#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:08:13 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/32/7233253.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_7233253
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
_atom_sites_solution_primary     dual
_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                104.438(4)
_cell_angle_beta                 108.872(4)
_cell_angle_gamma                96.664(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5213(5)
_cell_length_b                   10.9954(5)
_cell_length_c                   12.6323(5)
_cell_measurement_reflns_used    5749
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      31.7660
_cell_measurement_theta_min      1.9570
_cell_volume                     1307.93(11)
_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      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.681
_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      0.0603422000
_diffrn_orient_matrix_UB_12      -0.0139778000
_diffrn_orient_matrix_UB_13      0.0367913000
_diffrn_orient_matrix_UB_21      -0.0287492000
_diffrn_orient_matrix_UB_22      -0.0672353000
_diffrn_orient_matrix_UB_23      -0.0270670000
_diffrn_orient_matrix_UB_31      0.0304491000
_diffrn_orient_matrix_UB_32      -0.0002229000
_diffrn_orient_matrix_UB_33      -0.0430178000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.747
_diffrn_reflns_Laue_measured_fraction_max 0.681
_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            8611
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         1.968
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80216
_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    1.707
_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         1.162
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0288
_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)+(0.0600P)²+0.4583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4215
_reflns_number_total             4413
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_200K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_database_code               7233253
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
_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   0.830
_shelx_estimated_absorpt_t_min   0.607
_reflns_odcompleteness_completeness 73.48
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. 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
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.851
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 0.09897(2) 0.54735(2) 0.68294(2) 0.02660(9) Uani 1 1 d . . . . .
O2 O -0.0265(3) 0.3354(2) 0.5875(2) 0.0332(6) Uani 1 1 d . . . . .
O3 O 0.1581(3) 0.4899(2) 0.5197(3) 0.0353(5) Uani 1 1 d . U . . .
O4 O -0.0764(3) 0.2747(2) 0.3930(2) 0.0363(6) Uani 1 1 d . . . . .
O5 O 0.0633(3) 0.4831(3) 0.8402(2) 0.0428(7) Uani 1 1 d . . . . .
O6 O 0.1277(3) 0.4271(3) 0.3315(2) 0.0377(6) Uani 1 1 d . . . . .
O7 O 0.1696(3) 0.7597(2) 0.8502(2) 0.0372(6) Uani 1 1 d . . . . .
O8 O 0.3241(3) 0.6843(3) 0.7844(3) 0.0455(7) Uani 1 1 d . . . . .
O9 O 0.0453(5) -0.0498(3) 0.7116(3) 0.0600(10) Uani 1 1 d . . . . .
H9 H 0.0466 -0.1277 0.7044 0.090 Uiso 1 1 calc GR . . . .
O11 O 0.2588(3) 0.4121(3) 0.7395(3) 0.0579(9) Uani 1 1 d . . . . .
O12 O 0.6663(3) 0.6027(4) 0.7355(3) 0.0559(9) Uani 1 1 d . . . . .
H12 H 0.7491 0.6028 0.7452 0.084 Uiso 1 1 calc GR . . . .
N1 N -0.0072(5) 0.3118(4) 0.8924(4) 0.0518(10) Uani 1 1 d . . . . .
O1A O 0.2355(3) 0.9968(3) 0.9969(3) 0.0472(11) Uani 0.884(10) 1 d . . P A 1
H1A H 0.1803 0.9293 0.9486 0.071 Uiso 0.884(10) 1 calc GR . P A 1
O1B O 0.593(3) 0.804(2) 0.882(3) 0.060(10) Uani 0.116(10) 1 d . U P A 2
H1B H 0.5316 0.7375 0.8396 0.091 Uiso 0.116(10) 1 calc R . P A 2
N2 N 0.4329(5) 0.3310(5) 0.8316(4) 0.0643(12) Uani 1 1 d . . . . .
C1 C -0.0236(4) 0.1209(3) 0.4934(3) 0.0322(8) Uani 1 1 d . . . . .
C2 C 0.2061(4) 0.4657(3) 0.4396(4) 0.0338(6) Uani 1 1 d . U . . .
