#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:08:13 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/32/7233243.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_7233243
loop_
_publ_author_name
'Gładysiak, Andrzej'
'Moosavi, Seyed Mohamad'
'Sarkisov, Lev'
'Smit, Berend'
'Stylianou, Kyriakos C.'
_publ_section_title
;
 Guest-dependent negative thermal expansion in a lanthanide-based
 metal--organic framework
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5292
_journal_paper_doi               10.1039/C9CE00941H
_journal_volume                  21
_journal_year                    2019
_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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-03 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                104.759(4)
_cell_angle_beta                 107.340(5)
_cell_angle_gamma                97.380(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5096(6)
_cell_length_b                   10.9768(4)
_cell_length_c                   12.5019(6)
_cell_measurement_reflns_used    5009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4880
_cell_measurement_theta_min      2.0730
_cell_volume                     1298.23(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.714
_diffrn_measured_fraction_theta_max 0.652
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0597171000
_diffrn_orient_matrix_UB_12      -0.0137259000
_diffrn_orient_matrix_UB_13      0.0360613000
_diffrn_orient_matrix_UB_21      -0.0286008000
_diffrn_orient_matrix_UB_22      -0.0676179000
_diffrn_orient_matrix_UB_23      -0.0272211000
_diffrn_orient_matrix_UB_31      0.0307492000
_diffrn_orient_matrix_UB_32      0.0000326000
_diffrn_orient_matrix_UB_33      -0.0438156000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.714
_diffrn_reflns_Laue_measured_fraction_max 0.652
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8177
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.652
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.431
_diffrn_reflns_theta_min         1.977
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0330
_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)+(0.0705P)²+0.6708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3950
_reflns_number_total             4196
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_100K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_database_code               7233243
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb1'
_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   0.829
_shelx_estimated_absorpt_t_min   0.605
_reflns_odcompleteness_completeness 70.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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
 O1B-C11 \\sim C11-O1A
 with sigma of 0.02
 O1A-C12 \\sim O1B-C14
 with sigma of 0.02
3. Restrained planarity
 O1B, C14, C11, C12, O8, C7, O7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C2, O6, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1B)=Sof(H1BA)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(1)
 Sof(O1B)=Sof(H1B)=Sof(H12A)=1-FVAR(2)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
7.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
7.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,
 H3BB,H3BC)
7.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.872
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 0.09419(2) 0.54650(2) 0.68266(2) 0.02445(11) Uani 1 1 d . . . . .
O2 O -0.0365(3) 0.3346(3) 0.5869(3) 0.0267(7) Uani 1 1 d . . . . .
O3 O 0.1537(3) 0.4851(3) 0.5157(3) 0.0284(6) Uani 1 1 d . U . . .
O4 O -0.0827(3) 0.2727(3) 0.3919(3) 0.0295(7) Uani 1 1 d . . . . .
O5 O 0.0558(3) 0.4848(3) 0.8415(3) 0.0342(8) Uani 1 1 d . . . . .
O6 O 0.1304(3) 0.4227(3) 0.3275(3) 0.0308(7) Uani 1 1 d . U . . .
O7 O 0.1641(3) 0.7641(3) 0.8509(3) 0.0331(8) Uani 1 1 d . . . . .
O8 O 0.3193(3) 0.6806(3) 0.7868(3) 0.0342(8) Uani 1 1 d . . . . .
O9 O 0.0440(5) -0.0487(3) 0.7139(3) 0.0426(9) Uani 1 1 d . . . . .
H9 H 0.0660 -0.1201 0.7112 0.064 Uiso 1 1 calc GR . . . .
O11 O 0.2480(4) 0.4047(3) 0.7332(3) 0.0395(8) Uani 1 1 d . . . . .
O12 O 0.6584(4) 0.6069(4) 0.7373(3) 0.0445(9) Uani 1 1 d . . . . .
H12 H 0.7408 0.6046 0.7484 0.067 Uiso 1 1 calc GR . . . .
