#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:09:55 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261649 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/61/7706157.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_7706157
loop_
_publ_author_name
'Zhao, Xiao-Yang'
'Yang, Hui'
'Zhao, Wen-Yuan'
'Wang, Jia'
'Yang, Qi-Shan'
_publ_section_title
;
 A weakly luminescent Tb-MOF-based "turn-on" sensor for the
 highly selective and sensitive sensing of an anthrax biomarker.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1300
_journal_page_last               1306
_journal_paper_doi               10.1039/d0dt03906c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C18 H20 N2 O11 Tb, C3 H7 N O'
_chemical_formula_sum            'C21 H27 N3 O12 Tb'
_chemical_formula_weight         672.37
_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
_audit_block_doi                 10.5517/ccdc.csd.cc269b95
_audit_creation_date             2020-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-30 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                103.610(8)
_cell_angle_beta                 110.496(7)
_cell_angle_gamma                96.519(8)
_cell_formula_units_Z            2
_cell_length_a                   10.560(3)
_cell_length_b                   11.022(3)
_cell_length_c                   12.840(4)
_cell_measurement_reflns_used    6520
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.30
_cell_measurement_theta_min      2.96
_cell_volume                     1328.7(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22024
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.811
_diffrn_reflns_theta_min         3.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6102
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0838 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.8184.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0534
_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)+(0.0407P)²+0.3037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4422
_reflns_number_total             6225
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03906c2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7706157.cif.'
_cod_database_code               7706157
_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   0.702
_shelx_estimated_absorpt_t_min   0.549
_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, All O(H) groups
2. Restrained distances
 C16A-C17
 2.2 with sigma of 0.02
 C18-N2 \\sim N2-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C18 \\sim N2 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C16B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19B) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21B) = Uanis(C20A) = Uanis(C20B) = Uanis(C21A)
Uanis(C16B) = Uanis(C16A)
4. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C19A)=Sof(H19A)=1-FVAR(1)
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C19B)=Sof(H19B)=Sof(C21B)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(C16A)=Sof(H16A)=1-FVAR(2)
 Sof(C16B)=Sof(H16B)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3A), C7(H7), C13(H13), C16B(H16B), C19B(H19B), C19A(H19A),
 C16A(H16A)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C20B(H20A,H20B,H20C), C21B(H21A,H21B,H21C), C21A(H21D,H21E,H21F),
 C20A(H20D,H20E,H20F)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O9(H9), O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
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 0.39608(3) 0.45256(2) 0.31808(2) 0.02385(10) Uani 1 1 d . . . . .
O10 O 0.4293(5) 0.5210(4) 0.1643(3) 0.0485(12) Uani 1 1 d . . . . .
O5 O 0.4834(4) 0.3352(3) 0.5873(3) 0.0328(9) Uani 1 1 d . . . . .
O7 O 0.1718(4) 0.3102(4) 0.2198(4) 0.0504(12) Uani 1 1 d . . . . .
O3 O -0.1746(4) 0.4013(5) 0.2685(3) 0.0575(14) Uani 1 1 d . . . . .
H3 H -0.255111 0.403391 0.259445 0.086 Uiso 1 1 calc GR . . . .
O9 O 0.2640(5) 0.0158(5) 0.0039(5) 0.0721(16) Uani 1 1 d . . . . .
H9 H 0.317123 0.080570 0.053126 0.108 Uiso 1 1 calc GR . . . .
O2 O 0.3753(4) 0.5676(4) 0.6645(3) 0.0383(10) Uani 1 1 d . . . . .
O8 O 0.3248(4) 0.2465(4) 0.1524(3) 0.0390(10) Uani 1 1 d . . . . .
O6 O 0.4551(6) 0.0533(4) 0.2922(4) 0.0684(16) Uani 1 1 d . . . . .
H6 H 0.434093 0.123003 0.294300 0.103 Uiso 1 1 calc GR . . . .
O4 O 0.4272(4) 0.2759(3) 0.3942(3) 0.0368(10) Uani 1 1 d . . . . .
C12 C 0.1348(6) 0.0118(6) 0.0047(5) 0.0338(14) Uani 1 1 d . . . . .
