# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2235992'
loop_
_audit_author_name
_audit_author_address
'Hong-Xin Li'
;Shaanxi Normal University
China
;
_audit_update_record             
;
2023-01-13 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_audit_creation_date             2022-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H24 F4 N2 O17 Tb3 [+ solvent]'
_chemical_formula_sum            'C42 H24 F4 N2 O17 Tb3 [+ solvent]'
_chemical_formula_weight         1381.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   18.018(2)
_cell_length_b                   31.261(4)
_cell_length_c                   17.687(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.754(7)
_cell_angle_gamma                90
_cell_volume                     9253(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    243.0
_cell_measurement_theta_max      51.50
_cell_measurement_theta_min      4.96
_shelx_estimated_absorpt_T_max   0.460
_shelx_estimated_absorpt_T_min   0.261
_exptl_absorpt_coefficient_mu    11.473
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.3090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1462 before and 0.0957 after correction.
The Ratio of minimum to maximum transmission is 0.4120.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17740
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        51.755
_diffrn_reflns_theta_max         51.755
_diffrn_reflns_theta_min         4.963
_diffrn_ambient_temperature      243.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4241
_reflns_number_total             4968
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.053
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4968
_refine_ls_number_restraints     559
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0888
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1782P)²+64.6474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2528
_refine_ls_wR_factor_ref         0.2721
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C21-C20 = C22-C21 = C22-C23 = C22_$1-C23 = C22-C21 = C21_$1-C20
 1.43 with sigma of 0.001
 C23-C24
 1.43 with sigma of 0.01
 Tb1-O4
 2.4 with sigma of 0.01
 Tb2-O9
 2.4 with sigma of 0.01
 Tb2-O10
 2.4 with sigma of 0.01
 C23-C21_$1
 2.452 with sigma of 0.001
 C21-C23
 2.452 with sigma of 0.001
 C21-C21_$1
 2.452 with sigma of 0.001
 C22_$1-C20
 2.452 with sigma of 0.001
 C20-C22
 2.452 with sigma of 0.001
3. Restrained planarity
 C20, C21_$1, C21, C22_$1, C22, C23
 with sigma of 0.1
 N2, C20, C21, C21_$1, C22, C22_$1, C23
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O12 \\sim O12 \\sim N2 \\sim C20 \\sim C21 \\sim C21 \\sim C22 \\sim C22 \\sim
C23 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Tb1 \\sim Tb1 \\sim Tb2 \\sim Tb2 \\sim O1 \\sim O1 \\sim O2 \\sim O2 \\sim O3
\\sim O3 \\sim O5 \\sim O5 \\sim F3 \\sim F3 \\sim F1 \\sim F1 \\sim F2 \\sim
F2 \\sim O9 \\sim O9 \\sim O10 \\sim O10 \\sim O11 \\sim O11 \\sim O12 \\sim
O12 \\sim N1 \\sim N1 \\sim N2 \\sim C1 \\sim C1 \\sim C2 \\sim C2 \\sim C3
\\sim C3 \\sim C4 \\sim C4 \\sim C5 \\sim C5 \\sim C6 \\sim C6 \\sim C7 \\sim
C7 \\sim C8 \\sim C8 \\sim C9 \\sim C9 \\sim C10 \\sim C10 \\sim C11 \\sim C11
\\sim C12 \\sim C12 \\sim C13 \\sim C13 \\sim C14 \\sim C14 \\sim C15 \\sim C15
\\sim C16 \\sim C16 \\sim C17 \\sim C17 \\sim C18 \\sim C18 \\sim C19 \\sim C19
\\sim C20 \\sim C21 \\sim C21 \\sim C22 \\sim C22 \\sim C23 \\sim C24: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N2, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Tb2, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Tb1, Tb1, Tb2, Tb2, O1, O1, O2, O2, O3, O3, O5, O5, F3, F3, F1, F1, F2, F2,
 O9, O9, O10, O10, O11, O11, O12, O12, N1, N1, N2, C1, C1, C2, C2, C3, C3, C4,
 C4, C5, C5, C6, C6, C7, C7, C8, C8, C9, C9, C10, C10, C11, C11, C12, C12, C13,
 C13, C14, C14, C15, C15, C16, C16, C17, C17, C18, C18, C19, C19, C20, C21, C21,
  C22, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C11(H11), C7(H7), C8(H8), C15(H15), C16(H16),
 C18(H18), C19(H19), C21(H21), C22(H22)
6.b Fitted hexagon refined as free rotating group:
 C9(C10,C11,C6,C7,C8), C14(C15,C16,C17,C18,C19)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.40795(6) 0.500000 0.09591(7) 0.0633(4) Uani 1 2 d DS T P . .
Tb2 Tb 0.59684(4) 0.56309(2) 0.09751(5) 0.0635(4) Uani 1 1 d D . . . .
O1 O -0.0564(5) 0.1328(2) -0.0572(6) 0.073(2) Uani 1 1 d . U . . .
O2 O 0.2993(5) 0.4144(2) -0.0567(6) 0.077(2) Uani 1 1 d . U . . .
O3 O 0.3025(5) 0.4526(3) 0.0534(6) 0.075(2) Uani 1 1 d . U . . .
O4 O 0.324(3) 0.500000 0.175(3) 0.34(2) Uani 1 2 d DS TU P . .
O5 O 0.4502(6) 0.5486(3) 0.2016(6) 0.081(2) Uani 1 1 d . U . . .
F3 F 0.4613(3) 0.55527(16) 0.0466(5) 0.0619(17) Uani 1 1 d . . . . .
F1 F 0.5527(5) 0.500000 0.1385(6) 0.068(2) Uani 1 2 d S T P . .
F2 F 0.6371(5) 0.500000 0.0531(6) 0.065(2) Uani 1 2 d S T P . .
O9 O 0.7130(5) 0.5464(5) 0.2150(6) 0.135(4) Uani 1 1 d D . . . .
O10 O 0.6872(14) 0.6154(8) 0.1869(16) 0.273(12) Uani 1 1 d D . . . .
O11 O 0.5565(6) 0.5870(3) 0.2026(6) 0.085(2) Uani 1 1 d . U . . .
O12 O 0.588(2) 0.8702(15) 0.578(2) 0.364(13) Uani 1 1 d . U . . .
N1 N 0.000000 0.3324(4) 0.000000 0.097(5) Uani 1 2 d S TU P . .
N2 N 0.500000 0.6791(8) 0.500000 0.174(8) Uani 1 2 d S TU P . .
C1 C 0.000000 0.1508(5) 0.000000 0.065(4) Uani 1 2 d S TU P . .
C2 C 0.000000 0.1991(5) 0.000000 0.063(3) Uani 1 2 d S TU P . .
C3 C -0.0638(8) 0.2203(4) -0.0494(11) 0.088(4) Uani 1 1 d . U . . .
H3 H -0.108485 0.204886 -0.083589 0.106 Uiso 1 1 calc R U . . .
C4 C -0.0654(8) 0.2655(4) -0.0511(12) 0.093(4) Uani 1 1 d . U . . .
H4 H -0.110647 0.279817 -0.086769 0.112 Uiso 1 1 calc R U . . .
C5 C 0.000000 0.2891(5) 0.000000 0.090(5) Uani 1 2 d S TU P . .
C9 C 0.2016(4) 0.3995(2) -0.0008(6) 0.072(3) Uani 1 1 d G U . . .
C10 C 0.1621(5) 0.4132(2) 0.0491(6) 0.090(4) Uani 1 1 d G U . . .
H10 H 0.180567 0.437351 0.082389 0.108 Uiso 1 1 calc R U . . .
C11 C 0.0955(6) 0.3911(3) 0.0498(7) 0.113(5) Uani 1 1 d G U . . .
H11 H 0.068804 0.400305 0.083597 0.135 Uiso 1 1 calc R U . . .
C6 C 0.0682(5) 0.3553(3) 0.0006(7) 0.107(5) Uani 1 1 d G U . . .
C7 C 0.1077(5) 0.3416(2) -0.0493(7) 0.106(5) Uani 1 1 d G U . . .
H7 H 0.089229 0.317428 -0.082569 0.127 Uiso 1 1 calc R U . . .
C8 C 0.1743(5) 0.3637(2) -0.0500(6) 0.089(4) Uani 1 1 d G U . . .
H8 H 0.200993 0.354473 -0.083778 0.107 Uiso 1 1 calc R U . . .
C12 C 0.2726(7) 0.4231(4) -0.0039(10) 0.075(3) Uani 1 1 d . U . . .
C13 C 0.5026(10) 0.5781(4) 0.2288(10) 0.085(3) Uani 1 1 d . U . . .
C14 C 0.4989(8) 0.6053(3) 0.2993(6) 0.106(4) Uani 1 1 d G U . . .
C15 C 0.5501(8) 0.6401(3) 0.3250(8) 0.136(6) Uani 1 1 d G U . . .
H15 H 0.584810 0.647014 0.298115 0.164 Uiso 1 1 calc R U . . .
C16 C 0.5500(9) 0.6647(3) 0.3904(7) 0.162(7) Uani 1 1 d G U . . .
H16 H 0.584619 0.688248 0.407785 0.195 Uiso 1 1 calc R U . . .
C17 C 0.4987(10) 0.6545(4) 0.4301(7) 0.147(6) Uani 1 1 d G U . . .
C18 C 0.4475(8) 0.6196(4) 0.4044(8) 0.135(6) Uani 1 1 d G U . . .
H18 H 0.412804 0.612718 0.431303 0.162 Uiso 1 1 calc R U . . .
C19 C 0.4476(7) 0.5950(3) 0.3390(7) 0.113(5) Uani 1 1 d G U . . .
H19 H 0.412994 0.571483 0.321633 0.136 Uiso 1 1 calc R U . . .
C20 C 0.500000 0.7181(3) 0.500000 0.199(10) Uani 1 2 d DS TU P . .
C21 C 0.5518(9) 0.7415(3) 0.5686(5) 0.251(9) Uani 1 1 d D U . . .
H21 H 0.594974 0.728051 0.609151 0.301 Uiso 1 1 calc R U . . .
C22 C 0.5361(11) 0.7860(3) 0.57404(19) 0.280(9) Uani 1 1 d D U . . .
H22 H 0.549230 0.799484 0.624858 0.336 Uiso 1 1 calc R U . . .
C23 C 0.500000 0.8095(3) 0.500000 0.309(10) Uani 1 2 d DS TU P . .
C24 C 0.500000 0.8553(5) 0.500000 0.335(11) Uani 1 2 d DS TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb2 3.9245(10) 6_565 ?
Tb1 Tb2 3.9218(13) 2_655 ?
Tb1 Tb2 3.9218(13) 5_665 ?
Tb1 O3 2.305(8) . ?
Tb1 O3 2.305(8) 6_565 ?
Tb1 O4 2.406(10) . ?
Tb1 O5 2.309(10) . ?
Tb1 O5 2.309(10) 6_565 ?
Tb1 F3 2.300(5) . ?
Tb1 F3 2.300(5) 6_565 ?
Tb1 F1 2.432(9) . ?
Tb1 F2 2.454(10) 5_665 ?
Tb2 Tb2 3.8927(16) 2_655 ?
Tb2 O1 2.324(8) 4 ?
Tb2 O2 2.348(7) 5_665 ?
Tb2 F3 2.282(6) . ?
Tb2 F3 2.382(7) 2_655 ?
Tb2 F1 2.340(5) . ?
Tb2 F2 2.335(5) . ?
Tb2 O9 2.398(8) . ?
Tb2 O10 2.432(9) . ?
Tb2 O11 2.355(9) . ?
O1 C1 1.269(11) . ?
O2 C12 1.231(16) . ?
O3 C12 1.328(17) . ?
O5 C13 1.279(18) . ?
O11 C13 1.252(16) . ?
O12 C24 1.74(4) . ?
N1 C5 1.35(2) . ?
N1 C6 1.420(8) . ?
N1 C6 1.420(10) 2 ?
N2 C17 1.448(15) . ?
N2 C17 1.448(17) 2_656 ?
N2 C20 1.22(3) . ?
C1 C2 1.51(2) . ?
C2 C3 1.334(16) . ?