N1 N -0.0147(5) 0.3079(4) 0.8913(4) 0.0363(10) Uani 1 1 d . . . . .
O1A O 0.2339(4) 1.0071(4) 0.9930(4) 0.0361(13) Uani 0.866(11) 1 d D . P A 1
H1A H 0.1790 0.9373 0.9490 0.054 Uiso 0.866(11) 1 calc GR . P A 1
O1B O 0.587(2) 0.801(2) 0.8790(19) 0.061(12) Uani 0.134(11) 1 d D . P A 2
H1B H 0.5246 0.7349 0.8367 0.092 Uiso 0.134(11) 1 calc R . P A 2
N2 N 0.4273(5) 0.3326(4) 0.8312(4) 0.0413(11) Uani 1 1 d . . . . .
C1 C -0.0269(5) 0.1202(4) 0.4929(4) 0.0287(10) Uani 1 1 d . . . . .
C2 C 0.2055(5) 0.4625(4) 0.4370(4) 0.0286(8) Uani 1 1 d . U . . .
C3 C 0.3571(5) 0.4810(4) 0.4664(4) 0.0303(11) Uani 1 1 d . U . . .
C4 C -0.0502(4) 0.2526(4) 0.4906(4) 0.0270(10) Uani 1 1 d . . . . .
C5 C 0.4407(5) 0.5352(4) 0.5864(4) 0.0325(11) Uani 1 1 d . . . . .
H5 H 0.4005 0.5598 0.6450 0.039 Uiso 1 1 calc R . . . .
C6 C 0.5830(5) 0.5527(5) 0.6186(4) 0.0318(11) Uani 1 1 d . . . . .
C7 C 0.2867(4) 0.7725(4) 0.8503(4) 0.0269(10) Uani 1 1 d . . . . .
C8 C -0.0036(5) 0.0908(4) 0.5973(4) 0.0310(10) Uani 1 1 d . . . . .
H8 H -0.0054 0.1535 0.6647 0.037 Uiso 1 1 calc R . . . .
C9 C 0.0226(5) -0.0286(4) 0.6064(4) 0.0299(10) Uani 1 1 d . . . . .
C10 C -0.0338(5) 0.3876(4) 0.8281(4) 0.0360(12) Uani 1 1 d . . . . .
H10 H -0.1204 0.3712 0.7685 0.043 Uiso 1 1 calc R . . . .
N3 N 0.4762(5) 0.1527(5) 0.4539(5) 0.0476(11) Uani 1 1 d . U . . .
C11 C 0.3965(4) 0.8913(4) 0.9286(4) 0.0281(10) Uani 1 1 d D . . . .
C12 C 0.3636(5) 0.9989(4) 0.9949(4) 0.0309(11) Uani 1 1 d D . . . .
H12A H 0.2720 0.9984 0.9913 0.037 Uiso 0.134(11) 1 calc R . P A 2
C13 C 0.3683(5) 0.4226(5) 0.7952(5) 0.0367(11) Uani 1 1 d . . . . .
H13 H 0.4236 0.5071 0.8192 0.044 Uiso 1 1 calc R . . . .
C14 C 0.5312(5) 0.8932(4) 0.9338(4) 0.0291(10) Uani 1 1 d D . . . .
H14 H 0.5519 0.8200 0.8882 0.035 Uiso 0.866(11) 1 calc R . P A 1
C15 C -0.1244(7) 0.1968(5) 0.8707(6) 0.0490(14) Uani 1 1 d . . . . .
H15A H -0.1569 0.2116 0.9377 0.074 Uiso 1 1 calc GR . . . .
H15B H -0.0887 0.1180 0.8621 0.074 Uiso 1 1 calc GR . . . .
H15C H -0.2003 0.1871 0.7987 0.074 Uiso 1 1 calc GR . . . .
O10 O 0.6019(6) 0.2220(6) 0.6495(5) 0.0791(16) Uani 1 1 d . U . . .