C6 C 0.4782(6) 0.1214(5) 0.4928(5) 0.0319(14) Uani 1 1 d . . . . .
O11 O 0.2287(5) 0.5761(6) 0.2561(5) 0.0697(16) Uani 1 1 d . . . . .
C4 C -0.0910(6) 0.4512(6) 0.3844(5) 0.0324(14) Uani 1 1 d . . . . .
C5 C 0.4617(5) 0.2549(5) 0.4914(5) 0.0283(13) Uani 1 1 d . . . . .
C9 C 0.2048(6) 0.2291(6) 0.1538(5) 0.0340(14) Uani 1 1 d . . . . .
C8 C 0.4766(7) 0.0305(5) 0.3963(5) 0.0374(15) Uani 1 1 d . . . . .
C10 C 0.0996(6) 0.1096(5) 0.0747(5) 0.0320(14) Uani 1 1 d . . . . .
C11 C -0.0357(6) 0.0973(6) 0.0681(5) 0.0379(15) Uani 1 1 d . . . . .
H11 H -0.059750 0.162770 0.112968 0.046 Uiso 1 1 calc R . . . .
C1 C 0.2942(6) 0.5300(5) 0.5581(5) 0.0294(13) Uani 1 1 d . . . . .
C2 C 0.1430(5) 0.5149(5) 0.5293(5) 0.0275(13) Uani 1 1 d . . . . .
C3 C 0.0500(6) 0.4663(6) 0.4149(5) 0.0350(15) Uani 1 1 d . . . . .
H3A H 0.083487 0.443084 0.356659 0.042 Uiso 1 1 calc R . . . .
C7 C 0.5016(6) 0.0884(5) 0.5948(5) 0.0402(16) Uani 1 1 d . . . . .
H7 H 0.502748 0.148789 0.659514 0.048 Uiso 1 1 calc R . . . .
N1 N 0.5004(7) 0.6859(6) 0.1075(5) 0.0616(17) Uani 1 1 d . . . . .
C13 C 0.5172(8) 0.6125(7) 0.1748(6) 0.0524(18) Uani 1 1 d . . . . .
H13 H 0.602725 0.630251 0.236278 0.063 Uiso 1 1 calc R . . . .
O1 O 0.3377(4) 0.5050(4) 0.4778(4) 0.0365(10) Uani 1 1 d . . . . .
N2 N 0.0674(7) 0.6748(8) 0.1733(6) 0.080(2) Uani 1 1 d D U . . .
C16B C 0.1148(11) 0.5757(11) 0.2005(9) 0.049(3) Uani 0.648(12) 1 d . U P A 1
H16B H 0.051091 0.498421 0.172646 0.059 Uiso 0.648(12) 1 calc R . P A 1
C14 C 0.6095(11) 0.7913(9) 0.1259(9) 0.117(4) Uani 1 1 d . . . . .
H14A H 0.689721 0.796010 0.193076 0.175 Uiso 1 1 calc GR . . . .
H14B H 0.578017 0.869848 0.138068 0.175 Uiso 1 1 calc GR . . . .
H14C H 0.632746 0.777812 0.058820 0.175 Uiso 1 1 calc GR . . . .
C15 C 0.3727(12) 0.6678(11) 0.0116(9) 0.145(5) Uani 1 1 d . . . . .
H15A H 0.332764 0.578057 -0.023391 0.218 Uiso 1 1 calc GR . . . .
H15B H 0.389339 0.703646 -0.044935 0.218 Uiso 1 1 calc GR . . . .
H15C H 0.310140 0.709530 0.038474 0.218 Uiso 1 1 calc GR . . . .
C18 C -0.0788(12) 0.6370(12) 0.1057(11) 0.145(5) Uani 1 1 d D U . . .
H18A H -0.096557 0.632066 0.026090 0.218 Uiso 1 1 calc GR . . . .
H18B H -0.124271 0.698706 0.135725 0.218 Uiso 1 1 calc GR . . . .
H18C H -0.113603 0.554798 0.110180 0.218 Uiso 1 1 calc GR . . . .
C17 C 0.1236(13) 0.8078(11) 0.2016(10) 0.153(5) Uani 1 1 d D U . . .