C3 C 0.3580(4) 0.4828(3) 0.4683(3) 0.0332(9) Uani 1 1 d . . . . .
C4 C -0.0435(4) 0.2536(3) 0.4909(3) 0.0316(8) Uani 1 1 d . . . . .
C5 C 0.4452(4) 0.5350(4) 0.5868(3) 0.0375(9) Uani 1 1 d . . . . .
H5 H 0.4073 0.5591 0.6458 0.045 Uiso 1 1 calc R . . . .
C6 C 0.5870(4) 0.5515(4) 0.6181(3) 0.0366(9) Uani 1 1 d . . . . .
C7 C 0.2912(4) 0.7719(3) 0.8490(3) 0.0334(8) Uani 1 1 d . . . . .
C8 C -0.0006(4) 0.0907(3) 0.5970(4) 0.0394(9) Uani 1 1 d . . . . .
H8 H -0.0012 0.1533 0.6639 0.047 Uiso 1 1 calc R . . . .
C9 C 0.0234(5) -0.0291(3) 0.6059(3) 0.0380(9) Uani 1 1 d . . . . .
C10 C -0.0261(5) 0.3885(4) 0.8264(4) 0.0470(11) Uani 1 1 d . . . . .
H10 H -0.1127 0.3712 0.7645 0.056 Uiso 1 1 calc R . . . .
N3 N 0.4779(6) 0.1532(5) 0.4536(5) 0.0795(14) Uani 1 1 d . U . . .
C11 C 0.3981(4) 0.8909(3) 0.9276(3) 0.0336(8) Uani 1 1 d . . . . .
C12 C 0.3640(4) 0.9940(3) 0.9958(4) 0.0360(9) Uani 1 1 d . . . . .
H12A H 0.2722 0.9904 0.9927 0.043 Uiso 0.116(10) 1 calc R . P A 2
C13 C 0.3771(5) 0.4237(6) 0.7976(5) 0.0585(13) Uani 1 1 d . . . . .
H13 H 0.4358 0.5058 0.8214 0.070 Uiso 1 1 calc R . . . .
C14 C 0.5327(4) 0.8978(3) 0.9317(3) 0.0364(9) Uani 1 1 d . . . . .
H14 H 0.5545 0.8279 0.8844 0.044 Uiso 0.884(10) 1 calc R . P A 1
C15 C -0.1158(8) 0.2042(6) 0.8737(7) 0.0804(19) Uani 1 1 d . . . . .
H15A H -0.1365 0.2146 0.9452 0.121 Uiso 1 1 calc GR . . . .
H15B H -0.0850 0.1235 0.8547 0.121 Uiso 1 1 calc GR . . . .
H15C H -0.1986 0.2023 0.8085 0.121 Uiso 1 1 calc GR . . . .
O10 O 0.6112(8) 0.2268(8) 0.6457(6) 0.123(2) Uani 1 1 d . U . . .
C16 C 0.1191(8) 0.3307(7) 0.9899(6) 0.094(2) Uani 1 1 d . . . . .
H16A H 0.1688 0.4203 1.0159 0.141 Uiso 1 1 calc GR . . . .
H16B H 0.1761 0.2736 0.9653 0.141 Uiso 1 1 calc GR . . . .
H16C H 0.0982 0.3110 1.0547 0.141 Uiso 1 1 calc GR . . . .
C17 C 0.3604(9) 0.2010(8) 0.8007(8) 0.109(3) Uani 1 1 d . . . . .
H17A H 0.3494 0.1845 0.8704 0.163 Uiso 1 1 calc GR . . . .
H17B H 0.4125 0.1419 0.7708 0.163 Uiso 1 1 calc GR . . . .
H17C H 0.2696 0.1877 0.7400 0.163 Uiso 1 1 calc GR . . . .
C18 C 0.5802(8) 0.3626(9) 0.9018(8) 0.110(3) Uani 1 1 d . . . . .
H18A H 0.6257 0.3022 0.8641 0.164 Uiso 1 1 calc GR . . . .
H18B H 0.5939 0.3562 0.9806 0.164 Uiso 1 1 calc GR . . . .
H18C H 0.6197 0.4504 0.9078 0.164 Uiso 1 1 calc GR . . . .
