#------------------------------------------------------------------------------
#$Date: 2022-09-16 01:34:12 +0300 (Fri, 16 Sep 2022) $
#$Revision: 277902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/12/7711251.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7711251
loop_
_publ_author_name
'Liu, Weisai'
'Wang, Fei'
'Chen, Xiaoyi'
'Zhi, Wenke'
'Wang, Xuquan'
'Xu, Baoqiang'
'Yang, Bin'
_publ_section_title
;
 Design of “turn-off” luminescent Ln-MOFs for sensitive
 detection of cyanide anion
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01844F
_journal_year                    2022
_chemical_formula_moiety         'C18 H17 Br3 N2 O8 Tb, C3 H7 N O'
_chemical_formula_sum            'C21 H24 Br3 N3 O9 Tb'
_chemical_formula_weight         861.08
_chemical_name_systematic        Tb-DBTA
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                109.079(3)
_cell_angle_beta                 114.551(3)
_cell_angle_gamma                97.782(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2415(3)
_cell_length_b                   11.5520(3)
_cell_length_c                   12.9279(4)
_cell_measurement_reflns_used    14540
_cell_measurement_temperature    150.04(10)
_cell_measurement_theta_max      29.4260
_cell_measurement_theta_min      1.9150
_cell_volume                     1369.46(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.04(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  38.00   0.50    0.40    --   10.29 -57.00  60.00  206
  2  ω    -17.00  36.00   0.50    0.40    --   10.29  57.00-180.00  106
  3  ω     37.00  86.00   0.50    0.40    --   10.29  57.00-180.00   98
  4  ω    -90.00 -41.00   0.50    0.40    --  -11.46 159.00 -88.00   98
  5  ω    -67.00 -42.00   0.50    0.40    --  -11.46 118.00 118.00   50
  6  ω     -6.00  64.00   0.50    0.40    --  -11.46  57.00 -90.00  140
  7  ω    -87.00  23.00   0.50    0.40    --  -11.46 -77.00 -30.00  220
  8  ω    -87.00   9.00   0.50    0.40    --  -11.46 -57.00 150.00  192
  9  ω    -89.00  23.00   0.50    0.40    --  -11.46 -19.00 -60.00  224
 10  ω    -73.00 -24.00   0.50    0.40    --  -11.46 -57.00-120.00   98
 11  ω     -9.00  16.00   0.50    0.40    --  -11.46 -57.00-120.00   50
 12  ω     21.00  56.00   0.50    0.40    --   10.29 -99.00 -60.00   70
 13  ω    -11.00  18.00   0.50    0.40    --   10.29 -99.00 -60.00   58
 14  ω     48.00  90.00   0.50    0.40    --   10.29-159.00-121.00   84
 15  ω     14.00  65.00   0.50    0.40    --   10.29-118.00  31.00  102
 16  ω    -11.00  56.00   0.50    0.40    --   10.29 -99.00 120.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0111142000
_diffrn_orient_matrix_UB_12      0.0608021000
_diffrn_orient_matrix_UB_13      0.0171617000
_diffrn_orient_matrix_UB_21      0.0483161000
_diffrn_orient_matrix_UB_22      0.0178258000
_diffrn_orient_matrix_UB_23      0.0637279000
_diffrn_orient_matrix_UB_31      0.0537207000
_diffrn_orient_matrix_UB_32      0.0259430000
_diffrn_orient_matrix_UB_33      -0.0092386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31328
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.482
_diffrn_reflns_theta_min         1.913
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-Dimethylformamide?DMF?'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.318
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6425
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0414
_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)+(0.0703P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5384
_reflns_number_total             6425
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01844f2.cif
_cod_data_source_block           lws-150k_CCDC1
_cod_original_cell_volume        1369.46(8)
_cod_database_code               7711251
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N3 \\sim C19 \\sim C20 \\sim C21 \\sim O9A \\sim C19A \\sim N3A \\sim C20A
\\sim C21A \\sim O9: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
3. Others
 Sof(O9A)=Sof(C19A)=Sof(H19A)=Sof(N3A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(O9)=Sof(N3)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C11(H11), C13(H13), C16(H16), C19(H19), C19A(H19A)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C20A(H20D,H20E,H20F),
 C21A(H21D,H21E,H21F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.802
_oxdiff_exptl_absorpt_empirical_full_min 0.619
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.41062(2) 0.01071(2) 0.33226(2) 0.01640(9) Uani 1 1 d . . . . .