C2 C3 1.334(16) 2 ?
C3 H3 0.9400 . ?
C3 C4 1.414(18) . ?
C4 H4 0.9400 . ?
C4 C5 1.399(17) . ?
C9 C10 1.3900 . ?
C9 C8 1.3900 . ?
C9 C12 1.495(13) . ?
C10 H10 0.9400 . ?
C10 C11 1.3900 . ?
C11 H11 0.9400 . ?
C11 C6 1.3900 . ?
C6 C7 1.3900 . ?
C7 H7 0.9400 . ?
C7 C8 1.3900 . ?
C8 H8 0.9400 . ?
C13 C14 1.530(15) . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C15 H15 0.9400 . ?
C15 C16 1.3900 . ?
C16 H16 0.9400 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 H18 0.9400 . ?
C18 C19 1.3900 . ?
C19 H19 0.9400 . ?
C20 C21 1.4287(7) . ?
C20 C21 1.4287(7) 2_656 ?
C21 H21 0.9400 . ?
C21 C22 1.4292(8) . ?
C22 H22 0.9400 . ?
C22 C23 1.4296(7) . ?
C23 C24 1.434(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
Tb2 Tb1 Tb2 89.86(3) 2_655 6_565 ?
Tb2 Tb1 Tb2 60.38(3) 5_665 2_655 ?
Tb2 Tb1 Tb2 59.49(2) 5_665 6_565 ?
O3 Tb1 Tb2 69.1(2) . 5_665 ?
O3 Tb1 Tb2 106.66(19) . 6_565 ?
O3 Tb1 Tb2 158.9(2) 6_565 6_565 ?
O3 Tb1 Tb2 69.1(2) 6_565 2_655 ?
O3 Tb1 Tb2 106.9(2) . 2_655 ?
O3 Tb1 Tb2 106.9(2) 6_565 5_665 ?
O3 Tb1 O3 80.1(4) 6_565 . ?
O3 Tb1 O4 64.5(9) 6_565 . ?
O3 Tb1 O4 64.5(9) . . ?
O3 Tb1 O5 132.2(3) . . ?
O3 Tb1 O5 132.2(3) 6_565 6_565 ?
O3 Tb1 O5 79.9(3) . 6_565 ?
O3 Tb1 O5 79.9(3) 6_565 . ?
O3 Tb1 F1 139.5(2) . . ?
O3 Tb1 F1 139.5(2) 6_565 . ?
O3 Tb1 F2 75.3(3) . 5_665 ?
O3 Tb1 F2 75.3(3) 6_565 5_665 ?
O4 Tb1 Tb2 136.5(9) . 6_565 ?
O4 Tb1 Tb2 133.6(9) . 2_655 ?
O4 Tb1 Tb2 133.6(9) . 5_665 ?
O4 Tb1 F1 130.8(13) . . ?
O4 Tb1 F2 126.4(13) . 5_665 ?
O5 Tb1 Tb2 105.6(2) . 2_655 ?
O5 Tb1 Tb2 68.8(2) 6_565 6_565 ?
O5 Tb1 Tb2 107.5(2) . 6_565 ?
O5 Tb1 Tb2 158.7(2) 6_565 2_655 ?
O5 Tb1 Tb2 105.6(2) 6_565 5_665 ?
O5 Tb1 Tb2 158.7(2) . 5_665 ?
O5 Tb1 O4 67.7(9) 6_565 . ?
O5 Tb1 O4 67.7(9) . . ?
O5 Tb1 O5 82.3(4) 6_565 . ?
O5 Tb1 F1 75.8(3) 6_565 . ?
O5 Tb1 F1 75.8(3) . . ?
O5 Tb1 F2 138.5(2) . 5_665 ?
O5 Tb1 F2 138.5(2) 6_565 5_665 ?
F3 Tb1 Tb2 85.64(17) 6_565 2_655 ?
F3 Tb1 Tb2 85.64(17) . 5_665 ?
F3 Tb1 Tb2 33.77(18) 6_565 5_665 ?
F3 Tb1 Tb2 33.76(18) . 2_655 ?
F3 Tb1 Tb2 30.93(16) 6_565 6_565 ?
F3 Tb1 Tb2 84.09(14) . 6_565 ?
F3 Tb1 O3 78.6(2) . 6_565 ?
F3 Tb1 O3 78.6(2) 6_565 . ?
F3 Tb1 O3 140.3(3) . . ?
F3 Tb1 O3 140.3(3) 6_565 6_565 ?
F3 Tb1 O4 131.31(14) 6_565 . ?
F3 Tb1 O4 131.31(14) . . ?
F3 Tb1 O5 75.8(3) 6_565 6_565 ?
F3 Tb1 O5 138.0(3) . 6_565 ?
F3 Tb1 O5 75.8(3) . . ?
F3 Tb1 O5 138.0(3) 6_565 . ?
F3 Tb1 F3 97.4(3) 6_565 . ?
F3 Tb1 F1 64.3(2) . . ?
F3 Tb1 F1 64.3(2) 6_565 . ?
F3 Tb1 F2 67.1(2) . 5_665 ?
F3 Tb1 F2 67.1(2) 6_565 5_665 ?
F1 Tb1 Tb2 33.91(10) . 6_565 ?
F1 Tb1 Tb2 86.8(2) . 5_665 ?
F1 Tb1 Tb2 86.8(2) . 2_655 ?
F1 Tb1 F2 102.9(3) . 5_665 ?
F2 Tb1 Tb2 34.03(9) 5_665 2_655 ?
F2 Tb1 Tb2 87.03(17) 5_665 6_565 ?
F2 Tb1 Tb2 34.03(9) 5_665 5_665 ?
Tb1 Tb2 Tb1 90.13(3) 5_665 . ?
Tb2 Tb2 Tb1 60.22(2) 2_655 . ?
Tb2 Tb2 Tb1 60.29(2) 2_655 5_665 ?
O1 Tb2 Tb1 107.2(2) 4 . ?
O1 Tb2 Tb1 107.5(2) 4 5_665 ?
O1 Tb2 Tb2 69.6(2) 4 2_655 ?
O1 Tb2 O2 79.6(3) 4 5_665 ?
O1 Tb2 F3 78.7(3) 4 2_655 ?
O1 Tb2 F1 141.4(3) 4 . ?
O1 Tb2 F2 142.2(3) 4 . ?
O1 Tb2 O9 122.9(5) 4 . ?
O1 Tb2 O10 68.1(8) 4 . ?
O1 Tb2 O11 77.9(3) 4 . ?
O2 Tb2 Tb1 159.4(2) 5_665 . ?
O2 Tb2 Tb1 69.2(2) 5_665 5_665 ?
O2 Tb2 Tb2 106.4(2) 5_665 2_655 ?
O2 Tb2 F3 77.7(3) 5_665 2_655 ?
O2 Tb2 O9 78.0(4) 5_665 . ?
O2 Tb2 O10 65.2(7) 5_665 . ?
O2 Tb2 O11 131.4(3) 5_665 . ?
F3 Tb2 Tb1 31.22(15) . . ?
F3 Tb2 Tb1 32.47(12) 2_655 5_665 ?
F3 Tb2 Tb1 84.52(13) 2_655 . ?
F3 Tb2 Tb1 85.84(17) . 5_665 ?
F3 Tb2 Tb2 34.23(18) . 2_655 ?
F3 Tb2 Tb2 32.61(13) 2_655 2_655 ?
F3 Tb2 O1 79.1(2) . 4 ?
F3 Tb2 O2 140.3(3) . 5_665 ?
F3 Tb2 F3 65.5(2) . 2_655 ?
F3 Tb2 F1 66.1(3) . . ?
F3 Tb2 F2 101.4(3) . . ?
F3 Tb2 O9 143.3(3) 2_655 . ?
F3 Tb2 O9 141.4(4) . . ?
F3 Tb2 O10 133.6(7) . . ?
F3 Tb2 O10 133.4(7) 2_655 . ?
F3 Tb2 O11 75.4(3) . . ?
F1 Tb2 Tb1 86.9(2) . 5_665 ?
F1 Tb2 Tb1 35.4(2) . . ?
F1 Tb2 Tb2 88.8(2) . 2_655 ?
F1 Tb2 O2 138.5(3) . 5_665 ?
F1 Tb2 F3 100.4(3) . 2_655 ?
F1 Tb2 O9 80.6(5) . . ?
F1 Tb2 O10 126.0(8) . . ?
F1 Tb2 O11 77.5(3) . . ?
F2 Tb2 Tb1 36.0(2) . 5_665 ?
F2 Tb2 Tb1 87.11(18) . . ?
F2 Tb2 Tb2 89.4(2) . 2_655 ?
F2 Tb2 O2 76.6(3) . 5_665 ?
F2 Tb2 F3 67.8(3) . 2_655 ?
F2 Tb2 F1 64.9(3) . . ?
F2 Tb2 O9 80.1(5) . . ?
F2 Tb2 O10 124.8(7) . . ?
F2 Tb2 O11 139.4(3) . . ?
O9 Tb2 Tb1 112.2(4) . 5_665 ?
O9 Tb2 Tb1 111.9(3) . . ?
O9 Tb2 Tb2 167.5(4) . 2_655 ?
O9 Tb2 O10 54.8(8) . . ?
O10 Tb2 Tb1 134.3(7) . 5_665 ?
O10 Tb2 Tb1 135.4(7) . . ?
O10 Tb2 Tb2 137.7(8) . 2_655 ?
O11 Tb2 Tb1 69.2(2) . . ?
O11 Tb2 Tb1 159.2(2) . 5_665 ?
O11 Tb2 Tb2 105.2(2) . 2_655 ?
O11 Tb2 F3 137.3(3) . 2_655 ?
O11 Tb2 O9 79.1(4) . . ?
O11 Tb2 O10 66.5(7) . . ?
C1 O1 Tb2 136.7(9) . 4_545 ?
C12 O2 Tb2 138.4(8) . 5_665 ?
C12 O3 Tb1 138.5(8) . . ?
C13 O5 Tb1 139.0(8) . . ?
Tb1 F3 Tb2 113.8(3) . 2_655 ?
Tb2 F3 Tb1 117.9(3) . . ?
Tb2 F3 Tb2 113.2(2) . 2_655 ?
Tb2 F1 Tb1 110.6(3) 6_565 . ?
Tb2 F1 Tb1 110.6(3) . . ?
Tb2 F1 Tb2 114.9(4) 6_565 . ?
Tb2 F2 Tb1 109.9(3) 6_565 5_665 ?
Tb2 F2 Tb1 109.9(3) . 5_665 ?
Tb2 F2 Tb2 115.3(4) 6_565 . ?
C13 O11 Tb2 136.9(9) . . ?
C5 N1 C6 120.3(6) . . ?
C5 N1 C6 120.3(9) . 2 ?
C6 N1 C6 119.3(15) 2 . ?
C17 N2 C17 116(2) 2_656 . ?
C20 N2 C17 122.1(13) . 2_656 ?
C20 N2 C17 122.1(10) . . ?
O1 C1 O1 127.3(15) . 2 ?
O1 C1 C2 116.3(8) 2 . ?
O1 C1 C2 116.3(8) . . ?
C3 C2 C1 119.7(8) 2 . ?
C3 C2 C1 119.7(8) . . ?
C3 C2 C3 120.5(16) . 2 ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.0(14) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.5(14) . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C4 121.8(8) . 2 ?
N1 C5 C4 121.8(8) . . ?
C4 C5 C4 116.4(16) . 2 ?
C10 C9 C8 120.0 . . ?
C10 C9 C12 121.1(8) . . ?
C8 C9 C12 118.8(8) . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C6 120.0 . . ?
C6 C11 H11 120.0 . . ?
C11 C6 N1 121.0(6) . . ?
C7 C6 N1 119.0(6) . . ?
C7 C6 C11 120.0 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
O2 C12 O3 124.7(11) . . ?
O2 C12 C9 120.0(12) . . ?
O3 C12 C9 115.2(11) . . ?
O5 C13 C14 117.2(12) . . ?
O11 C13 O5 125.9(12) . . ?
O11 C13 C14 116.9(13) . . ?
