#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:08:13 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/32/7233248.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_7233248
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                104.317(4)
_cell_angle_beta                 109.262(4)
_cell_angle_gamma                96.536(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5190(6)
_cell_length_b                   10.9933(5)
_cell_length_c                   12.6565(5)
_cell_measurement_reflns_used    5759
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      31.9260
_cell_measurement_theta_min      2.0920
_cell_volume                     1307.83(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      220.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.684
_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      0.0605786000
_diffrn_orient_matrix_UB_12      -0.0139922000
_diffrn_orient_matrix_UB_13      0.0370018000
_diffrn_orient_matrix_UB_21      -0.0287806000
_diffrn_orient_matrix_UB_22      -0.0671920000
_diffrn_orient_matrix_UB_23      -0.0270263000
_diffrn_orient_matrix_UB_31      0.0303666000
_diffrn_orient_matrix_UB_32      -0.0002225000
_diffrn_orient_matrix_UB_33      -0.0428559000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.747
_diffrn_reflns_Laue_measured_fraction_max 0.684
_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            8658
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.431
_diffrn_reflns_theta_min         1.967
_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  0.77258
_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         1.689
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4433
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0664P)²+0.6025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4230
_reflns_number_total             4433
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00941h5.cif
_cod_data_source_block           SION2_220K
_cod_depositor_comments
'Adding full bibliography for 7233243--7233257.cif.'
_cod_database_code               7233248
_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 73.65
_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 1.166
_oxdiff_exptl_absorpt_empirical_full_min 0.828
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 0.10010(2) 0.54749(2) 0.68289(2) 0.02727(9) Uani 1 1 d . . . . .
O2 O -0.0238(3) 0.3356(2) 0.5875(2) 0.0358(6) Uani 1 1 d . . . . .
O3 O 0.1592(3) 0.4908(3) 0.5202(3) 0.0369(5) Uani 1 1 d . U . . .
O4 O -0.0752(3) 0.2753(2) 0.3934(2) 0.0365(6) Uani 1 1 d . . . . .
O5 O 0.0650(3) 0.4825(3) 0.8393(3) 0.0445(7) Uani 1 1 d . . . . .
O6 O 0.1272(3) 0.4279(3) 0.3323(3) 0.0395(7) Uani 1 1 d . . . . .
O7 O 0.1710(3) 0.7584(3) 0.8498(3) 0.0386(7) Uani 1 1 d . . . . .
O8 O 0.3249(3) 0.6852(3) 0.7837(3) 0.0480(8) Uani 1 1 d . . . . .
O9 O 0.0454(5) -0.0500(3) 0.7111(3) 0.0653(12) Uani 1 1 d . . . . .
H9 H 0.0472 -0.1268 0.7042 0.098 Uiso 1 1 calc GR . . . .
O11 O 0.2619(4) 0.4143(4) 0.7410(4) 0.0632(10) Uani 1 1 d . . . . .
O12 O 0.6682(3) 0.6023(4) 0.7349(3) 0.0591(10) Uani 1 1 d . . . . .
H12 H 0.7504 0.6044 0.7442 0.089 Uiso 1 1 calc GR . . . .
N1 N -0.0054(5) 0.3121(4) 0.8923(4) 0.0565(11) Uani 1 1 d . . . . .
O1A O 0.2350(4) 0.9942(4) 0.9971(4) 0.0500(13) Uani 0.881(11) 1 d . . P A 1
H1A H 0.1827 0.9239 0.9552 0.075 Uiso 0.881(11) 1 calc GR . P A 1
O1B O 0.591(3) 0.806(3) 0.884(3) 0.065(11) Uani 0.119(11) 1 d . U P A 2
H1B H 0.5307 0.7408 0.8425 0.098 Uiso 0.119(11) 1 calc R . P A 2
N2 N 0.4332(5) 0.3300(5) 0.8314(5) 0.0700(14) Uani 1 1 d . . . . .
C1 C -0.0232(4) 0.1209(3) 0.4932(3) 0.0340(9) Uani 1 1 d . . . . .