C16 C 0.1117(7) 0.3265(6) 0.9886(6) 0.0570(17) Uani 1 1 d . . . . .
H16A H 0.1756 0.4046 0.9972 0.086 Uiso 1 1 calc GR . . . .
H16B H 0.1527 0.2516 0.9724 0.086 Uiso 1 1 calc GR . . . .
H16C H 0.0917 0.3357 1.0616 0.086 Uiso 1 1 calc GR . . . .
C17 C 0.3507(7) 0.1997(5) 0.7974(6) 0.0519(15) Uani 1 1 d . . . . .
H17A H 0.3282 0.1849 0.8644 0.078 Uiso 1 1 calc GR . . . .
H17B H 0.4064 0.1398 0.7742 0.078 Uiso 1 1 calc GR . . . .
H17C H 0.2662 0.1852 0.7310 0.078 Uiso 1 1 calc GR . . . .
C18 C 0.5728(7) 0.3637(7) 0.9027(6) 0.0596(18) Uani 1 1 d . . . . .
H18A H 0.6200 0.3068 0.8624 0.089 Uiso 1 1 calc GR . . . .
H18B H 0.5829 0.3514 0.9795 0.089 Uiso 1 1 calc GR . . . .
H18C H 0.6126 0.4539 0.9142 0.089 Uiso 1 1 calc GR . . . .
C1A C 0.5934(11) 0.1920(10) 0.5447(10) 0.054(2) Uani 0.625(10) 1 d . U P B 1
H1AA H 0.6761 0.1974 0.5280 0.065 Uiso 0.625(10) 1 calc R . P B 1
C2A C 0.4708(14) 0.1144(12) 0.3318(11) 0.064(3) Uani 0.625(10) 1 d . U P B 1
H2AA H 0.5622 0.1402 0.3290 0.096 Uiso 0.625(10) 1 calc GR . P B 1
H2AB H 0.4077 0.1567 0.2869 0.096 Uiso 0.625(10) 1 calc GR . P B 1
H2AC H 0.4387 0.0204 0.2974 0.096 Uiso 0.625(10) 1 calc GR . P B 1
C3A C 0.3440(12) 0.1370(12) 0.4722(12) 0.063(3) Uani 0.625(10) 1 d . U P B 1
H3AA H 0.3013 0.0449 0.4469 0.094 Uiso 0.625(10) 1 calc GR . P B 1
H3AB H 0.2841 0.1806 0.4259 0.094 Uiso 0.625(10) 1 calc GR . P B 1
H3AC H 0.3584 0.1751 0.5559 0.094 Uiso 0.625(10) 1 calc GR . P B 1
C1B C 0.490(2) 0.201(2) 0.5675(17) 0.063(4) Uani 0.375(10) 1 d . U P B 2
H1BA H 0.4119 0.2198 0.5867 0.076 Uiso 0.375(10) 1 calc R . P B 2
C2B C 0.600(2) 0.145(2) 0.4241(19) 0.063(5) Uani 0.375(10) 1 d . U P B 2
H2BA H 0.6807 0.1822 0.4959 0.094 Uiso 0.375(10) 1 calc GR . P B 2
H2BB H 0.6034 0.1926 0.3683 0.094 Uiso 0.375(10) 1 calc GR . P B 2
H2BC H 0.5993 0.0540 0.3883 0.094 Uiso 0.375(10) 1 calc GR . P B 2
C3B C 0.344(2) 0.122(2) 0.357(2) 0.073(6) Uani 0.375(10) 1 d . U P B 2
H3BA H 0.2709 0.1325 0.3899 0.109 Uiso 0.375(10) 1 calc GR . P B 2
H3BB H 0.3263 0.0327 0.3068 0.109 Uiso 0.375(10) 1 calc GR . P B 2
H3BC H 0.3472 0.1808 0.3100 0.109 Uiso 0.375(10) 1 calc GR . P B 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
O2 Tb1 O4 127.00(10) . 2_566
O2 Tb1 O5 78.11(11) . .
