#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:08:13 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/32/7233246.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_7233246
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                104.707(4)
_cell_angle_beta                 107.578(5)
_cell_angle_gamma                97.265(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5156(6)
_cell_length_b                   10.9858(4)
_cell_length_c                   12.5290(6)
_cell_measurement_reflns_used    5160
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.4680
_cell_measurement_theta_min      1.9480
_cell_volume                     1301.80(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      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.716
_diffrn_measured_fraction_theta_max 0.654
_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      0.0598284000
_diffrn_orient_matrix_UB_12      -0.0136848000
_diffrn_orient_matrix_UB_13      0.0361699000
_diffrn_orient_matrix_UB_21      -0.0285537000
_diffrn_orient_matrix_UB_22      -0.0675335000
_diffrn_orient_matrix_UB_23      -0.0271222000
_diffrn_orient_matrix_UB_31      0.0306586000
_diffrn_orient_matrix_UB_32      -0.0000295000
_diffrn_orient_matrix_UB_33      -0.0436884000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.716
_diffrn_reflns_Laue_measured_fraction_max 0.654
_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            8235
_diffrn_reflns_point_group_measured_fraction_full 0.716
_diffrn_reflns_point_group_measured_fraction_max 0.654
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.426
_diffrn_reflns_theta_min         1.974
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81926
_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    1.715
_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         1.516
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4216
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0309
_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)+(0.0695P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3969
_reflns_number_total             4216
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_120K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_database_code               7233246
_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   0.829
_shelx_estimated_absorpt_t_min   0.606
_reflns_odcompleteness_completeness 70.54
_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 planarity
 O1B, C14, C11, C12, O8, C7, O7
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
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
 O3, C2, O6, C3
 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 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.895
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 0.09500(2) 0.54663(2) 0.68273(2) 0.02506(10) Uani 1 1 d . . . . .
O2 O -0.0353(3) 0.3348(2) 0.5868(3) 0.0277(6) Uani 1 1 d . . . . .
O3 O 0.1547(3) 0.4857(3) 0.5161(3) 0.0298(6) Uani 1 1 d . U . . .
O4 O -0.0816(3) 0.2731(2) 0.3920(2) 0.0310(7) Uani 1 1 d . . . . .
O5 O 0.0572(3) 0.4845(3) 0.8411(3) 0.0367(7) Uani 1 1 d . . . . .
O6 O 0.1298(3) 0.4231(3) 0.3285(3) 0.0320(7) Uani 1 1 d . U . . .
O7 O 0.1650(3) 0.7632(3) 0.8508(3) 0.0340(7) Uani 1 1 d . . . . .
O8 O 0.3201(3) 0.6809(3) 0.7867(3) 0.0358(7) Uani 1 1 d . . . . .
O9 O 0.0442(4) -0.0491(3) 0.7135(3) 0.0468(9) Uani 1 1 d . . . . .
H9 H 0.0500 -0.1260 0.7073 0.070 Uiso 1 1 calc GR . . . .
O11 O 0.2495(3) 0.4058(3) 0.7346(3) 0.0431(8) Uani 1 1 d . . . . .
O12 O 0.6598(3) 0.6062(4) 0.7369(3) 0.0473(9) Uani 1 1 d . . . . .
H12 H 0.7420 0.6032 0.7481 0.071 Uiso 1 1 calc GR . . . .
N1 N -0.0130(4) 0.3084(4) 0.8911(4) 0.0392(9) Uani 1 1 d . . . . .
O1A O 0.2343(4) 1.0051(3) 0.9936(4) 0.0394(12) Uani 0.865(10) 1 d . . P A 1
H1A H 0.1802 0.9342 0.9514 0.059 Uiso 0.865(10) 1 calc GR . P A 1
O1B O 0.594(3) 0.801(2) 0.8769(19) 0.061(11) Uani 0.135(10) 1 d . . P A 2
H1B H 0.5340 0.7337 0.8339 0.092 Uiso 0.135(10) 1 calc R . P A 2
N2 N 0.4286(4) 0.3325(4) 0.8312(4) 0.0446(10) Uani 1 1 d . . . . .
C1 C -0.0264(4) 0.1205(3) 0.4930(4) 0.0290(9) Uani 1 1 d . . . . .
