#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/07/2220786.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2220786
loop_
_publ_author_name
'Hao, Lujiang'
'Liu, Xia'
_publ_section_title
Tetrakis(μ-2,4-difluorobenzoato)bis[(2,2'-bipyridine)(2,4-difluorobenzoato)terbium(III)]
_journal_coeditor_code           HB2812
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m150
_journal_paper_doi               10.1107/S1600536808043936
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Tb2 (C7 H3 F2 O2)6 (C10 H8 N2)2]'
_chemical_formula_moiety         'C62 H34 F12 Tb2 N4 O12'
_chemical_formula_sum            'C62 H34 F12 N4 O12 Tb2'
_chemical_formula_weight         1572.77
_chemical_name_systematic
;
Tetrakis(μ-2,4-difluorobenzoato)bis[(2,2'-bipyridine)(2,4-
difluorobenzoato)terbium(III)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.99(2)
_cell_angle_beta                 102.90(2)
_cell_angle_gamma                113.58(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4010(10)
_cell_length_b                   12.1890(10)
_cell_length_c                   12.588(2)
_cell_measurement_reflns_used    5557
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.79
_cell_volume                     1451.5(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5557
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.572
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0345P)²+0.822P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                4813
_reflns_number_total             5557
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2812.cif
_cod_data_source_block           I
_cod_original_cell_volume        1451.5(3)
_cod_database_code               2220786
_cod_database_fobs_code          2220786
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb Tb1 0.39615(2) 0.804496(17) 0.439773(18) 0.03337(8) Uani d . 1 . .
F F1 0.8156(4) 1.1600(3) 0.2648(3) 0.0809(11) Uani d . 1 . .
F F2 0.3952(4) 0.7245(4) -0.0812(3) 0.1009(13) Uani d . 1 . .
F F3 0.7957(4) 0.9340(4) 0.8322(3) 0.0947(13) Uani d . 1 . .
F F4 1.1389(4) 1.1727(5) 0.6340(6) 0.136(2) Uani d . 1 . .
F F5 -0.1318(6) 0.5659(8) 0.2091(5) 0.131(3) Uani d P 0.672(10) . .
F F6 -0.0100(8) 0.6768(9) -0.1480(6) 0.155(4) Uani d P 0.672(10) . .
F F7 0.1797(11) 0.7301(13) 0.0303(10) 0.100(5) Uani d P 0.328(10) . .
F F8 -0.3317(10) 0.5145(17) 0.0353(11) 0.126(7) Uani d P 0.328(10) . .
O O1 0.1421(3) 0.6937(3) 0.3366(3) 0.0459(8) Uani d . 1 . .
O O2 0.2722(3) 0.7141(3) 0.2304(3) 0.0497(8) Uani d . 1 . .
O O3 0.6259(3) 1.0197(2) 0.5936(3) 0.0361(7) Uani d . 1 . .
O O4 0.5990(3) 0.8317(3) 0.5898(3) 0.0492(9) Uani d . 1 . .
O O5 0.5614(3) 0.8920(3) 0.3552(3) 0.0392(7) Uani d . 1 . .
O O6 0.6504(3) 1.1034(3) 0.3975(3) 0.0449(8) Uani d . 1 . .
N N1 0.2901(4) 0.6091(3) 0.4973(4) 0.0459(10) Uani d . 1 . .
N N2 0.4379(4) 0.6128(3) 0.3584(3) 0.0431(9) Uani d . 1 . .
C C1 0.5204(5) 0.6201(5) 0.2990(5) 0.0539(13) Uani d . 1 . .
H H1 0.5613 0.6955 0.2850 0.065 Uiso calc R 1 . .
C C2 0.5503(7) 0.5218(6) 0.2559(5) 0.0681(17) Uani d . 1 . .
H H2 0.6097 0.5311 0.2146 0.082 Uiso calc R 1 . .
C C3 0.4902(7) 0.4132(5) 0.2760(5) 0.0704(18) Uani d . 1 . .
H H3 0.5076 0.3455 0.2486 0.085 Uiso calc R 1 . .
C C4 0.4042(7) 0.4023(5) 0.3364(5) 0.0638(17) Uani d . 1 . .
H H4 0.3626 0.3270 0.3504 0.077 Uiso calc R 1 . .
C C5 0.3780(5) 0.5031(4) 0.3773(4) 0.0446(12) Uani d . 1 . .
C C6 0.6742(4) 0.9489(4) 0.6192(4) 0.0345(9) Uani d . 1 . .
C C7 0.8260(4) 1.0066(4) 0.6802(4) 0.0385(10) Uani d . 1 . .