O2 Tb1 O6 78.76(11) . 2_566
O2 Tb1 O7 151.29(12) . .
O2 Tb1 O8 146.03(11) . .
O2 Tb1 O11 73.94(11) . .
O3 Tb1 O2 77.23(11) . .
O3 Tb1 O4 75.88(11) . 2_566
O3 Tb1 O5 145.85(11) . .
O3 Tb1 O6 122.15(11) . 2_566
O3 Tb1 O7 131.34(11) . .
O3 Tb1 O8 89.07(12) . .
O3 Tb1 O11 78.05(13) . .
O4 Tb1 O7 68.10(11) 2_566 .
O4 Tb1 O11 140.54(13) 2_566 .
O5 Tb1 O4 138.26(12) . 2_566
O5 Tb1 O6 75.02(12) . 2_566
O5 Tb1 O7 76.67(11) . .
O5 Tb1 O8 98.55(12) . .
O5 Tb1 O11 72.65(13) . .
O6 Tb1 O4 78.32(11) 2_566 2_566
O6 Tb1 O7 81.66(11) 2_566 .
O6 Tb1 O11 141.10(12) 2_566 .
O8 Tb1 O4 77.59(11) . 2_566
O8 Tb1 O6 133.62(11) . 2_566
O8 Tb1 O7 52.62(11) . .
O8 Tb1 O11 72.86(11) . .
O11 Tb1 O7 110.80(11) . .
C4 O2 Tb1 132.5(3) . .
C2 O3 Tb1 170.3(3) . .
C4 O4 Tb1 138.1(3) . 2_566
C10 O5 Tb1 123.9(3) . .
C2 O6 Tb1 107.0(3) . 2_566
C7 O7 Tb1 88.2(3) . .
C7 O8 Tb1 97.7(3) . .
C9 O9 H9 109.5 . .
C13 O11 Tb1 134.4(3) . .
C6 O12 H12 109.5 . .
C10 N1 C15 121.2(5) . .
C10 N1 C16 122.7(5) . .
C16 N1 C15 116.0(5) . .
C12 O1A H1A 109.5 . .
C14 O1B H1B 109.5 . .
C13 N2 C17 121.3(5) . .
C13 N2 C18 120.5(5) . .
C17 N2 C18 118.1(5) . .
C8 C1 C4 119.0(4) . .
C8 C1 C9 119.2(4) . 2_556
C9 C1 C4 121.8(4) 2_556 .
O3 C2 O6 121.1(4) . .
O3 C2 C3 121.4(4) . .
O6 C2 C3 117.6(5) . .
C5 C3 C2 117.8(5) . .
C6 C3 C2 122.6(4) 2_666 .
C6 C3 C5 119.6(4) 2_666 .
O2 C4 O4 124.8(4) . .
O2 C4 C1 117.8(4) . .
O4 C4 C1 117.3(4) . .
C3 C5 H5 120.0 . .
C6 C5 C3 119.9(5) . .
C6 C5 H5 120.0 . .
O12 C6 C3 122.7(4) . 2_666
O12 C6 C5 116.8(5) . .
C3 C6 C5 120.5(4) 2_666 .
O7 C7 C11 120.3(4) . .
O8 C7 O7 121.1(4) . .
O8 C7 C11 118.6(4) . .
C1 C8 H8 119.0 . .
C1 C8 C9 121.9(4) . .
C9 C8 H8 119.0 . .
O9 C9 C1 123.6(4) . 2_556
O9 C9 C8 117.5(4) . .
C8 C9 C1 118.9(4) . 2_556
O5 C10 N1 124.4(5) . .
O5 C10 H10 117.8 . .
N1 C10 H10 117.8 . .
C1A N3 C2A 122.6(8) . .
C1A N3 C3A 121.1(8) . .
C2A N3 C3A 116.2(8) . .
C1B N3 C2B 118.4(13) . .