C2 C 0.2054(4) 0.4629(4) 0.4373(4) 0.0294(8) Uani 1 1 d . U . . .
C3 C 0.3576(4) 0.4814(4) 0.4674(4) 0.0296(9) Uani 1 1 d . U . . .
C4 C -0.0487(4) 0.2529(3) 0.4906(4) 0.0279(9) Uani 1 1 d . . . . .
C5 C 0.4417(4) 0.5356(4) 0.5864(4) 0.0343(10) Uani 1 1 d . . . . .
H5 H 0.4021 0.5609 0.6451 0.041 Uiso 1 1 calc R . . . .
C6 C 0.5839(5) 0.5524(4) 0.6183(4) 0.0330(10) Uani 1 1 d . . . . .
C7 C 0.2873(4) 0.7724(4) 0.8499(4) 0.0300(9) Uani 1 1 d . . . . .
C8 C -0.0026(5) 0.0912(4) 0.5973(4) 0.0330(9) Uani 1 1 d . . . . .
H8 H -0.0039 0.1539 0.6647 0.040 Uiso 1 1 calc R . . . .
C9 C 0.0234(5) -0.0288(4) 0.6060(4) 0.0312(9) Uani 1 1 d . . . . .
C10 C -0.0327(5) 0.3877(4) 0.8280(4) 0.0401(11) Uani 1 1 d . . . . .
H10 H -0.1197 0.3717 0.7687 0.048 Uiso 1 1 calc R . . . .
N3 N 0.4764(5) 0.1528(4) 0.4541(5) 0.0523(11) Uani 1 1 d . U . . .
C11 C 0.3967(4) 0.8913(3) 0.9287(3) 0.0287(9) Uani 1 1 d . . . . .
C12 C 0.3641(4) 0.9983(4) 0.9948(4) 0.0330(10) Uani 1 1 d . . . . .
H12A H 0.2723 0.9976 0.9907 0.040 Uiso 0.135(10) 1 calc R . P A 2
C13 C 0.3702(5) 0.4232(5) 0.7954(4) 0.0411(11) Uani 1 1 d . . . . .
H13 H 0.4260 0.5070 0.8187 0.049 Uiso 1 1 calc R . . . .
C14 C 0.5313(4) 0.8939(4) 0.9331(4) 0.0296(9) Uani 1 1 d . . . . .
H14 H 0.5520 0.8217 0.8865 0.036 Uiso 0.865(10) 1 calc R . P A 1
C15 C -0.1234(6) 0.1980(5) 0.8720(6) 0.0539(14) Uani 1 1 d . . . . .
H15A H -0.1547 0.2140 0.9395 0.081 Uiso 1 1 calc GR . . . .
H15B H -0.0883 0.1189 0.8637 0.081 Uiso 1 1 calc GR . . . .
H15C H -0.2000 0.1882 0.8003 0.081 Uiso 1 1 calc GR . . . .
O10 O 0.6042(7) 0.2227(6) 0.6485(5) 0.0896(17) Uani 1 1 d . U . . .
C16 C 0.1124(7) 0.3274(6) 0.9890(6) 0.0644(17) Uani 1 1 d . . . . .
H16A H 0.1767 0.4049 0.9972 0.097 Uiso 1 1 calc GR . . . .
H16B H 0.1532 0.2523 0.9742 0.097 Uiso 1 1 calc GR . . . .
H16C H 0.0918 0.3379 1.0616 0.097 Uiso 1 1 calc GR . . . .
C17 C 0.3520(7) 0.2002(5) 0.7983(6) 0.0578(15) Uani 1 1 d . . . . .
H17A H 0.3304 0.1860 0.8656 0.087 Uiso 1 1 calc GR . . . .
H17B H 0.4072 0.1401 0.7750 0.087 Uiso 1 1 calc GR . . . .
H17C H 0.2669 0.1858 0.7323 0.087 Uiso 1 1 calc GR . . . .
C18 C 0.5733(7) 0.3637(7) 0.9021(6) 0.0667(17) Uani 1 1 d . . . . .
H18A H 0.6202 0.3057 0.8627 0.100 Uiso 1 1 calc GR . . . .