C2 C 0.2062(4) 0.4665(4) 0.4403(4) 0.0355(6) Uani 1 1 d . U . . .
C3 C 0.3579(4) 0.4834(4) 0.4684(4) 0.0356(10) Uani 1 1 d . . . . .
C4 C -0.0418(4) 0.2538(3) 0.4914(3) 0.0329(9) Uani 1 1 d . . . . .
C5 C 0.4458(4) 0.5351(4) 0.5870(4) 0.0380(9) Uani 1 1 d . . . . .
H5 H 0.4087 0.5589 0.6453 0.046 Uiso 1 1 calc R . . . .
C6 C 0.5883(4) 0.5512(4) 0.6181(4) 0.0375(10) Uani 1 1 d . . . . .
C7 C 0.2919(4) 0.7719(3) 0.8485(3) 0.0355(9) Uani 1 1 d . . . . .
C8 C -0.0002(5) 0.0907(4) 0.5966(4) 0.0419(10) Uani 1 1 d . . . . .
H8 H 0.0000 0.1530 0.6627 0.050 Uiso 1 1 calc R . . . .
C9 C 0.0229(5) -0.0294(4) 0.6061(4) 0.0404(10) Uani 1 1 d . . . . .
C10 C -0.0239(5) 0.3886(5) 0.8264(4) 0.0491(11) Uani 1 1 d . . . . .
H10 H -0.1100 0.3717 0.7651 0.059 Uiso 1 1 calc R . . . .
N3 N 0.4784(7) 0.1537(6) 0.4537(6) 0.0877(17) Uani 1 1 d . U . . .
C11 C 0.3986(4) 0.8911(3) 0.9271(3) 0.0354(9) Uani 1 1 d . . . . .
C12 C 0.3643(4) 0.9924(4) 0.9962(4) 0.0374(9) Uani 1 1 d . . . . .
H12A H 0.2734 0.9875 0.9936 0.045 Uiso 0.119(11) 1 calc R . P A 2
C13 C 0.3789(6) 0.4243(6) 0.7987(5) 0.0662(16) Uani 1 1 d . . . . .
H13 H 0.4380 0.5052 0.8234 0.079 Uiso 1 1 calc R . . . .
C14 C 0.5329(4) 0.8990(4) 0.9309(4) 0.0381(9) Uani 1 1 d . . . . .
H14 H 0.5547 0.8304 0.8839 0.046 Uiso 0.881(11) 1 calc R . P A 1
C15 C -0.1147(9) 0.2061(7) 0.8741(7) 0.088(2) Uani 1 1 d . . . . .
H15A H -0.1311 0.2144 0.9464 0.132 Uiso 1 1 calc GR . . . .
H15B H -0.0874 0.1253 0.8511 0.132 Uiso 1 1 calc GR . . . .
H15C H -0.1985 0.2078 0.8126 0.132 Uiso 1 1 calc GR . . . .
O10 O 0.6117(9) 0.2268(8) 0.6444(6) 0.133(3) Uani 1 1 d . U . . .
C16 C 0.1199(10) 0.3319(8) 0.9910(7) 0.105(3) Uani 1 1 d . . . . .
H16A H 0.1564 0.4233 1.0294 0.158 Uiso 1 1 calc GR . . . .
H16B H 0.1868 0.2936 0.9643 0.158 Uiso 1 1 calc GR . . . .
H16C H 0.1012 0.2920 1.0462 0.158 Uiso 1 1 calc GR . . . .
C17 C 0.3653(11) 0.2004(9) 0.8013(9) 0.129(4) Uani 1 1 d . . . . .
H17A H 0.3625 0.1814 0.8715 0.194 Uiso 1 1 calc GR . . . .
H17B H 0.4149 0.1441 0.7663 0.194 Uiso 1 1 calc GR . . . .
H17C H 0.2720 0.1868 0.7456 0.194 Uiso 1 1 calc GR . . . .
C18 C 0.5796(10) 0.3614(11) 0.9032(10) 0.126(4) Uani 1 1 d . . . . .