C1A C 0.5994(17) 0.1931(14) 0.5409(14) 0.091(4) Uani 0.548(11) 1 d . U P B 1
H1AA H 0.6803 0.1960 0.5227 0.110 Uiso 0.548(11) 1 calc R . P B 1
C2A C 0.455(2) 0.1146(18) 0.3307(15) 0.112(6) Uani 0.548(11) 1 d . U P B 1
H2AA H 0.5389 0.1463 0.3192 0.168 Uiso 0.548(11) 1 calc GR . P B 1
H2AB H 0.3799 0.1505 0.2892 0.168 Uiso 0.548(11) 1 calc GR . P B 1
H2AC H 0.4301 0.0205 0.2995 0.168 Uiso 0.548(11) 1 calc GR . P B 1
C3A C 0.3473(16) 0.1420(17) 0.4781(16) 0.104(5) Uani 0.548(11) 1 d . U P B 1
H3AA H 0.3428 0.0763 0.5176 0.156 Uiso 0.548(11) 1 calc GR . P B 1
H3AB H 0.2682 0.1175 0.4039 0.156 Uiso 0.548(11) 1 calc GR . P B 1
H3AC H 0.3456 0.2249 0.5287 0.156 Uiso 0.548(11) 1 calc GR . P B 1
C1B C 0.500(2) 0.203(2) 0.5640(17) 0.105(5) Uani 0.452(11) 1 d . U P B 2
H1BA H 0.4231 0.2220 0.5837 0.126 Uiso 0.452(11) 1 calc R . P B 2
C2B C 0.600(2) 0.143(2) 0.423(2) 0.110(6) Uani 0.452(11) 1 d . U P B 2
H2BA H 0.6599 0.2281 0.4506 0.164 Uiso 0.452(11) 1 calc GR . P B 2
H2BB H 0.5718 0.1075 0.3381 0.164 Uiso 0.452(11) 1 calc GR . P B 2
H2BC H 0.6492 0.0856 0.4614 0.164 Uiso 0.452(11) 1 calc GR . P B 2
C3B C 0.346(2) 0.120(2) 0.3605(18) 0.103(6) Uani 0.452(11) 1 d . U P B 2
H3BA H 0.2789 0.1551 0.3911 0.155 Uiso 0.452(11) 1 calc GR . P B 2
H3BB H 0.3161 0.0260 0.3287 0.155 Uiso 0.452(11) 1 calc GR . P B 2
H3BC H 0.3523 0.1554 0.2982 0.155 Uiso 0.452(11) 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 126.50(9) . 2_566
O2 Tb1 O5 77.81(9) . .
O2 Tb1 O6 78.85(9) . 2_566
O2 Tb1 O7 151.65(10) . .
O2 Tb1 O8 145.64(9) . .
O2 Tb1 O11 74.25(11) . .
O3 Tb1 O2 77.33(9) . .
O3 Tb1 O4 76.06(9) . 2_566
O3 Tb1 O5 145.94(10) . .
O3 Tb1 O6 122.06(9) . 2_566
O3 Tb1 O7 131.00(9) . .
O3 Tb1 O8 87.50(10) . .
O3 Tb1 O11 78.97(12) . .
O4 Tb1 O5 137.95(10) 2_566 .
O4 Tb1 O6 77.43(10) 2_566 2_566
O4 Tb1 O7 69.16(9) 2_566 .
O4 Tb1 O8 77.64(10) 2_566 .
O4 Tb1 O11 141.70(12) 2_566 .
O5 Tb1 O7 76.55(9) . .
O5 Tb1 O8 100.38(11) . .
O5 Tb1 O11 72.10(12) . .
O6 Tb1 O5 74.83(10) 2_566 .
O6 Tb1 O7 82.94(9) 2_566 .
O6 Tb1 O8 134.41(10) 2_566 .
O6 Tb1 O11 140.86(11) 2_566 .
O8 Tb1 O7 52.57(10) . .
O8 Tb1 O11 72.67(11) . .
O11 Tb1 O7 108.68(11) . .
C4 O2 Tb1 133.6(2) . .
C2 O3 Tb1 172.5(2) . .
