#------------------------------------------------------------------------------
#$Date: 2022-09-08 02:06:00 +0300 (Thu, 08 Sep 2022) $
#$Revision: 277724 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/12/7711203.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_7711203
loop_
_publ_author_name
'Ren, Tai-Lin'
'Zhang, Xiao-Nuan'
'Hu, Jun-Jie'
'Wen, He-Rui'
'Liu, Sui-Jun'
'Peng, Yan'
_publ_section_title
;
 Stable Terbium Metal-organic Framework with Turn-on and Blue-shift
 Fluorescence Sensing for Acidic Amino Acids (L-aspartate, L-glutamine)
 and Cations (Al3+, Ga3+)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02632E
_journal_year                    2022
_chemical_formula_moiety
'0.25(C244 H144 O80 Tb8), 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C67 H54 N2 O24 Tb2'
_chemical_formula_weight         1588.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-17 deposited with the CCDC.	2022-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.2490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0733(7)
_cell_length_b                   28.8085(14)
_cell_length_c                   16.2113(5)
_cell_measurement_reflns_used    6513
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.01
_cell_volume                     7840.0(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      297.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.1588
_diffrn_reflns_av_unetI/netI     0.1261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59245
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.828
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0751 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.8628.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       rod
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8966
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0559
_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)+(0.0675P)²+43.6645P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4879
_reflns_number_total             8966
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02632e2.cif
_cod_data_source_block           1_a_sq_s
_cod_database_code               7711203
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H20(0.5) O13(0.5) H13(0.5)
4.a Riding coordinates:
 O15(H15A,H15B), O13(H13)
4.b Rotating group:
 O9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7A), C35(H35), C8(H8), C15(H15), C20(H20), C22(H22), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
4.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
4.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.42078(2) 0.35610(2) 0.59018(3) 0.03228(13) Uani 1 1 d . . . . .
C1 C -0.0686(5) 0.4714(3) 0.4512(7) 0.049(2) Uani 1 1 d . . . . .
O1 O 0.500000 0.3947(3) 0.750000 0.051(2) Uani 1 2 d S T P A .
O2 O 0.5305(3) 0.3089(2) 0.6450(4) 0.0471(16) Uani 1 1 d . . . . .
O7 O 0.0826(4) 0.5656(2) 0.2061(5) 0.0528(16) Uani 1 1 d . . . . .
H7 H 0.077043 0.575960 0.155598 0.079 Uiso 1 1 calc GR . . . .
O8 O 0.3393(4) 0.4168(3) 0.4744(6) 0.077(2) Uani 1 1 d . . . . .
O9 O 0.5099(5) 0.3987(3) 0.5654(6) 0.086(2) Uani 1 1 d . . . . .
H9A H 0.558378 0.393052 0.613703 0.128 Uiso 1 1 d GR . . . .
H9B H 0.504147 0.427784 0.570110 0.128 Uiso 1 1 d GR . . . .
C2 C 0.3000(6) 0.4238(4) 0.5131(7) 0.054(3) Uani 1 1 d . . . . .
O3 O 0.2048(5) 0.5485(3) 0.2445(6) 0.078(2) Uani 1 1 d . . . . .
C3 C 0.1184(5) 0.4938(3) 0.4492(7) 0.044(2) Uani 1 1 d . . . . .
C16 C 0.5897(5) 0.2994(3) 0.7289(6) 0.039(2) Uani 1 1 d . . . . .
O4 O 0.9285(6) 0.3677(3) 0.9048(7) 0.102(3) Uani 1 1 d . . . . .
C4 C 0.6565(5) 0.2724(3) 0.7361(5) 0.0339(18) Uani 1 1 d . . . . .
C5 C 0.7805(5) 0.2235(3) 0.7489(5) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.822632 0.207276 0.753748 0.046 Uiso 1 1 calc R . . . .
O5 O 0.5975(3) 0.3101(2) 0.8085(4) 0.0474(16) Uani 1 1 d . . . . .
C6 C 0.7713(5) 0.2231(3) 0.8273(6) 0.0372(19) Uani 1 1 d . . . . .