C C8 0.9148(5) 1.0685(5) 0.6301(5) 0.0592(14) Uani d . 1 . .
H H8 0.8820 1.0786 0.5605 0.071 Uiso calc R 1 . .
C C9 1.0537(6) 1.1153(6) 0.6853(7) 0.0772(19) Uani d . 1 . .
C C10 1.1062(6) 1.1066(6) 0.7881(8) 0.086(2) Uani d . 1 . .
H H10 1.2005 1.1417 0.8242 0.103 Uiso calc R 1 . .
C C11 1.0191(6) 1.0454(7) 0.8389(6) 0.0792(19) Uani d . 1 . .
H H11 1.0532 1.0379 0.9095 0.095 Uiso calc R 1 . .
C C12 0.8806(5) 0.9955(5) 0.7837(5) 0.0525(13) Uani d . 1 . .
C C13 0.1575(5) 0.6867(4) 0.2397(4) 0.0385(10) Uani d . 1 . .
C C14 0.0384(5) 0.6523(4) 0.1333(4) 0.0400(10) Uani d . 1 . .
C C15 -0.0962(5) 0.5956(6) 0.1252(5) 0.0591(14) Uani d . 1 . .
H H15 -0.1166 0.5754 0.1877 0.071 Uiso d PR 0.328(10) . .
C C16 -0.2018(6) 0.5664(7) 0.0283(6) 0.0759(18) Uani d . 1 . .
H H16 -0.2913 0.5274 0.0267 0.091 Uiso d PR 0.672(10) . .
C C17 -0.1771(6) 0.5947(6) -0.0640(5) 0.0720(18) Uani d . 1 . .
H H17 -0.2484 0.5771 -0.1298 0.086 Uiso calc R 1 . .
C C18 -0.0453(7) 0.6497(6) -0.0581(5) 0.0716(17) Uani d . 1 . .
H H18 -0.0263 0.6684 -0.1216 0.086 Uiso d PR 0.328(10) . .
C C19 0.0606(6) 0.6780(5) 0.0380(5) 0.0569(14) Uani d . 1 . .
H H19 0.1495 0.7160 0.0381 0.068 Uiso d PR 0.672(10) . .
C C20 0.6086(4) 0.9903(4) 0.3307(4) 0.0363(10) Uani d . 1 . .
C C21 0.6107(5) 0.9677(4) 0.2092(4) 0.0418(11) Uani d . 1 . .
C C22 0.7081(6) 1.0524(5) 0.1800(5) 0.0531(13) Uani d . 1 . .
C C23 0.7024(7) 1.0276(6) 0.0660(6) 0.0652(16) Uani d . 1 . .
H H23 0.7709 1.0859 0.0489 0.078 Uiso calc R 1 . .
C C24 0.5965(7) 0.9176(6) -0.0230(5) 0.0681(16) Uani d . 1 . .
H H24 0.5903 0.9012 -0.1007 0.082 Uiso calc R 1 . .
C C25 0.5015(6) 0.8340(6) 0.0064(5) 0.0636(15) Uani d . 1 . .
C C26 0.5055(5) 0.8547(5) 0.1189(4) 0.0491(12) Uani d . 1 . .
H H26 0.4385 0.7939 0.1352 0.059 Uiso calc R 1 . .
C C27 0.2154(5) 0.6091(5) 0.5643(6) 0.0599(15) Uani d . 1 . .
H H27 0.2191 0.6867 0.6022 0.072 Uiso calc R 1 . .
C C28 0.1331(6) 0.5017(6) 0.5811(6) 0.0762(19) Uani d . 1 . .
H H28 0.0830 0.5066 0.6294 0.091 Uiso calc R 1 . .
C C29 0.1267(7) 0.3900(6) 0.5266(7) 0.087(2) Uani d . 1 . .
H H29 0.0705 0.3154 0.5355 0.105 Uiso calc R 1 . .
C C30 0.2036(7) 0.3854(5) 0.4570(6) 0.080(2) Uani d . 1 . .
H H30 0.1997 0.3077 0.4189 0.095 Uiso calc R 1 . .
C C31 0.2873(5) 0.4976(4) 0.4440(4) 0.0496(13) Uani d . 1 . .
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'
F F 0.0171 0.0103 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O6 Tb1 O3 2_676 2_676 75.94(10) ?
O6 Tb1 O5 2_676 . 132.93(10) ?
O3 Tb1 O5 2_676 . 74.31(10) ?
O6 Tb1 O2 2_676 . 132.91(12) ?
O3 Tb1 O2 2_676 . 78.22(11) ?
O5 Tb1 O2 . . 74.15(11) ?
O6 Tb1 O4 2_676 . 84.77(12) ?