C15 C14 C13 118.5(9) . . ?
C15 C14 C19 120.0 . . ?
C19 C14 C13 121.5(9) . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 N2 120.4(10) . . ?
C16 C17 C18 120.0 . . ?
C18 C17 N2 119.6(10) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C14 C19 H19 120.0 . . ?
C18 C19 C14 120.0 . . ?
C18 C19 H19 120.0 . . ?
N2 C20 C21 120.86(6) . . ?
N2 C20 C21 120.86(6) . 2_656 ?
C21 C20 C21 118.28(12) . 2_656 ?
C20 C21 H21 120.9 . . ?
C20 C21 C22 118.23(9) . . ?
C22 C21 H21 120.9 . . ?
C21 C22 H22 120.9 . . ?
C21 C22 C23 118.14(9) . . ?
C23 C22 H22 120.9 . . ?
C22 C23 C22 118.32(15) 2_656 . ?
C22 C23 C24 120.84(8) 2_656 . ?
C22 C23 C24 120.84(8) . . ?
O12 C24 O12 149(3) . 2_656 ?
C23 C24 O12 105.5(16) . . ?
C23 C24 O12 105.5(16) . 2_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O3 C12 O2 -2(2) . . . . ?
Tb1 O3 C12 C9 177.4(7) . . . . ?
Tb1 O5 C13 O11 -7(3) . . . . ?
Tb1 O5 C13 C14 173.1(9) . . . . ?
Tb2 O1 C1 O1 0.4(5) 4_545 . . 2 ?
Tb2 O1 C1 C2 -179.6(5) 4_545 . . . ?
Tb2 O2 C12 O3 -1(2) 5_665 . . . ?
Tb2 O2 C12 C9 179.7(7) 5_665 . . . ?
Tb2 O11 C13 O5 2(3) . . . . ?
Tb2 O11 C13 C14 -177.2(9) . . . . ?
O1 C1 C2 C3 11.2(9) . . . . ?
O1 C1 C2 C3 11.2(9) 2 . . 2 ?
O1 C1 C2 C3 -168.8(9) 2 . . . ?
O1 C1 C2 C3 -168.8(9) . . . 2 ?
O5 C13 C14 C15 -174.0(11) . . . . ?
O5 C13 C14 C19 7.9(19) . . . . ?
O11 C13 C14 C15 5.6(18) . . . . ?
O11 C13 C14 C19 -172.5(11) . . . . ?
N1 C6 C7 C8 179.7(11) . . . . ?
N2 C17 C18 C19 -178.0(14) . . . . ?
N2 C20 C21 C22 -165.0(3) . . . . ?
C1 C2 C3 C4 -179.6(11) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C3 C2 C3 C4 0.4(11) 2 . . . ?
C3 C4 C5 N1 -179.6(11) . . . . ?
C3 C4 C5 C4 0.4(11) . . . 2 ?
C5 N1 C6 C11 -137.4(5) . . . . ?
C5 N1 C6 C7 43.0(9) . . . . ?
C9 C10 C11 C6 0.0 . . . . ?
C10 C9 C8 C7 0.0 . . . . ?
C10 C9 C12 O2 -169.3(10) . . . . ?
C10 C9 C12 O3 11.1(15) . . . . ?
C10 C11 C6 N1 -179.6(11) . . . . ?
C10 C11 C6 C7 0.0 . . . . ?
C11 C6 C7 C8 0.0 . . . . ?
C6 N1 C5 C4 -135.6(14) 2 . . 2 ?
C6 N1 C5 C4 44.4(14) 2 . . . ?
C6 N1 C5 C4 44.4(10) . . . 2 ?
C6 N1 C5 C4 -135.6(10) . . . . ?
C6 N1 C6 C11 42.6(9) 2 . . . ?
C6 N1 C6 C7 -137.0(16) 2 . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C8 C9 C12 O2 9.7(16) . . . . ?
C8 C9 C12 O3 -169.9(9) . . . . ?
C12 C9 C10 C11 179.0(11) . . . . ?
C12 C9 C8 C7 -179.0(10) . . . . ?
C13 C14 C15 C16 -178.1(13) . . . . ?
C13 C14 C19 C18 178.1(13) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C15 C14 C19 C18 0.0 . . . . ?
C15 C16 C17 N2 178.0(14) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 N2 C17 C16 -133(2) 2_656 . . . ?
C17 N2 C17 C18 45.0(13) 2_656 . . . ?
C17 N2 C20 C21 -136.1(13) . . . . ?
C17 N2 C20 C21 -136.1(18) 2_656 . . 2_656 ?
C17 N2 C20 C21 43.9(18) 2_656 . . . ?
C17 N2 C20 C21 43.9(13) . . . 2_656 ?
C17 C18 C19 C14 0.0 . . . . ?
C19 C14 C15 C16 0.0 . . . . ?
C20 N2 C17 C16 47.0(11) . . . . ?
C20 N2 C17 C18 -135.0(7) . . . . ?
C20 C21 C22 C23 -30.3(6) . . . . ?
C21 C20 C21 C22 15.0(3) 2_656 . . . ?
C21 C22 C23 C22 15.0(3) . . . 2_656 ?
C21 C22 C23 C24 -165.0(3) . . . . ?
C22 C23 C24 O12 -147.8(16) 2_656 . . . ?
C22 C23 C24 O12 32.2(16) 2_656 . . 2_656 ?
C22 C23 C24 O12 -147.8(16) . . . 2_656 ?
C22 C23 C24 O12 32.2(16) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.675 -0.014 -0.565 5818.6 524.9 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
#==============================================================================
# Start Validation Reply Form
#=============================================================================
_vrf_THETM01_a                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however these crystals  
were small and weakly diffracting. Thus the very high angle data was 
dominated by noise because of the weak diffraction and thus was omitted.
;
####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2235996'
loop_
_audit_author_name
_audit_author_address
'Hong-Xin Li'
;Shaanxi Normal University
China
;
_audit_update_record             
;
2023-01-13 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_audit_creation_date             2022-12-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6427)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H24 F4 N4 O18 Tb3'
_chemical_formula_sum            'C45 H24 F4 N4 O18 Tb3'
_chemical_formula_weight         1461.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           162
_space_group_name_H-M_alt        'P -3 1 m'
_space_group_name_Hall           '-P 3 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z'
'x, x-y, -z'
'-x+y, y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z'
'-x, -x+y, z'
'x-y, -y, z'

_cell_length_a                   18.0964(8)
_cell_length_b                   18.0964(8)
_cell_length_c                   15.2035(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4311.8(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    243.0
_cell_measurement_theta_max      50.48
_cell_measurement_theta_min      5.64
_shelx_estimated_absorpt_T_max   0.371
_shelx_estimated_absorpt_T_min   0.319
_exptl_absorpt_coefficient_mu    12.353
_exptl_absorpt_correction_T_max  0.291
_exptl_absorpt_correction_T_min  0.284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1268 before and 0.0619 after correction.
The Ratio of minimum to maximum transmission is 0.5669.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12979
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        50.490
_diffrn_reflns_theta_max         50.490
_diffrn_reflns_theta_min         5.646
_diffrn_ambient_temperature      243.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1558
_reflns_number_total             1618
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.273
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0714
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1062P)²+48.2153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.1892
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C1-N42 = N42-C6 = C2-C13 = C3-C13 = C3-C1
 1.39 with sigma of 0.02
 O82-C6 = C6-N42
 1.2 with sigma of 0.02
 O82-O82_$2
 2.7 with sigma of 0.02
 C6-C6_$2
 1.43 with sigma of 0.01
 C3-C13 = C13-C2
 1.39 with sigma of 0.02
 N42-O82
 2.408 with sigma of 0.04
 O82-N42
 2.078 with sigma of 0.04
 C3-C2
 2.408 with sigma of 0.04
2. Restrained planarity
 C6, O82, C6_$2, O82_$2, N42, C6_$1, O82_$1, N42_$3, C6_$3, O82_$3
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C3 \\sim C1 \\sim C4 \\sim C13 \\sim C2 \\sim N42 \\sim C6 \\sim O82: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C6(0.5) O82(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C00O(H00O), C13(H13), C00Y(H00Y)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb01 Tb 0.87383(4) 0.87383(4) 0.39559(5) 0.0302(5) Uani 1 2 d S T P . .
F2 F 0.8853(4) 0.8853(4) 0.5487(5) 0.0266(17) Uani 1 2 d S T P . .
F6 F 1.000000 1.000000 0.3510(9) 0.044(3) Uani 1 6 d S T P . .
O4 O 0.8299(6) 0.9272(6) 0.2780(5) 0.069(2) Uani 1 1 d . . . . .
O008 O 0.8315(5) 0.7338(4) 0.4394(5) 0.051(2) Uani 1 1 d . . . . .
O2 O 0.7580(14) 0.7580(14) 0.2875(12) 0.172(10) Uani 1 2 d S T P . .
N00M N 0.666667 0.333333 0.500000 0.074(9) Uani 1 6 d S T P . .
C3 C 0.6425(15) 0.9257(15) 0.1212(19) 0.204(7) Uani 1 1 d D U . . .
H3 H 0.595916 0.874079 0.101540 0.245 Uiso 1 1 calc R U . . .
C1 C 0.6451(17) 1.000000 0.093(3) 0.199(7) Uani 1 2 d DS TU P . .
C00J C 0.8010(4) 0.6021(8) 0.500000 0.045(4) Uani 1 2 d S T P . .
C00N C 0.8487(6) 0.6974(11) 0.500000 0.050(4) Uani 1 2 d S T P . .
C4 C 0.844(2) 1.000000 0.254(2) 0.147(7) Uani 1 2 d S TU P . .
C00O C 0.8258(7) 0.5568(6) 0.5532(8) 0.050(3) Uani 1 1 d . . . . .
H00O H 0.874428 0.587411 0.588598 0.060 Uiso 1 1 calc R U . . .
C00R C 0.7112(5) 0.4225(10) 0.500000 0.065(5) Uani 1 2 d S T P . .
C13 C 0.7021(12) 0.9186(12) 0.1763(17) 0.181(6) Uani 1 1 d D U . . .
H13 H 0.695304 0.866405 0.196086 0.218 Uiso 1 1 calc R U . . .
C00Y C 0.7831(7) 0.4691(7) 0.5574(12) 0.075(4) Uani 1 1 d . . . . .
H00Y H 0.800500 0.440456 0.596527 0.090 Uiso 1 1 calc R U . . .
C2 C 0.7735(16) 1.000000 0.198(2) 0.153(6) Uani 1 2 d DS TU P . .
N42 N 0.5764(14) 1.000000 0.046(2) 0.212(8) Uani 1 2 d DS TU P . .
C6 C 0.5028(9) 0.9349(14) 0.0213(11) 0.214(10) Uani 0.5 1 d D U P . .
O82 O 0.4988(13) 0.8659(14) 0.040(2) 0.289(17) Uani 0.5 1 d D U P . .


_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
Tb01 Tb01 3.9104(13) 8_566 ?
Tb01 Tb01 3.9545(13) 2_765 ?
Tb01 Tb01 3.9104(13) 9_656 ?
Tb01 F2 2.345(4) 9_656 ?
Tb01 F2 2.337(7) . ?
Tb01 F2 2.345(4) 8_566 ?
Tb01 F6 2.382(4) . ?
Tb01 O4 2.351(8) . ?
Tb01 O4 2.351(8) 10 ?
Tb01 O008 2.348(7) . ?
Tb01 O008 2.348(7) 10 ?
Tb01 O2 2.66(2) . ?
O4 C4 1.266(15) . ?
O008 C00N 1.258(11) . ?
N00M C00R 1.397(16) 2_655 ?
N00M C00R 1.397(16) . ?
N00M C00R 1.397(16) 3_665 ?
C3 H3 0.9400 . ?
C3 C1 1.391(17) . ?
C3 C13 1.421(13) . ?
C1 N42 1.433(18) . ?
C00J C00N 1.49(2) . ?
C00J C00O 1.376(13) . ?
C00J C00O 1.376(13) 6_656 ?
C4 C2 1.53(4) . ?
C00O H00O 0.9400 . ?