O6 O 0.8878(4) 0.1771(2) 0.9311(4) 0.0532(17) Uani 1 1 d . . . . .
C7 C 0.6657(5) 0.2711(3) 0.6570(6) 0.040(2) Uani 1 1 d . . . . .
H7A H 0.629113 0.286338 0.598766 0.048 Uiso 1 1 calc R . . . .
C35 C 0.1818(6) 0.4640(3) 0.4960(7) 0.052(2) Uani 1 1 d . . . . .
H35 H 0.190029 0.446819 0.549319 0.063 Uiso 1 1 calc R . . . .
C8 C 0.7091(5) 0.2483(3) 0.8209(6) 0.0366(19) Uani 1 1 d . . . . .
H8 H 0.703190 0.248737 0.873926 0.044 Uiso 1 1 calc R . . . .
C9 C 0.2348(5) 0.4588(3) 0.4656(7) 0.048(2) Uani 1 1 d . . . . .
O10 O 0.8122(4) 0.1934(2) 0.9847(4) 0.0581(19) Uani 1 1 d . . . . .
C10 C 0.7396(5) 0.2484(3) 0.5786(6) 0.036(2) Uani 1 1 d . . . . .
C11 C 0.7928(5) 0.2801(3) 0.5811(6) 0.040(2) Uani 1 1 d . . . . .
O12 O 0.3143(4) 0.4010(2) 0.5869(5) 0.0532(17) Uani 1 1 d . . . . .
C12 C 0.8022(5) 0.2825(3) 0.4983(6) 0.039(2) Uani 1 1 d . . . . .
C13 C 0.1598(5) 0.5155(3) 0.3404(6) 0.044(2) Uani 1 1 d . . . . .
C14 C 0.1515(6) 0.5448(3) 0.2586(7) 0.048(2) Uani 1 1 d . . . . .
C15 C 0.2227(6) 0.4851(3) 0.3869(7) 0.050(2) Uani 1 1 d . . . . .
H15 H 0.257241 0.482240 0.365792 0.060 Uiso 1 1 calc R . . . .
O15 O 0.6608(9) 0.4084(5) 0.7272(10) 0.188(6) Uani 1 1 d . U . . .
H15A H 0.655283 0.416490 0.773151 0.282 Uiso 1 1 d R . . . .
H15B H 0.709343 0.408900 0.744122 0.282 Uiso 1 1 d R . . . .
C17 C 0.0582(5) 0.4966(3) 0.4772(6) 0.044(2) Uani 1 1 d . . . . .
C20 C 0.500000 0.4377(6) 0.750000 0.076(5) Uani 1 2 d S T P . .
H20 H 0.473053 0.454379 0.691329 0.091 Uiso 0.5 1 calc R . . A .
C19 C -0.0086(6) 0.4688(3) 0.4292(7) 0.048(2) Uani 1 1 d . . . . .
N1 N 0.9049(5) 0.3258(3) 1.0036(7) 0.063(2) Uani 1 1 d . . . . .
C22 C 0.1065(5) 0.5200(3) 0.3692(7) 0.046(2) Uani 1 1 d . . . . .
H22 H 0.063478 0.540196 0.335899 0.056 Uiso 1 1 calc R . . . .
C21 C 0.7283(5) 0.2474(3) 0.6637(5) 0.037(2) Uani 1 1 d . . . . .
C24 C 0.8981(7) 0.3444(4) 0.5791(9) 0.077(4) Uani 1 1 d . . . . .
H24 H 0.933489 0.365365 0.579463 0.092 Uiso 1 1 calc R . . . .
C23 C 0.8266(5) 0.1963(3) 0.9192(6) 0.041(2) Uani 1 1 d . . . . .
C25 C -0.1464(8) 0.4125(4) 0.3304(9) 0.080(4) Uani 1 1 d . . . . .
H25 H -0.191682 0.393922 0.297693 0.096 Uiso 1 1 calc R . . . .
C26 C -0.0226(7) 0.4362(4) 0.3550(8) 0.067(3) Uani 1 1 d . . . . .
