#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:08:13 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/32/7233247.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_7233247
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                104.175(4)
_cell_angle_beta                 109.639(4)
_cell_angle_gamma                96.452(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5121(6)
_cell_length_b                   10.9835(5)
_cell_length_c                   12.6782(5)
_cell_measurement_reflns_used    5799
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      31.8610
_cell_measurement_theta_min      2.1000
_cell_volume                     1305.96(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      240.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.743
_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      0.0607900000
_diffrn_orient_matrix_UB_12      -0.0140685000
_diffrn_orient_matrix_UB_13      0.0372153000
_diffrn_orient_matrix_UB_21      -0.0289161000
_diffrn_orient_matrix_UB_22      -0.0671874000
_diffrn_orient_matrix_UB_23      -0.0270054000
_diffrn_orient_matrix_UB_31      0.0303309000
_diffrn_orient_matrix_UB_32      -0.0002330000
_diffrn_orient_matrix_UB_33      -0.0426888000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.743
_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            8597
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.428
_diffrn_reflns_theta_min         1.967
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78641
_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    1.710
_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         1.431
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4401
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0267
_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)+(0.0552P)²+0.5328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4188
_reflns_number_total             4401
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_240K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_database_code               7233247
_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 73.37
_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 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.866
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 0.10126(2) 0.54756(2) 0.68277(2) 0.02683(8) Uani 1 1 d . . . . .
O2 O -0.0216(3) 0.3356(2) 0.5872(2) 0.0359(6) Uani 1 1 d . . . . .
O3 O 0.1601(3) 0.4922(2) 0.5212(3) 0.0379(5) Uani 1 1 d . U . . .
O4 O -0.0740(3) 0.2756(2) 0.3938(2) 0.0374(6) Uani 1 1 d . . . . .
O5 O 0.0667(3) 0.4816(3) 0.8386(2) 0.0463(7) Uani 1 1 d . . . . .
O6 O 0.1263(3) 0.4288(3) 0.3334(2) 0.0396(6) Uani 1 1 d . . . . .
O7 O 0.1720(3) 0.7572(2) 0.8493(2) 0.0389(6) Uani 1 1 d . . . . .
O8 O 0.3259(3) 0.6865(3) 0.7828(3) 0.0509(8) Uani 1 1 d . . . . .
O9 O 0.0453(5) -0.0506(3) 0.7106(3) 0.0669(11) Uani 1 1 d . . . . .
H9 H 0.0559 -0.1252 0.7057 0.100 Uiso 1 1 calc GR . . . .
O11 O 0.2648(4) 0.4168(4) 0.7425(4) 0.0673(10) Uani 1 1 d . . . . .
O12 O 0.6698(3) 0.6007(4) 0.7340(3) 0.0601(10) Uani 1 1 d . . . . .
H12 H 0.7524 0.6144 0.7423 0.090 Uiso 1 1 calc GR . . . .
N1 N -0.0031(5) 0.3129(4) 0.8932(4) 0.0584(11) Uani 1 1 d . . . . .
O1A O 0.2356(3) 0.9916(4) 0.9973(4) 0.0512(12) Uani 0.884(9) 1 d . . P A 1
H1A H 0.1842 0.9203 0.9572 0.077 Uiso 0.884(9) 1 calc GR . P A 1
O1B O 0.595(2) 0.808(2) 0.879(3) 0.061(9) Uani 0.116(9) 1 d . U P A 2
H1B H 0.5349 0.7420 0.8370 0.091 Uiso 0.116(9) 1 calc R . P A 2
N2 N 0.4336(5) 0.3283(5) 0.8297(5) 0.0753(14) Uani 1 1 d . . . . .
C1 C -0.0223(4) 0.1213(3) 0.4935(3) 0.0337(8) Uani 1 1 d . . . . .
C2 C 0.2063(4) 0.4676(3) 0.4403(4) 0.0359(6) Uani 1 1 d . U . . .
C3 C 0.3579(4) 0.4839(3) 0.4690(3) 0.0343(9) Uani 1 1 d . . . . .
C4 C -0.0405(4) 0.2544(3) 0.4921(3) 0.0318(8) Uani 1 1 d . . . . .