C00O C00Y 1.377(16) . ?
C00R C00Y 1.438(16) . ?
C00R C00Y 1.438(16) 6_656 ?
C13 H13 0.9400 . ?
C13 C2 1.431(13) . ?
C00Y H00Y 0.9400 . ?
N42 C6 1.315(13) . ?
N42 C6 1.315(13) 12_675 ?
C6 C6 2.04(4) 12_675 ?
C6 C6 1.435(10) 6 ?
C6 O82 1.247(17) . ?

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
Tb01 Tb01 Tb01 59.626(13) 9_656 2_765 ?
Tb01 Tb01 Tb01 60.75(3) 9_656 8_566 ?
Tb01 Tb01 Tb01 90.0 8_566 2_765 ?
F2 Tb01 Tb01 85.60(15) 8_566 2_765 ?
F2 Tb01 Tb01 33.29(16) 9_656 9_656 ?
F2 Tb01 Tb01 86.51(17) 8_566 9_656 ?
F2 Tb01 Tb01 85.58(14) . 2_765 ?
F2 Tb01 Tb01 86.51(17) 9_656 8_566 ?
F2 Tb01 Tb01 33.43(7) . 8_566 ?
F2 Tb01 Tb01 32.53(15) 9_656 2_765 ?
F2 Tb01 Tb01 33.43(7) . 9_656 ?
F2 Tb01 Tb01 33.29(16) 8_566 8_566 ?
F2 Tb01 F2 100.1(3) 9_656 8_566 ?
F2 Tb01 F2 66.0(2) . 8_566 ?
F2 Tb01 F2 66.0(2) . 9_656 ?
F2 Tb01 F6 66.0(2) 8_566 . ?
F2 Tb01 F6 66.0(2) 9_656 . ?
F2 Tb01 F6 101.4(4) . . ?
F2 Tb01 O4 139.0(2) . . ?
F2 Tb01 O4 138.8(3) 9_656 . ?
F2 Tb01 O4 76.0(3) 8_566 . ?
F2 Tb01 O4 76.0(3) 9_656 10 ?
F2 Tb01 O4 139.0(2) . 10 ?
F2 Tb01 O4 138.8(3) 8_566 10 ?
F2 Tb01 O008 140.4(2) 8_566 . ?
F2 Tb01 O008 76.7(2) 8_566 10 ?
F2 Tb01 O008 77.3(2) . 10 ?
F2 Tb01 O008 76.7(2) 9_656 . ?
F2 Tb01 O008 77.3(2) . . ?
F2 Tb01 O008 140.4(2) 9_656 10 ?
F2 Tb01 O2 129.86(16) 9_656 . ?
F2 Tb01 O2 133.2(5) . . ?
F2 Tb01 O2 129.86(17) 8_566 . ?
F6 Tb01 Tb01 87.2(3) . 9_656 ?
F6 Tb01 Tb01 87.2(3) . 8_566 ?
F6 Tb01 Tb01 33.88(15) . 2_765 ?
F6 Tb01 O2 125.4(6) . . ?
O4 Tb01 Tb01 159.2(2) 10 8_566 ?
O4 Tb01 Tb01 106.2(2) 10 9_656 ?
O4 Tb01 Tb01 69.2(2) 10 2_765 ?
O4 Tb01 Tb01 159.2(2) . 9_656 ?
O4 Tb01 Tb01 106.2(2) . 8_566 ?
O4 Tb01 Tb01 107.0(2) . 2_765 ?
O4 Tb01 F6 75.4(3) 10 . ?
O4 Tb01 F6 75.4(3) . . ?
O4 Tb01 O4 80.8(5) 10 . ?
O4 Tb01 O2 63.9(4) 10 . ?
O4 Tb01 O2 63.9(4) . . ?
O008 Tb01 Tb01 106.41(19) . 2_765 ?
O008 Tb01 Tb01 159.20(19) 10 2_765 ?
O008 Tb01 Tb01 69.21(19) . 9_656 ?
O008 Tb01 Tb01 107.74(19) 10 9_656 ?
O008 Tb01 Tb01 69.21(19) 10 8_566 ?
O008 Tb01 Tb01 107.74(19) . 8_566 ?
O008 Tb01 F6 139.0(2) . . ?
O008 Tb01 F6 139.0(2) 10 . ?
O008 Tb01 O4 79.5(3) 10 . ?
O008 Tb01 O4 131.6(3) 10 10 ?
O008 Tb01 O4 131.6(3) . . ?
O008 Tb01 O4 79.5(3) . 10 ?
O008 Tb01 O008 81.4(4) . 10 ?
O008 Tb01 O2 67.8(4) . . ?
O008 Tb01 O2 67.8(4) 10 . ?
O2 Tb01 Tb01 136.9(3) . 8_566 ?
O2 Tb01 Tb01 133.0(4) . 2_765 ?
O2 Tb01 Tb01 136.9(3) . 9_656 ?
Tb01 F2 Tb01 113.28(18) . 8_566 ?
Tb01 F2 Tb01 114.9(3) 9_656 8_566 ?
Tb01 F2 Tb01 113.28(18) . 9_656 ?
Tb01 F6 Tb01 112.2(3) 3_675 2_765 ?
Tb01 F6 Tb01 112.2(3) 3_675 . ?
Tb01 F6 Tb01 112.2(3) 2_765 . ?
C4 O4 Tb01 135.6(15) . . ?
C00N O008 Tb01 137.7(9) . . ?
C00R N00M C00R 120.000(1) 3_665 2_655 ?
C00R N00M C00R 119.999(4) . 2_655 ?
C00R N00M C00R 120.001(5) 3_665 . ?
C1 C3 H3 116.2 . . ?
C1 C3 C13 128(2) . . ?
C13 C3 H3 116.2 . . ?
C3 C1 C3 114(2) 12_675 . ?
C3 C1 N42 123.0(12) 12_675 . ?
C3 C1 N42 123.0(12) . . ?
C00O C00J C00N 121.0(6) 6_656 . ?
C00O C00J C00N 121.0(7) . . ?
C00O C00J C00O 117.9(13) 6_656 . ?
O008 C00N O008 126.2(16) 6_656 . ?
O008 C00N C00J 116.9(8) 6_656 . ?
O008 C00N C00J 116.9(8) . . ?
O4 C4 O4 129(3) . 12_675 ?
O4 C4 C2 115.4(14) . . ?
O4 C4 C2 115.4(14) 12_675 . ?
C00J C00O H00O 118.2 . . ?
C00J C00O C00Y 123.5(12) . . ?
C00Y C00O H00O 118.2 . . ?
N00M C00R C00Y 120.5(8) . 6_656 ?
N00M C00R C00Y 120.5(8) . . ?
C00Y C00R C00Y 119.0(15) 6_656 . ?
C3 C13 H13 123.8 . . ?
C3 C13 C2 112.5(19) . . ?
C2 C13 H13 123.8 . . ?
C00O C00Y C00R 118.0(13) . . ?
C00O C00Y H00Y 121.0 . . ?
C00R C00Y H00Y 121.0 . . ?
C13 C2 C4 117.0(11) . . ?
C13 C2 C4 117.0(11) 12_675 . ?
C13 C2 C13 126(2) . 12_675 ?
C6 N42 C1 129.1(12) . . ?
C6 N42 C1 129.1(12) 12_675 . ?
C6 N42 C6 102(2) . 12_675 ?
N42 C6 C6 39.2(12) . 12_675 ?
N42 C6 C6 129.2(12) . 6 ?
C6 C6 C6 90.000(1) 6 12_675 ?
O82 C6 N42 111.1(12) . . ?
O82 C6 C6 150.3(7) . 12_675 ?
O82 C6 C6 119.7(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
Tb01 O4 C4 O4 17(6) . . . 12_675 ?
Tb01 O4 C4 C2 -154(2) . . . . ?
Tb01 O008 C00N O008 -1.2(5) . . . 6_656 ?
Tb01 O008 C00N C00J 178.8(5) . . . . ?
O4 C4 C2 C13 2(5) 12_675 . . 12_675 ?
O4 C4 C2 C13 -2(5) . . . . ?
O4 C4 C2 C13 -175(3) 12_675 . . . ?
O4 C4 C2 C13 175(3) . . . 12_675 ?
N00M C00R C00Y C00O 178.6(10) . . . . ?
C3 C1 N42 C6 0(7) . . . . ?
C3 C1 N42 C6 174(3) . . . 12_675 ?
C3 C1 N42 C6 0(7) 12_675 . . 12_675 ?
C3 C1 N42 C6 -174(3) 12_675 . . . ?
C3 C13 C2 C4 -177(3) . . . . ?
C3 C13 C2 C13 6(6) . . . 12_675 ?
C1 C3 C13 C2 -4(6) . . . . ?
C1 N42 C6 C6 176(5) . . . 12_675 ?
C1 N42 C6 C6 176(4) . . . 6 ?
C1 N42 C6 O82 -4(4) . . . . ?
C00J C00O C00Y C00R 3(2) . . . . ?
C00N C00J C00O C00Y 178.5(11) . . . . ?
C00O C00J C00N O008 -11.9(7) . . . 6_656 ?
C00O C00J C00N O008 168.1(7) . . . . ?
C00O C00J C00N O008 -11.9(7) 6_656 . . . ?
C00O C00J C00N O008 168.1(7) 6_656 . . 6_656 ?
C00O C00J C00O C00Y -1.5(11) 6_656 . . . ?
C00R N00M C00R C00Y -44.8(7) 3_665 . . . ?
C00R N00M C00R C00Y 135.2(7) 2_655 . . . ?
C00R N00M C00R C00Y 135.2(7) 3_665 . . 6_656 ?
C00R N00M C00R C00Y -44.8(7) 2_655 . . 6_656 ?
C13 C3 C1 C3 2(8) . . . 12_675 ?
C13 C3 C1 N42 -172(3) . . . . ?
C00Y C00R C00Y C00O -1.4(10) 6_656 . . . ?
C6 N42 C6 C6 0(4) 12_675 . . 6 ?
C6 N42 C6 O82 -180.0(15) 12_675 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.415 -0.431 -0.206 2320.9 439.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
#==============================================================================
# Start Validation Reply Form
#=============================================================================
_vrf_THETM01_a                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however these crystals  
were small and weakly diffracting. Thus the very high angle data was 
dominated by noise because of the weak diffraction and thus was omitted.
;
####################################################################### 
# 
# 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_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2235993'
loop_
_audit_author_name
_audit_author_address
'Hong-Xin Li'
;Shaanxi Normal University
China
;
_audit_update_record             
;
2023-01-13 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_audit_creation_date             2022-12-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H18 F4 N1 O12 Tb3'
_chemical_formula_sum            'C33 H18 F4 N O12 Tb3'
_chemical_formula_weight         1173.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_H-M_alt        'P 63/m c m'
_space_group_name_Hall           '-P 6c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   18.0166(4)
_cell_length_b                   18.0166(4)
_cell_length_c                   27.4264(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7709.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8714
_cell_measurement_temperature    243.0
_cell_measurement_theta_max      54.24
_cell_measurement_theta_min      5.67
_shelx_estimated_absorpt_T_max   0.685
_shelx_estimated_absorpt_T_min   0.408
_exptl_absorpt_coefficient_mu    13.639
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.6168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0600 before and 0.0401 after correction.
The Ratio of minimum to maximum transmission is 0.8234.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2200
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17728
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        54.238
_diffrn_reflns_theta_max         54.238
_diffrn_reflns_theta_min         4.292
_diffrn_ambient_temperature      243.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1555
_reflns_number_total             1719
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.889
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1719
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0582
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1106P)²+64.0412P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.1916
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 1.000000 0.87468(4) 0.55830(2) 0.0256(4) Uani 1 2 d S T P . .
F1 F 1.000000 1.000000 0.5817(4) 0.030(2) Uani 1 6 d S T P . .
F2 F 0.8862(4) 0.8862(4) 0.5268(3) 0.0315(17) Uani 1 2 d S T P . .
O1 O 1.0957(4) 0.9280(4) 0.62443(19) 0.0395(15) Uani 1 1 d . . . . .