H26 H 0.014982 0.433589 0.338661 0.080 Uiso 1 1 calc R . . . .
C27 C 0.8551(6) 0.3157(4) 0.5003(7) 0.058(3) Uani 1 1 d . . . . .
H27 H 0.860610 0.317851 0.447028 0.069 Uiso 1 1 calc R . . . .
C28 C -0.1361(6) 0.4429(4) 0.4001(8) 0.064(3) Uani 1 1 d . . . . .
H28 H -0.174900 0.444993 0.414546 0.077 Uiso 1 1 calc R . . . .
C29 C 0.8385(6) 0.3121(4) 0.6599(7) 0.056(3) Uani 1 1 d . . . . .
H29 H 0.832830 0.311926 0.713144 0.068 Uiso 1 1 calc R . . . .
C30 C 0.8900(7) 0.3430(4) 0.6601(9) 0.078(4) Uani 1 1 d . . . . .
H30 H 0.919621 0.363036 0.713231 0.094 Uiso 1 1 calc R . . . .
C31 C 0.8868(8) 0.3573(4) 0.9341(9) 0.080(3) Uani 1 1 d . . . . .
H31 H 0.838190 0.372520 0.906051 0.096 Uiso 1 1 calc R . . . .
C32 C -0.0878(8) 0.4090(4) 0.3077(9) 0.075(3) Uani 1 1 d . . . . .
H32 H -0.094412 0.388091 0.260123 0.090 Uiso 1 1 calc R . . . .
C33 C 0.8552(9) 0.3165(5) 1.0379(11) 0.118(6) Uani 1 1 d . . . . .
H33A H 0.882872 0.324021 1.106794 0.177 Uiso 1 1 calc GR . . . .
H33B H 0.841089 0.284243 1.028602 0.177 Uiso 1 1 calc GR . . . .
H33C H 0.807776 0.335024 1.001758 0.177 Uiso 1 1 calc GR . . . .
O13 O 0.5377(14) 0.4579(7) 0.8321(16) 0.144(9) Uani 0.5 1 d . . . A -1
H13 H 0.587208 0.449544 0.863444 0.215 Uiso 0.5 1 d R . . A -1
C34 C 0.9787(8) 0.3004(5) 1.0477(12) 0.119(6) Uani 1 1 d . . . . .
H34A H 0.972486 0.275286 1.005190 0.179 Uiso 1 1 calc GR . . . .
H34B H 0.992495 0.288293 1.110360 0.179 Uiso 1 1 calc GR . . . .
H34C H 1.020103 0.320795 1.057005 0.179 Uiso 1 1 calc GR . . . .
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'
Tb Tb -0.1723 4.1537 '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'
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 O6 158.09(14) . 8_455 ?
O1 Tb1 O12 80.62(18) . . ?
O1 Tb1 C23 173.1(2) . 8_455 ?
O2 Tb1 O1 86.03(19) . . ?
O2 Tb1 O8 144.8(2) . . ?
O2 Tb1 O9 73.9(3) . . ?
O2 Tb1 O6 80.0(2) . 8_455 ?
O2 Tb1 O10 103.3(2) . 8_455 ?
O2 Tb1 O12 161.03(19) . . ?
O2 Tb1 C23 92.7(2) . 8_455 ?
O8 Tb1 O1 105.3(3) . . ?
O8 Tb1 O6 77.9(2) . 8_455 ?
O8 Tb1 O12 53.0(2) . . ?
O8 Tb1 C23 79.6(3) . 8_455 ?
O9 Tb1 O1 80.3(2) . . ?
O9 Tb1 O8 75.4(3) . . ?
O9 Tb1 O6 79.6(2) . 8_455 ?
O9 Tb1 O12 116.6(3) . . ?
O9 Tb1 C23 105.9(3) . 8_455 ?
O5 Tb1 O1 76.7(2) 2_656 . ?
O5 Tb1 O2 83.0(2) 2_656 . ?
O5 Tb1 O8 131.8(2) 2_656 . ?
O5 Tb1 O9 148.3(3) 2_656 . ?
O5 Tb1 O6 117.8(2) 2_656 8_455 ?