C1B N3 C3B 122.7(15) . .
C2B N3 C3B 118.5(14) . .
C12 C11 C7 120.6(4) . .
C14 C11 C7 119.1(4) . .
C14 C11 C12 120.3(4) . .
O1A C12 C11 124.5(4) . .
O1A C12 C14 117.0(4) . 2_677
C11 C12 H12A 120.7 . .
C14 C12 C11 118.6(4) 2_677 .
C14 C12 H12A 120.7 2_677 .
O11 C13 N2 125.0(5) . .
O11 C13 H13 117.5 . .
N2 C13 H13 117.5 . .
O1B C14 C11 130.5(12) . .
O1B C14 C12 108.4(12) . 2_677
C11 C14 C12 121.1(4) . 2_677
C11 C14 H14 119.5 . .
C12 C14 H14 119.5 2_677 .
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 . .
N1 C16 H16A 109.5 . .
N1 C16 H16B 109.5 . .
N1 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 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 . .
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 . .
N3 C1A H1AA 117.8 . .
O10 C1A N3 124.4(10) . .
O10 C1A H1AA 117.8 . .
N3 C2A H2AA 109.5 . .
N3 C2A H2AB 109.5 . .
N3 C2A H2AC 109.5 . .
H2AA C2A H2AB 109.5 . .
H2AA C2A H2AC 109.5 . .
H2AB C2A H2AC 109.5 . .
N3 C3A H3AA 109.5 . .
N3 C3A H3AB 109.5 . .
N3 C3A H3AC 109.5 . .
H3AA C3A H3AB 109.5 . .
H3AA C3A H3AC 109.5 . .
H3AB C3A H3AC 109.5 . .
N3 C1B H1BA 119.0 . .
O10 C1B N3 122.0(18) . .
O10 C1B H1BA 119.0 . .
N3 C2B H2BA 109.5 . .
N3 C2B H2BB 109.5 . .
N3 C2B H2BC 109.5 . .
H2BA C2B H2BB 109.5 . .
H2BA C2B H2BC 109.5 . .
H2BB C2B H2BC 109.5 . .
N3 C3B H3BA 109.5 . .
N3 C3B H3BB 109.5 . .
N3 C3B H3BC 109.5 . .
H3BA C3B H3BB 109.5 . .
H3BA C3B H3BC 109.5 . .
H3BB C3B H3BC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2 2.348(3) .
Tb1 O3 2.318(4) .
Tb1 O4 2.400(3) 2_566
Tb1 O5 2.378(4) .
Tb1 O6 2.398(3) 2_566
Tb1 O7 2.596(3) .
Tb1 O8 2.398(3) .
Tb1 O11 2.444(3) .
O2 C4 1.261(6) .
O3 C2 1.248(7) .
O4 Tb1 2.400(3) 2_566
O4 C4 1.263(6) .
O5 C10 1.269(6) .
O6 Tb1 2.398(3) 2_566
O6 C2 1.284(6) .
O7 C7 1.283(6) .
O8 C7 1.267(6) .
O9 H9 0.8400 .
O9 C9 1.375(6) .
O11 C13 1.230(6) .
O12 H12 0.8400 .
O12 C6 1.382(6) .
N1 C10 1.316(6) .
N1 C15 1.478(7) .
N1 C16 1.458(7) .
O1A H1A 0.8400 .
O1A C12 1.372(7) .
O1B H1B 0.8400 .
O1B C14 1.367(15) .
N2 C13 1.335(6) .
N2 C17 1.461(7) .
N2 C18 1.466(7) .
C1 C4 1.510(5) .
C1 C8 1.382(7) .
C1 C9 1.401(7) 2_556
C2 C3 1.498(7) .
C3 C5 1.415(6) .
C3 C6 1.387(8) 2_666
C5 H5 0.9500 .
C5 C6 1.401(7) .
C6 C3 1.387(8) 2_666
C7 C11 1.510(5) .
C8 H8 0.9500 .