H18B H 0.5840 0.3534 0.9796 0.100 Uiso 1 1 calc GR . . . .
H18C H 0.6132 0.4532 0.9118 0.100 Uiso 1 1 calc GR . . . .
C1A C 0.5938(11) 0.1924(10) 0.5440(9) 0.060(2) Uani 0.630(9) 1 d . U P B 1
H1AA H 0.6759 0.1979 0.5267 0.073 Uiso 0.630(9) 1 calc R . P B 1
C2A C 0.4685(14) 0.1133(13) 0.3311(11) 0.072(3) Uani 0.630(9) 1 d . U P B 1
H2AA H 0.5598 0.1364 0.3273 0.109 Uiso 0.630(9) 1 calc GR . P B 1
H2AB H 0.4067 0.1573 0.2869 0.109 Uiso 0.630(9) 1 calc GR . P B 1
H2AC H 0.4337 0.0197 0.2968 0.109 Uiso 0.630(9) 1 calc GR . P B 1
C3A C 0.3441(12) 0.1380(12) 0.4742(11) 0.070(3) Uani 0.630(9) 1 d . U P B 1
H3AA H 0.2862 0.0531 0.4246 0.105 Uiso 0.630(9) 1 calc GR . P B 1
H3AB H 0.2980 0.2055 0.4542 0.105 Uiso 0.630(9) 1 calc GR . P B 1
H3AC H 0.3608 0.1456 0.5572 0.105 Uiso 0.630(9) 1 calc GR . P B 1
C1B C 0.489(2) 0.198(2) 0.5640(17) 0.072(5) Uani 0.370(9) 1 d . U P B 2
H1BA H 0.4106 0.2124 0.5828 0.087 Uiso 0.370(9) 1 calc R . P B 2
C2B C 0.599(2) 0.144(2) 0.4238(19) 0.072(5) Uani 0.370(9) 1 d . U P B 2
H2BA H 0.6778 0.2039 0.4875 0.109 Uiso 0.370(9) 1 calc GR . P B 2
H2BB H 0.5875 0.1654 0.3509 0.109 Uiso 0.370(9) 1 calc GR . P B 2
H2BC H 0.6126 0.0554 0.4127 0.109 Uiso 0.370(9) 1 calc GR . P B 2
C3B C 0.344(2) 0.123(2) 0.3577(19) 0.076(5) Uani 0.370(9) 1 d . U P B 2
H3BA H 0.2726 0.1407 0.3907 0.114 Uiso 0.370(9) 1 calc GR . P B 2
H3BB H 0.3221 0.0311 0.3119 0.114 Uiso 0.370(9) 1 calc GR . P B 2
H3BC H 0.3497 0.1756 0.3065 0.114 Uiso 0.370(9) 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 126.84(9) . 2_566
O2 Tb1 O5 78.07(10) . .
O2 Tb1 O6 78.75(10) . 2_566
O2 Tb1 O7 151.31(10) . .
O2 Tb1 O8 146.01(10) . .
O2 Tb1 O11 74.06(10) . .
O3 Tb1 O2 77.28(10) . .
O3 Tb1 O4 75.95(10) . 2_566
O3 Tb1 O5 145.80(10) . .
O3 Tb1 O6 122.04(10) . 2_566
O3 Tb1 O7 131.29(10) . .
O3 Tb1 O8 88.86(11) . .
O3 Tb1 O11 78.31(12) . .
O4 Tb1 O7 68.28(10) 2_566 .
O4 Tb1 O11 140.88(12) 2_566 .
O5 Tb1 O4 138.23(11) . 2_566
O5 Tb1 O6 75.21(11) . 2_566
O5 Tb1 O7 76.65(10) . .
O5 Tb1 O8 98.71(11) . .
O5 Tb1 O11 72.37(12) . .
O6 Tb1 O4 77.98(10) 2_566 2_566
O6 Tb1 O7 81.87(10) 2_566 .
O6 Tb1 O8 133.73(10) 2_566 .
O6 Tb1 O11 141.11(11) 2_566 .
O8 Tb1 O4 77.73(10) . 2_566
O8 Tb1 O7 52.60(11) . .
O8 Tb1 O11 72.79(11) . .
O11 Tb1 O7 110.39(11) . .