H18A H 0.6282 0.3135 0.8601 0.190 Uiso 1 1 calc GR . . . .
H18B H 0.5929 0.3388 0.9750 0.190 Uiso 1 1 calc GR . . . .
H18C H 0.6151 0.4527 0.9226 0.190 Uiso 1 1 calc GR . . . .
C1A C 0.601(2) 0.1942(16) 0.5403(16) 0.099(4) Uani 0.539(12) 1 d . U P B 1
H1AA H 0.6806 0.1983 0.5225 0.118 Uiso 0.539(12) 1 calc R . P B 1
C2A C 0.451(3) 0.113(2) 0.3300(18) 0.131(7) Uani 0.539(12) 1 d . U P B 1
H2AA H 0.5254 0.1572 0.3150 0.197 Uiso 0.539(12) 1 calc GR . P B 1
H2AB H 0.3650 0.1337 0.2880 0.197 Uiso 0.539(12) 1 calc GR . P B 1
H2AC H 0.4441 0.0211 0.3034 0.197 Uiso 0.539(12) 1 calc GR . P B 1
C3A C 0.348(2) 0.1438(18) 0.4800(19) 0.114(5) Uani 0.539(12) 1 d . U P B 1
H3AA H 0.3275 0.0621 0.4937 0.171 Uiso 0.539(12) 1 calc GR . P B 1
H3AB H 0.2722 0.1497 0.4137 0.171 Uiso 0.539(12) 1 calc GR . P B 1
H3AC H 0.3609 0.2134 0.5494 0.171 Uiso 0.539(12) 1 calc GR . P B 1
C1B C 0.502(3) 0.205(2) 0.5627(19) 0.110(6) Uani 0.461(12) 1 d . U P B 2
H1BA H 0.4270 0.2273 0.5817 0.132 Uiso 0.461(12) 1 calc R . P B 2
C2B C 0.602(2) 0.143(2) 0.424(2) 0.113(6) Uani 0.461(12) 1 d . U P B 2
H2BA H 0.6605 0.2273 0.4500 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H2BB H 0.5740 0.1061 0.3402 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H2BC H 0.6515 0.0876 0.4639 0.170 Uiso 0.461(12) 1 calc GR . P B 2
C3B C 0.345(2) 0.118(2) 0.360(2) 0.113(7) Uani 0.461(12) 1 d . U P B 2
H3BA H 0.2784 0.1514 0.3903 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H3BB H 0.3177 0.0252 0.3290 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H3BC H 0.3500 0.1538 0.2984 0.170 Uiso 0.461(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 126.42(9) . 2_566
O2 Tb1 O5 77.73(10) . .
O2 Tb1 O6 79.05(10) . 2_566
O2 Tb1 O7 151.79(11) . .
O2 Tb1 O8 145.53(10) . .
O2 Tb1 O11 74.41(12) . .
O3 Tb1 O2 77.26(10) . .
O3 Tb1 O4 76.12(10) . 2_566
O3 Tb1 O5 145.88(10) . .
O3 Tb1 O6 122.13(10) . 2_566
O3 Tb1 O7 130.93(10) . .
O3 Tb1 O8 87.17(11) . .
O3 Tb1 O11 79.11(13) . .
O4 Tb1 O5 137.93(11) 2_566 .
O4 Tb1 O6 77.23(10) 2_566 2_566
O4 Tb1 O7 69.42(9) 2_566 .
O4 Tb1 O8 77.57(11) 2_566 .
O4 Tb1 O11 141.77(13) 2_566 .
O5 Tb1 O6 74.76(11) . 2_566
O5 Tb1 O7 76.58(10) . .
O5 Tb1 O8 100.86(12) . .
O5 Tb1 O11 72.06(13) . .
O6 Tb1 O7 83.15(10) 2_566 .
O6 Tb1 O8 134.42(10) 2_566 .
O6 Tb1 O11 141.00(13) 2_566 .
O8 Tb1 O7 52.49(10) . .