C5 C 0.4465(4) 0.5343(4) 0.5868(3) 0.0377(9) Uani 1 1 d . . . . .
H5 H 0.4100 0.5570 0.6454 0.045 Uiso 1 1 calc R . . . .
C6 C 0.5892(4) 0.5508(4) 0.6175(3) 0.0389(9) Uani 1 1 d . . . . .
C7 C 0.2933(4) 0.7718(3) 0.8485(3) 0.0349(8) Uani 1 1 d . . . . .
C8 C 0.0006(5) 0.0902(3) 0.5967(3) 0.0423(9) Uani 1 1 d . . . . .
H8 H 0.0011 0.1520 0.6629 0.051 Uiso 1 1 calc R . . . .
C9 C 0.0231(5) -0.0298(3) 0.6054(3) 0.0405(9) Uani 1 1 d . . . . .
C10 C -0.0226(5) 0.3882(4) 0.8256(4) 0.0509(11) Uani 1 1 d . . . . .
H10 H -0.1089 0.3707 0.7638 0.061 Uiso 1 1 calc R . . . .
N3 N 0.4782(7) 0.1531(6) 0.4527(6) 0.0939(17) Uani 1 1 d . U . . .
C11 C 0.3989(4) 0.8910(3) 0.9268(3) 0.0347(8) Uani 1 1 d . . . . .
C12 C 0.3643(4) 0.9912(4) 0.9959(4) 0.0390(9) Uani 1 1 d . . . . .
H12A H 0.2732 0.9858 0.9930 0.047 Uiso 0.116(9) 1 calc R . P A 2
C13 C 0.3807(6) 0.4238(7) 0.7983(5) 0.0752(17) Uani 1 1 d . . . . .
H13 H 0.4414 0.5039 0.8231 0.090 Uiso 1 1 calc R . . . .
C14 C 0.5329(4) 0.9001(4) 0.9306(3) 0.0388(9) Uani 1 1 d . . . . .
H14 H 0.5549 0.8323 0.8831 0.047 Uiso 0.884(9) 1 calc R . P A 1
C15 C -0.1128(9) 0.2065(7) 0.8742(8) 0.099(2) Uani 1 1 d . . . . .
H15A H -0.1390 0.2214 0.9420 0.148 Uiso 1 1 calc GR . . . .
H15B H -0.0802 0.1270 0.8631 0.148 Uiso 1 1 calc GR . . . .
H15C H -0.1924 0.2005 0.8049 0.148 Uiso 1 1 calc GR . . . .
O10 O 0.6137(9) 0.2266(9) 0.6444(7) 0.149(3) Uani 1 1 d . U . . .
C16 C 0.1215(10) 0.3323(9) 0.9903(7) 0.120(3) Uani 1 1 d . . . . .
H16A H 0.1614 0.4236 1.0253 0.180 Uiso 1 1 calc GR . . . .
H16B H 0.1860 0.2892 0.9641 0.180 Uiso 1 1 calc GR . . . .
H16C H 0.1026 0.2975 1.0481 0.180 Uiso 1 1 calc GR . . . .
C17 C 0.3695(11) 0.1977(10) 0.7994(9) 0.147(5) Uani 1 1 d . . . . .
H17A H 0.3749 0.1757 0.8701 0.220 Uiso 1 1 calc GR . . . .
H17B H 0.4163 0.1441 0.7588 0.220 Uiso 1 1 calc GR . . . .
H17C H 0.2733 0.1837 0.7484 0.220 Uiso 1 1 calc GR . . . .
C18 C 0.5853(10) 0.3643(10) 0.9008(9) 0.125(3) Uani 1 1 d . . . . .
H18A H 0.6307 0.3024 0.8670 0.188 Uiso 1 1 calc GR . . . .
H18B H 0.6014 0.3648 0.9809 0.188 Uiso 1 1 calc GR . . . .
H18C H 0.6225 0.4492 0.9007 0.188 Uiso 1 1 calc GR . . . .