O2 O 0.9046(4) 0.7353(4) 0.5334(2) 0.0412(15) Uani 1 1 d . . . . .
N1 N 0.666667 0.333333 0.500000 0.056(6) Uani 1 6 d S T P . .
C1 C 1.1828(9) 1.0709(10) 0.7240(5) 0.085(4) Uani 1 1 d . U . . .
H1 H 1.210360 1.123360 0.707204 0.102 Uiso 1 1 calc R U . . .
C2 C 1.1457(7) 1.000000 0.6995(4) 0.025(3) Uani 1 2 d S T P . .
C3 C 1.1361(6) 1.000000 0.6446(5) 0.0298(19) Uani 1 2 d S TU P . .
C4 C 0.8492(4) 0.6984(8) 0.500000 0.037(3) Uani 1 2 d S T P . .
C5 C 0.8016(4) 0.6031(7) 0.500000 0.036(3) Uani 1 2 d S T P . .
C6 C 0.7288(6) 0.5564(6) 0.4722(4) 0.052(3) Uani 1 1 d . . . . .
H6 H 0.708779 0.585959 0.452986 0.063 Uiso 1 1 calc R U . . .
C7 C 0.6849(6) 0.4690(6) 0.4714(5) 0.054(3) Uani 1 1 d . . . . .
H7 H 0.636349 0.439430 0.451408 0.065 Uiso 1 1 calc R U . . .
C8 C 0.7120(4) 0.4241(8) 0.500000 0.044(3) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb1 3.9147(12) 14_566 ?
Tb1 Tb1 3.9106(12) 3_675 ?
Tb1 Tb1 3.9106(12) 2_765 ?
Tb1 Tb1 3.9146(12) 15_656 ?
Tb1 F1 2.348(3) . ?
Tb1 F2 2.328(4) . ?
Tb1 F2 2.344(7) 15_656 ?
Tb1 F2 2.328(4) 2_765 ?
Tb1 O1 2.351(6) . ?
Tb1 O1 2.351(5) 24_765 ?
Tb1 O2 2.326(6) 24_765 ?
Tb1 O2 2.326(6) . ?
O1 C3 1.255(8) . ?
O2 C4 1.270(8) . ?
N1 C8 1.416(12) 3_665 ?
N1 C8 1.416(12) . ?
N1 C8 1.416(12) 2_655 ?
C1 C1 1.43(3) 16_557 ?
C1 H1 0.9400 . ?
C1 C2 1.295(15) . ?
C2 C3 1.514(18) . ?
C4 C5 1.487(17) . ?
C5 C6 1.380(12) 11_656 ?
C5 C6 1.380(12) . ?
C6 H6 0.9400 . ?
C6 C7 1.364(13) . ?
C7 H7 0.9400 . ?
C7 C8 1.380(12) . ?

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
Tb1 Tb1 Tb1 59.93(2) 14_566 15_656 ?
Tb1 Tb1 Tb1 90.0 3_675 15_656 ?
Tb1 Tb1 Tb1 60.036(11) 2_765 15_656 ?
Tb1 Tb1 Tb1 60.036(11) 3_675 14_566 ?
Tb1 Tb1 Tb1 90.0 2_765 14_566 ?
Tb1 Tb1 Tb1 60.0 2_765 3_675 ?
F1 Tb1 Tb1 33.60(10) . 3_675 ?
F1 Tb1 Tb1 33.60(10) . 2_765 ?
F1 Tb1 Tb1 86.9(2) . 15_656 ?
F1 Tb1 Tb1 86.9(2) . 14_566 ?
F1 Tb1 O1 75.4(2) . . ?
F1 Tb1 O1 75.4(2) . 24_765 ?
F2 Tb1 Tb1 85.59(15) . 2_765 ?
F2 Tb1 Tb1 32.95(6) 15_656 14_566 ?
F2 Tb1 Tb1 85.73(17) 2_765 14_566 ?
F2 Tb1 Tb1 32.86(14) 2_765 2_765 ?
F2 Tb1 Tb1 85.59(14) 2_765 3_675 ?
F2 Tb1 Tb1 33.20(16) 2_765 15_656 ?
F2 Tb1 Tb1 85.62(14) 15_656 2_765 ?
F2 Tb1 Tb1 32.86(14) . 3_675 ?
F2 Tb1 Tb1 33.20(16) . 14_566 ?
F2 Tb1 Tb1 85.73(17) . 15_656 ?
F2 Tb1 Tb1 32.95(6) 15_656 15_656 ?
F2 Tb1 Tb1 85.62(14) 15_656 3_675 ?
F2 Tb1 F1 100.8(3) 15_656 . ?
F2 Tb1 F1 65.95(18) . . ?
F2 Tb1 F1 65.95(19) 2_765 . ?
F2 Tb1 F2 65.4(2) 2_765 15_656 ?
F2 Tb1 F2 99.5(3) . 2_765 ?
F2 Tb1 F2 65.4(2) . 15_656 ?
F2 Tb1 O1 77.2(2) 2_765 . ?
F2 Tb1 O1 138.4(2) 2_765 24_765 ?
F2 Tb1 O1 77.2(2) . 24_765 ?
F2 Tb1 O1 139.88(15) 15_656 24_765 ?
F2 Tb1 O1 138.4(2) . . ?
F2 Tb1 O1 139.88(16) 15_656 . ?
O1 Tb1 Tb1 106.31(14) . 3_675 ?
O1 Tb1 Tb1 69.26(15) 24_765 3_675 ?
O1 Tb1 Tb1 107.51(15) 24_765 14_566 ?
O1 Tb1 Tb1 107.51(15) . 15_656 ?
O1 Tb1 Tb1 159.25(15) 24_765 15_656 ?
O1 Tb1 Tb1 69.26(15) . 2_765 ?
O1 Tb1 Tb1 106.31(14) 24_765 2_765 ?
O1 Tb1 Tb1 159.25(15) . 14_566 ?
O1 Tb1 O1 78.8(3) 24_765 . ?
O2 Tb1 Tb1 106.54(16) . 15_656 ?
O2 Tb1 Tb1 159.24(16) . 2_765 ?
O2 Tb1 Tb1 107.17(16) 24_765 2_765 ?
O2 Tb1 Tb1 106.54(16) 24_765 14_566 ?
O2 Tb1 Tb1 69.24(16) 24_765 15_656 ?
O2 Tb1 Tb1 159.24(16) 24_765 3_675 ?
O2 Tb1 Tb1 107.17(16) . 3_675 ?
O2 Tb1 Tb1 69.24(16) . 14_566 ?
O2 Tb1 F1 139.78(16) 24_765 . ?
O2 Tb1 F1 139.78(16) . . ?
O2 Tb1 F2 139.1(2) 24_765 . ?
O2 Tb1 F2 139.1(2) . 2_765 ?
O2 Tb1 F2 77.2(2) . . ?
O2 Tb1 F2 76.7(2) . 15_656 ?
O2 Tb1 F2 77.2(2) 24_765 2_765 ?
O2 Tb1 F2 76.7(2) 24_765 15_656 ?
O2 Tb1 O1 131.5(2) . . ?
O2 Tb1 O1 81.4(2) 24_765 . ?
O2 Tb1 O1 131.5(2) 24_765 24_765 ?
O2 Tb1 O1 81.4(2) . 24_765 ?
O2 Tb1 O2 79.6(3) . 24_765 ?
Tb1 F1 Tb1 112.8(2) 2_765 . ?
Tb1 F1 Tb1 112.8(2) 3_675 . ?
Tb1 F1 Tb1 112.8(2) 2_765 3_675 ?
Tb1 F2 Tb1 114.3(3) . 3_675 ?
Tb1 F2 Tb1 113.85(19) 3_675 14_566 ?
Tb1 F2 Tb1 113.85(19) . 14_566 ?
C3 O1 Tb1 133.8(6) . . ?
C4 O2 Tb1 137.7(6) . . ?
C8 N1 C8 120.001(5) 3_665 . ?
C8 N1 C8 119.996(3) . 2_655 ?
C8 N1 C8 120.003(1) 3_665 2_655 ?
C1 C1 H1 119.4 16_557 . ?
C2 C1 C1 121.3(8) . 16_557 ?
C2 C1 H1 119.4 . . ?
C1 C2 C1 117.3(16) 23_675 . ?
C1 C2 C3 121.3(8) 23_675 . ?
C1 C2 C3 121.3(8) . . ?
O1 C3 O1 126.9(12) 23_675 . ?
O1 C3 C2 116.5(6) 23_675 . ?
O1 C3 C2 116.5(6) . . ?
O2 C4 O2 126.2(11) . 11_656 ?
O2 C4 C5 116.9(6) . . ?
O2 C4 C5 116.9(6) 11_656 . ?
C6 C5 C4 121.9(6) . . ?
C6 C5 C4 121.9(6) 11_656 . ?
C6 C5 C6 116.2(11) 11_656 . ?
C5 C6 H6 118.7 . . ?
C7 C6 C5 122.6(10) . . ?
C7 C6 H6 118.7 . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.8(10) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 N1 120.5(6) 11_656 . ?
C7 C8 N1 120.5(6) . . ?
C7 C8 C7 119.0(12) . 11_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C3 O1 -34.7(18) . . . 23_675 ?
Tb1 O1 C3 C2 143.2(8) . . . . ?
Tb1 O2 C4 O2 1.0(4) . . . 11_656 ?
Tb1 O2 C4 C5 -179.0(4) . . . . ?
O2 C4 C5 C6 166.7(7) 11_656 . . 11_656 ?
O2 C4 C5 C6 -13.3(7) 11_656 . . . ?
O2 C4 C5 C6 166.7(7) . . . . ?
O2 C4 C5 C6 -13.3(7) . . . 11_656 ?
C1 C1 C2 C1 -3.1(19) 16_557 . . 23_675 ?
C1 C1 C2 C3 172.4(8) 16_557 . . . ?
C1 C2 C3 O1 -176.8(12) . . . . ?
C1 C2 C3 O1 -1.4(18) 23_675 . . . ?
C1 C2 C3 O1 176.8(12) 23_675 . . 23_675 ?
C1 C2 C3 O1 1.4(18) . . . 23_675 ?
C4 C5 C6 C7 179.3(9) . . . . ?
C5 C6 C7 C8 1.4(18) . . . . ?
C6 C5 C6 C7 -0.7(9) 11_656 . . . ?
C6 C7 C8 N1 179.3(8) . . . . ?
C6 C7 C8 C7 -0.7(8) . . . 11_656 ?
C8 N1 C8 C7 -41.3(6) 2_655 . . . ?
C8 N1 C8 C7 138.7(6) 2_655 . . 11_656 ?
C8 N1 C8 C7 138.7(6) 3_665 . . . ?
C8 N1 C8 C7 -41.3(6) 3_665 . . 11_656 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.250 7.3 3.5 ?
2 0.000 0.000 0.750 7.3 0.0 ?
3 -0.953 -0.905 -0.482 5144.2 821.6 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
#==============================================================================
# Start Validation Reply Form
#=============================================================================
_vrf_THETM01_a                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however these crystals  
were small and weakly diffracting. Thus the very high angle data was 
dominated by noise because of the weak diffraction and thus was omitted.
;
####################################################################### 
# 
# 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_a_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2235994'
loop_
_audit_author_name
_audit_author_address
'Hong-Xin Li'
;Shaanxi Normal University
China
;
_audit_update_record             
;
2023-01-13 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_audit_creation_date             2022-12-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H21 F4 N1 O15 Tb3, 3(C2 N)'
_chemical_formula_sum            'C45 H42 F4 N4 O15 Tb3'
_chemical_formula_weight         1431.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_H-M_alt        'P 63/m c m'
_space_group_name_Hall           '-P 6c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   18.0378(4)
_cell_length_b                   18.0378(4)
_cell_length_c                   27.5886(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7773.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    243
_cell_measurement_theta_max      54.24
_cell_measurement_theta_min      5.66
_shelx_estimated_absorpt_T_max   0.611
_shelx_estimated_absorpt_T_min   0.408
_exptl_absorpt_coefficient_mu    13.657
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.6277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0622 before and 0.0386 after correction.