C8 C9 1.399(6) .
C9 C1 1.401(7) 2_556
C10 H10 0.9500 .
N3 C1A 1.331(11) .
N3 C2A 1.457(13) .
N3 C3A 1.470(13) .
N3 C1B 1.34(2) .
N3 C2B 1.46(2) .
N3 C3B 1.48(2) .
C11 C12 1.407(6) .
C11 C14 1.394(7) .
C12 H12A 0.9500 .
C12 C14 1.399(6) 2_677
C13 H13 0.9500 .
C14 C12 1.399(6) 2_677
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
O10 C1A 1.240(13) .
O10 C1B 1.26(2) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C1A H1AA 0.9500 .
C2A H2AA 0.9800 .
C2A H2AB 0.9800 .
C2A H2AC 0.9800 .
C3A H3AA 0.9800 .
C3A H3AB 0.9800 .
C3A H3AC 0.9800 .
C1B H1BA 0.9500 .
C2B H2BA 0.9800 .
C2B H2BB 0.9800 .
C2B H2BC 0.9800 .
C3B H3BA 0.9800 .
C3B H3BB 0.9800 .
C3B H3BC 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_4
Tb1 O2 C4 O4 -53.6(6) . .
Tb1 O2 C4 C1 126.6(4) . .
Tb1 O4 C4 O2 15.2(8) 2_566 .
Tb1 O4 C4 C1 -165.1(3) 2_566 .
Tb1 O5 C10 N1 139.1(4) . .
Tb1 O6 C2 O3 12.8(5) 2_566 .
Tb1 O6 C2 C3 -166.9(3) 2_566 .
Tb1 O7 C7 O8 -6.0(4) . .
Tb1 O7 C7 C11 175.8(4) . .
Tb1 O8 C7 O7 6.6(5) . .
Tb1 O8 C7 C11 -175.2(3) . .
Tb1 O11 C13 N2 165.5(4) . .
O3 C2 C3 C5 -5.1(6) . .
O3 C2 C3 C6 174.9(4) . 2_666
O6 C2 C3 C5 174.6(4) . .
O6 C2 C3 C6 -5.3(6) . 2_666
O7 C7 C11 C12 -5.9(7) . .
O7 C7 C11 C14 174.5(4) . .
O8 C7 C11 C12 175.9(4) . .
O8 C7 C11 C14 -3.7(6) . .
C1 C8 C9 O9 -179.8(5) . .
C1 C8 C9 C1 0.8(8) . 2_556
C2 C3 C5 C6 179.0(4) . .
C3 C5 C6 O12 179.6(4) . .
C3 C5 C6 C3 1.0(8) . 2_666
C4 C1 C8 C9 -178.2(4) . .
C6 C3 C5 C6 -1.0(8) 2_666 .
C7 C11 C12 O1A -1.4(7) . .
C7 C11 C12 C14 180.0(4) . 2_677
C7 C11 C14 O1B -1.1(12) . .
C7 C11 C14 C12 -180.0(4) . 2_677
C8 C1 C4 O2 5.6(6) . .
C8 C1 C4 O4 -174.1(4) . .
C9 C1 C4 O2 -171.7(4) 2_556 .
C9 C1 C4 O4 8.5(7) 2_556 .
C9 C1 C8 C9 -0.8(8) 2_556 .
C12 C11 C14 O1B 179.3(12) . .
C12 C11 C14 C12 0.4(8) . 2_677
C14 C11 C12 O1A 178.3(5) . .
C14 C11 C12 C14 -0.4(7) . 2_677
C15 N1 C10 O5 179.8(5) . .
C16 N1 C10 O5 2.9(9) . .
C17 N2 C13 O11 0.7(9) . .
C18 N2 C13 O11 178.5(6) . .
C2A N3 C1A O10 -177.9(10) . .
C3A N3 C1A O10 -2.4(15) . .
C2B N3 C1B O10 -10(2) . .
C3B N3 C1B O10 177.2(15) . .
