#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:44:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180094 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/40/7054073.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_7054073
loop_
_publ_author_name
'Kim, Tae Kyung'
'Lee, Kyung Joo'
'Choi, Min'
'Park, Noejung'
'Moon, Dohyun'
'Moon, Hoi Ri'
_publ_section_title
;
 Metal--organic frameworks constructed from flexible ditopic ligands:
 conformational diversity of an aliphatic ligand
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4130
_journal_paper_doi               10.1039/c3nj00812f
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C33 H50 N2 O20 Tb3'
_chemical_formula_sum            'C33 H50 N2 O20 Tb3'
_chemical_formula_weight         1271.51
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.99(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.108(2)
_cell_length_b                   17.477(4)
_cell_length_c                   20.111(4)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.26
_cell_volume                     4253.2(15)
_computing_cell_refinement       DENZO
_computing_data_collection       DENZO
_computing_data_reduction        DENZO
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013-XL (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013-XS (Sheldrick, 2013)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Enraf-Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16558
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.013
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DENZO Scalepack'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_description       'parallel piped'
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.634
_refine_diff_density_min         -2.285
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0396
_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)+(0.0301P)²+14.5087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7249
_reflns_number_total             9670
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3nj00812f.txt
_cod_data_source_block           TbC4DC
_cod_original_cell_volume        4253.1(15)
_cod_database_code               7054073
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_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 1.01934(2) 0.75097(2) 0.69472(2) 0.01781(7) Uani 1 1 d . . . . .
Tb2 Tb 0.86642(2) 0.76382(2) 0.86985(2) 0.02093(8) Uani 1 1 d . . . . .
Tb3 Tb 0.69952(2) 0.73938(2) 1.03073(2) 0.01591(7) Uani 1 1 d . . . . .
O1A O 1.1105(3) 0.8685(2) 0.7297(2) 0.0355(10) Uani 1 1 d . . . . .
O2A O 1.0164(3) 0.8135(2) 0.80689(17) 0.0273(9) Uani 1 1 d . . . . .
O3A O 1.1309(3) 1.1141(3) 1.0780(2) 0.0366(10) Uani 1 1 d . . . . .
O4A O 1.1730(3) 1.1659(2) 0.9813(2) 0.0335(10) Uani 1 1 d . . . . .
C1A C 1.0656(5) 0.8720(3) 0.7849(3) 0.0299(13) Uani 1 1 d . . . . .
C2A C 1.0634(6) 0.9475(4) 0.8209(3) 0.0506(19) Uani 1 1 d . . . . .
H2A1 H 1.0948 0.9864 0.7928 0.061 Uiso 1 1 calc R U . . .
H2A2 H 0.9871 0.9614 0.8278 0.061 Uiso 1 1 calc R U . . .
C3A C 1.1240(7) 0.9477(4) 0.8857(3) 0.0510(19) Uani 1 1 d . . . . .
H3A1 H 1.2002 0.9330 0.8797 0.061 Uiso 1 1 calc R U . . .
H3A2 H 1.0911 0.9108 0.9152 0.061 Uiso 1 1 calc R U . . .
C4A C 1.1199(8) 1.0285(4) 0.9172(4) 0.065(2) Uani 1 1 d . . . . .
H4A1 H 1.1662 1.0626 0.8922 0.078 Uiso 1 1 calc R U . . .
H4A2 H 1.0447 1.0475 0.9131 0.078 Uiso 1 1 calc R U . . .
C5A C 1.1558(6) 1.0311(4) 0.9866(3) 0.0449(17) Uani 1 1 d . . . . .
H5A1 H 1.2307 1.0115 0.9907 0.054 Uiso 1 1 calc R U . . .
H5A2 H 1.1091 0.9972 1.0116 0.054 Uiso 1 1 calc R U . . .
C6A C 1.1530(4) 1.1094(4) 1.0176(3) 0.0304(14) Uani 1 1 d . . . . .
O1B O 0.8631(3) 0.8288(2) 0.68839(19) 0.0333(10) Uani 1 1 d . . . . .
O2B O 0.7806(3) 0.8383(2) 0.78512(19) 0.0304(9) Uani 1 1 d . . . . .
O3B O 0.6103(3) 1.1887(2) 0.74074(19) 0.0295(9) Uani 1 1 d . . . . .
O4B O 0.7557(3) 1.1681(2) 0.6823(2) 0.0344(10) Uani 1 1 d . . . . .
C1B C 0.7893(5) 0.8537(3) 0.7245(3) 0.0276(13) Uani 1 1 d . . . . .
C2B C 0.7048(6) 0.9066(4) 0.6930(3) 0.0434(17) Uani 1 1 d . . . . .
H2B1 H 0.6381 0.8775 0.6829 0.052 Uiso 1 1 calc R U . . .
H2B2 H 0.7325 0.9246 0.6511 0.052 Uiso 1 1 calc R U . . .
C3B C 0.6743(6) 0.9758(4) 0.7343(4) 0.0477(18) Uani 1 1 d . . . . .
H3B1 H 0.6375 0.9587 0.7737 0.057 Uiso 1 1 calc R U . . .
H3B2 H 0.6228 1.0076 0.7086 0.057 Uiso 1 1 calc R U . . .
C4B C 0.7752(6) 1.0233(4) 0.7552(4) 0.060(2) Uani 1 1 d . . . . .
H4B1 H 0.8191 0.9949 0.7881 0.073 Uiso 1 1 calc R U . . .