O3 Tb1 O4 2_676 . 123.24(9) ?
O5 Tb1 O4 . . 82.03(11) ?
O2 Tb1 O4 . . 142.07(12) ?
O6 Tb1 O1 2_676 . 84.52(12) ?
O3 Tb1 O1 2_676 . 81.13(10) ?
O5 Tb1 O1 . . 125.07(10) ?
O2 Tb1 O1 . . 52.89(11) ?
O4 Tb1 O1 . . 149.70(10) ?
O6 Tb1 N1 2_676 . 79.45(12) ?
O3 Tb1 N1 2_676 . 145.03(12) ?
O5 Tb1 N1 . . 139.96(12) ?
O2 Tb1 N1 . . 101.74(13) ?
O4 Tb1 N1 . . 78.13(11) ?
O1 Tb1 N1 . . 72.07(11) ?
O6 Tb1 N2 2_676 . 138.65(12) ?
O3 Tb1 N2 2_676 . 145.39(12) ?
O5 Tb1 N2 . . 78.18(11) ?
O2 Tb1 N2 . . 74.34(12) ?
O4 Tb1 N2 . . 72.15(11) ?
O1 Tb1 N2 . . 98.32(12) ?
N1 Tb1 N2 . . 62.76(14) ?
O6 Tb1 O3 2_676 . 70.68(10) ?
O3 Tb1 O3 2_676 . 73.82(10) ?
O5 Tb1 O3 . . 66.47(10) ?
O2 Tb1 O3 . . 136.36(10) ?
O4 Tb1 O3 . . 49.42(9) ?
O1 Tb1 O3 . . 148.14(10) ?
N1 Tb1 O3 . . 120.33(11) ?
N2 Tb1 O3 . . 113.49(10) ?
C15 F5 H15 . . 8.4 ?
C18 F6 H18 . . 8.0 ?
C19 F7 H19 . . 11.1 ?
C16 F8 H16 . . 9.1 ?
C13 O1 Tb1 . . 90.5(3) ?
C13 O2 Tb1 . . 94.3(3) ?
C6 O3 Tb1 . 2_676 163.2(3) ?
C6 O3 Tb1 . . 88.4(2) ?
Tb1 O3 Tb1 2_676 . 106.18(10) ?
C6 O4 Tb1 . . 99.1(2) ?
C20 O5 Tb1 . . 136.0(3) ?
C20 O6 Tb1 . 2_676 134.3(3) ?
C27 N1 C31 . . 118.3(4) ?
C27 N1 Tb1 . . 119.6(3) ?
C31 N1 Tb1 . . 121.0(3) ?
C1 N2 C5 . . 117.7(4) ?
C1 N2 Tb1 . . 121.2(3) ?
C5 N2 Tb1 . . 121.1(3) ?
N2 C1 C2 . . 124.0(5) ?
N2 C1 H1 . . 118.0 ?
C2 C1 H1 . . 118.0 ?
C3 C2 C1 . . 117.5(6) ?
C3 C2 H2 . . 121.2 ?
C1 C2 H2 . . 121.2 ?
C2 C3 C4 . . 120.0(5) ?
C2 C3 H3 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C3 C4 C5 . . 120.1(5) ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
N2 C5 C4 . . 120.7(6) ?
N2 C5 C31 . . 116.6(4) ?
C4 C5 C31 . . 122.6(5) ?
O4 C6 O3 . . 120.9(4) ?
O4 C6 C7 . . 119.8(4) ?
O3 C6 C7 . . 119.2(4) ?
O4 C6 Tb1 . . 56.3(2) ?
O3 C6 Tb1 . . 66.3(2) ?
C7 C6 Tb1 . . 162.8(3) ?
C8 C7 C12 . . 118.1(5) ?
C8 C7 C6 . . 119.9(4) ?
C12 C7 C6 . . 122.0(4) ?
C7 C8 C9 . . 118.6(5) ?
C7 C8 H8 . . 120.7 ?
C9 C8 H8 . . 120.7 ?
F4 C9 C10 . . 119.3(6) ?
F4 C9 C8 . . 118.0(6) ?
C10 C9 C8 . . 122.7(6) ?
C9 C10 C11 . . 119.2(6) ?
C9 C10 H10 . . 120.4 ?
C11 C10 H10 . . 120.4 ?
C10 C11 C12 . . 118.9(6) ?
C10 C11 H11 . . 120.5 ?
C12 C11 H11 . . 120.5 ?
F3 C12 C11 . . 118.8(5) ?
F3 C12 C7 . . 118.7(4) ?
C11 C12 C7 . . 122.4(6) ?
O2 C13 O1 . . 121.4(4) ?