Br1 Br 0.37019(5) 0.35331(5) 0.70960(5) 0.02734(13) Uani 1 1 d . . . . .
Br2 Br 0.83531(5) 0.61845(5) 0.60364(5) 0.02921(14) Uani 1 1 d . . . . .
Br3 Br -0.11364(6) 0.22472(6) 0.42854(6) 0.03615(16) Uani 1 1 d . . . . .
O1 O 0.5299(3) 0.1392(3) 0.5485(3) 0.0198(7) Uani 1 1 d . . . . .
O2 O 0.6411(4) 0.2273(3) 0.7544(3) 0.0261(8) Uani 1 1 d . . . . .
O3 O 0.6865(3) 0.8086(3) 0.6419(4) 0.0274(8) Uani 1 1 d . . . . .
O4 O 0.5143(4) 0.7892(3) 0.6807(4) 0.0297(8) Uani 1 1 d . . . . .
O5 O 0.2548(3) -0.0355(3) 0.4016(3) 0.0211(7) Uani 1 1 d . . . . .
O6 O 0.3570(3) -0.0112(3) 0.6024(3) 0.0218(7) Uani 1 1 d . . . . .
O7 O 0.1819(3) -0.0691(4) 0.1522(3) 0.0289(8) Uani 1 1 d . . . . .
O8 O 0.4288(3) -0.0528(3) 0.1447(3) 0.0269(8) Uani 1 1 d . . . . .
N1 N -0.0464(5) -0.0937(5) 0.0649(5) 0.0359(11) Uani 1 1 d . . . . .
N2 N 0.4569(5) -0.1948(5) -0.0050(5) 0.0392(12) Uani 1 1 d . . . . .
C1 C 0.5905(5) 0.3671(4) 0.6527(4) 0.0192(10) Uani 1 1 d . . . . .
C2 C 0.5026(5) 0.4305(4) 0.6770(4) 0.0193(9) Uani 1 1 d . . . . .
C3 C 0.5078(5) 0.5504(4) 0.6748(4) 0.0202(10) Uani 1 1 d . . . . .
H3 H 0.442892 0.590091 0.686638 0.024 Uiso 1 1 calc R U . . .
C4 C 0.6055(5) 0.6140(4) 0.6555(4) 0.0186(9) Uani 1 1 d . . . . .
C5 C 0.6949(5) 0.5489(5) 0.6324(5) 0.0207(10) Uani 1 1 d . . . . .
C6 C 0.6856(5) 0.4268(5) 0.6294(5) 0.0234(10) Uani 1 1 d . . . . .
H6 H 0.745319 0.383585 0.611115 0.028 Uiso 1 1 calc R U . . .
C7 C 0.5869(5) 0.2359(4) 0.6526(5) 0.0197(10) Uani 1 1 d . . . . .
C8 C 0.6019(5) 0.7449(4) 0.6584(4) 0.0197(10) Uani 1 1 d . . . . .
C9 C 0.2574(5) -0.0221(4) 0.5026(5) 0.0195(10) Uani 1 1 d . . . . .
C10 C 0.1247(5) -0.0117(4) 0.5049(5) 0.0194(10) Uani 1 1 d . . . . .
C11 C 0.0706(5) 0.0789(5) 0.4692(5) 0.0210(10) Uani 1 1 d . . . . .
H11 H 0.117456 0.132539 0.446679 0.025 Uiso 1 1 calc R U . . .
C12 C -0.0511(5) 0.0911(5) 0.4665(5) 0.0206(10) Uani 1 1 d . . . . .
C13 C 0.0821(5) -0.0382(5) 0.1568(5) 0.0287(11) Uani 1 1 d . . . . .
H13 H 0.099546 0.030185 0.231866 0.034 Uiso 1 1 calc R U . . .
C14 C -0.1567(6) -0.0484(8) 0.0776(8) 0.062(2) Uani 1 1 d . . . . .
H14A H -0.219620 -0.116116 0.077536 0.092 Uiso 1 1 calc R U . . .