H4B2 H 0.8202 1.0312 0.7168 0.073 Uiso 1 1 calc R U . . .
C5B C 0.7461(6) 1.1001(4) 0.7840(3) 0.0416(16) Uani 1 1 d . . . . .
H5B1 H 0.6912 1.0929 0.8175 0.050 Uiso 1 1 calc R U . . .
H5B2 H 0.8115 1.1220 0.8059 0.050 Uiso 1 1 calc R U . . .
C6B C 0.7023(5) 1.1547(3) 0.7329(3) 0.0272(13) Uani 1 1 d . . . . .
O1C O 0.9401(3) 0.6241(3) 0.8950(2) 0.0387(11) Uani 1 1 d . . . . .
O2C O 0.8248(3) 0.6778(2) 0.96167(18) 0.0261(9) Uani 1 1 d . . . . .
C1C C 0.8780(4) 0.6187(3) 0.9420(3) 0.0265(13) Uani 1 1 d . . . . .
C2C C 0.8566(5) 0.5441(4) 0.9763(3) 0.0408(16) Uani 1 1 d . . . . .
H2C1 H 0.7927 0.5201 0.9547 0.049 Uiso 1 1 calc R U . . .
H2C2 H 0.8382 0.5547 1.0220 0.049 Uiso 1 1 calc R U . . .
C3C C 0.9519(5) 0.4882(4) 0.9768(3) 0.0409(16) Uani 1 1 d . . . . .
H3C1 H 0.9781 0.4834 0.9319 0.049 Uiso 1 1 calc R U . . .
H3C2 H 0.9255 0.4383 0.9903 0.049 Uiso 1 1 calc R U . . .
O1D O 0.6853(3) 0.7847(2) 0.91212(17) 0.0237(8) Uani 1 1 d . . . . .
O2D O 0.5570(3) 0.7073(3) 0.94637(19) 0.0351(10) Uani 1 1 d . . . . .
O3D O 0.3502(3) 0.7915(3) 0.6145(2) 0.0350(10) Uani 1 1 d . . . . .
O4D O 0.2016(3) 0.7368(2) 0.65090(18) 0.0270(9) Uani 1 1 d . . . . .
C1D C 0.5943(4) 0.7480(3) 0.9022(3) 0.0251(12) Uani 1 1 d . . . . .
C2D C 0.5312(5) 0.7582(4) 0.8368(3) 0.0328(14) Uani 1 1 d . . . . .
H2D1 H 0.4807 0.8009 0.8408 0.039 Uiso 1 1 calc R U . . .
H2D2 H 0.5830 0.7711 0.8029 0.039 Uiso 1 1 calc R U . . .
C3D C 0.4665(5) 0.6892(4) 0.8146(3) 0.0441(17) Uani 1 1 d . . . . .
H3D1 H 0.4056 0.6819 0.8440 0.053 Uiso 1 1 calc R U . . .
H3D2 H 0.5138 0.6445 0.8183 0.053 Uiso 1 1 calc R U . . .
C4D C 0.4204(6) 0.6953(5) 0.7427(3) 0.0478(18) Uani 1 1 d . . . . .
H4D1 H 0.4815 0.6982 0.7129 0.057 Uiso 1 1 calc R U . . .
H4D2 H 0.3787 0.6493 0.7318 0.057 Uiso 1 1 calc R U . . .
C5D C 0.3474(5) 0.7633(4) 0.7314(3) 0.0416(17) Uani 1 1 d . . . . .
H5D1 H 0.3900 0.8096 0.7394 0.050 Uiso 1 1 calc R U . . .
H5D2 H 0.2884 0.7623 0.7629 0.050 Uiso 1 1 calc R U . . .
C6D C 0.2978(4) 0.7649(3) 0.6613(3) 0.0269(12) Uani 1 1 d . . . . .
O1E O 0.6616(3) 0.6093(2) 1.05855(19) 0.0306(9) Uani 1 1 d . . . . .
O2E O 0.5301(3) 0.6851(2) 1.09093(17) 0.0240(8) Uani 1 1 d . . . . .
C1E C 0.5656(4) 0.6182(3) 1.0790(2) 0.0225(12) Uani 1 1 d . . . . .
C2E C 0.4925(6) 0.5500(4) 1.0858(3) 0.0381(16) Uani 1 1 d . . . . .
H2E1 H 0.4161 0.5662 1.0806 0.046 Uiso 1 1 calc R U . . .
H2E2 H 0.5031 0.5293 1.1303 0.046 Uiso 1 1 calc R U . . .
C3E C 0.5139(6) 0.4869(3) 1.0355(3) 0.0393(16) Uani 1 1 d . . . . .
H3E1 H 0.5910 0.4720 1.0390 0.047 Uiso 1 1 calc R U . . .
H3E2 H 0.4695 0.4425 1.0456 0.047 Uiso 1 1 calc R U . . .
O1F O 0.5816(3) 0.8441(2) 1.0368(2) 0.0393(11) Uani 1 1 d . . . . .
O2F O 0.4687(4) 0.8433(3) 1.1207(2) 0.0432(12) Uani 1 1 d . . . . .
C1F C 0.4960(5) 0.8641(4) 1.0639(3) 0.0357(15) Uani 1 1 d . . . . .
C2F C 0.4188(6) 0.9174(6) 1.0259(4) 0.077(3) Uani 1 1 d . . . . .
H2F1 H 0.3617 0.8868 1.0038 0.092 Uiso 1 1 calc R U . . .
