C36 F32 -69.2(12) . . . . ?
C33 C32 C36 F32 109.1(11) . . . . ?
O31 C32 C36 F31 49.1(12) . . . . ?
C33 C32 C36 F31 -132.7(10) . . . . ?
O35 C34 C37 F34B 17.4(17) . . . . ?
C33 C34 C37 F34B -161.5(15) . . . . ?
O35 C34 C37 F35A 66(2) . . . . ?
C33 C34 C37 F35A -112(2) . . . . ?
O35 C34 C37 F36B 140.7(18) . . . . ?
C33 C34 C37 F36B -38(2) . . . . ?
O35 C34 C37 F36A -54(2) . . . . ?
C33 C34 C37 F36A 128(2) . . . . ?
O35 C34 C37 F34A -171(2) . . . . ?
C33 C34 C37 F34A 10(2) . . . . ?
O35 C34 C37 F35B -99.8(15) . . . . ?
C33 C34 C37 F35B 81.4(16) . . . . ?
Sm1 O41 C42 C43 22.6(16) . . . . ?
Sm1 O41 C42 C46 -156.5(6) . . . . ?
O41 C42 C43 C44 -4.9(18) . . . . ?
C46 C42 C43 C44 174.2(9) . . . . ?
C42 C43 C44 O45 2.0(19) . . . . ?
C42 C43 C44 C47 -175.5(10) . . . . ?
C43 C44 O45 Sm1 -16.5(17) . . . . ?
C47 C44 O45 Sm1 161.0(6) . . . . ?
O41 C42 C46 F42A -52.2(12) . . . . ?
C43 C42 C46 F42A 128.6(10) . . . . ?
O41 C42 C46 F42B 123(2) . . . . ?
C43 C42 C46 F42B -57(3) . . . . ?
O41 C42 C46 F41A 72.4(13) . . . . ?
C43 C42 C46 F41A -106.9(13) . . . . ?
O41 C42 C46 F41B -111(3) . . . . ?
C43 C42 C46 F41B 70(3) . . . . ?
O41 C42 C46 F43A -173.2(9) . . . . ?
C43 C42 C46 F43A 7.6(13) . . . . ?
O41 C42 C46 F43B 5(2) . . . . ?
C43 C42 C46 F43B -174(2) . . . . ?
O45 C44 C47 F44 -119.4(11) . . . . ?
C43 C44 C47 F44 58.4(14) . . . . ?
O45 C44 C47 F45 121.0(11) . . . . ?
C43 C44 C47 F45 -61.1(14) . . . . ?
O45 C44 C47 F46 2.6(14) . . . . ?
C43 C44 C47 F46 -179.6(10) . . . . ?
C56 N51 C52 C53 -3.3(14) . . . . ?
Sm2 N51 C52 C53 -163.9(8) . . . . ?
N51 C52 C53 C54 6.3(16) . . . . ?
C52 C53 C54 C55 -5.6(18) . . . . ?
C53 C54 C55 C56 2.2(18) . . . . ?
C52 N51 C56 C55 -0.2(14) . . . . ?
Sm2 N51 C56 C55 160.3(8) . . . . ?
C52 N51 C56 C57 179.2(8) . . . . ?
Sm2 N51 C56 C57 -20.2(11) . . . . ?
C54 C55 C56 N51 0.8(16) . . . . ?
C54 C55 C56 C57 -178.6(9) . . . . ?
N51 C56 C57 C58 -172.7(9) . . . . ?
C55 C56 C57 C58 6.7(16) . . . . ?
N51 C56 C57 N62 5.3(13) . . . . ?
C55 C56 C57 N62 -175.2(9) . . . . ?
N62 C57 C58 C59 -0.3(15) . . . . ?
C56 C57 C58 C59 177.6(9) . . . . ?
C57 C58 C59 C60 -0.9(16) . . . . ?
C58 C59 C60 C61 1.5(16) . . . . ?
C59 C60 C61 N62 -0.8(16) . . . . ?
C60 C61 N62 C57 -0.4(14) . . . . ?
C60 C61 N62 Sm2 170.5(7) . . . . ?
C58 C57 N62 C61 1.0(14) . . . . ?
C56 C57 N62 C61 -177.1(8) . . . . ?
C58 C57 N62 Sm2 -169.9(7) . . . . ?
C56 C57 N62 Sm2 12.0(11) . . . . ?
Sm2 O71 C72 C73 -19.3(17) . . . . ?
Sm2 O71 C72 C76 158.3(7) . . . . ?
O71 C72 C73 C74 1.6(18) . . . . ?
C76 C72 C73 C74 -175.9(10) . . . . ?
C72 C73 C74 O75 -3.2(18) . . . . ?
C72 C73 C74 C77 174.7(10) . . . . ?
C73 C74 O75 Sm2 22.8(17) . . . . ?
C77 C74 O75 Sm2 -155.1(6) . . . . ?
O71 C72 C76 F71 -117.8(12) . . . . ?
C73 C72 C76 F71 60.0(14) . . . . ?
O71 C72 C76 F72 1.3(15) . . . . ?
C73 C72 C76 F72 179.2(10) . . . . ?