C1A C 0.602(2) 0.1939(17) 0.5438(18) 0.113(5) Uani 0.527(12) 1 d . U P B 1
H1AA H 0.6830 0.1966 0.5272 0.136 Uiso 0.527(12) 1 calc R . P B 1
C2A C 0.454(3) 0.114(2) 0.3311(19) 0.138(7) Uani 0.527(12) 1 d . U P B 1
H2AA H 0.5354 0.1482 0.3193 0.207 Uiso 0.527(12) 1 calc GR . P B 1
H2AB H 0.3761 0.1462 0.2891 0.207 Uiso 0.527(12) 1 calc GR . P B 1
H2AC H 0.4331 0.0209 0.3017 0.207 Uiso 0.527(12) 1 calc GR . P B 1
C3A C 0.351(2) 0.143(2) 0.480(2) 0.130(6) Uani 0.527(12) 1 d . U P B 1
H3AA H 0.3250 0.0577 0.4848 0.195 Uiso 0.527(12) 1 calc GR . P B 1
H3AB H 0.2761 0.1589 0.4183 0.195 Uiso 0.527(12) 1 calc GR . P B 1
H3AC H 0.3681 0.2063 0.5544 0.195 Uiso 0.527(12) 1 calc GR . P B 1
C1B C 0.504(3) 0.203(2) 0.5631(19) 0.118(6) Uani 0.473(12) 1 d . U P B 2
H1BA H 0.4282 0.2239 0.5825 0.142 Uiso 0.473(12) 1 calc R . P B 2
C2B C 0.601(3) 0.140(2) 0.420(2) 0.127(7) Uani 0.473(12) 1 d . U P B 2
H2BA H 0.6322 0.2183 0.4042 0.191 Uiso 0.473(12) 1 calc GR . P B 2
H2BB H 0.5752 0.0677 0.3497 0.191 Uiso 0.473(12) 1 calc GR . P B 2
H2BC H 0.6745 0.1270 0.4836 0.191 Uiso 0.473(12) 1 calc GR . P B 2
C3B C 0.345(2) 0.115(2) 0.356(2) 0.124(7) Uani 0.473(12) 1 d . U P B 2
H3BA H 0.2767 0.1502 0.3833 0.187 Uiso 0.473(12) 1 calc GR . P B 2
H3BB H 0.3172 0.0223 0.3273 0.187 Uiso 0.473(12) 1 calc GR . P B 2
H3BC H 0.3514 0.1481 0.2933 0.187 Uiso 0.473(12) 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 126.27(9) . 2_566
O2 Tb1 O5 77.70(10) . .
O2 Tb1 O6 79.19(10) . 2_566
O2 Tb1 O7 151.85(10) . .
O2 Tb1 O8 145.56(10) . .
O2 Tb1 O11 74.73(12) . .
O3 Tb1 O2 77.22(10) . .
O3 Tb1 O4 76.13(9) . 2_566
O3 Tb1 O5 145.92(10) . .
O3 Tb1 O6 122.08(9) . 2_566
O3 Tb1 O7 130.92(9) . .
O3 Tb1 O8 86.81(10) . .
O3 Tb1 O11 79.37(12) . .
O4 Tb1 O5 137.87(10) 2_566 .
O4 Tb1 O6 76.95(10) 2_566 2_566
O4 Tb1 O7 69.64(9) 2_566 .
O4 Tb1 O8 77.41(10) 2_566 .
O4 Tb1 O11 141.84(12) 2_566 .
O5 Tb1 O7 76.55(9) . .
O5 Tb1 O8 101.41(11) . .
O5 Tb1 O11 72.01(13) . .
O6 Tb1 O5 74.75(11) 2_566 .
O6 Tb1 O7 83.24(9) 2_566 .
O6 Tb1 O8 134.41(10) 2_566 .
O6 Tb1 O11 141.21(12) 2_566 .
O8 Tb1 O7 52.55(10) . .
O8 Tb1 O11 72.42(12) . .
O11 Tb1 O7 107.50(12) . .
C4 O2 Tb1 134.8(2) . .
C2 O3 Tb1 173.5(2) . .
C4 O4 Tb1 138.8(2) . 2_566
C10 O5 Tb1 125.1(3) . .
C2 O6 Tb1 109.5(3) . 2_566
C7 O7 Tb1 89.5(2) . .
C7 O8 Tb1 97.1(2) . .
C9 O9 H9 109.5 . .
C13 O11 Tb1 142.0(4) . .
C6 O12 H12 109.5 . .