H2F2 H 0.3830 0.9499 1.0578 0.092 Uiso 1 1 calc R U . . .
C3F C 0.4685(8) 0.9668(5) 0.9758(4) 0.085(3) Uani 1 1 d . . . . .
H3F1 H 0.4126 0.9894 0.9462 0.101 Uiso 1 1 calc R U . . .
H3F2 H 0.5211 0.9389 0.9497 0.101 Uiso 1 1 calc R U . . .
O1G O 1.1153(4) 0.6607(3) 0.7614(3) 0.0515(13) Uani 1 1 d . . . . .
N1G N 1.1495(5) 0.5387(4) 0.7911(4) 0.0554(17) Uani 1 1 d . . . . .
C1G C 1.1331(12) 0.6125(9) 0.7985(8) 0.051(4) Uani 0.557(14) 1 d . . P A 1
H1G H 1.1367 0.6285 0.8426 0.061 Uiso 0.557(14) 1 calc R U P A 1
C2G C 1.1374(15) 0.5155(12) 0.7152(9) 0.095(7) Uani 0.557(14) 1 d . . P A 1
H2G1 H 1.1180 0.5599 0.6891 0.142 Uiso 0.557(14) 1 calc R U P A 1
H2G2 H 1.0807 0.4775 0.7095 0.142 Uiso 0.557(14) 1 calc R U P A 1
H2G3 H 1.2063 0.4952 0.7008 0.142 Uiso 0.557(14) 1 calc R U P A 1
C3G C 1.168(2) 0.4802(14) 0.8311(12) 0.124(12) Uani 0.557(14) 1 d . . P A 1
H3G1 H 1.1675 0.4973 0.8765 0.186 Uiso 0.557(14) 1 calc R U P A 1
H3G2 H 1.2385 0.4581 0.8223 0.186 Uiso 0.557(14) 1 calc R U P A 1
H3G3 H 1.1110 0.4426 0.8237 0.186 Uiso 0.557(14) 1 calc R U P A 1
C11G C 1.1009(13) 0.5866(9) 0.7580(9) 0.034(4) Uani 0.443(14) 1 d . . P A 2
H11G H 1.0480 0.5690 0.7271 0.041 Uiso 0.443(14) 1 calc R U P A 2
C21G C 1.130(2) 0.4541(11) 0.7870(15) 0.074(9) Uani 0.443(14) 1 d . . P A 2
H21A H 1.0845 0.4384 0.8226 0.111 Uiso 0.443(14) 1 calc R U P A 2
H21B H 1.1998 0.4278 0.7906 0.111 Uiso 0.443(14) 1 calc R U P A 2
H21C H 1.0941 0.4419 0.7451 0.111 Uiso 0.443(14) 1 calc R U P A 2
C31G C 1.217(2) 0.5595(12) 0.8547(11) 0.098(10) Uani 0.443(14) 1 d . . P A 2
H31A H 1.2854 0.5320 0.8558 0.148 Uiso 0.443(14) 1 calc R U P A 2
H31B H 1.1755 0.5459 0.8929 0.148 Uiso 0.443(14) 1 calc R U P A 2
H31C H 1.2312 0.6135 0.8553 0.148 Uiso 0.443(14) 1 calc R U P A 2
O1H O 1.0307(4) 0.7656(3) 0.9399(3) 0.0605(16) Uani 1 1 d . . . . .
N1H N 1.1758(5) 0.7417(4) 1.0061(3) 0.0520(16) Uani 0.564(17) 1 d . . P B 1
C1H C 1.1164(10) 0.7420(8) 0.9489(7) 0.044(4) Uani 0.564(17) 1 d . . P B 1
H1H H 1.1497 0.7204 0.9124 0.053 Uiso 0.564(17) 1 calc R U P B 1
C2H C 1.2854(13) 0.7016(13) 1.0079(12) 0.093(7) Uani 0.564(17) 1 d . . P B 1
H2H1 H 1.2766 0.6506 1.0246 0.140 Uiso 0.564(17) 1 calc R U P B 1
H2H2 H 1.3366 0.7291 1.0365 0.140 Uiso 0.564(17) 1 calc R U P B 1
H2H3 H 1.3131 0.6995 0.9638 0.140 Uiso 0.564(17) 1 calc R U P B 1
C3H C 1.136(2) 0.7682(15) 1.0654(9) 0.112(9) Uani 0.564(17) 1 d . . P B 1
H3H1 H 1.0625 0.7873 1.0581 0.167 Uiso 0.564(17) 1 calc R U P B 1
H3H2 H 1.1831 0.8086 1.0822 0.167 Uiso 0.564(17) 1 calc R U P B 1
H3H3 H 1.1357 0.7271 1.0971 0.167 Uiso 0.564(17) 1 calc R U P B 1
N11H N 1.1758(5) 0.7417(4) 1.0061(3) 0.0520(16) Uani 0.436(17) 1 d . . P B 2
C11H C 1.0714(13) 0.7545(8) 0.9866(9) 0.034(5) Uani 0.436(17) 1 d . . P B 2
H11H H 1.0233 0.7537 1.0216 0.041 Uiso 0.436(17) 1 calc R U P B 2
C21H C 1.2630(17) 0.7378(17) 0.9612(14) 0.090(10) Uani 0.436(17) 1 d . . P B 2
H21D H 1.2864 0.6856 0.9568 0.135 Uiso 0.436(17) 1 calc R U P B 2
H21E H 1.3239 0.7683 0.9778 0.135 Uiso 0.436(17) 1 calc R U P B 2
H21F H 1.2378 0.7569 0.9185 0.135 Uiso 0.436(17) 1 calc R U P B 2
C31H C 1.207(2) 0.7478(18) 1.0803(11) 0.097(10) Uani 0.436(17) 1 d . . P B 2
H31D H 1.2507 0.7927 1.0881 0.145 Uiso 0.436(17) 1 calc R U P B 2
H31E H 1.2480 0.7033 1.0941 0.145 Uiso 0.436(17) 1 calc R U P B 2
H31F H 1.1406 0.7511 1.1052 0.145 Uiso 0.436(17) 1 calc R U 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
O2F Tb1 O1B 100.72(16) 4_675 .