C4 O2 Tb1 132.4(3) . .
C2 O3 Tb1 170.8(3) . .
C4 O4 Tb1 138.2(2) . 2_566
C10 O5 Tb1 124.1(3) . .
C2 O6 Tb1 107.5(3) . 2_566
C7 O7 Tb1 88.4(2) . .
C7 O8 Tb1 97.6(2) . .
C9 O9 H9 109.5 . .
C13 O11 Tb1 134.9(3) . .
C6 O12 H12 109.5 . .
C10 N1 C15 121.4(4) . .
C10 N1 C16 122.9(4) . .
C16 N1 C15 115.5(4) . .
C12 O1A H1A 109.5 . .
C14 O1B H1B 109.5 . .
C13 N2 C17 121.8(4) . .
C13 N2 C18 119.9(5) . .
C18 N2 C17 118.3(4) . .
C8 C1 C4 119.0(4) . .
C8 C1 C9 119.2(4) . 2_556
C9 C1 C4 121.7(4) 2_556 .
O3 C2 O6 121.1(4) . .
O3 C2 C3 120.8(4) . .
O6 C2 C3 118.1(4) . .
C5 C3 C2 118.3(4) . .
C6 C3 C2 122.0(4) 2_666 .
C6 C3 C5 119.8(4) 2_666 .
O2 C4 C1 117.8(4) . .
O4 C4 O2 124.8(3) . .
O4 C4 C1 117.5(4) . .
C3 C5 H5 120.0 . .
C6 C5 C3 120.0(5) . .
C6 C5 H5 120.0 . .
O12 C6 C3 123.1(4) . 2_666
O12 C6 C5 116.6(4) . .
C3 C6 C5 120.2(4) 2_666 .
O7 C7 C11 120.2(4) . .
O8 C7 O7 121.0(3) . .
O8 C7 C11 118.8(4) . .
C1 C8 H8 119.2 . .
C1 C8 C9 121.7(4) . .
C9 C8 H8 119.2 . .
O9 C9 C1 123.7(4) . 2_556
O9 C9 C8 117.2(4) . .
C1 C9 C8 119.1(4) 2_556 .
O5 C10 N1 124.2(4) . .
O5 C10 H10 117.9 . .
N1 C10 H10 117.9 . .
C1A N3 C2A 123.1(8) . .
C1A N3 C3A 120.7(8) . .
C2A N3 C3A 116.1(8) . .
C1B N3 C2B 118.9(14) . .
C1B N3 C3B 122.6(14) . .
C2B N3 C3B 118.3(13) . .
C12 C11 C7 121.0(4) . .
C14 C11 C7 118.8(4) . .
C14 C11 C12 120.3(3) . .
O1A C12 C11 124.1(4) . .
O1A C12 C14 116.9(4) . 2_677
C11 C12 H12A 120.5 . .
C14 C12 C11 119.0(4) 2_677 .
C14 C12 H12A 120.5 2_677 .
O11 C13 N2 124.7(5) . .
O11 C13 H13 117.6 . .
N2 C13 H13 117.6 . .
O1B C14 C11 132.5(11) . .
O1B C14 C12 106.8(11) . 2_677
C11 C14 C12 120.7(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 117.6 . .
O10 C1A N3 124.8(10) . .
O10 C1A H1AA 117.6 . .
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 118.6 . .
O10 C1B N3 122.9(18) . .
O10 C1B H1BA 118.6 . .
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 2.349(3) .
Tb1 O3 2.321(3) .
Tb1 O4 2.399(3) 2_566
Tb1 O5 2.379(3) .
Tb1 O6 2.396(3) 2_566
Tb1 O7 2.591(3) .
Tb1 O8 2.399(3) .
Tb1 O11 2.442(3) .
O2 C4 1.264(5) .
O3 C2 1.244(6) .
O4 Tb1 2.399(3) 2_566
O4 C4 1.263(5) .
O5 C10 1.270(6) .
O6 Tb1 2.396(3) 2_566
O6 C2 1.279(5) .
O7 C7 1.281(6) .
O8 C7 1.267(5) .
O9 H9 0.8400 .
O9 C9 1.378(6) .
O11 C13 1.228(6) .
O12 H12 0.8400 .