C4 O4 Tb1 138.8(2) . 2_566
C10 O5 Tb1 124.3(3) . .
C2 O6 Tb1 108.7(3) . 2_566
C7 O7 Tb1 89.0(2) . .
C7 O8 Tb1 97.2(2) . .
C9 O9 H9 109.5 . .
C13 O11 Tb1 138.7(4) . .
C6 O12 H12 109.5 . .
C10 N1 C15 121.7(5) . .
C10 N1 C16 122.6(5) . .
C16 N1 C15 115.7(5) . .
C12 O1A H1A 109.5 . .
C14 O1B H1B 109.5 . .
C13 N2 C17 124.7(5) . .
C13 N2 C18 117.7(6) . .
C17 N2 C18 117.6(5) . .
C8 C1 C4 119.1(3) . .
C8 C1 C9 119.5(3) . 2_556
C9 C1 C4 121.3(3) 2_556 .
O3 C2 O6 121.4(3) . .
O3 C2 C3 120.8(3) . .
O6 C2 C3 117.8(4) . .
C5 C3 C2 118.0(4) . .
C6 C3 C2 121.9(3) 2_666 .
C6 C3 C5 120.1(3) 2_666 .
O2 C4 C1 117.3(3) . .
O4 C4 O2 125.1(3) . .
O4 C4 C1 117.6(3) . .
C3 C5 H5 119.9 . .
C6 C5 C3 120.1(4) . .
C6 C5 H5 119.9 . .
O12 C6 C3 123.1(3) . 2_666
O12 C6 C5 117.2(4) . .
C3 C6 C5 119.7(3) 2_666 .
O7 C7 C11 119.9(4) . .
O8 C7 O7 121.0(3) . .
O8 C7 C11 119.1(4) . .
C1 C8 H8 119.1 . .
C1 C8 C9 121.8(4) . .
C9 C8 H8 119.1 . .
O9 C9 C1 123.7(3) . 2_556
O9 C9 C8 117.6(3) . .
C8 C9 C1 118.7(4) . 2_556
O5 C10 N1 124.0(4) . .
O5 C10 H10 118.0 . .
N1 C10 H10 118.0 . .
C1A N3 C2A 126.0(14) . .
C1A N3 C3A 120.8(11) . .
C2A N3 C3A 113.2(12) . .
C1B N3 C2B 116.2(15) . .
C1B N3 C3B 124.9(16) . .
C3B N3 C2B 118.7(14) . .
C12 C11 C7 121.0(4) . .
C14 C11 C7 118.9(3) . .
C14 C11 C12 120.1(3) . .
O1A C12 C11 124.5(3) . .
O1A C12 C14 116.7(4) . 2_677
C11 C12 H12A 120.6 . .
C14 C12 C11 118.8(4) 2_677 .
C14 C12 H12A 120.6 2_677 .
O11 C13 N2 125.2(6) . .
O11 C13 H13 117.4 . .
N2 C13 H13 117.4 . .
O1B C14 C12 108.6(11) . 2_677
C11 C14 O1B 130.0(11) . .
C11 C14 C12 121.0(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 118.8 . .
O10 C1A N3 122.3(15) . .
O10 C1A H1AA 118.8 . .
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 117.1 . .
O10 C1B N3 126(2) . .
O10 C1B H1BA 117.1 . .
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 2.342(2) .
Tb1 O3 2.304(3) .
Tb1 O4 2.388(2) 2_566
Tb1 O5 2.388(3) .
Tb1 O6 2.388(3) 2_566
Tb1 O7 2.567(3) .
Tb1 O8 2.401(3) .
Tb1 O11 2.426(3) .
O2 C4 1.266(5) .
O3 C2 1.256(5) .
O4 Tb1 2.388(2) 2_566
O4 C4 1.260(5) .
O5 C10 1.254(5) .
O6 Tb1 2.388(3) 2_566
O6 C2 1.275(5) .
O7 C7 1.277(5) .
O8 C7 1.257(5) .
O9 H9 0.8400 .
O9 C9 1.361(5) .
O11 C13 1.196(6) .
O12 H12 0.8400 .
O12 C6 1.373(5) .