O5 Tb1 O10 74.0(2) 2_656 8_455 ?
O5 Tb1 O12 80.9(2) 2_656 . ?
O5 Tb1 C23 96.4(2) 2_656 8_455 ?
O6 Tb1 C23 26.89(19) 8_455 8_455 ?
O10 Tb1 O1 147.75(16) 8_455 . ?
O10 Tb1 O8 84.9(3) 8_455 . ?
O10 Tb1 O9 131.9(2) 8_455 . ?
O10 Tb1 O6 53.23(18) 8_455 8_455 ?
O10 Tb1 O12 81.8(2) 8_455 . ?
O10 Tb1 C23 26.4(2) 8_455 8_455 ?
O12 Tb1 O6 116.5(2) . 8_455 ?
O12 Tb1 C23 98.9(2) . 8_455 ?
C17 C1 C19 118.4(9) 5_566 . ?
C28 C1 C17 122.0(9) . 5_566 ?
C28 C1 C19 119.6(10) . . ?
Tb1 O1 Tb1 125.8(4) . 2_656 ?
C20 O1 Tb1 117.07(19) . . ?
C20 O1 Tb1 117.08(19) . 2_656 ?
C16 O2 Tb1 133.2(5) . . ?
C14 O7 H7 109.5 . . ?
C2 O8 Tb1 94.0(6) . . ?
Tb1 O9 H9A 109.0 . . ?
Tb1 O9 H9B 109.9 . . ?
H9A O9 H9B 104.1 . . ?
O8 C2 C9 117.5(8) . . ?
O12 C2 O8 120.7(8) . . ?
O12 C2 C9 121.8(8) . . ?
C35 C3 C17 121.4(8) . . ?
C35 C3 C22 119.0(8) . . ?
C22 C3 C17 119.5(8) . . ?
O2 C16 C4 118.4(7) . . ?
O5 C16 O2 125.0(8) . . ?
O5 C16 C4 116.6(7) . . ?
C7 C4 C16 120.5(7) . . ?
C8 C4 C16 120.2(7) . . ?
C8 C4 C7 119.2(7) . . ?
C6 C5 H5 119.5 . . ?
C21 C5 H5 119.5 . . ?
C21 C5 C6 120.9(7) . . ?
C16 O5 Tb1 154.8(6) . 2_656 ?
C5 C6 C8 119.5(7) . . ?
C5 C6 C23 121.3(7) . . ?
C8 C6 C23 119.2(7) . . ?
C23 O6 Tb1 90.6(5) . 8_556 ?
C4 C7 H7A 119.5 . . ?
C21 C7 C4 121.1(7) . . ?
C21 C7 H7A 119.5 . . ?
C3 C35 H35 119.1 . . ?
C3 C35 C9 121.8(8) . . ?
C9 C35 H35 119.1 . . ?
C4 C8 C6 120.1(7) . . ?
C4 C8 H8 120.0 . . ?
C6 C8 H8 120.0 . . ?
C35 C9 C2 120.8(8) . . ?
C15 C9 C2 120.5(8) . . ?
C15 C9 C35 118.7(8) . . ?
C23 O10 Tb1 96.0(5) . 8_556 ?
C11 C10 C21 118.8(7) . . ?
C12 C10 C11 121.8(7) 7_656 . ?
C12 C10 C21 119.4(8) 7_656 . ?
C10 C11 C12 119.3(7) . . ?
C10 C11 C29 123.9(7) . . ?
C29 C11 C12 116.8(8) . . ?
C2 O12 Tb1 92.2(5) . . ?
C10 C12 C11 118.8(8) 7_656 . ?
C10 C12 C27 122.1(7) 7_656 . ?
C27 C12 C11 119.1(8) . . ?
C15 C13 C14 117.8(8) . . ?
C15 C13 C22 121.4(8) . . ?
C22 C13 C14 120.7(8) . . ?
O7 C14 C13 113.5(8) . . ?
O3 C14 O7 124.3(9) . . ?
O3 C14 C13 122.2(9) . . ?
C9 C15 H15 120.1 . . ?