H17A H 0.198558 0.835616 0.276717 0.230 Uiso 1 1 calc GR . . . .
H17B H 0.052917 0.855049 0.203021 0.230 Uiso 1 1 calc GR . . . .
H17C H 0.157171 0.822398 0.144152 0.230 Uiso 1 1 calc GR . . . .
N3 N -0.0177(10) 0.1536(7) 0.4553(8) 0.094(2) Uani 1 1 d . . . . .
O12 O 0.1184(13) 0.2286(10) 0.6418(9) 0.169(4) Uani 1 1 d . . . . .
C20B C -0.147(3) 0.115(2) 0.357(3) 0.132(5) Uani 0.509(10) 1 d . . P B 1
H20A H -0.174793 0.023729 0.330795 0.198 Uiso 0.509(10) 1 calc GR . P B 1
H20B H -0.136571 0.145222 0.295274 0.198 Uiso 0.509(10) 1 calc GR . P B 1
H20C H -0.215916 0.151176 0.378579 0.198 Uiso 0.509(10) 1 calc GR . P B 1
C19B C 0.005(3) 0.204(3) 0.567(3) 0.124(9) Uani 0.509(10) 1 d . U P B 1
H19B H -0.069210 0.220574 0.587718 0.149 Uiso 0.509(10) 1 calc R . P B 1
C21B C 0.104(3) 0.142(2) 0.417(2) 0.132(5) Uani 0.509(10) 1 d . . P B 1
H21A H 0.125119 0.059067 0.415346 0.198 Uiso 0.509(10) 1 calc GR . P B 1
H21B H 0.184079 0.206646 0.471713 0.198 Uiso 0.509(10) 1 calc GR . P B 1
H21C H 0.080270 0.152918 0.341276 0.198 Uiso 0.509(10) 1 calc GR . P B 1
C21A C -0.148(3) 0.142(2) 0.475(2) 0.132(5) Uani 0.491(10) 1 d . . P B 2
H21D H -0.209437 0.185522 0.429081 0.198 Uiso 0.491(10) 1 calc GR . P B 2
H21E H -0.128471 0.180626 0.555759 0.198 Uiso 0.491(10) 1 calc GR . P B 2
H21F H -0.192118 0.053770 0.452350 0.198 Uiso 0.491(10) 1 calc GR . P B 2
C20A C -0.038(3) 0.112(2) 0.340(3) 0.132(5) Uani 0.491(10) 1 d . . P B 2
H20D H -0.010333 0.032420 0.324319 0.198 Uiso 0.491(10) 1 calc GR . P B 2
H20E H 0.015773 0.174641 0.322469 0.198 Uiso 0.491(10) 1 calc GR . P B 2
H20F H -0.134498 0.101274 0.292825 0.198 Uiso 0.491(10) 1 calc GR . P B 2
C19A C 0.105(4) 0.195(3) 0.546(3) 0.117(9) Uani 0.491(10) 1 d . U P B 2
H19A H 0.184862 0.197161 0.530472 0.140 Uiso 0.491(10) 1 calc R . P B 2
C16A C 0.203(2) 0.6505(19) 0.2465(18) 0.049(3) Uani 0.352(12) 1 d D . P A 2
H16A H 0.272157 0.723749 0.289505 0.059 Uiso 0.352(12) 1 calc R . 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'
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
O10 Tb1 O7 102.50(15) . . ?
O10 Tb1 O8 76.30(14) . . ?
O10 Tb1 C9 90.32(16) . . ?
O5 Tb1 O10 77.47(14) 2_666 . ?
O5 Tb1 O7 145.64(15) 2_666 . ?
O5 Tb1 O2 79.39(14) 2_666 2_666 ?
O5 Tb1 O8 151.73(13) 2_666 . ?
O5 Tb1 O4 126.48(13) 2_666 . ?
O5 Tb1 O11 75.49(17) 2_666 . ?
O5 Tb1 C9 162.88(15) 2_666 . ?
O7 Tb1 O8 52.47(14) . . ?
O7 Tb1 C9 25.97(15) . . ?
O2 Tb1 O10 74.39(15) 2_666 . ?
O2 Tb1 O7 134.30(14) 2_666 . ?