C10 N1 C15 121.0(5) . .
C10 N1 C16 122.7(5) . .
C16 N1 C15 116.2(5) . .
C12 O1A H1A 109.5 . .
C14 O1B H1B 109.5 . .
C13 N2 C17 129.4(7) . .
C13 N2 C18 114.1(6) . .
C17 N2 C18 116.4(7) . .
C8 C1 C4 118.9(3) . .
C8 C1 C9 119.3(3) . 2_556
C9 C1 C4 121.7(3) 2_556 .
O3 C2 O6 121.4(3) . .
O3 C2 C3 120.4(3) . .
O6 C2 C3 118.2(4) . .
C5 C3 C2 118.2(4) . .
C6 C3 C2 121.6(3) 2_666 .
C6 C3 C5 120.3(3) 2_666 .
O2 C4 O4 125.0(3) . .
O2 C4 C1 118.0(3) . .
O4 C4 C1 117.0(3) . .
C3 C5 H5 120.0 . .
C3 C5 C6 120.0(4) . .
C6 C5 H5 120.0 . .
O12 C6 C3 123.3(4) . 2_666
O12 C6 C5 117.0(4) . .
C3 C6 C5 119.7(3) 2_666 .
O7 C7 C11 120.0(3) . .
O8 C7 O7 120.6(3) . .
O8 C7 C11 119.3(4) . .
C1 C8 H8 119.0 . .
C1 C8 C9 121.9(4) . .
C9 C8 H8 119.0 . .
O9 C9 C1 123.9(3) . 2_556
O9 C9 C8 117.4(3) . .
C8 C9 C1 118.7(4) . 2_556
O5 C10 N1 123.9(4) . .
O5 C10 H10 118.1 . .
N1 C10 H10 118.1 . .
C1A N3 C2A 127.4(18) . .
C1A N3 C3A 118.1(15) . .
C2A N3 C3A 114.5(15) . .
C1B N3 C2B 116.4(17) . .
C1B N3 C3B 127.4(19) . .
C3B N3 C2B 116.0(16) . .
C12 C11 C7 120.9(4) . .
C14 C11 C7 118.8(3) . .
C14 C11 C12 120.3(3) . .
O1A C12 C11 124.6(3) . .
O1A C12 C14 116.6(4) . 2_677
C11 C12 H12A 120.6 . .
C11 C12 C14 118.9(4) . 2_677
C14 C12 H12A 120.6 2_677 .
O11 C13 N2 125.5(7) . .
O11 C13 H13 117.3 . .
N2 C13 H13 117.3 . .
O1B C14 C11 130.3(11) . .
O1B C14 C12 108.5(10) . 2_677
C11 C14 C12 120.8(4) . 2_677
C11 C14 H14 119.6 . .
C12 C14 H14 119.6 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 118.4 . .
O10 C1A N3 123(2) . .
O10 C1A H1AA 118.4 . .
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 116.4 . .
O10 C1B N3 127(3) . .
O10 C1B H1BA 116.4 . .
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 2.334(2) .
Tb1 O3 2.297(3) .
Tb1 O4 2.378(2) 2_566
Tb1 O5 2.384(3) .
Tb1 O6 2.381(3) 2_566
Tb1 O7 2.548(3) .
Tb1 O8 2.396(3) .
Tb1 O11 2.409(3) .
O2 C4 1.250(5) .
O3 C2 1.260(5) .
O4 Tb1 2.378(2) 2_566
O4 C4 1.264(5) .
O5 C10 1.247(6) .
O6 Tb1 2.381(3) 2_566
O6 C2 1.263(5) .
O7 C7 1.271(5) .
O8 C7 1.253(5) .
O9 H9 0.8300 .
O9 C9 1.356(5) .
O11 C13 1.167(6) .
O12 H12 0.8300 .
O12 C6 1.363(5) .
N1 C10 1.315(6) .
N1 C15 1.458(8) .
N1 C16 1.414(8) .
O1A H1A 0.8300 .
O1A C12 1.359(6) .
O1B H1B 0.8300 .
O1B C14 1.41(3) .
N2 C13 1.324(6) .
N2 C17 1.414(10) .
N2 C18 1.493(10) .