O2F Tb1 O3B 81.71(14) 4_675 2_646
O1B Tb1 O3B 75.11(14) . 2_646
O2F Tb1 O1G 90.21(19) 4_675 .
O1B Tb1 O1G 143.82(15) . .
O3B Tb1 O1G 72.50(15) 2_646 .
O2F Tb1 O2E 77.83(15) 4_675 4_675
O1B Tb1 O2E 75.31(13) . 4_675
O3B Tb1 O2E 139.88(14) 2_646 4_675
O1G Tb1 O2E 140.87(15) . 4_675
O2F Tb1 O4D 85.20(14) 4_675 1_655
O1B Tb1 O4D 142.16(13) . 1_655
O3B Tb1 O4D 142.46(14) 2_646 1_655
O1G Tb1 O4D 72.52(15) . 1_655
O2E Tb1 O4D 69.47(13) 4_675 1_655
O2F Tb1 O1A 155.12(14) 4_675 .
O1B Tb1 O1A 83.21(15) . .
O3B Tb1 O1A 122.74(13) 2_646 .
O1G Tb1 O1A 101.07(17) . .
O2E Tb1 O1A 79.51(13) 4_675 .
O4D Tb1 O1A 77.33(13) 1_655 .
O2F Tb1 O2A 152.40(14) 4_675 .
O1B Tb1 O2A 75.98(13) . .
O3B Tb1 O2A 70.90(13) 2_646 .
O1G Tb1 O2A 78.55(16) . .
O2E Tb1 O2A 126.05(13) 4_675 .
O4D Tb1 O2A 114.49(12) 1_655 .
O1A Tb1 O2A 52.46(13) . .
O2F Tb1 C1A 175.66(17) 4_675 .
O1B Tb1 C1A 74.96(16) . .
O3B Tb1 C1A 96.55(16) 2_646 .
O1G Tb1 C1A 93.06(19) . .
O2E Tb1 C1A 101.28(16) 4_675 .
O4D Tb1 C1A 98.50(15) 1_655 .
O1A Tb1 C1A 26.20(14) . .
O2A Tb1 C1A 26.69(14) . .
O2B Tb2 O3A 79.78(15) . 3_777
O2B Tb2 O1H 138.92(16) . .
O3A Tb2 O1H 74.39(18) 3_777 .
O2B Tb2 O1D 77.73(12) . .
O3A Tb2 O1D 72.91(13) 3_777 .
O1H Tb2 O1D 122.53(17) . .
O2B Tb2 O2A 75.07(13) . .
O3A Tb2 O2A 84.84(14) 3_777 .
O1H Tb2 O2A 71.33(16) . .
O1D Tb2 O2A 147.42(13) . .
O2B Tb2 O4B 79.80(15) . 2_646
O3A Tb2 O4B 143.34(14) 3_777 2_646
O1H Tb2 O4B 137.54(17) . 2_646
O1D Tb2 O4B 73.19(13) . 2_646
O2A Tb2 O4B 118.43(12) . 2_646
O2B Tb2 O2C 141.97(13) . .
O3A Tb2 O2C 102.58(14) 3_777 .
O1H Tb2 O2C 75.68(15) . .
O1D Tb2 O2C 67.21(12) . .
O2A Tb2 O2C 142.77(13) . .
O4B Tb2 O2C 76.47(13) 2_646 .
O2B Tb2 O3B 73.70(13) . 2_646
O3A Tb2 O3B 145.97(13) 3_777 2_646
O1H Tb2 O3B 113.33(18) . 2_646
O1D Tb2 O3B 120.31(12) . 2_646
O2A Tb2 O3B 68.13(12) . 2_646
O4B Tb2 O3B 51.00(12) 2_646 2_646
O2C Tb2 O3B 111.45(13) . 2_646
O2B Tb2 O1C 141.83(14) . .
O3A Tb2 O1C 138.20(15) 3_777 .
O1H Tb2 O1C 68.39(17) . .
O1D Tb2 O1C 112.23(13) . .
O2A Tb2 O1C 100.25(13) . .
O4B Tb2 O1C 69.19(14) 2_646 .
O2C Tb2 O1C 50.59(12) . .
O3B Tb2 O1C 69.63(13) 2_646 .
O2B Tb2 C6B 74.98(15) . 2_646
O3A Tb2 C6B 154.18(15) 3_777 2_646
O1H Tb2 C6B 129.51(19) . 2_646
O1D Tb2 C6B 96.23(15) . 2_646
O2A Tb2 C6B 93.73(14) . 2_646
O4B Tb2 C6B 24.99(14) 2_646 2_646
O2C Tb2 C6B 94.11(14) . 2_646
O3B Tb2 C6B 26.02(14) 2_646 2_646
O1C Tb2 C6B 67.47(15) . 2_646
O2B Tb2 C1C 148.27(16) . .