C13 C15 C9 119.9(8) . . ?
C13 C15 H15 120.1 . . ?
H15A O15 H15B 113.0 . . ?
C1 C17 C3 120.2(9) 5_566 . ?
C19 C17 C1 120.3(8) . 5_566 ?
C19 C17 C3 119.5(8) . . ?
O1 C20 H20 121.175(2) . 2_656 ?
O1 C20 H20 121.2 . . ?
O1 C20 O13 117.6(13) . . ?
H20 C20 H20 117.6 . 2_656 ?
O13 C20 H20 3.5(13) . 2_656 ?
O13 C20 H20 121.2 . . ?
C17 C19 C1 121.3(9) . . ?
C17 C19 C26 122.5(9) . . ?
C26 C19 C1 116.1(10) . . ?
C31 N1 C33 122.6(12) . . ?
C31 N1 C34 119.7(10) . . ?
C33 N1 C34 117.7(11) . . ?
C3 C22 H22 120.4 . . ?
C13 C22 C3 119.2(8) . . ?
C13 C22 H22 120.4 . . ?
C5 C21 C7 119.1(7) . . ?
C5 C21 C10 120.7(7) . . ?
C7 C21 C10 120.2(7) . . ?
C27 C24 H24 119.3 . . ?
C27 C24 C30 121.4(10) . . ?
C30 C24 H24 119.3 . . ?
C6 C23 Tb1 176.1(6) . 8_556 ?
O6 C23 Tb1 62.5(4) . 8_556 ?
O6 C23 C6 120.5(7) . . ?
O10 C23 Tb1 57.7(4) . 8_556 ?
O10 C23 C6 119.4(7) . . ?
O10 C23 O6 120.1(8) . . ?
C28 C25 H25 120.2 . . ?
C28 C25 C32 119.6(11) . . ?
C32 C25 H25 120.2 . . ?
C19 C26 H26 118.6 . . ?
C32 C26 C19 122.9(10) . . ?
C32 C26 H26 118.6 . . ?
C12 C27 H27 119.6 . . ?
C24 C27 C12 120.8(9) . . ?
C24 C27 H27 119.6 . . ?
C1 C28 H28 119.1 . . ?
C25 C28 C1 121.9(10) . . ?
C25 C28 H28 119.1 . . ?
C11 C29 H29 118.7 . . ?
C30 C29 C11 122.6(8) . . ?
C30 C29 H29 118.7 . . ?
C24 C30 H30 120.3 . . ?
C29 C30 C24 119.4(10) . . ?
C29 C30 H30 120.3 . . ?
O4 C31 N1 125.2(12) . . ?
O4 C31 H31 117.4 . . ?
N1 C31 H31 117.4 . . ?
C25 C32 H32 120.1 . . ?
C26 C32 C25 119.9(11) . . ?
C26 C32 H32 120.1 . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C20 O13 H20 10(4) . 2_656 ?
C20 O13 H13 108.8 . . ?
H13 O13 H20 113.6 . 2_656 ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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 2.441(4) . ?
Tb1 O2 2.311(5) . ?
Tb1 O8 2.427(6) . ?
Tb1 O9 2.379(7) . ?
Tb1 O5 2.291(5) 2_656 ?
Tb1 O6 2.476(6) 8_455 ?
Tb1 O10 2.371(6) 8_455 ?
Tb1 O12 2.473(6) . ?
Tb1 C23 2.791(8) 8_455 ?
C1 C17 1.406(13) 5_566 ?
C1 C19 1.432(12) . ?
C1 C28 1.401(13) . ?
O1 C20 1.239(17) . ?
O2 C16 1.252(9) . ?
O7 H7 0.8200 . ?
O7 C14 1.306(11) . ?
O8 C2 1.266(10) . ?
O9 H9A 0.8671 . ?
O9 H9B 0.8538 . ?
C2 C9 1.488(12) . ?
C2 O12 1.253(10) . ?
O3 C14 1.214(11) . ?
C3 C35 1.369(11) . ?
C3 C17 1.508(11) . ?
C3 C22 1.403(11) . ?