H14B H -0.207583 -0.027788 0.007099 0.092 Uiso 1 1 calc R U . . .
H14C H -0.117174 0.029036 0.156726 0.092 Uiso 1 1 calc R U . . .
C15 C -0.0813(7) -0.2009(6) -0.0508(7) 0.060(2) Uani 1 1 d . . . . .
H15A H 0.003287 -0.209964 -0.052726 0.090 Uiso 1 1 calc R U . . .
H15B H -0.139373 -0.185045 -0.122501 0.090 Uiso 1 1 calc R U . . .
H15C H -0.131444 -0.280466 -0.055463 0.090 Uiso 1 1 calc R U . . .
C16 C 0.4794(6) -0.1350(5) 0.1101(5) 0.0321(12) Uani 1 1 d . . . . .
H16 H 0.540157 -0.157269 0.172071 0.039 Uiso 1 1 calc R U . . .
C17 C 0.5147(10) -0.2960(7) -0.0370(8) 0.071(2) Uani 1 1 d . . . . .
H17A H 0.579811 -0.300092 0.039799 0.107 Uiso 1 1 calc R U . . .
H17B H 0.563017 -0.277990 -0.080819 0.107 Uiso 1 1 calc R U . . .
H17C H 0.440669 -0.378734 -0.091869 0.107 Uiso 1 1 calc R U . . .
C18 C 0.3687(7) -0.1654(7) -0.1063(6) 0.0508(17) Uani 1 1 d . . . . .
H18A H 0.281025 -0.235740 -0.161627 0.076 Uiso 1 1 calc R U . . .
H18B H 0.414336 -0.156005 -0.154610 0.076 Uiso 1 1 calc R U . . .
H18C H 0.351361 -0.084764 -0.070925 0.076 Uiso 1 1 calc R U . . .
O9 O -0.2699(11) -0.4037(10) -0.0242(11) 0.075(4) Uani 0.500(8) 1 d . U P A 1
N3 N -0.1345(15) -0.4592(14) 0.1230(14) 0.050(3) Uani 0.500(8) 1 d . U P A 1
C19 C -0.239(2) -0.4835(18) 0.0094(17) 0.042(3) Uani 0.500(8) 1 d . U P A 1
H19 H -0.291422 -0.571073 -0.047290 0.051 Uiso 0.500(8) 1 calc R U P A 1
C20 C -0.050(2) -0.3311(18) 0.212(2) 0.076(5) Uani 0.500(8) 1 d . U P A 1
H20A H 0.024700 -0.304856 0.195904 0.114 Uiso 0.500(8) 1 calc R U P A 1
H20B H -0.010404 -0.327370 0.297163 0.114 Uiso 0.500(8) 1 calc R U P A 1
H20C H -0.105309 -0.272589 0.205677 0.114 Uiso 0.500(8) 1 calc R U P A 1
C21 C -0.0981(19) -0.5621(16) 0.1523(18) 0.086(5) Uani 0.500(8) 1 d . U P A 1
H21A H -0.155927 -0.644487 0.078704 0.129 Uiso 0.500(8) 1 calc R U P A 1
H21B H -0.112220 -0.561439 0.222386 0.129 Uiso 0.500(8) 1 calc R U P A 1
H21C H -0.001004 -0.551337 0.176151 0.129 Uiso 0.500(8) 1 calc R U P A 1
O9A O -0.1735(10) -0.2564(9) 0.2083(10) 0.058(3) Uani 0.500(8) 1 d . U P A 2
C19A C -0.0846(16) -0.2954(16) 0.1967(16) 0.042(3) Uani 0.500(8) 1 d . U P A 2
H19A H 0.006991 -0.237817 0.250468 0.050 Uiso 0.500(8) 1 calc R U P A 2
N3A N -0.1007(14) -0.4125(14) 0.1154(13) 0.045(3) Uani 0.500(8) 1 d . U P A 2
C20A C 0.0149(15) -0.4474(16) 0.1046(15) 0.071(5) Uani 0.500(8) 1 d . U P A 2
H20D H 0.098479 -0.372424 0.159523 0.106 Uiso 0.500(8) 1 calc R U P A 2
H20E H -0.004798 -0.475062 0.017356 0.106 Uiso 0.500(8) 1 calc R U P A 2
H20F H 0.028561 -0.518057 0.129566 0.106 Uiso 0.500(8) 1 calc R U P A 2
C21A C -0.232(2) -0.511(2) 0.040(2) 0.063(5) Uani 0.500(8) 1 d . U P A 2
H21D H -0.247792 -0.551975 0.090447 0.094 Uiso 0.500(8) 1 calc R U P A 2
H21E H -0.232651 -0.575733 -0.031961 0.094 Uiso 0.500(8) 1 calc R U P A 2
H21F H -0.304162 -0.472507 0.009960 0.094 Uiso 0.500(8) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 71.01(11) . 2_656 ?