O3A Tb2 C1C 124.03(16) 3_777 .
O1H Tb2 C1C 72.23(17) . .
O1D Tb2 C1C 89.13(14) . .
O2A Tb2 C1C 123.32(14) . .
O4B Tb2 C1C 68.72(15) 2_646 .
O2C Tb2 C1C 25.83(13) . .
O3B Tb2 C1C 88.96(14) 2_646 .
O1C Tb2 C1C 24.93(13) . .
C6B Tb2 C1C 77.97(16) 2_646 .
O2B Tb2 Tb3 115.64(9) . .
O3A Tb2 Tb3 74.40(10) 3_777 .
O1H Tb2 Tb3 87.52(14) . .
O1D Tb2 Tb3 38.60(8) . .
O2A Tb2 Tb3 153.79(9) . .
O4B Tb2 Tb3 87.59(9) 2_646 .
O2C Tb2 Tb3 34.89(9) . .
O3B Tb2 Tb3 136.69(8) 2_646 .
O1C Tb2 Tb3 85.47(8) . .
C6B Tb2 Tb3 111.93(11) 2_646 .
C1C Tb2 Tb3 60.65(11) . .
O4A Tb3 O1F 81.56(15) 3_777 .
O4A Tb3 O2C 79.47(14) 3_777 .
O1F Tb3 O2C 143.12(14) . .
O4A Tb3 O1E 148.35(14) 3_777 .
O1F Tb3 O1E 127.79(14) . .
O2C Tb3 O1E 80.58(13) . .
O4A Tb3 O2D 123.86(14) 3_777 .
O1F Tb3 O2D 78.27(16) . .
O2C Tb3 O2D 86.53(14) . .
O1E Tb3 O2D 78.90(14) . .
O4A Tb3 O4D 89.82(14) 3_777 4_676
O1F Tb3 O4D 78.46(14) . 4_676
O2C Tb3 O4D 132.47(12) . 4_676
O1E Tb3 O4D 85.79(13) . 4_676
O2D Tb3 O4D 134.94(13) . 4_676
O4A Tb3 O3D 75.36(15) 3_777 4_676
O1F Tb3 O3D 124.73(15) . 4_676
O2C Tb3 O3D 80.13(13) . 4_676
O1E Tb3 O3D 77.21(14) . 4_676
O2D Tb3 O3D 154.20(16) . 4_676
O4D Tb3 O3D 52.42(12) 4_676 4_676
O4A Tb3 O1D 72.26(13) 3_777 .
O1F Tb3 O1D 77.27(13) . .
O2C Tb3 O1D 66.94(12) . .
O1E Tb3 O1D 120.98(13) . .
O2D Tb3 O1D 52.40(12) . .
O4D Tb3 O1D 151.61(13) 4_676 .
O3D Tb3 O1D 137.06(12) 4_676 .
O4A Tb3 O2E 149.58(13) 3_777 .
O1F Tb3 O2E 76.53(13) . .
O2C Tb3 O2E 130.08(13) . .
O1E Tb3 O2E 51.82(12) . .
O2D Tb3 O2E 71.91(12) . .
O4D Tb3 O2E 65.41(12) 4_676 .
O3D Tb3 O2E 100.19(13) 4_676 .
O1D Tb3 O2E 121.89(12) . .
O4A Tb3 C1D 98.56(15) 3_777 .
O1F Tb3 C1D 75.51(16) . .
O2C Tb3 C1D 76.42(14) . .
O1E Tb3 C1D 100.32(15) . .
O2D Tb3 C1D 25.59(14) . .
O4D Tb3 C1D 151.08(14) 4_676 .
O3D Tb3 C1D 156.49(14) 4_676 .
O1D Tb3 C1D 26.84(13) . .
O2E Tb3 C1D 96.13(14) . .
O4A Tb3 C6D 81.60(15) 3_777 4_676
O1F Tb3 C6D 102.13(17) . 4_676
O2C Tb3 C6D 105.98(15) . 4_676
O1E Tb3 C6D 80.59(15) . 4_676
O2D Tb3 C6D 153.81(14) . 4_676
O4D Tb3 C6D 26.54(14) 4_676 4_676
O3D Tb3 C6D 25.88(14) 4_676 4_676
O1D Tb3 C6D 153.70(14) . 4_676
O2E Tb3 C6D 82.65(14) . 4_676
C1D Tb3 C6D 177.57(16) . 4_676
O4A Tb3 C1E 165.33(14) 3_777 .
O1F Tb3 C1E 102.04(16) . .
O2C Tb3 C1E 104.29(15) . .
O1E Tb3 C1E 25.77(14) . .
O2D Tb3 C1E 70.76(14) . .
O4D Tb3 C1E 77.15(14) 4_676 .
O3D Tb3 C1E 91.18(15) 4_676 .
O1D Tb3 C1E 122.35(13) . .
O2E Tb3 C1E 26.39(13) . .
C1D Tb3 C1E 96.10(15) . .
C6D Tb3 C1E 83.74(15) 4_676 .
C1A O1A Tb1 95.2(3) . .
C1A O2A Tb2 147.5(4) . .
C1A O2A Tb1 90.9(3) . .
Tb2 O2A Tb1 110.51(15) . .