The Ratio of minimum to maximum transmission is 0.8362.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16985
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        54.235
_diffrn_reflns_theta_max         54.235
_diffrn_reflns_theta_min         5.159
_diffrn_ambient_temperature      243
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1541
_reflns_number_total             1681
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1681
_refine_ls_number_restraints     348
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0583
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0997P)²+77.4622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.1852
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6-C7
 1.39 with sigma of 0.001
 C14-C15
 1.39 with sigma of 0.001
 C7-C8
 1.39 with sigma of 0.001
 C16-C7
 1.39 with sigma of 0.001
 C8-C9
 1.39 with sigma of 0.001
 C13-C14
 1.39 with sigma of 0.001
 C9-C10
 1.39 with sigma of 0.001
 C15-C16
 1.39 with sigma of 0.001
 C10-C11
 1.39 with sigma of 0.001
 C11-C12
 1.39 with sigma of 0.001
 C12-C13
 1.39 with sigma of 0.001
 C6-C7 = C7-C16
 1.39 with sigma of 0.02
 C7-C16 = C16-C11
 1.39 with sigma of 0.02
 C8-C7 = C7-C16
 1.39 with sigma of 0.02
 C16-C11 = C11-C10
 1.39 with sigma of 0.02
 C12-C11 = C11-C16
 1.39 with sigma of 0.02
 C11-C16 = C16-C15
 1.39 with sigma of 0.02
 C11-C10 = C10-C9
 1.39 with sigma of 0.02
 C14-C13 = C13-C12
 1.39 with sigma of 0.02
 C10-C9 = C9-C8
 1.39 with sigma of 0.02
 C13-C12 = C12-C11
 1.39 with sigma of 0.02
 C9-C8 = C8-C7
 1.39 with sigma of 0.02
 C16-C15 = C15-C14
 1.39 with sigma of 0.02
 C15-C14 = C14-C13
 1.39 with sigma of 0.02
 C8-C16
 2.408 with sigma of 0.04
 C10-C8
 2.408 with sigma of 0.04
 C15-C13
 2.408 with sigma of 0.04
 C16-C14
 2.408 with sigma of 0.04
 C6-C16
 2.408 with sigma of 0.04
 C14-C12
 2.408 with sigma of 0.04
 C7-C11
 2.408 with sigma of 0.04
 C12-C16
 2.408 with sigma of 0.04
 C11-C9
 2.408 with sigma of 0.04
 C9-C7
 2.408 with sigma of 0.04
 C13-C11
 2.408 with sigma of 0.04
 C11-C15
 2.408 with sigma of 0.04
 C16-C10
 2.408 with sigma of 0.04
 C8-C7 \\sim C16-C7 \\sim C16-C11 \\sim C11-C10 \\sim C8-C9 \\sim C9-C10 \\sim
C12-C11 \\sim C13-C12 \\sim C14-
 C13 \\sim C14-C15 \\sim C15-C16
 with sigma of 0.02
3. Restrained planarity
 C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O2) \\sim Ueq: with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C17) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 Tb1, O3, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C7(0.25) C8(0.25) H8(0.25) C9(0.25) H9(0.25) C10(0.25) C11(0.25)
 C12(0.25) H12(0.25) C13(0.25) H13(0.25) C14(0.25) H14(0.25) C15(0.25)
 H15(0.25) C16(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.87466(4) 1.000000 0.55756(2) 0.0189(4) Uani 1 2 d S T P . .
F1 F 1.000000 1.1149(4) 0.5267(2) 0.0222(16) Uani 1 2 d S T P . .
F2 F 1.000000 1.000000 0.5800(4) 0.023(2) Uani 1 6 d S T P . .
O1 O 0.7349(4) 0.9035(4) 0.5329(2) 0.0394(16) Uani 1 1 d . U . . .
O2 O 0.743(2) 1.000000 0.6140(15) 0.284(5) Uani 1 2 d S TU P . .
O3 O 0.9280(4) 1.0943(4) 0.62436(18) 0.0275(14) Uani 1 1 d . . . . .
N1 N 0.333333 0.666667 0.500000 0.0466(13) Uani 1 6 d S TU P . .
C1 C 0.4247(9) 0.7124(4) 0.500000 0.039(2) Uani 1 2 d S TU P . .
C2 C 0.4692(7) 0.6857(7) 0.4719(4) 0.046(3) Uani 1 1 d . U . . .
H2 H 0.439495 0.636855 0.452354 0.055 Uiso 1 1 calc R U . . .
C3 C 0.5569(7) 0.7297(7) 0.4720(4) 0.045(3) Uani 1 1 d . U . . .
H3 H 0.586333 0.710341 0.452426 0.055 Uiso 1 1 calc R U . . .
C4 C 0.6027(8) 0.8014(4) 0.500000 0.0317(19) Uani 1 2 d S TU P . .
C5 C 0.6985(9) 0.8492(4) 0.500000 0.0339(19) Uani 1 2 d S TU P . .
C6 C 1.000000 1.1360(6) 0.6457(4) 0.0229(18) Uani 1 2 d DS TU P . .
C7 C 0.9937(8) 1.1439(6) 0.6954(4) 0.020(3) Uani 0.25 1 d D U P A -1
C8 C 1.0570(11) 1.1384(12) 0.7212(6) 0.022(4) Uani 0.25 1 d D U P A -1
H8 H 1.097138 1.129712 0.704212 0.026 Uiso 0.25 1 calc R U P A -1
C9 C 1.0627(12) 1.1454(16) 0.7714(6) 0.022(4) Uani 0.25 1 d D U P A -1
H9 H 1.109091 1.146675 0.787751 0.026 Uiso 0.25 1 calc R U P A -1
C10 C 0.9994(11) 1.1506(14) 0.7973(6) 0.019(4) Uani 0.25 1 d D U P A -1
C11 C 0.9381(11) 1.1604(15) 0.7720(7) 0.023(3) Uani 0.25 1 d D U P A -1
C12 C 0.8831(11) 1.1773(15) 0.7989(7) 0.030(4) Uani 0.25 1 d D U P A -1
H12 H 0.887289 1.180348 0.832882 0.036 Uiso 0.25 1 calc R U P A -1
C13 C 0.8219(14) 1.1899(17) 0.7756(8) 0.036(4) Uani 0.25 1 d D U P A -1
H13 H 0.791607 1.211693 0.792372 0.043 Uiso 0.25 1 calc R U P A -1
C14 C 0.8070(13) 1.1691(18) 0.7267(8) 0.037(4) Uani 0.25 1 d D U P A -1
H14 H 0.756935 1.162141 0.711892 0.044 Uiso 0.25 1 calc R U P A -1
C15 C 0.8663(11) 1.1588(16) 0.6997(7) 0.028(4) Uani 0.25 1 d D U P A -1
H15 H 0.860270 1.153866 0.665826 0.033 Uiso 0.25 1 calc R U P A -1
C16 C 0.9342(10) 1.1555(16) 0.7213(7) 0.022(3) Uani 0.25 1 d D U P A -1
N2 N 0.616(2) 0.616(2) 0.5825(13) 0.176(2) Uani 1 2 d S TU P . .
C17 C 0.547(3) 0.547(3) 0.5509(15) 0.186(4) Uani 1 2 d S TU P . .
C18 C 0.699(2) 0.699(2) 0.5686(12) 0.130(4) Uani 1 2 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb1 3.8986(11) 15_656 ?
Tb1 Tb1 3.9161(12) 3_675 ?
Tb1 Tb1 3.8986(11) 14_566 ?
Tb1 F1 2.334(4) 2_765 ?
Tb1 F1 2.333(7) 15_656 ?
Tb1 F1 2.334(4) . ?
Tb1 F2 2.344(3) . ?
Tb1 O1 2.337(7) 23_675 ?
Tb1 O1 2.337(7) . ?
Tb1 O2 2.83(4) . ?
Tb1 O3 2.362(5) 23_675 ?
Tb1 O3 2.362(5) . ?
O1 C5 1.254(9) . ?
O3 C6 1.273(7) . ?
N1 C1 1.427(14) . ?
N1 C1 1.427(14) 2_665 ?
N1 C1 1.427(14) 3_565 ?
C1 C2 1.364(13) . ?
C1 C2 1.364(13) 12_566 ?
C2 H2 0.9400 . ?
C2 C3 1.369(15) . ?
C3 H3 0.9400 . ?
C3 C4 1.371(13) . ?
C4 C5 1.50(2) . ?
C6 C7 1.3901(11) . ?
C7 C8 1.3900(11) . ?
C7 C16 1.3901(11) . ?
C8 H8 0.9400 . ?
C8 C9 1.3901(11) . ?
C9 H9 0.9400 . ?
C9 C10 1.3900(11) . ?
C10 C11 1.3901(11) . ?
C11 C12 1.3901(11) . ?
C11 C16 1.401(8) . ?
C12 H12 0.9400 . ?
C12 C13 1.3900(11) . ?
C13 H13 0.9400 . ?
C13 C14 1.3901(11) . ?
C14 H14 0.9400 . ?
C14 C15 1.3900(11) . ?
C15 H15 0.9400 . ?
C15 C16 1.3901(11) . ?
N2 C17 1.52(5) . ?
N2 C18 1.54(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
Tb1 Tb1 Tb1 59.851(11) 14_566 3_675 ?
Tb1 Tb1 Tb1 60.30(2) 15_656 14_566 ?
Tb1 Tb1 Tb1 90.000(1) 15_656 3_675 ?
F1 Tb1 Tb1 86.38(16) . 15_656 ?
F1 Tb1 Tb1 33.34(7) 15_656 15_656 ?
F1 Tb1 Tb1 85.98(15) 2_765 3_675 ?
F1 Tb1 Tb1 33.34(7) 15_656 14_566 ?
F1 Tb1 Tb1 85.98(14) 15_656 3_675 ?
F1 Tb1 Tb1 32.96(14) . 3_675 ?
F1 Tb1 Tb1 33.32(16) 2_765 15_656 ?
F1 Tb1 Tb1 33.32(16) . 14_566 ?
F1 Tb1 Tb1 86.38(17) 2_765 14_566 ?
F1 Tb1 F1 66.0(2) 15_656 2_765 ?
F1 Tb1 F1 66.0(2) 15_656 . ?
F1 Tb1 F1 100.5(3) 2_765 . ?
F1 Tb1 F2 65.81(19) . . ?
F1 Tb1 F2 65.81(19) 2_765 . ?
F1 Tb1 F2 100.7(3) 15_656 . ?
F1 Tb1 O1 76.6(2) . 23_675 ?
F1 Tb1 O1 139.5(2) 2_765 23_675 ?
F1 Tb1 O1 139.5(2) . . ?
F1 Tb1 O1 76.6(2) 2_765 . ?
F1 Tb1 O1 76.6(2) 15_656 23_675 ?
F1 Tb1 O1 76.6(2) 15_656 . ?
F1 Tb1 O2 129.72(16) 2_765 . ?
F1 Tb1 O2 127.9(9) 15_656 . ?
F1 Tb1 O2 129.72(16) . . ?
F1 Tb1 O3 137.7(2) . 23_675 ?
F1 Tb1 O3 77.3(2) 2_765 23_675 ?
F1 Tb1 O3 140.69(14) 15_656 23_675 ?
F1 Tb1 O3 137.7(2) 2_765 . ?
F1 Tb1 O3 77.3(2) . . ?
F1 Tb1 O3 140.69(15) 15_656 . ?
F2 Tb1 Tb1 33.36(10) . 3_675 ?
F2 Tb1 Tb1 86.3(2) . 15_656 ?
F2 Tb1 Tb1 86.3(2) . 14_566 ?
F2 Tb1 O2 131.4(9) . . ?
F2 Tb1 O3 75.4(2) . 23_675 ?
F2 Tb1 O3 75.4(2) . . ?
O1 Tb1 Tb1 106.98(16) . 14_566 ?
O1 Tb1 Tb1 159.15(16) . 3_675 ?
O1 Tb1 Tb1 106.83(17) 23_675 3_675 ?
O1 Tb1 Tb1 106.98(16) 23_675 15_656 ?
O1 Tb1 Tb1 69.15(16) . 15_656 ?
O1 Tb1 Tb1 69.16(16) 23_675 14_566 ?