O1 Tb1 O2 121.43(11) . 2_656 ?
O1 Tb1 O3 75.74(11) . 2_666 ?
O1 Tb1 O4 84.06(12) . 2_666 ?
O1 Tb1 O5 75.18(11) . . ?
O1 Tb1 O6 75.17(11) . 2_656 ?
O1 Tb1 O7 140.86(11) . . ?
O1 Tb1 O8 144.23(11) . . ?
O2 Tb1 O1 50.42(10) 2_656 2_656 ?
O3 Tb1 O1 133.70(11) 2_666 2_656 ?
O3 Tb1 O2 145.82(11) 2_666 2_656 ?
O4 Tb1 O1 147.82(12) 2_666 2_656 ?
O4 Tb1 O2 147.79(11) 2_666 2_656 ?
O4 Tb1 O3 53.08(11) 2_666 2_666 ?
O5 Tb1 O1 67.14(10) . 2_656 ?
O5 Tb1 O2 82.13(11) . 2_656 ?
O5 Tb1 O3 73.91(11) . 2_666 ?
O5 Tb1 O4 126.41(11) . 2_666 ?
O5 Tb1 O6 133.28(11) . 2_656 ?
O5 Tb1 O7 73.33(11) . . ?
O5 Tb1 O8 140.51(12) . . ?
O6 Tb1 O1 69.46(10) 2_656 2_656 ?
O6 Tb1 O2 83.49(11) 2_656 2_656 ?
O6 Tb1 O3 130.69(11) 2_656 2_666 ?
O6 Tb1 O4 84.99(11) 2_656 2_666 ?
O6 Tb1 O7 143.96(12) 2_656 . ?
O6 Tb1 O8 74.73(11) 2_656 . ?
O7 Tb1 O1 115.79(11) . 2_656 ?
O7 Tb1 O2 76.34(12) . 2_656 ?
O7 Tb1 O3 73.67(12) . 2_666 ?
O7 Tb1 O4 96.39(12) . 2_666 ?
O8 Tb1 O1 114.90(10) . 2_656 ?
O8 Tb1 O2 73.46(11) . 2_656 ?
O8 Tb1 O3 110.98(12) . 2_666 ?
O8 Tb1 O4 74.51(12) . 2_666 ?
O8 Tb1 O7 71.06(12) . . ?
Tb1 O1 Tb1 108.99(11) . 2_656 ?
C7 O1 Tb1 161.5(3) . . ?
C7 O1 Tb1 89.5(3) . 2_656 ?
C7 O2 Tb1 97.6(3) . 2_656 ?
C8 O3 Tb1 91.9(3) . 2_666 ?
C8 O4 Tb1 93.6(3) . 2_666 ?
C9 O5 Tb1 138.4(3) . . ?
C9 O6 Tb1 135.3(3) . 2_656 ?
C13 O7 Tb1 123.7(3) . . ?
C16 O8 Tb1 126.1(3) . . ?
C13 N1 C14 120.7(6) . . ?
C13 N1 C15 120.8(5) . . ?
C15 N1 C14 118.5(5) . . ?
C16 N2 C17 121.1(6) . . ?
C16 N2 C18 121.6(5) . . ?
C17 N2 C18 117.2(5) . . ?
C2 C1 C7 122.0(4) . . ?
C6 C1 C2 118.8(4) . . ?
C6 C1 C7 119.2(4) . . ?
C1 C2 Br1 120.6(3) . . ?
C1 C2 C3 120.4(4) . . ?
C3 C2 Br1 119.0(3) . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.7(4) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 117.1(4) . . ?