C16 C4 1.497(11) . ?
C16 O5 1.251(9) . ?
O4 C31 1.204(14) . ?
C4 C7 1.393(10) . ?
C4 C8 1.377(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.381(10) . ?
C5 C21 1.377(10) . ?
C6 C8 1.398(11) . ?
C6 C23 1.496(11) . ?
O6 C23 1.262(9) . ?
C7 H7A 0.9300 . ?
C7 C21 1.380(10) . ?
C35 H35 0.9300 . ?
C35 C9 1.403(11) . ?
C8 H8 0.9300 . ?
C9 C15 1.387(12) . ?
O10 C23 1.246(9) . ?
C10 C11 1.389(11) . ?
C10 C12 1.379(11) 7_656 ?
C10 C21 1.517(10) . ?
C11 C12 1.456(10) . ?
C11 C29 1.428(12) . ?
C12 C27 1.417(12) . ?
C13 C14 1.503(12) . ?
C13 C15 1.372(12) . ?
C13 C22 1.388(11) . ?
C15 H15 0.9300 . ?
O15 H15A 0.8430 . ?
O15 H15B 0.8560 . ?
C17 C19 1.379(13) . ?
C20 H20 0.9299 2_656 ?
C20 H20 0.9300 . ?
C20 O13 1.257(18) . ?
C19 C26 1.428(13) . ?
N1 C31 1.332(14) . ?
N1 C33 1.410(13) . ?
N1 C34 1.441(14) . ?
C22 H22 0.9300 . ?
C24 H24 0.9300 . ?
C24 C27 1.361(14) . ?
C24 C30 1.409(14) . ?
C25 H25 0.9300 . ?
C25 C28 1.354(14) . ?
C25 C32 1.415(15) . ?
C26 H26 0.9300 . ?
C26 C32 1.347(15) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C29 C30 1.364(13) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
O13 H13 0.8659 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
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 C20 O13 -3.1(12) 2_656 . . . ?
Tb1 O1 C20 O13 176.9(12) . . . . ?
Tb1 O2 C16 C4 -170.9(5) . . . . ?
Tb1 O2 C16 O5 10.0(14) . . . . ?
Tb1 O8 C2 C9 -177.4(8) . . . . ?
Tb1 O8 C2 O12 0.5(11) . . . . ?
Tb1 O6 C23 C6 -177.3(8) 8_556 . . . ?
Tb1 O6 C23 O10 3.6(9) 8_556 . . . ?
Tb1 O10 C23 C6 177.1(7) 8_556 . . . ?
Tb1 O10 C23 O6 -3.7(10) 8_556 . . . ?
C1 C17 C19 C1 -0.6(14) 5_566 . . . ?
C1 C17 C19 C26 179.0(8) 5_566 . . . ?
C1 C19 C26 C32 -0.2(15) . . . . ?
O2 C16 C4 C7 20.6(13) . . . . ?
O2 C16 C4 C8 -158.8(8) . . . . ?
O2 C16 O5 Tb1 -32(2) . . . 2_656 ?
O8 C2 C9 C35 171.4(10) . . . . ?
O8 C2 C9 C15 -5.3(15) . . . . ?
O8 C2 O12 Tb1 -0.5(11) . . . . ?
C2 C9 C15 C13 176.5(9) . . . . ?
C3 C35 C9 C2 -175.8(9) . . . . ?
C3 C35 C9 C15 1.0(15) . . . . ?
C3 C17 C19 C1 -177.9(8) . . . . ?
C3 C17 C19 C26 1.8(13) . . . . ?
C16 C4 C7 C21 178.2(8) . . . . ?
C16 C4 C8 C6 179.9(8) . . . . ?
C4 C16 O5 Tb1 149.0(10) . . . 2_656 ?
C4 C7 C21 C5 2.4(14) . . . . ?
C4 C7 C21 C10 -176.9(8) . . . . ?
C5 C6 C8 C4 1.4(13) . . . . ?
C5 C6 C23 O6 7.2(14) . . . . ?
C5 C6 C23 O10 -173.6(9) . . . . ?