N1 C10 1.314(6) .
N1 C15 1.460(7) .
N1 C16 1.441(7) .
O1A H1A 0.8400 .
O1A C12 1.361(5) .
O1B H1B 0.8400 .
O1B C14 1.39(3) .
N2 C13 1.327(6) .
N2 C17 1.434(9) .
N2 C18 1.463(8) .
C1 C4 1.505(4) .
C1 C8 1.383(6) .
C1 C9 1.401(6) 2_556
C2 C3 1.498(5) .
C3 C5 1.405(5) .
C3 C6 1.386(7) 2_666
C5 H5 0.9500 .
C5 C6 1.391(6) .
C6 C3 1.386(7) 2_666
C7 C11 1.500(4) .
C8 H8 0.9500 .
C8 C9 1.394(5) .
C9 C1 1.401(6) 2_556
C10 H10 0.9500 .
N3 C1A 1.327(15) .
N3 C2A 1.434(18) .
N3 C3A 1.500(17) .
N3 C1B 1.29(2) .
N3 C2B 1.46(2) .
N3 C3B 1.434(18) .
C11 C12 1.401(6) .
C11 C14 1.393(6) .
C12 H12A 0.9500 .
C12 C14 1.395(5) 2_677
C13 H13 0.9500 .
C14 C12 1.395(5) 2_677
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
O10 C1A 1.243(17) .
O10 C1B 1.23(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 -49.6(5) . .
Tb1 O2 C4 C1 130.7(3) . .
Tb1 O4 C4 O2 10.0(7) 2_566 .
Tb1 O4 C4 C1 -170.3(3) 2_566 .
Tb1 O5 C10 N1 142.5(4) . .
Tb1 O6 C2 O3 11.1(4) 2_566 .
Tb1 O6 C2 C3 -168.2(2) 2_566 .
Tb1 O7 C7 O8 -5.4(4) . .
Tb1 O7 C7 C11 176.1(3) . .
Tb1 O8 C7 O7 5.8(4) . .
Tb1 O8 C7 C11 -175.7(3) . .
Tb1 O11 C13 N2 166.5(4) . .
O3 C2 C3 C5 -4.3(5) . .
O3 C2 C3 C6 175.5(4) . 2_666
O6 C2 C3 C5 175.0(3) . .
O6 C2 C3 C6 -5.1(5) . 2_666
O7 C7 C11 C12 -5.3(5) . .
O7 C7 C11 C14 175.0(3) . .
O8 C7 C11 C12 176.2(4) . .
O8 C7 C11 C14 -3.6(5) . .
C1 C8 C9 O9 179.8(4) . .
C1 C8 C9 C1 -0.2(7) . 2_556
C2 C3 C5 C6 179.3(4) . .
C3 C5 C6 O12 -179.9(4) . .
C3 C5 C6 C3 0.6(7) . 2_666
C4 C1 C8 C9 -177.7(4) . .
C6 C3 C5 C6 -0.6(7) 2_666 .
C7 C11 C12 O1A -0.4(6) . .
C7 C11 C12 C14 179.5(3) . 2_677
C7 C11 C14 O1B -8(2) . .
C7 C11 C14 C12 -179.4(4) . 2_677
C8 C1 C4 O2 5.9(5) . .
C8 C1 C4 O4 -173.8(4) . .
C9 C1 C4 O2 -172.0(4) 2_556 .
C9 C1 C4 O4 8.3(6) 2_556 .
C9 C1 C8 C9 0.2(7) 2_556 .
C12 C11 C14 O1B 173(2) . .
C12 C11 C14 C12 0.8(7) . 2_677
C14 C11 C12 O1A 179.4(4) . .
C14 C11 C12 C14 -0.8(6) . 2_677
C15 N1 C10 O5 178.9(5) . .
C16 N1 C10 O5 1.2(9) . .
C17 N2 C13 O11 1.9(10) . .
C18 N2 C13 O11 179.5(7) . .
C2A N3 C1A O10 179.0(13) . .
C3A N3 C1A O10 -2.5(18) . .
C2B N3 C1B O10 -9(3) . .
C3B N3 C1B O10 176.6(16) . .