C3 C4 C8 116.3(4) . . ?
C5 C4 C8 126.6(4) . . ?
C4 C5 Br2 123.8(3) . . ?
C6 C5 Br2 115.3(3) . . ?
C6 C5 C4 121.0(4) . . ?
C1 C6 C5 121.0(4) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
O1 C7 Tb1 65.1(2) . 2_656 ?
O1 C7 C1 118.1(4) . . ?
O2 C7 Tb1 57.4(2) . 2_656 ?
O2 C7 O1 122.5(4) . . ?
O2 C7 C1 119.4(4) . . ?
C1 C7 Tb1 176.8(3) . 2_656 ?
O3 C8 Tb1 61.6(2) . 2_666 ?
O3 C8 O4 121.4(4) . . ?
O3 C8 C4 120.3(4) . . ?
O4 C8 Tb1 59.8(2) . 2_666 ?
O4 C8 C4 118.3(4) . . ?
C4 C8 Tb1 178.0(3) . 2_666 ?
O5 C9 O6 128.0(4) . . ?
O5 C9 C10 114.8(4) . . ?
O6 C9 C10 117.1(4) . . ?
C11 C10 C9 117.3(4) . . ?
C11 C10 C12 118.3(4) . 2_556 ?
C12 C10 C9 124.3(4) 2_556 . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.1(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C12 Br3 120.1(3) 2_556 . ?
C11 C12 Br3 118.3(3) . . ?
C11 C12 C10 121.6(4) . 2_556 ?
O7 C13 N1 124.5(5) . . ?
O7 C13 H13 117.7 . . ?
N1 C13 H13 117.7 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 N2 125.8(5) . . ?
O8 C16 H16 117.1 . . ?
N2 C16 H16 117.1 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 N3 C20 121.3(15) . . ?
C19 N3 C21 120.7(16) . . ?
C20 N3 C21 117.8(15) . . ?
O9 C19 N3 124.5(18) . . ?
O9 C19 H19 117.7 . . ?
N3 C19 H19 117.7 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O9A C19A H19A 116.6 . . ?
O9A C19A N3A 126.7(16) . . ?
N3A C19A H19A 116.6 . . ?
C19A N3A C20A 122.0(14) . . ?
C19A N3A C21A 121.1(16) . . ?
C21A N3A C20A 116.8(16) . . ?
N3A C20A H20D 109.5 . . ?
N3A C20A H20E 109.5 . . ?
N3A C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
N3A C21A H21D 109.5 . . ?
N3A C21A H21E 109.5 . . ?
N3A C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.335(3) . ?
Tb1 O1 2.650(3) 2_656 ?
Tb1 O2 2.483(3) 2_656 ?
Tb1 O3 2.475(3) 2_666 ?
Tb1 O4 2.434(3) 2_666 ?
Tb1 O5 2.350(3) . ?
Tb1 O6 2.387(3) 2_656 ?
Tb1 O7 2.421(3) . ?
Tb1 O8 2.397(3) . ?
Br1 C2 1.895(5) . ?
Br2 C5 1.901(5) . ?
Br3 C12 1.902(4) . ?
O1 C7 1.255(6) . ?
O2 C7 1.245(6) . ?
O3 C8 1.254(6) . ?
O4 C8 1.261(6) . ?
O5 C9 1.251(6) . ?
O6 C9 1.261(6) . ?
O7 C13 1.241(6) . ?
O8 C16 1.227(6) . ?
N1 C13 1.316(7) . ?
N1 C14 1.459(8) . ?
N1 C15 1.448(8) . ?
N2 C16 1.313(7) . ?
N2 C17 1.440(7) . ?
N2 C18 1.455(7) . ?
C1 C2 1.385(6) . ?
C1 C6 1.383(6) . ?
C1 C7 1.509(6) . ?
C2 C3 1.390(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(6) . ?
C4 C5 1.405(6) . ?
C4 C8 1.507(6) . ?
C5 C6 1.386(6) . ?
C6 H6 0.9500 . ?
C9 C10 1.525(6) . ?
C10 C11 1.390(6) . ?
C10 C12 1.391(6) 2_556 ?
C11 H11 0.9500 . ?
C11 C12 1.382(6) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O9 C19 1.175(18) . ?