O8 Tb1 O11 72.53(12) . .
O11 Tb1 O7 108.07(12) . .
C4 O2 Tb1 134.2(3) . .
C2 O3 Tb1 173.0(3) . .
C4 O4 Tb1 139.0(2) . 2_566
C10 O5 Tb1 124.9(3) . .
C2 O6 Tb1 108.9(3) . 2_566
C7 O7 Tb1 89.3(2) . .
C7 O8 Tb1 97.1(2) . .
C9 O9 H9 109.5 . .
C13 O11 Tb1 140.0(4) . .
C6 O12 H12 109.5 . .
C10 N1 C15 121.7(5) . .
C10 N1 C16 122.4(5) . .
C16 N1 C15 115.7(5) . .
C12 O1A H1A 109.5 . .
C14 O1B H1B 109.5 . .
C13 N2 C17 127.2(6) . .
C13 N2 C18 116.9(7) . .
C17 N2 C18 115.9(7) . .
C8 C1 C4 118.8(4) . .
C8 C1 C9 119.8(3) . 2_556
C9 C1 C4 121.3(4) 2_556 .
O3 C2 O6 121.6(4) . .
O3 C2 C3 121.0(4) . .
O6 C2 C3 117.4(4) . .
C5 C3 C2 117.6(4) . .
C6 C3 C2 122.0(4) 2_666 .
C6 C3 C5 120.4(4) 2_666 .
O2 C4 C1 117.8(3) . .
O4 C4 O2 124.8(3) . .
O4 C4 C1 117.4(3) . .
C3 C5 H5 120.0 . .
C6 C5 C3 119.9(4) . .
C6 C5 H5 120.0 . .
O12 C6 C3 123.2(4) . 2_666
O12 C6 C5 117.1(4) . .
C3 C6 C5 119.7(4) 2_666 .
O7 C7 C11 120.0(4) . .
O8 C7 O7 120.9(3) . .
O8 C7 C11 119.1(4) . .
C1 C8 H8 119.0 . .
C1 C8 C9 122.1(4) . .
C9 C8 H8 119.0 . .
O9 C9 C1 123.9(3) . 2_556
O9 C9 C8 117.9(4) . .
C8 C9 C1 118.2(4) . 2_556
O5 C10 N1 124.6(5) . .
O5 C10 H10 117.7 . .
N1 C10 H10 117.7 . .
C1A N3 C2A 127.0(17) . .
C1A N3 C3A 120.4(13) . .
C2A N3 C3A 112.6(15) . .
C1B N3 C2B 115.2(17) . .
C1B N3 C3B 125.4(19) . .
C3B N3 C2B 119.1(16) . .
C12 C11 C7 120.8(4) . .
C14 C11 C7 118.9(4) . .
C14 C11 C12 120.3(3) . .
O1A C12 C11 124.5(4) . .
O1A C12 C14 116.5(4) . 2_677
C11 C12 H12A 120.5 . .
C14 C12 C11 118.9(4) 2_677 .
C14 C12 H12A 120.5 2_677 .
O11 C13 N2 125.0(6) . .
O11 C13 H13 117.5 . .
N2 C13 H13 117.5 . .
O1B C14 C11 129.4(14) . .
O1B C14 C12 109.2(13) . 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 119.3 . .
O10 C1A N3 121.4(19) . .
O10 C1A H1AA 119.3 . .
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 116.6 . .
O10 C1B N3 127(2) . .
O10 C1B H1BA 116.6 . .
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 2.337(2) .
Tb1 O3 2.305(3) .
Tb1 O4 2.383(2) 2_566
Tb1 O5 2.385(3) .
Tb1 O6 2.387(3) 2_566
Tb1 O7 2.557(3) .
Tb1 O8 2.398(3) .
Tb1 O11 2.420(3) .
O2 C4 1.262(5) .
O3 C2 1.250(6) .
O4 Tb1 2.383(2) 2_566
O4 C4 1.262(5) .
O5 C10 1.250(6) .
O6 Tb1 2.387(3) 2_566
O6 C2 1.274(5) .