O1 Tb1 F2 139.33(17) 23_675 . ?
O1 Tb1 F2 139.33(17) . . ?
O1 Tb1 O1 80.3(3) . 23_675 ?
O1 Tb1 O2 64.5(6) 23_675 . ?
O1 Tb1 O2 64.5(6) . . ?
O1 Tb1 O3 131.5(2) 23_675 23_675 ?
O1 Tb1 O3 81.8(2) 23_675 . ?
O1 Tb1 O3 131.5(2) . . ?
O1 Tb1 O3 81.8(2) . 23_675 ?
O2 Tb1 Tb1 133.6(6) . 14_566 ?
O2 Tb1 Tb1 133.6(6) . 15_656 ?
O2 Tb1 Tb1 136.4(6) . 3_675 ?
O3 Tb1 Tb1 107.97(14) . 14_566 ?
O3 Tb1 Tb1 69.33(14) . 3_675 ?
O3 Tb1 Tb1 159.25(14) 23_675 14_566 ?
O3 Tb1 Tb1 107.97(14) 23_675 15_656 ?
O3 Tb1 Tb1 159.25(14) . 15_656 ?
O3 Tb1 Tb1 105.72(14) 23_675 3_675 ?
O3 Tb1 O2 67.1(6) . . ?
O3 Tb1 O2 67.1(6) 23_675 . ?
O3 Tb1 O3 77.2(3) 23_675 . ?
Tb1 F1 Tb1 114.1(3) 3_675 . ?
Tb1 F1 Tb1 113.35(18) 14_566 3_675 ?
Tb1 F1 Tb1 113.35(18) 14_566 . ?
Tb1 F2 Tb1 113.3(2) . 2_765 ?
Tb1 F2 Tb1 113.3(2) . 3_675 ?
Tb1 F2 Tb1 113.3(2) 3_675 2_765 ?
C5 O1 Tb1 137.8(7) . . ?
C6 O3 Tb1 135.5(5) . . ?
C1 N1 C1 120.001(1) 3_565 . ?
C1 N1 C1 120.000(2) 2_665 3_565 ?
C1 N1 C1 119.999(5) 2_665 . ?
C2 C1 N1 120.6(7) 12_566 . ?
C2 C1 N1 120.6(7) . . ?
C2 C1 C2 118.7(14) 12_566 . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.5(11) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.7(11) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C3 117.0(13) 12_566 . ?
C3 C4 C5 121.5(7) . . ?
C3 C4 C5 121.5(7) 12_566 . ?
O1 C5 O1 126.1(12) . 12_566 ?
O1 C5 C4 116.9(6) . . ?
O1 C5 C4 116.9(6) 12_566 . ?
O3 C6 O3 124.1(9) . 24_765 ?
O3 C6 C7 122.0(7) 24_765 . ?
O3 C6 C7 113.9(7) . . ?
C8 C7 C6 112.8(12) . . ?
C16 C7 C6 129.2(14) . . ?
C16 C7 C8 118.1(12) . . ?
C7 C8 H8 119.0 . . ?
C7 C8 C9 122.1(17) . . ?
C9 C8 H8 119.0 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.5(17) . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 118.9(14) . . ?
C10 C11 C12 117.4(16) . . ?
C10 C11 C16 120.8(15) . . ?
C12 C11 C16 121.8(14) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.1(15) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 121.0 . . ?
C14 C13 C12 117.9(18) . . ?
C14 C13 H13 121.0 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(18) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 122.0(15) . . ?
C16 C15 H15 119.0 . . ?
C7 C16 C11 120.3(14) . . ?
C7 C16 C15 123.3(16) . . ?
C15 C16 C11 116.3(14) . . ?
C17 N2 C18 131(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C5 O1 -0.2(4) . . . 12_566 ?
Tb1 O1 C5 C4 179.8(4) . . . . ?
Tb1 O3 C6 O3 32.3(17) . . . 24_765 ?
Tb1 O3 C6 C7 -145.9(7) . . . . ?
O3 C6 C7 C8 142.5(10) . . . . ?
O3 C6 C7 C8 -35.7(10) 24_765 . . . ?
O3 C6 C7 C16 -37.0(17) . . . . ?
O3 C6 C7 C16 144.8(17) 24_765 . . . ?
N1 C1 C2 C3 -180.0(8) . . . . ?
C1 N1 C1 C2 -138.7(5) 3_565 . . 12_566 ?
C1 N1 C1 C2 41.3(5) 3_565 . . . ?
C1 N1 C1 C2 -138.7(5) 2_665 . . . ?
C1 N1 C1 C2 41.3(5) 2_665 . . 12_566 ?
C1 C2 C3 C4 0.0(16) . . . . ?
C2 C1 C2 C3 0.0(8) 12_566 . . . ?
C2 C3 C4 C3 0.0(8) . . . 12_566 ?
C2 C3 C4 C5 -180.0(8) . . . . ?
C3 C4 C5 O1 13.1(6) 12_566 . . . ?
C3 C4 C5 O1 -166.9(6) 12_566 . . 12_566 ?
C3 C4 C5 O1 -166.9(6) . . . . ?
C3 C4 C5 O1 13.1(6) . . . 12_566 ?
C6 C7 C8 C9 179(2) . . . . ?
C6 C7 C16 C11 178.7(18) . . . . ?
C6 C7 C16 C15 2(3) . . . . ?
C7 C8 C9 C10 6(3) . . . . ?
C8 C7 C16 C11 -1(3) . . . . ?
C8 C7 C16 C15 -177.6(19) . . . . ?
C8 C9 C10 C11 -9(4) . . . . ?
C9 C10 C11 C12 -171(2) . . . . ?
C9 C10 C11 C16 7(4) . . . . ?
C10 C11 C12 C13 178(2) . . . . ?
C10 C11 C16 C7 -2(4) . . . . ?
C10 C11 C16 C15 175(2) . . . . ?
C11 C12 C13 C14 12(4) . . . . ?
C12 C11 C16 C7 175.8(18) . . . . ?
C12 C11 C16 C15 -7(4) . . . . ?
C12 C13 C14 C15 -17(4) . . . . ?
C13 C14 C15 C16 10(4) . . . . ?
C14 C15 C16 C7 179(2) . . . . ?
C14 C15 C16 C11 2(4) . . . . ?
C16 C7 C8 C9 -1(2) . . . . ?
C16 C11 C12 C13 0(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
#==============================================================================
# Start Validation Reply Form
#=============================================================================
_vrf_PLAT602_a                   
;
PROBLEM: Solvent Accessible VOID(S) in Structure 
RESPONSE: This alert is inherent to MOF structures.
;

#==============================================================================
# Start Validation Reply Form
#=============================================================================
_vrf_THETM01_a                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however these crystals  
were small and weakly diffracting. Thus the very high angle data was 
dominated by noise because of the weak diffraction and thus was omitted.
;
####################################################################### 
# 
# 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_a_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2235995'
loop_
_audit_author_name
_audit_author_address
'Hong-Xin Li'
;Shaanxi Normal University
China
;
_audit_update_record             
;
2023-01-13 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_audit_creation_date             2022-12-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H15 F4 N1 O15 S4.5 Tb3'
_chemical_formula_sum            'C36 H21 F4 N O15 S4.50 Tb3'
_chemical_formula_weight         1404.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_H-M_alt        'P 63/m c m'
_space_group_name_Hall           '-P 6c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   17.8807(6)
_cell_length_b                   17.8807(6)
_cell_length_c                   34.2217(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9475.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8666
_cell_measurement_temperature    243.0
_cell_measurement_theta_max      50.19
_cell_measurement_theta_min      3.85
_shelx_estimated_absorpt_T_max   0.583
_shelx_estimated_absorpt_T_min   0.378
_exptl_absorpt_coefficient_mu    12.092
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.4028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1268 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.5371.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.985
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25841
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        50.460
_diffrn_reflns_theta_max         50.460
_diffrn_reflns_theta_min         2.582
_diffrn_ambient_temperature      243.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1598
_reflns_number_total             1820
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         1820
_refine_ls_number_restraints     273
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0750
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1019P)²+92.0855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2082
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6-C7
 1.39 with sigma of 0.001
 C8-S1
 2.5 with sigma of 0.001
 C11-C14
 2.56 with sigma of 0.01
 S1-C7 \\sim S1-C10 \\sim S2-C9 \\sim S2-C12 \\sim S3-C11 \\sim S3-C14
 with sigma of 0.02
 C7-C6 \\sim C8-C7 \\sim C8-C9 \\sim C9-C10 \\sim C10-C11 \\sim C12-C11 \\sim
C13-C12 \\sim C13-C14
 with sigma of 0.02
3. Restrained planarity
 C6, S1, S2, S3, C7, C8, C9, C10, C11, C12, C13, C14
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(S3) \\sim
Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O2) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S3) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S3) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(S3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S3) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(S2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 Tb1, O3, C6, S1, S2, S3, C7, C8, C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: S1(0.25) S2(0.25) S3(0.25) C7(0.25) C8(0.25) H8(0.25) C9(0.25)
 C10(0.25) C11(0.25) C12(0.25) C13(0.25) H13(0.25) C14(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.000000 0.12725(5) 0.45188(3) 0.0618(5) Uani 1 2 d S T P . .
F1 F -0.1101(7) 0.000000 0.4810(3) 0.096(3) Uani 1 2 d S T P . .
F2 F 0.000000 0.000000 0.4355(6) 0.096(5) Uani 1 6 d S T P . .
O1 O 0.0956(6) 0.2637(6) 0.4724(2) 0.084(2) Uani 1 1 d . U . . .
O2 O 0.000000 0.2563(18) 0.4033(9) 0.264(5) Uani 1 2 d S TU P . .
O3 O -0.0959(7) 0.0700(7) 0.4004(3) 0.114(3) Uani 1 1 d . U . . .
N1 N 0.333333 0.666667 0.500000 0.0851(13) Uani 1 6 d S TU P . .
C1 C 0.2870(5) 0.5739(11) 0.500000 0.071(2) Uani 1 2 d S TU P . .
C2 C 0.2171(8) 0.5308(8) 0.4765(4) 0.083(4) Uani 1 1 d . U . . .
H2 H 0.199674 0.561581 0.460123 0.099 Uiso 1 1 calc R U . . .
C3 C 0.1713(8) 0.4410(8) 0.4765(4) 0.076(3) Uani 1 1 d . U . . .
H3 H 0.122248 0.411073 0.460609 0.091 Uiso 1 1 calc R U . . .
C4 C 0.1978(5) 0.3957(11) 0.500000 0.067(2) Uani 1 2 d S TU P . .
C5 C 0.1490(6) 0.2980(11) 0.500000 0.077(2) Uani 1 2 d S TU P . .
C6 C -0.1348(10) 0.000000 0.3852(4) 0.090(5) Uani 1 2 d DS T P . .
S1 S -0.0928(10) 0.0579(10) 0.3068(6) 0.049(7) Uani 0.25 1 d D U P A -1
S2 S -0.2793(7) -0.1661(7) 0.2514(13) 0.095(3) Uani 0.25 1 d D U P A -1
S3 S -0.0998(15) 0.0589(17) 0.1921(10) 0.094(12) Uani 0.25 1 d D U P A -1
C7 C -0.1487(16) -0.0139(18) 0.3453(4) 0.070(6) Uani 0.25 1 d D U P A -1
C8 C -0.2101(11) -0.0875(12) 0.3284(8) 0.065(6) Uani 0.25 1 d D U P A -1
H8 H -0.247615 -0.134736 0.343983 0.078 Uiso 0.25 1 calc R U P A -1
C9 C -0.2176(18) -0.093(2) 0.2887(8) 0.058(5) Uani 0.25 1 d D U P A -1
C10 C -0.1574(15) -0.0181(18) 0.2718(8) 0.056(5) Uani 0.25 1 d D U P A -1
C11 C -0.151(2) -0.007(3) 0.2325(7) 0.053(5) Uani 0.25 1 d D U P A -1
C12 C -0.2148(18) -0.084(2) 0.2182(9) 0.055(5) Uani 0.25 1 d D U P A -1
C13 C -0.224(2) -0.093(2) 0.1787(9) 0.058(6) Uani 0.25 1 d D U P A -1
H13 H -0.266320 -0.143351 0.166560 0.070 Uiso 0.25 1 calc R U P A -1
C14 C -0.1672(18) -0.021(2) 0.1583(7) 0.052(6) Uani 0.25 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb1 3.9409(17) 3 ?