N3 C19 1.35(2) . ?
N3 C20 1.42(2) . ?
N3 C21 1.422(19) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
O9A C19A 1.194(17) . ?
C19A H19A 0.9500 . ?
C19A N3A 1.35(2) . ?
N3A C20A 1.458(18) . ?
N3A C21A 1.43(3) . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
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 C7 Tb1 178.1(9) . . . 2_656 ?
Tb1 O1 C7 O2 178.5(6) . . . . ?
Tb1 O1 C7 O2 0.4(4) 2_656 . . . ?
Tb1 O1 C7 C1 179.7(4) 2_656 . . . ?
Tb1 O1 C7 C1 -2.2(11) . . . . ?
Tb1 O2 C7 O1 -0.4(5) 2_656 . . . ?
Tb1 O2 C7 C1 -179.8(3) 2_656 . . . ?
Tb1 O3 C8 O4 -1.1(5) 2_666 . . . ?
Tb1 O3 C8 C4 -179.4(4) 2_666 . . . ?
Tb1 O4 C8 O3 1.1(5) 2_666 . . . ?
Tb1 O4 C8 C4 179.5(4) 2_666 . . . ?
Tb1 O5 C9 O6 -24.1(8) . . . . ?
Tb1 O5 C9 C10 152.7(3) . . . . ?
Tb1 O6 C9 O5 -1.0(8) 2_656 . . . ?
Tb1 O6 C9 C10 -177.8(3) 2_656 . . . ?
Tb1 O7 C13 N1 -170.1(4) . . . . ?
Tb1 O8 C16 N2 160.1(4) . . . . ?
Br1 C2 C3 C4 177.8(4) . . . . ?
Br2 C5 C6 C1 178.0(4) . . . . ?
O5 C9 C10 C11 -51.5(6) . . . . ?
O5 C9 C10 C12 124.8(5) . . . 2_556 ?
O6 C9 C10 C11 125.6(5) . . . . ?
O6 C9 C10 C12 -58.0(6) . . . 2_556 ?
C1 C2 C3 C4 -3.8(7) . . . . ?
C2 C1 C6 C5 1.1(8) . . . . ?
C2 C1 C7 O1 102.9(5) . . . . ?
C2 C1 C7 O2 -77.7(6) . . . . ?
C2 C3 C4 C5 3.0(7) . . . . ?
C2 C3 C4 C8 -178.5(4) . . . . ?
C3 C4 C5 Br2 179.9(4) . . . . ?
C3 C4 C5 C6 -0.2(7) . . . . ?
C3 C4 C8 O3 -180.0(4) . . . . ?
C3 C4 C8 O4 1.6(7) . . . . ?
C4 C5 C6 C1 -1.9(8) . . . . ?
C5 C4 C8 O3 -1.6(7) . . . . ?
C5 C4 C8 O4 179.9(5) . . . . ?
C6 C1 C2 Br1 180.0(4) . . . . ?
C6 C1 C2 C3 1.6(7) . . . . ?
C6 C1 C7 O1 -77.9(6) . . . . ?
C6 C1 C7 O2 101.5(5) . . . . ?
C7 C1 C2 Br1 -0.8(7) . . . . ?
C7 C1 C2 C3 -179.2(4) . . . . ?
C7 C1 C6 C5 -178.1(5) . . . . ?
C8 C4 C5 Br2 1.6(7) . . . . ?
C8 C4 C5 C6 -178.5(5) . . . . ?
C9 C10 C11 C12 178.5(4) . . . . ?
C10 C11 C12 Br3 175.6(4) . . . . ?
C10 C11 C12 C10 -2.0(8) . . . 2_556 ?
C12 C10 C11 C12 1.9(8) 2_556 . . . ?
C14 N1 C13 O7 -178.3(5) . . . . ?
C15 N1 C13 O7 1.8(8) . . . . ?
C17 N2 C16 O8 -175.9(6) . . . . ?
C18 N2 C16 O8 1.7(9) . . . . ?
C20 N3 C19 O9 -1(3) . . . . ?
C21 N3 C19 O9 -175.3(19) . . . . ?
O9A C19A N3A C20A 176.6(16) . . . . ?
O9A C19A N3A C21A -7(3) . . . . ?