O2 Tb1 O8 83.57(13) 2_666 . ?
O2 Tb1 C9 109.12(16) 2_666 . ?
O8 Tb1 C9 26.53(15) . . ?
O4 Tb1 O10 137.63(15) . . ?
O4 Tb1 O7 76.72(15) . . ?
O4 Tb1 O2 76.88(14) . 2_666 ?
O4 Tb1 O8 70.09(13) . . ?
O4 Tb1 O11 141.34(17) . . ?
O4 Tb1 C9 70.55(15) . . ?
O11 Tb1 O10 72.36(18) . . ?
O11 Tb1 O7 71.98(18) . . ?
O11 Tb1 O2 141.77(17) . 2_666 ?
O11 Tb1 O8 106.06(17) . . ?
O11 Tb1 C9 89.49(19) . . ?
O1 Tb1 O10 145.94(15) . . ?
O1 Tb1 O5 77.23(13) . 2_666 ?
O1 Tb1 O7 86.20(14) . . ?
O1 Tb1 O2 122.24(13) . 2_666 ?
O1 Tb1 O8 131.05(13) . . ?
O1 Tb1 O4 76.31(14) . . ?
O1 Tb1 O11 79.49(17) . . ?
O1 Tb1 C9 108.49(16) . . ?
C13 O10 Tb1 126.7(4) . . ?
C5 O5 Tb1 135.1(4) . 2_666 ?
C9 O7 Tb1 96.5(3) . . ?
C4 O3 H3 109.5 . . ?
C12 O9 H9 109.5 . . ?
C1 O2 Tb1 109.6(3) . 2_666 ?
C9 O8 Tb1 89.7(3) . . ?
C8 O6 H6 109.5 . . ?
C5 O4 Tb1 138.3(3) . . ?
O9 C12 C10 124.0(5) . . ?
O9 C12 C11 116.1(5) . 2 ?
C11 C12 C10 119.9(5) 2 . ?
C8 C6 C5 122.2(6) . . ?
C8 C6 C7 118.4(5) . . ?
C7 C6 C5 119.3(5) . . ?
C16B O11 Tb1 147.0(7) . . ?
C16A O11 Tb1 153.1(15) . . ?
O3 C4 C2 122.7(5) . 2_566 ?
O3 C4 C3 117.5(5) . . ?
C3 C4 C2 119.7(5) . 2_566 ?
O5 C5 C6 117.4(5) . . ?
O4 C5 O5 126.0(5) . . ?
O4 C5 C6 116.6(5) . . ?
O7 C9 Tb1 57.5(3) . . ?
O7 C9 O8 121.2(5) . . ?
O7 C9 C10 119.0(5) . . ?
O8 C9 Tb1 63.8(3) . . ?
O8 C9 C10 119.8(5) . . ?
C10 C9 Tb1 175.2(4) . . ?
O6 C8 C6 123.1(5) . . ?
O6 C8 C7 117.8(5) . 2_656 ?
C7 C8 C6 119.1(6) 2_656 . ?
C12 C10 C9 121.0(5) . . ?
C11 C10 C12 119.7(5) . . ?
C11 C10 C9 119.3(5) . . ?
C12 C11 C10 120.4(6) 2 . ?
C12 C11 H11 119.8 2 . ?
C10 C11 H11 119.8 . . ?
O2 C1 C2 118.0(5) . . ?
O1 C1 O2 122.1(5) . . ?
O1 C1 C2 119.9(5) . . ?
C4 C2 C1 121.6(5) 2_566 . ?
C3 C2 C4 118.3(5) . 2_566 ?
C3 C2 C1 120.1(5) . . ?
C4 C3 C2 122.0(5) . . ?
C4 C3 H3A 119.0 . . ?
C2 C3 H3A 119.0 . . ?
C6 C7 H7 118.8 . . ?
C8 C7 C6 122.5(6) 2_656 . ?
C8 C7 H7 118.8 2_656 . ?
C13 N1 C14 122.2(7) . . ?
C13 N1 C15 121.6(7) . . ?
C15 N1 C14 116.2(7) . . ?
O10 C13 N1 125.7(7) . . ?
O10 C13 H13 117.1 . . ?