Tb1 Tb1 4.0029(17) 14_556 ?
Tb1 Tb1 3.9409(17) 2 ?
Tb1 F1 2.316(11) 14_556 ?
Tb1 F1 2.360(6) 3 ?
Tb1 F1 2.360(6) . ?
Tb1 F2 2.344(5) . ?
Tb1 O1 2.280(9) 24 ?
Tb1 O1 2.280(9) . ?
Tb1 O2 2.84(3) . ?
Tb1 O3 2.310(11) 24 ?
Tb1 O3 2.310(11) . ?
O1 C5 1.263(11) . ?
O3 C6 1.204(12) . ?
N1 C1 1.436(16) . ?
N1 C1 1.436(17) 2_665 ?
N1 C1 1.436(16) 3_565 ?
C1 C2 1.357(15) . ?
C1 C2 1.357(14) 11_556 ?
C2 H2 0.9400 . ?
C2 C3 1.391(16) . ?
C3 H3 0.9400 . ?
C3 C4 1.382(14) . ?
C4 C5 1.51(2) . ?
C6 C7 1.3899(11) . ?
S1 C7 1.761(17) . ?
S1 C10 1.745(17) . ?
S2 C9 1.761(18) . ?
S2 C12 1.753(18) . ?
S3 C11 1.752(17) . ?
S3 C14 1.767(17) . ?
C7 C8 1.352(16) . ?
C8 H8 0.9400 . ?
C8 C9 1.364(17) . ?
C9 C10 1.362(17) . ?
C10 C11 1.356(16) . ?
C11 C12 1.362(18) . ?
C12 C13 1.361(17) . ?
C13 H13 0.9400 . ?
C13 C14 1.359(17) . ?

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
Tb1 Tb1 Tb1 60.510(15) 3 14_556 ?
Tb1 Tb1 Tb1 90.0 2 14_556 ?
Tb1 Tb1 Tb1 60.0 2 3 ?
F1 Tb1 Tb1 83.6(3) . 3 ?
F1 Tb1 Tb1 81.5(3) . 14_556 ?
F1 Tb1 Tb1 33.4(2) . 2 ?
F1 Tb1 Tb1 33.4(2) 3 3 ?
F1 Tb1 Tb1 30.8(2) 3 14_556 ?
F1 Tb1 Tb1 83.4(3) 14_556 2 ?
F1 Tb1 Tb1 83.4(3) 14_556 3 ?
F1 Tb1 Tb1 31.45(10) 14_556 14_556 ?
F1 Tb1 Tb1 83.6(3) 3 2 ?
F1 Tb1 F1 60.6(4) 14_556 . ?
F1 Tb1 F1 92.5(6) . 3 ?
F1 Tb1 F1 60.6(4) 14_556 3 ?
F1 Tb1 F2 96.3(6) 14_556 . ?
F1 Tb1 O2 133.7(3) 3 . ?
F1 Tb1 O2 133.7(3) . . ?
F1 Tb1 O2 133.4(7) 14_556 . ?
F2 Tb1 Tb1 85.5(4) . 14_556 ?
F2 Tb1 Tb1 32.77(18) . 3 ?
F2 Tb1 Tb1 32.77(18) . 2 ?
F2 Tb1 F1 64.6(4) . . ?
F2 Tb1 F1 64.6(4) . 3 ?
F2 Tb1 O2 130.4(8) . . ?
O1 Tb1 Tb1 105.3(2) 24 14_556 ?
O1 Tb1 Tb1 157.9(2) 24 3 ?
O1 Tb1 Tb1 106.1(2) 24 2 ?
O1 Tb1 Tb1 67.9(2) . 14_556 ?
O1 Tb1 Tb1 157.9(2) . 2 ?
O1 Tb1 Tb1 106.1(2) . 3 ?
O1 Tb1 F1 77.3(3) 24 . ?
O1 Tb1 F1 77.7(3) . 14_556 ?
O1 Tb1 F1 77.3(3) . 3 ?
O1 Tb1 F1 136.0(3) . . ?
O1 Tb1 F1 77.7(3) 24 14_556 ?
O1 Tb1 F1 136.0(3) 24 3 ?
O1 Tb1 F2 138.5(2) . . ?
O1 Tb1 F2 138.5(2) 24 . ?
O1 Tb1 O1 81.0(4) 24 . ?
O1 Tb1 O2 67.4(5) . . ?
O1 Tb1 O2 67.4(5) 24 . ?
O1 Tb1 O3 134.6(3) . . ?
O1 Tb1 O3 82.4(3) 24 . ?
O1 Tb1 O3 134.6(4) 24 24 ?
O1 Tb1 O3 82.4(3) . 24 ?
O2 Tb1 Tb1 134.6(5) . 2 ?
O2 Tb1 Tb1 135.4(5) . 14_556 ?
O2 Tb1 Tb1 134.6(5) . 3 ?
O3 Tb1 Tb1 67.4(3) . 2 ?
O3 Tb1 Tb1 67.4(3) 24 3 ?
O3 Tb1 Tb1 157.4(3) . 14_556 ?
O3 Tb1 Tb1 105.0(3) 24 2 ?
O3 Tb1 Tb1 105.0(3) . 3 ?
O3 Tb1 Tb1 106.9(3) 24 14_556 ?
O3 Tb1 F1 138.3(3) . 14_556 ?
O3 Tb1 F1 138.3(3) 24 14_556 ?
O3 Tb1 F1 138.4(3) . 3 ?
O3 Tb1 F1 79.5(4) . . ?
O3 Tb1 F1 138.4(3) 24 . ?
O3 Tb1 F1 79.5(4) 24 3 ?
O3 Tb1 F2 75.4(4) . . ?
O3 Tb1 F2 75.4(4) 24 . ?
O3 Tb1 O2 67.2(5) 24 . ?
O3 Tb1 O2 67.2(5) . . ?
O3 Tb1 O3 80.0(5) . 24 ?
Tb1 F1 Tb1 117.8(3) 15_556 2 ?
Tb1 F1 Tb1 113.2(4) 2 . ?
Tb1 F1 Tb1 117.8(3) 15_556 . ?
Tb1 F2 Tb1 114.5(4) 2 3 ?
Tb1 F2 Tb1 114.5(4) 3 . ?
Tb1 F2 Tb1 114.5(4) 2 . ?
C5 O1 Tb1 136.9(10) . . ?
C6 O3 Tb1 134.8(10) . . ?
C1 N1 C1 119.999(4) 3_565 . ?
C1 N1 C1 120.001(2) . 2_665 ?
C1 N1 C1 120.000(7) 3_565 2_665 ?
C2 C1 N1 119.5(8) 11_556 . ?
C2 C1 N1 119.5(8) . . ?
C2 C1 C2 121.0(17) . 11_556 ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.9(13) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.1(13) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C3 119.0(16) . 11_556 ?
C3 C4 C5 120.5(8) . . ?
C3 C4 C5 120.5(8) 11_556 . ?
O1 C5 O1 130.2(17) . 11_556 ?
O1 C5 C4 114.9(9) 11_556 . ?
O1 C5 C4 114.9(8) . . ?
O3 C6 O3 128.4(16) 23 . ?
O3 C6 C7 106.9(13) 23 . ?
O3 C6 C7 124.7(16) . . ?
C10 S1 C7 91.8(11) . . ?
C12 S2 C9 86.8(11) . . ?
C11 S3 C14 93.0(11) . . ?
C6 C7 S1 128(2) . . ?
C8 C7 C6 126(2) . . ?
C8 C7 S1 106.1(9) . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2(17) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 S2 141(3) . . ?
C10 C9 S2 108(2) . . ?
C10 C9 C8 110(3) . . ?
C9 C10 S1 112(2) . . ?
C11 C10 S1 126(3) . . ?
C11 C10 C9 122(3) . . ?
C10 C11 S3 149(4) . . ?
C10 C11 C12 104(3) . . ?
C12 C11 S3 106.9(18) . . ?
C11 C12 S2 119(2) . . ?
C13 C12 S2 124(4) . . ?
C13 C12 C11 117(3) . . ?
C12 C13 H13 122.7 . . ?
C14 C13 C12 115(3) . . ?
C14 C13 H13 122.7 . . ?
C13 C14 S3 108.1(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C5 O1 0.2(5) . . . 11_556 ?
Tb1 O1 C5 C4 -179.8(5) . . . . ?
Tb1 O3 C6 O3 36(3) . . . 23 ?
Tb1 O3 C6 C7 -141.3(10) . . . . ?
O3 C6 C7 S1 -158.7(14) 23 . . . ?
O3 C6 C7 S1 19.0(17) . . . . ?
O3 C6 C7 C8 21.5(16) 23 . . . ?
O3 C6 C7 C8 -160.8(16) . . . . ?
N1 C1 C2 C3 -179.4(9) . . . . ?
C1 N1 C1 C2 43.0(6) 3_565 . . . ?
C1 N1 C1 C2 -137.0(6) 3_565 . . 11_556 ?
C1 N1 C1 C2 43.0(6) 2_665 . . 11_556 ?
C1 N1 C1 C2 -137.0(6) 2_665 . . . ?
C1 C2 C3 C4 -1.2(17) . . . . ?
C2 C1 C2 C3 0.6(9) 11_556 . . . ?
C2 C3 C4 C3 0.6(9) . . . 11_556 ?
C2 C3 C4 C5 -179.4(9) . . . . ?
C3 C4 C5 O1 -166.9(7) . . . 11_556 ?
C3 C4 C5 O1 13.1(7) 11_556 . . 11_556 ?
C3 C4 C5 O1 13.1(7) . . . . ?
C3 C4 C5 O1 -166.9(7) 11_556 . . . ?
C6 C7 C8 C9 179.9(8) . . . . ?
S1 C7 C8 C9 0.0(11) . . . . ?
S1 C10 C11 S3 0(2) . . . . ?
S1 C10 C11 C12 179.8(7) . . . . ?
S2 C9 C10 S1 -179.8(4) . . . . ?
S2 C9 C10 C11 0.1(11) . . . . ?
S2 C12 C13 C14 -179.7(7) . . . . ?
S3 C11 C12 S2 179.8(6) . . . . ?
S3 C11 C12 C13 0.1(11) . . . . ?
C7 S1 C10 C9 0.0(7) . . . . ?
C7 S1 C10 C11 -179.9(9) . . . . ?
C7 C8 C9 S2 179.7(8) . . . . ?
C7 C8 C9 C10 -0.1(12) . . . . ?
C8 C9 C10 S1 0.1(10) . . . . ?
C8 C9 C10 C11 179.9(9) . . . . ?
C9 S2 C12 C11 0.1(7) . . . . ?
C9 S2 C12 C13 179.8(9) . . . . ?
C9 C10 C11 S3 -179.9(12) . . . . ?
C9 C10 C11 C12 0.0(12) . . . . ?
C10 S1 C7 C6 -179.8(7) . . . . ?
C10 S1 C7 C8 0.0(7) . . . . ?
C10 C11 C12 S2 -0.1(10) . . . . ?
C10 C11 C12 C13 -179.8(8) . . . . ?
C11 S3 C14 C13 0.2(8) . . . . ?
C11 C12 C13 C14 0.0(12) . . . . ?
C12 S2 C9 C8 -179.9(12) . . . . ?
C12 S2 C9 C10 -0.1(7) . . . . ?
C12 C13 C14 S3 -0.1(10) . . . . ?
C14 S3 C11 C10 179.7(15) . . . . ?
C14 S3 C11 C12 -0.1(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.938 -0.009 -0.443 5992.9 1507.7 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
#==============================================================================
# Start Validation Reply Form
#=============================================================================
_vrf_THETM01_a                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however these crystals  
were small and weakly diffracting. Thus the very high angle data was 
dominated by noise because of the weak diffraction and thus was omitted.
;