C1 C4 1.499(4) .
C1 C8 1.383(5) .
C1 C9 1.399(6) 2_556
C2 C3 1.489(5) .
C3 C5 1.395(5) .
C3 C6 1.382(7) 2_666
C5 H5 0.9400 .
C5 C6 1.395(5) .
C6 C3 1.382(7) 2_666
C7 C11 1.493(4) .
C8 H8 0.9400 .
C8 C9 1.388(5) .
C9 C1 1.398(6) 2_556
C10 H10 0.9400 .
N3 C1A 1.36(2) .
N3 C2A 1.42(2) .
N3 C3A 1.49(2) .
N3 C1B 1.29(2) .
N3 C2B 1.49(2) .
N3 C3B 1.45(2) .
C11 C12 1.394(6) .
C11 C14 1.385(6) .
C12 H12A 0.9400 .
C12 C14 1.396(5) 2_677
C13 H13 0.9400 .
C14 C12 1.396(5) 2_677
C14 H14 0.9400 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 H15C 0.9700 .
O10 C1A 1.20(2) .
O10 C1B 1.21(2) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16 H16C 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 H17C 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 H18C 0.9700 .
C1A H1AA 0.9400 .
C2A H2AA 0.9700 .
C2A H2AB 0.9700 .
C2A H2AC 0.9700 .
C3A H3AA 0.9700 .
C3A H3AB 0.9700 .
C3A H3AC 0.9700 .
C1B H1BA 0.9400 .
C2B H2BA 0.9700 .
C2B H2BB 0.9700 .
C2B H2BC 0.9700 .
C3B H3BA 0.9700 .
C3B H3BB 0.9700 .
C3B H3BC 0.9700 .
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 -47.7(5) . .
Tb1 O2 C4 C1 132.4(3) . .
Tb1 O4 C4 O2 7.5(6) 2_566 .
Tb1 O4 C4 C1 -172.5(3) 2_566 .
Tb1 O5 C10 N1 143.8(4) . .
Tb1 O6 C2 O3 11.0(4) 2_566 .
Tb1 O6 C2 C3 -168.9(2) 2_566 .
Tb1 O7 C7 O8 -4.5(4) . .
Tb1 O7 C7 C11 175.9(3) . .
Tb1 O8 C7 O7 4.8(4) . .
Tb1 O8 C7 C11 -175.6(3) . .
Tb1 O11 C13 N2 167.3(4) . .
O3 C2 C3 C5 -3.8(5) . .
O3 C2 C3 C6 175.4(4) . 2_666
O6 C2 C3 C5 176.1(3) . .
O6 C2 C3 C6 -4.6(5) . 2_666
O7 C7 C11 C12 -4.3(5) . .
O7 C7 C11 C14 175.2(4) . .
O8 C7 C11 C12 176.1(4) . .
O8 C7 C11 C14 -4.4(5) . .
C1 C8 C9 O9 179.7(4) . .
C1 C8 C9 C1 0.0(7) . 2_556
C2 C3 C5 C6 179.8(4) . .
C3 C5 C6 O12 179.8(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 -1.2(6) . .
C7 C11 C12 C14 178.8(3) . 2_677
C7 C11 C14 O1B -7(2) . .
C7 C11 C14 C12 -178.8(4) . 2_677
C8 C1 C4 O2 6.4(5) . .
C8 C1 C4 O4 -173.6(4) . .
C9 C1 C4 O2 -171.3(4) 2_556 .
C9 C1 C4 O4 8.8(5) 2_556 .
C9 C1 C8 C9 0.0(7) 2_556 .
C12 C11 C14 O1B 172.8(19) . .
C12 C11 C14 C12 0.6(7) . 2_677
C14 C11 C12 O1A 179.4(4) . .
C14 C11 C12 C14 -0.6(6) . 2_677
C15 N1 C10 O5 179.0(6) . .
C16 N1 C10 O5 1.6(10) . .
C17 N2 C13 O11 4.4(13) . .
C18 N2 C13 O11 179.8(7) . .
C2A N3 C1A O10 179.2(17) . .
C3A N3 C1A O10 -3(2) . .
C2B N3 C1B O10 -10(3) . .
C3B N3 C1B O10 174.5(18) . .