O12 C6 1.383(5) .
N1 C10 1.313(6) .
N1 C15 1.484(7) .
N1 C16 1.453(7) .
O1A H1A 0.8400 .
O1A C12 1.372(6) .
O1B H1B 0.8400 .
O1B C14 1.43(2) .
N2 C13 1.336(6) .
N2 C17 1.459(7) .
N2 C18 1.456(7) .
C1 C4 1.508(5) .
C1 C8 1.382(6) .
C1 C9 1.397(6) 2_556
C2 C3 1.503(6) .
C3 C5 1.407(6) .
C3 C6 1.388(7) 2_666
C5 H5 0.9500 .
C5 C6 1.400(6) .
C6 C3 1.388(7) 2_666
C7 C11 1.511(5) .
C8 H8 0.9500 .
C8 C9 1.404(5) .
C9 C1 1.397(6) 2_556
C10 H10 0.9500 .
N3 C1A 1.326(11) .
N3 C2A 1.464(13) .
N3 C3A 1.484(13) .
N3 C1B 1.30(2) .
N3 C2B 1.45(2) .
N3 C3B 1.47(2) .
C11 C12 1.402(6) .
C11 C14 1.396(6) .
C12 H12A 0.9500 .
C12 C14 1.399(5) 2_677
C13 H13 0.9500 .
C14 C12 1.399(5) 2_677
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
O10 C1A 1.232(12) .
O10 C1B 1.28(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 -53.9(6) . .
Tb1 O2 C4 C1 127.3(3) . .
Tb1 O4 C4 O2 15.1(7) 2_566 .
Tb1 O4 C4 C1 -166.1(3) 2_566 .
Tb1 O5 C10 N1 139.2(4) . .
Tb1 O6 C2 O3 13.0(4) 2_566 .
Tb1 O6 C2 C3 -167.1(3) 2_566 .
Tb1 O7 C7 O8 -6.4(4) . .
Tb1 O7 C7 C11 176.1(3) . .
Tb1 O8 C7 O7 7.0(4) . .
Tb1 O8 C7 C11 -175.5(3) . .
Tb1 O11 C13 N2 166.0(4) . .
O3 C2 C3 C5 -5.5(6) . .
O3 C2 C3 C6 175.1(4) . 2_666
O6 C2 C3 C5 174.6(4) . .
O6 C2 C3 C6 -4.8(6) . 2_666
O7 C7 C11 C12 -6.5(6) . .
O7 C7 C11 C14 174.7(4) . .
O8 C7 C11 C12 176.0(4) . .
O8 C7 C11 C14 -2.8(6) . .
C1 C8 C9 O9 -179.3(4) . .
C1 C8 C9 C1 0.5(7) . 2_556
C2 C3 C5 C6 178.9(4) . .
C3 C5 C6 O12 -179.9(4) . .
C3 C5 C6 C3 1.6(7) . 2_666
C4 C1 C8 C9 -177.8(4) . .
C6 C3 C5 C6 -1.6(7) 2_666 .
C7 C11 C12 O1A -0.4(7) . .
C7 C11 C12 C14 179.8(4) . 2_677
C7 C11 C14 O1B -1.5(11) . .
C7 C11 C14 C12 -179.7(4) . 2_677
C8 C1 C4 O2 4.7(6) . .
C8 C1 C4 O4 -174.1(4) . .
C9 C1 C4 O2 -172.5(4) 2_556 .
C9 C1 C4 O4 8.6(6) 2_556 .
C9 C1 C8 C9 -0.5(7) 2_556 .
C12 C11 C14 O1B 179.6(11) . .
C12 C11 C14 C12 1.4(7) . 2_677
C14 C11 C12 O1A 178.4(4) . .
C14 C11 C12 C14 -1.4(7) . 2_677
C15 N1 C10 O5 179.2(5) . .
C16 N1 C10 O5 4.0(9) . .
C17 N2 C13 O11 1.1(8) . .
C18 N2 C13 O11 179.3(6) . .
C2A N3 C1A O10 -177.7(10) . .
C3A N3 C1A O10 -1.9(15) . .
C2B N3 C1B O10 -7(3) . .
C3B N3 C1B O10 179.1(15) . .