C6A O3A Tb2 119.1(4) . 3_777
C6A O4A Tb3 140.9(4) . 3_777
O1A C1A O2A 119.5(5) . .
O1A C1A C2A 118.9(6) . .
O2A C1A C2A 121.4(5) . .
O1A C1A Tb1 58.6(3) . .
O2A C1A Tb1 62.4(3) . .
C2A C1A Tb1 163.1(5) . .
C3A C2A C1A 114.3(6) . .
C2A C3A C4A 110.0(6) . .
C5A C4A C3A 114.2(6) . .
C4A C5A C6A 114.6(6) . .
O4A C6A O3A 124.3(6) . .
O4A C6A C5A 117.8(5) . .
O3A C6A C5A 117.9(6) . .
C1B O1B Tb1 140.1(4) . .
C1B O2B Tb2 140.4(4) . .
C6B O3B Tb1 152.9(4) . 2_656
C6B O3B Tb2 90.5(3) . 2_656
Tb1 O3B Tb2 109.47(15) 2_656 2_656
C6B O4B Tb2 99.0(3) . 2_656
O1B C1B O2B 125.1(5) . .
O1B C1B C2B 117.4(5) . .
O2B C1B C2B 117.5(5) . .
C1B C2B C3B 115.7(6) . .
C2B C3B C4B 112.1(6) . .
C5B C4B C3B 113.3(6) . .
C6B C5B C4B 112.8(6) . .
O4B C6B O3B 119.5(5) . .
O4B C6B C5B 120.2(5) . .
O3B C6B C5B 120.3(5) . .
O4B C6B Tb2 56.0(3) . 2_656
O3B C6B Tb2 63.5(3) . 2_656
C5B C6B Tb2 175.7(5) . 2_656
C1C O1C Tb2 90.3(3) . .
C1C O2C Tb3 152.7(4) . .
C1C O2C Tb2 98.2(3) . .
Tb3 O2C Tb2 108.59(15) . .
O1C C1C O2C 120.0(5) . .
O1C C1C C2C 122.6(5) . .
O2C C1C C2C 117.4(5) . .
O1C C1C Tb2 64.7(3) . .
O2C C1C Tb2 55.9(3) . .
C2C C1C Tb2 167.3(4) . .
C1C C2C C3C 114.9(5) . .
C2C C3C C3C 113.2(7) . 3_767
C1D O1D Tb2 131.0(3) . .
C1D O1D Tb3 91.1(3) . .
Tb2 O1D Tb3 104.71(13) . .
C1D O2D Tb3 95.7(3) . .
C6D O3D Tb3 92.8(3) . 4_575
C6D O4D Tb1 137.8(4) . 1_455
C6D O4D Tb3 94.2(3) . 4_575
Tb1 O4D Tb3 111.33(14) 1_455 4_575
O2D C1D O1D 120.6(5) . .
O2D C1D C2D 120.5(5) . .
O1D C1D C2D 118.8(5) . .
O2D C1D Tb3 58.7(3) . .
O1D C1D Tb3 62.0(3) . .
C2D C1D Tb3 174.5(4) . .
C3D C2D C1D 114.2(5) . .
C2D C3D C4D 113.3(6) . .
C5D C4D C3D 113.1(6) . .
C4D C5D C6D 111.7(5) . .
O3D C6D O4D 120.5(5) . .
O3D C6D C5D 121.1(5) . .
O4D C6D C5D 118.4(5) . .
O3D C6D Tb3 61.3(3) . 4_575
O4D C6D Tb3 59.2(3) . 4_575
C5D C6D Tb3 177.1(5) . 4_575
C1E O1E Tb3 98.4(3) . .
C1E O2E Tb1 128.9(3) . 4_576
C1E O2E Tb3 88.3(3) . .
Tb1 O2E Tb3 107.81(14) 4_576 .
O1E C1E O2E 119.9(5) . .
O1E C1E C2E 119.2(5) . .
O2E C1E C2E 120.8(5) . .
O1E C1E Tb3 55.8(3) . .
O2E C1E Tb3 65.3(3) . .
C2E C1E Tb3 165.3(4) . .
C1E C2E C3E 113.7(5) . .
C3E C3E C2E 111.6(7) 3_667 .
C1F O1F Tb3 140.3(4) . .
C1F O2F Tb1 136.7(4) . 4_576
O1F C1F O2F 124.8(6) . .
O1F C1F C2F 117.7(6) . .
O2F C1F C2F 117.5(6) . .
C3F C2F C1F 116.6(7) . .
C2F C3F C3F 101.3(9) . 3_677
C1G O1G Tb1 161.2(8) . .
C11G O1G Tb1 125.0(9) . .
C1G N1G C3G 135.8(16) . .
C11G N1G C21G 125.5(15) . .
C11G N1G C31G 121.9(13) . .
C21G N1G C31G 110.9(14) . .
C1G N1G C2G 110.5(12) . .
C3G N1G C2G 113.6(15) . .
O1G C1G N1G 132.6(17) . .
N1G C11G O1G 126.6(16) . .
C11H O1H Tb2 150.1(10) . .
C1H O1H Tb2 146.3(9) . .
C1H N1H C3H 123.4(11) . .
C1H N1H C2H 118.2(11) . .
C3H N1H C2H 118.0(12) . .
O1H C1H N1H 127.3(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2F 2.290(4) 4_675
Tb1 O1B 2.330(4) .
Tb1 O3B 2.340(4) 2_646
Tb1 O1G 2.350(5) .