O71 C72 C76 F73 123.4(12) . . . . ?
C73 C72 C76 F73 -58.8(15) . . . . ?
O75 C74 C77 F75B 161(3) . . . . ?
C73 C74 C77 F75B -17(3) . . . . ?
O75 C74 C77 F76B -73(3) . . . . ?
C73 C74 C77 F76B 109(3) . . . . ?
O75 C74 C77 F75A -49(2) . . . . ?
C73 C74 C77 F75A 133(2) . . . . ?
O75 C74 C77 F74A -168.8(17) . . . . ?
C73 C74 C77 F74A 13(2) . . . . ?
O75 C74 C77 F76A 77(2) . . . . ?
C73 C74 C77 F76A -101(2) . . . . ?
O75 C74 C77 F74B 32(2) . . . . ?
C73 C74 C77 F74B -146(2) . . . . ?
Sm2 O81 C82 C83 -15.8(15) . . . . ?
Sm2 O81 C82 C86 165.8(5) . . . . ?
O81 C82 C83 C84 -5.4(16) . . . . ?
C86 C82 C83 C84 173.1(8) . . . . ?
C82 C83 C84 O85 2.8(17) . . . . ?
C82 C83 C84 C87 -178.6(9) . . . . ?
C83 C84 O85 Sm2 20.9(16) . . . . ?
C87 C84 O85 Sm2 -157.7(6) . . . . ?
O81 C82 C86 F81A 44(3) . . . . ?
C83 C82 C86 F81A -135(2) . . . . ?
O81 C82 C86 F81B -151(2) . . . . ?
C83 C82 C86 F81B 30(2) . . . . ?
O81 C82 C86 F83A -78(2) . . . . ?
C83 C82 C86 F83A 104(2) . . . . ?
O81 C82 C86 F83B 83(2) . . . . ?
C83 C82 C86 F83B -95(2) . . . . ?
O81 C82 C86 F82A 161.9(19) . . . . ?
C83 C82 C86 F82A -17(2) . . . . ?
O81 C82 C86 F82B -30(2) . . . . ?
C83 C82 C86 F82B 151(2) . . . . ?
O85 C84 C87 F85 -71.4(13) . . . . ?
C83 C84 C87 F85 109.8(11) . . . . ?
O85 C84 C87 F84 50.5(13) . . . . ?
C83 C84 C87 F84 -128.3(11) . . . . ?
O85 C84 C87 F86 169.3(9) . . . . ?
C83 C84 C87 F86 -9.5(14) . . . . ?
Sm2 O91 C92 C93 -10.4(16) . . . . ?
Sm2 O91 C92 C96 169.5(7) . . . . ?
O91 C92 C93 C94 -4.0(17) . . . . ?
C96 C92 C93 C94 176.1(10) . . . . ?
C92 C93 C94 O95 -0.3(17) . . . . ?
C92 C93 C94 C97 178.3(9) . . . . ?
C93 C94 O95 Sm2 19.3(16) . . . . ?
C97 C94 O95 Sm2 -159.4(6) . . . . ?
O91 C92 C96 F91 61.2(14) . . . . ?
C93 C92 C96 F91 -118.8(12) . . . . ?
O91 C92 C96 F93 -176.0(10) . . . . ?
C93 C92 C96 F93 3.9(15) . . . . ?
O91 C92 C96 F92 -57.1(13) . . . . ?
C93 C92 C96 F92 122.9(11) . . . . ?
O95 C94 C97 F95 -62.5(13) . . . . ?
C93 C94 C97 F95 118.7(12) . . . . ?
O95 C94 C97 F96 61.2(13) . . . . ?
C93 C94 C97 F96 -117.6(12) . . . . ?
O95 C94 C97 F94 177.5(10) . . . . ?
C93 C94 C97 F94 -1.3(15) . . . . ?

_refine_diff_density_max         1.044
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.152


# start Validation Reply Form
_vrf_PLAT213_eh110               
;
PROBLEM: Atom F35A            has ADP max/min Ratio .....        4.5 prolat
RESPONSE: There are 5 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully
;
_vrf_PLAT214_eh110               
;
PROBLEM: Atom F74B      (Anion/Solvent) ADP max/min Ratio        5.2 prolat
RESPONSE: There are 5 disordered -CF3 groups which are modelled anisotropically as two PARTs.  This F atom is at partial occupancy and thus on the edge of what can be modelled successfully
;
# end Validation Reply Form

_chemical_properties_physical    Moisture-sensitive,Hygroscopic