O7 C7 1.269(5) .
O8 C7 1.255(5) .
O9 H9 0.8300 .
O9 C9 1.352(6) .
O11 C13 1.182(6) .
O12 H12 0.8300 .
O12 C6 1.367(5) .
N1 C10 1.311(6) .
N1 C15 1.456(8) .
N1 C16 1.435(8) .
O1A H1A 0.8300 .
O1A C12 1.366(6) .
O1B H1B 0.8300 .
O1B C14 1.36(3) .
N2 C13 1.327(6) .
N2 C17 1.417(10) .
N2 C18 1.455(10) .
C1 C4 1.501(5) .
C1 C8 1.379(6) .
C1 C9 1.403(6) 2_556
C2 C3 1.495(5) .
C3 C5 1.405(5) .
C3 C6 1.383(7) 2_666
C5 H5 0.9400 .
C5 C6 1.395(6) .
C6 C3 1.383(7) 2_666
C7 C11 1.500(5) .
C8 H8 0.9400 .
C8 C9 1.397(5) .
C9 C1 1.403(6) 2_556
C10 H10 0.9400 .
N3 C1A 1.323(18) .
N3 C2A 1.44(2) .
N3 C3A 1.51(2) .
N3 C1B 1.28(2) .
N3 C2B 1.47(2) .
N3 C3B 1.44(2) .
C11 C12 1.397(6) .
C11 C14 1.389(6) .
C12 H12A 0.9400 .
C12 C14 1.397(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 1.24(2) .
O10 C1B 1.22(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 -48.8(6) . .
Tb1 O2 C4 C1 131.8(3) . .
Tb1 O4 C4 O2 9.0(7) 2_566 .
Tb1 O4 C4 C1 -171.5(3) 2_566 .
Tb1 O5 C10 N1 142.8(4) . .
Tb1 O6 C2 O3 10.8(4) 2_566 .
Tb1 O6 C2 C3 -168.4(3) 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 166.7(5) . .
O3 C2 C3 C5 -3.9(6) . .
O3 C2 C3 C6 175.5(4) . 2_666
O6 C2 C3 C5 175.3(4) . .
O6 C2 C3 C6 -5.3(6) . 2_666
O7 C7 C11 C12 -4.7(6) . .
O7 C7 C11 C14 174.9(4) . .
O8 C7 C11 C12 176.8(4) . .
O8 C7 C11 C14 -3.6(6) . .
C1 C8 C9 O9 179.6(5) . .
C1 C8 C9 C1 0.4(7) . 2_556
C2 C3 C5 C6 179.1(4) . .
C3 C5 C6 O12 179.8(4) . .
C3 C5 C6 C3 0.4(7) . 2_666
C4 C1 C8 C9 -177.7(4) . .
C6 C3 C5 C6 -0.4(7) 2_666 .
C7 C11 C12 O1A -1.4(7) . .
C7 C11 C12 C14 179.3(4) . 2_677
C7 C11 C14 O1B -10(2) . .
C7 C11 C14 C12 -179.3(4) . 2_677
C8 C1 C4 O2 5.8(6) . .
C8 C1 C4 O4 -173.7(4) . .
C9 C1 C4 O2 -171.3(4) 2_556 .
C9 C1 C4 O4 9.2(6) 2_556 .
C9 C1 C8 C9 -0.4(8) 2_556 .
C12 C11 C14 O1B 170(2) . .
C12 C11 C14 C12 0.3(7) . 2_677
C14 C11 C12 O1A 179.0(4) . .
C14 C11 C12 C14 -0.3(7) . 2_677
C15 N1 C10 O5 178.6(6) . .
C16 N1 C10 O5 2.5(10) . .
C17 N2 C13 O11 2.3(12) . .
C18 N2 C13 O11 -179.6(8) . .
C2A N3 C1A O10 -180.0(16) . .
C3A N3 C1A O10 -1(2) . .
C2B N3 C1B O10 -12(3) . .
C3B N3 C1B O10 174.1(18) . .