Tb1 O2E 2.375(4) 4_675
Tb1 O4D 2.417(4) 1_655
Tb1 O1A 2.425(4) .
Tb1 O2A 2.508(4) .
Tb1 C1A 2.830(6) .
Tb2 O2B 2.357(4) .
Tb2 O3A 2.377(4) 3_777
Tb2 O1H 2.397(5) .
Tb2 O1D 2.407(3) .
Tb2 O2A 2.411(4) .
Tb2 O4B 2.445(4) 2_646
Tb2 O2C 2.447(4) .
Tb2 O3B 2.607(4) 2_646
Tb2 O1C 2.643(4) .
Tb2 C6B 2.912(6) 2_646
Tb2 C1C 2.923(6) .
Tb2 Tb3 3.8972(11) .
Tb3 O4A 2.282(4) 3_777
Tb3 O1F 2.328(4) .
Tb3 O2C 2.352(4) .
Tb3 O1E 2.390(4) .
Tb3 O2D 2.443(4) .
Tb3 O4D 2.452(4) 4_676
Tb3 O3D 2.499(4) 4_676
Tb3 O1D 2.514(3) .
Tb3 O2E 2.597(4) .
Tb3 C1D 2.845(5) .
Tb3 C6D 2.846(5) 4_676
Tb3 C1E 2.858(5) .
O1A C1A 1.255(7) .
O2A C1A 1.271(7) .
O3A C6A 1.255(7) .
O3A Tb2 2.377(4) 3_777
O4A C6A 1.255(7) .
O4A Tb3 2.282(4) 3_777
C1A C2A 1.506(9) .
C2A C3A 1.473(9) .
C3A C4A 1.548(10) .
C4A C5A 1.449(9) .
C5A C6A 1.506(8) .
O1B C1B 1.249(6) .
O2B C1B 1.257(6) .
O3B C6B 1.278(7) .
O3B Tb1 2.340(4) 2_656
O3B Tb2 2.607(4) 2_656
O4B C6B 1.246(7) .
O4B Tb2 2.445(4) 2_656
C1B C2B 1.503(8) .
C2B C3B 1.520(9) .
C3B C4B 1.525(10) .
C4B C5B 1.508(10) .
C5B C6B 1.487(8) .
C6B Tb2 2.912(6) 2_656
O1C C1C 1.232(6) .
O2C C1C 1.287(7) .
C1C C2C 1.501(8) .
C2C C3C 1.512(8) .
C3C C3C 1.525(13) 3_767
O1D C1D 1.285(6) .
O2D C1D 1.235(6) .
O3D C6D 1.244(7) .
O3D Tb3 2.499(4) 4_575
O4D C6D 1.275(7) .
O4D Tb1 2.417(4) 1_455
O4D Tb3 2.452(4) 4_575
C1D C2D 1.509(7) .
C2D C3D 1.498(9) .
C3D C4D 1.534(8) .
C4D C5D 1.494(9) .
C5D C6D 1.514(8) .
C6D Tb3 2.846(5) 4_575
O1E C1E 1.256(6) .
O2E C1E 1.271(6) .
O2E Tb1 2.376(4) 4_576
C1E C2E 1.494(8) .
C2E C3E 1.525(8) .
C3E C3E 1.524(12) 3_667
O1F C1F 1.238(7) .
O2F C1F 1.254(7) .
O2F Tb1 2.290(4) 4_576
C1F C2F 1.508(9) .
C2F C3F 1.472(11) .
C3F C3F 1.682(19) 3_677
O1G C1G 1.142(13) .
O1G C11G 1.308(16) .
N1G C11G 1.210(17) .
N1G C1G 1.314(16) .
N1G C3G 1.31(2) .
N1G C21G 1.499(19) .
N1G C31G 1.536(19) .
N1G C2G 1.582(17) .
O1H C11H 1.062(16) .
O1H C1H 1.126(13) .
N1H C1H 1.335(14) .
N1H C3H 1.38(2) .
N1H C2H 1.500(17) .
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_3
_geom_torsion_site_symmetry_4
Tb1 O1A C1A O2A 14.5(6) . . .
Tb1 O1A C1A C2A -160.7(5) . . .
Tb2 O2A C1A O1A -146.5(5) . . .
Tb1 O2A C1A O1A -13.9(6) . . .
Tb2 O2A C1A C2A 28.5(11) . . .
Tb1 O2A C1A C2A 161.1(6) . . .
Tb2 O2A C1A Tb1 -132.6(7) . . .
O1A C1A C2A C3A -117.3(7) . . .
O2A C1A C2A C3A 67.7(9) . . .
Tb1 C1A C2A C3A 165.9(12) . . .
C1A C2A C3A C4A 178.0(6) . . .
C2A C3A C4A C5A 167.3(7) . . .
C3A C4A C5A C6A 179.5(6) . . .
Tb3 O4A C6A O3A 65.7(8) 3_777 . .
Tb3 O4A C6A C5A -114.3(6) 3_777 . .
Tb2 O3A C6A O4A -2.7(8) 3_777 . .
Tb2 O3A C6A C5A 177.3(4) 3_777 . .
C4A C5A C6A O4A -33.1(9) . . .
C4A C5A C6A O3A 146.9(7) . . .
Tb1 O1B C1B O2B -0.8(11) . . .
Tb1 O1B C1B C2B 178.6(5) . . .
Tb2 O2B C1B O1B -2.4(10) . . .