N1 C13 H13 117.1 . . ?
C1 O1 Tb1 174.6(4) . . ?
C16B N2 C18 109.6(9) . . ?
C16B N2 C17 135.8(9) . . ?
C18 N2 C16A 152.3(11) . . ?
C17 N2 C18 114.4(8) . . ?
C17 N2 C16A 92.7(9) . . ?
O11 C16B N2 126.2(10) . . ?
O11 C16B H16B 116.9 . . ?
N2 C16B H16B 116.9 . . ?
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 . . ?
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 . . ?
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 . . ?
C20B N3 C21B 111.2(16) . . ?
C19B N3 C20B 128(2) . . ?
C19B N3 C21B 120.6(18) . . ?
C20A N3 C21A 113.2(17) . . ?
C19A N3 C21A 120.3(18) . . ?
C19A N3 C20A 126(2) . . ?
N3 C20B H20A 109.5 . . ?
N3 C20B H20B 109.5 . . ?
N3 C20B H20C 109.5 . . ?
H20A C20B H20B 109.5 . . ?
H20A C20B H20C 109.5 . . ?
H20B C20B H20C 109.5 . . ?
N3 C19B H19B 119.4 . . ?
O12 C19B N3 121(3) . . ?
O12 C19B H19B 119.4 . . ?
N3 C21B H21A 109.5 . . ?
N3 C21B H21B 109.5 . . ?
N3 C21B H21C 109.5 . . ?
H21A C21B H21B 109.5 . . ?
H21A C21B H21C 109.5 . . ?
H21B C21B H21C 109.5 . . ?
N3 C21A H21D 109.5 . . ?
N3 C21A H21E 109.5 . . ?
N3 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
N3 C20A H20D 109.5 . . ?
N3 C20A H20E 109.5 . . ?
N3 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
N3 C19A H19A 117.8 . . ?
O12 C19A N3 124(3) . . ?
O12 C19A H19A 117.8 . . ?
O11 C16A N2 131(2) . . ?
O11 C16A H16A 114.5 . . ?
N2 C16A H16A 114.5 . . ?
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 O10 2.390(4) . ?
Tb1 O5 2.339(3) 2_666 ?
Tb1 O7 2.407(4) . ?
Tb1 O2 2.387(4) 2_666 ?
Tb1 O8 2.543(4) . ?
Tb1 O4 2.382(4) . ?
Tb1 O11 2.384(5) . ?
Tb1 C9 2.835(5) . ?
Tb1 O1 2.309(4) . ?
O10 C13 1.238(8) . ?
O5 C5 1.263(6) . ?
O7 C9 1.249(7) . ?
O3 H3 0.8200 . ?
O3 C4 1.371(7) . ?
O9 H9 0.8200 . ?
O9 C12 1.363(7) . ?
O2 C1 1.267(6) . ?
O8 C9 1.266(7) . ?
O6 H6 0.8200 . ?
O6 C8 1.363(7) . ?
O4 C5 1.257(6) . ?
C12 C10 1.406(8) . ?
C12 C11 1.384(7) 2 ?
C6 C5 1.505(8) . ?
C6 C8 1.392(8) . ?
C6 C7 1.387(8) . ?
O11 C16B 1.163(11) . ?
O11 C16A 0.915(16) . ?
C4 C2 1.396(8) 2_566 ?
C4 C3 1.379(7) . ?
C9 C10 1.500(7) . ?
C8 C7 1.381(8) 2_656 ?
C10 C11 1.390(8) . ?
C11 H11 0.9300 . ?
C1 C2 1.488(7) . ?
C1 O1 1.255(6) . ?
C2 C3 1.382(7) . ?
C3 H3A 0.9300 . ?
C7 H7 0.9300 . ?
N1 C13 1.299(8) . ?
N1 C14 1.452(10) . ?
N1 C15 1.427(11) . ?
C13 H13 0.9300 . ?
N2 C16B 1.321(12) . ?
N2 C18 1.435(10) . ?
N2 C17 1.426(10) . ?
N2 C16A 1.505(19) . ?
C16B H16B 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
N3 C20B 1.43(3) . ?
N3 C19B 1.34(3) . ?