O5 C16 C4 C7 -160.2(8) . . . . ?
O5 C16 C4 C8 20.5(12) . . . . ?
C6 C5 C21 C7 -0.4(14) . . . . ?
C6 C5 C21 C10 178.9(8) . . . . ?
C7 C4 C8 C6 0.5(13) . . . . ?
C35 C3 C17 C1 91.6(11) . . . 5_566 ?
C35 C3 C17 C19 -91.1(11) . . . . ?
C35 C3 C22 C13 -0.8(14) . . . . ?
C35 C9 C15 C13 -0.2(15) . . . . ?
C8 C4 C7 C21 -2.5(13) . . . . ?
C8 C6 C23 O6 -172.8(8) . . . . ?
C8 C6 C23 O10 6.4(13) . . . . ?
C9 C2 O12 Tb1 177.3(9) . . . . ?
C10 C11 C12 C10 -3.0(13) . . . 7_656 ?
C10 C11 C12 C27 178.5(8) . . . . ?
C10 C11 C29 C30 -179.6(10) . . . . ?
C10 C12 C27 C24 -177.2(10) 7_656 . . . ?
C11 C10 C21 C5 -82.6(11) . . . . ?
C11 C10 C21 C7 96.7(10) . . . . ?
C11 C12 C27 C24 1.3(15) . . . . ?
C11 C29 C30 C24 1.2(18) . . . . ?
O12 C2 C9 C35 -6.4(16) . . . . ?
O12 C2 C9 C15 176.9(10) . . . . ?
C12 C10 C11 C12 3.1(14) 7_656 . . . ?
C12 C10 C11 C29 -178.8(9) 7_656 . . . ?
C12 C10 C21 C5 96.4(10) 7_656 . . . ?
C12 C10 C21 C7 -84.3(11) 7_656 . . . ?
C12 C11 C29 C30 -1.5(15) . . . . ?
C14 C13 C15 C9 177.3(9) . . . . ?
C14 C13 C22 C3 -176.7(9) . . . . ?
C15 C13 C14 O7 167.2(9) . . . . ?
C15 C13 C14 O3 -13.3(15) . . . . ?
C15 C13 C22 C3 1.5(15) . . . . ?
C17 C1 C19 C17 0.6(14) 5_566 . . . ?
C17 C1 C19 C26 -179.1(8) 5_566 . . . ?
C17 C1 C28 C25 179.2(10) 5_566 . . . ?
C17 C3 C35 C9 175.2(9) . . . . ?
C17 C3 C22 C13 -176.5(9) . . . . ?
C17 C19 C26 C32 -179.8(10) . . . . ?
C19 C1 C28 C25 0.5(15) . . . . ?
C19 C26 C32 C25 0.5(18) . . . . ?
C22 C3 C35 C9 -0.5(15) . . . . ?
C22 C3 C17 C1 -92.7(11) . . . 5_566 ?
C22 C3 C17 C19 84.6(11) . . . . ?
C22 C13 C14 O7 -14.4(13) . . . . ?
C22 C13 C14 O3 165.0(10) . . . . ?
C22 C13 C15 C9 -1.0(15) . . . . ?
C21 C5 C6 C8 -1.5(13) . . . . ?
C21 C5 C6 C23 178.6(8) . . . . ?
C21 C10 C11 C12 -177.9(7) . . . . ?
C21 C10 C11 C29 0.2(13) . . . . ?
C23 C6 C8 C4 -178.6(8) . . . . ?
C27 C24 C30 C29 0.4(19) . . . . ?
C28 C1 C19 C17 179.3(9) . . . . ?
C28 C1 C19 C26 -0.3(13) . . . . ?
C28 C25 C32 C26 -0.3(19) . . . . ?
C29 C11 C12 C10 178.7(8) . . . 7_656 ?
C29 C11 C12 C27 0.2(12) . . . . ?
C30 C24 C27 C12 -1.6(18) . . . . ?
C32 C25 C28 C1 -0.1(18) . . . . ?
C33 N1 C31 O4 177.2(13) . . . . ?
C34 N1 C31 O4 -2(2) . . . . ?