Tb2 O2B C1B C2B 178.1(4) . . .
O1B C1B C2B C3B -137.2(6) . . .
O2B C1B C2B C3B 42.3(9) . . .
C1B C2B C3B C4B 55.6(8) . . .
C2B C3B C4B C5B 168.4(6) . . .
C3B C4B C5B C6B -72.3(8) . . .
Tb2 O4B C6B O3B 1.7(6) 2_656 . .
Tb2 O4B C6B C5B -177.6(5) 2_656 . .
Tb1 O3B C6B O4B -139.9(6) 2_656 . .
Tb2 O3B C6B O4B -1.6(5) 2_656 . .
Tb1 O3B C6B C5B 39.4(11) 2_656 . .
Tb2 O3B C6B C5B 177.7(5) 2_656 . .
Tb1 O3B C6B Tb2 -138.3(8) 2_656 . 2_656
C4B C5B C6B O4B -53.4(8) . . .
C4B C5B C6B O3B 127.3(6) . . .
Tb2 O1C C1C O2C -9.0(6) . . .
Tb2 O1C C1C C2C 168.0(5) . . .
Tb3 O2C C1C O1C 178.5(5) . . .
Tb2 O2C C1C O1C 9.8(6) . . .
Tb3 O2C C1C C2C 1.4(11) . . .
Tb2 O2C C1C C2C -167.4(5) . . .
Tb3 O2C C1C Tb2 168.7(8) . . .
O1C C1C C2C C3C 30.5(9) . . .
O2C C1C C2C C3C -152.4(6) . . .
Tb2 C1C C2C C3C 152.3(16) . . .
C1C C2C C3C C3C 71.8(9) . . 3_767
Tb3 O2D C1D O1D 3.5(6) . . .
Tb3 O2D C1D C2D -173.6(5) . . .
Tb2 O1D C1D O2D 107.3(6) . . .
Tb3 O1D C1D O2D -3.4(6) . . .
Tb2 O1D C1D C2D -75.5(6) . . .
Tb3 O1D C1D C2D 173.8(5) . . .
Tb2 O1D C1D Tb3 110.7(4) . . .
O2D C1D C2D C3D -33.4(8) . . .
O1D C1D C2D C3D 149.4(6) . . .
C1D C2D C3D C4D -169.5(5) . . .
C2D C3D C4D C5D -57.8(8) . . .
C3D C4D C5D C6D -176.5(6) . . .
Tb3 O3D C6D O4D -0.4(6) 4_575 . .
Tb3 O3D C6D C5D 178.0(5) 4_575 . .
Tb1 O4D C6D O3D -128.2(5) 1_455 . .
Tb3 O4D C6D O3D 0.4(6) 4_575 . .
Tb1 O4D C6D C5D 53.3(8) 1_455 . .
Tb3 O4D C6D C5D -178.0(5) 4_575 . .
Tb1 O4D C6D Tb3 -128.7(5) 1_455 . 4_575
C4D C5D C6D O3D -83.3(8) . . .
C4D C5D C6D O4D 95.2(7) . . .
Tb3 O1E C1E O2E -13.2(5) . . .
Tb3 O1E C1E C2E 163.8(4) . . .
Tb1 O2E C1E O1E -99.6(5) 4_576 . .
Tb3 O2E C1E O1E 12.0(5) . . .
Tb1 O2E C1E C2E 83.4(6) 4_576 . .
Tb3 O2E C1E C2E -164.9(5) . . .
Tb1 O2E C1E Tb3 -111.7(3) 4_576 . .
O1E C1E C2E C3E -31.2(8) . . .
O2E C1E C2E C3E 145.8(5) . . .
Tb3 C1E C2E C3E 35(2) . . .
C1E C2E C3E C3E -65.0(9) . . 3_667
Tb3 O1F C1F O2F 33.4(12) . . .
Tb3 O1F C1F C2F -146.6(6) . . .
Tb1 O2F C1F O1F -16.0(12) 4_576 . .
Tb1 O2F C1F C2F 163.9(6) 4_576 . .
O1F C1F C2F C3F -25.8(12) . . .
O2F C1F C2F C3F 154.3(8) . . .
C1F C2F C3F C3F -75.7(11) . . 3_677
C11G O1G C1G N1G 23.0(14) . . .
Tb1 O1G C1G N1G 96(3) . . .
C11G N1G C1G O1G -25.5(15) . . .
C3G N1G C1G O1G -178(2) . . .
C21G N1G C1G O1G -96(5) . . .
C31G N1G C1G O1G 151(2) . . .
C2G N1G C1G O1G -2(2) . . .
C1G N1G C11G O1G 20.1(11) . . .
C3G N1G C11G O1G 126(5) . . .
C21G N1G C11G O1G 179.0(16) . . .
C31G N1G C11G O1G 16(2) . . .
C2G N1G C11G O1G -136.3(18) . . .
C1G O1G C11G N1G -22.9(13) . . .
Tb1 O1G C11G N1G 179.3(10) . . .
C11H O1H C1H N1H -14.0(13) . . .
Tb2 O1H C1H N1H -159.3(7) . . .
C3H N1H C1H O1H 3(2) . . .
C2H N1H C1H O1H 175.3(15) . . .
C2C C3C C3C C2C 180.000(3) . 3_767 3_767
C2E C3E C3E C2E 180.000(4) . 3_667 3_667
C2F C3F C3F C2F 180.000(3) . 3_677 3_677