N3 C21B 1.54(3) . ?
N3 C21A 1.49(3) . ?
N3 C20A 1.37(3) . ?
N3 C19A 1.34(3) . ?
O12 C19B 1.19(3) . ?
O12 C19A 1.15(3) . ?
C20B H20A 0.9600 . ?
C20B H20B 0.9600 . ?
C20B H20C 0.9600 . ?
C19B H19B 0.9300 . ?
C21B H21A 0.9600 . ?
C21B H21B 0.9600 . ?
C21B H21C 0.9600 . ?
C21A H21D 0.9600 . ?
C21A H21E 0.9600 . ?
C21A H21F 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C19A H19A 0.9300 . ?
C16A H16A 0.9300 . ?
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 O10 C13 N1 -145.6(6) . . . . ?
Tb1 O5 C5 O4 -45.2(8) 2_666 . . . ?
Tb1 O5 C5 C6 134.9(4) 2_666 . . . ?
Tb1 O7 C9 O8 -4.1(6) . . . . ?
Tb1 O7 C9 C10 176.2(4) . . . . ?
Tb1 O2 C1 C2 170.3(4) 2_666 . . . ?
Tb1 O2 C1 O1 -9.4(6) 2_666 . . . ?
Tb1 O8 C9 O7 3.9(6) . . . . ?
Tb1 O8 C9 C10 -176.4(5) . . . . ?
Tb1 O4 C5 O5 5.7(9) . . . . ?
Tb1 O4 C5 C6 -174.4(4) . . . . ?
Tb1 O11 C16B N2 -166.6(7) . . . . ?
Tb1 O11 C16A N2 165.3(12) . . . . ?
O7 C9 C10 C12 -175.6(6) . . . . ?
O7 C9 C10 C11 6.3(9) . . . . ?
O3 C4 C3 C2 -179.6(6) . . . . ?
O9 C12 C10 C9 1.1(9) . . . . ?
O9 C12 C10 C11 179.1(6) . . . . ?
O2 C1 C2 C4 4.2(8) . . . 2_566 ?
O2 C1 C2 C3 -175.8(5) . . . . ?
O8 C9 C10 C12 4.7(9) . . . . ?
O8 C9 C10 C11 -173.4(5) . . . . ?
C12 C10 C11 C12 1.5(10) . . . 2 ?
C4 C2 C3 C4 0.2(10) 2_566 . . . ?
C5 C6 C8 O6 -2.5(10) . . . . ?
C5 C6 C8 C7 177.2(5) . . . 2_656 ?
C5 C6 C7 C8 -177.3(6) . . . 2_656 ?
C9 C10 C11 C12 179.6(5) . . . 2 ?
C8 C6 C5 O5 -170.5(5) . . . . ?
C8 C6 C5 O4 9.6(8) . . . . ?
C8 C6 C7 C8 0.0(10) . . . 2_656 ?
C11 C12 C10 C9 -179.6(5) 2 . . . ?
C11 C12 C10 C11 -1.5(10) 2 . . . ?
C1 C2 C3 C4 -179.8(5) . . . . ?
C2 C4 C3 C2 -0.2(10) 2_566 . . . ?
C7 C6 C5 O5 6.7(8) . . . . ?
C7 C6 C5 O4 -173.2(5) . . . . ?
C7 C6 C8 O6 -179.7(6) . . . . ?
C7 C6 C8 C7 0.0(10) . . . 2_656 ?
O1 C1 C2 C4 -176.2(5) . . . 2_566 ?
O1 C1 C2 C3 3.8(8) . . . . ?
C14 N1 C13 O10 -179.8(8) . . . . ?
C15 N1 C13 O10 0.7(13) . . . . ?
C18 N2 C16B O11 -178.9(10) . . . . ?
C18 N2 C16A O11 17(4) . . . . ?
C17 N2 C16B O11 -4(2) . . . . ?
C17 N2 C16A O11 -175(3) . . . . ?
C20B N3 C19B O12 177.8(19) . . . . ?
C21B N3 C19B O12 -8(3) . . . . ?
C21A N3 C19A O12 -3(3) . . . . ?
C20A N3 C19A O12 -180(2) . . . . ?