O2 C13 C14 . . 118.7(4) ?
O1 C13 C14 . . 119.8(4) ?
O2 C13 Tb1 . . 59.2(2) ?
O1 C13 Tb1 . . 62.9(2) ?
C14 C13 Tb1 . . 167.8(3) ?
C19 C14 C15 . . 115.9(5) ?
C19 C14 C13 . . 120.2(4) ?
C15 C14 C13 . . 123.9(4) ?
F5 C15 C16 . . 115.0(6) ?
F5 C15 C14 . . 122.3(5) ?
C16 C15 C14 . . 122.7(5) ?
F5 C15 H15 . . 3.3 ?
C16 C15 H15 . . 118.3 ?
C14 C15 H15 . . 119.0 ?
C17 C16 C15 . . 120.4(6) ?
C17 C16 F8 . . 123.5(7) ?
C15 C16 F8 . . 115.9(7) ?
C17 C16 H16 . . 120.1 ?
C15 C16 H16 . . 119.5 ?
F8 C16 H16 . . 4.6 ?
C16 C17 C18 . . 117.8(5) ?
C16 C17 H17 . . 121.1 ?
C18 C17 H17 . . 121.1 ?
C17 C18 F6 . . 122.6(6) ?
C17 C18 C19 . . 122.0(6) ?
F6 C18 C19 . . 115.3(7) ?
C17 C18 H18 . . 119.2 ?
F6 C18 H18 . . 3.7 ?
C19 C18 H18 . . 118.8 ?
F7 C19 C18 . . 114.6(7) ?
F7 C19 C14 . . 124.2(6) ?
C18 C19 C14 . . 121.1(5) ?
F7 C19 H19 . . 4.4 ?
C18 C19 H19 . . 119.0 ?
C14 C19 H19 . . 119.9 ?
O5 C20 O6 . . 125.8(4) ?
O5 C20 C21 . . 115.8(4) ?
O6 C20 C21 . . 118.4(4) ?
C22 C21 C26 . . 117.6(5) ?
C22 C21 C20 . . 124.3(4) ?
C26 C21 C20 . . 118.1(4) ?
F1 C22 C21 . . 119.9(5) ?
F1 C22 C23 . . 118.5(5) ?
C21 C22 C23 . . 121.5(5) ?
C24 C23 C22 . . 120.5(5) ?
C24 C23 H23 . . 119.7 ?
C22 C23 H23 . . 119.7 ?
C25 C24 C23 . . 117.6(5) ?
C25 C24 H24 . . 121.2 ?
C23 C24 H24 . . 121.2 ?
C24 C25 C26 . . 123.2(6) ?
C24 C25 F2 . . 118.2(5) ?
C26 C25 F2 . . 118.5(5) ?
C25 C26 C21 . . 119.4(5) ?
C25 C26 H26 . . 120.3 ?
C21 C26 H26 . . 120.3 ?
N1 C27 C28 . . 124.0(6) ?
N1 C27 H27 . . 118.0 ?
C28 C27 H27 . . 118.0 ?
C29 C28 C27 . . 118.4(7) ?
C29 C28 H28 . . 120.8 ?
C27 C28 H28 . . 120.8 ?
C28 C29 C30 . . 119.8(5) ?
C28 C29 H29 . . 120.1 ?
C30 C29 H29 . . 120.1 ?
C29 C30 C31 . . 119.7(6) ?
C29 C30 H30 . . 120.2 ?
C31 C30 H30 . . 120.2 ?
N1 C31 C30 . . 119.9(6) ?
N1 C31 C5 . . 116.7(4) ?
C30 C31 C5 . . 123.4(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tb1 N1 . 2.565(3) y
Tb1 N2 . 2.586(4) y
Tb1 O6 2_676 2.364(3) y
Tb1 O3 2_676 2.377(3) y
Tb1 O5 . 2.379(3) y
Tb1 O2 . 2.418(3) y
Tb1 O4 . 2.481(3) y
Tb1 O1 . 2.498(3) y
Tb1 O3 . 2.696(3) y
F1 C22 . 1.347(6) ?
F2 C25 . 1.365(7) ?
F3 C12 . 1.331(6) ?
F4 C9 . 1.344(7) ?
F5 C15 . 1.294(7) ?
F5 H15 . 0.3691 ?
F6 C18 . 1.353(9) ?
F6 H18 . 0.4290 ?
F7 C19 . 1.286(11) ?
F7 H19 . 0.3654 ?
F8 C16 . 1.392(13) ?
F8 H16 . 0.4706 ?
O1 C13 . 1.258(6) ?
O2 C13 . 1.254(6) ?
O3 C6 . 1.259(5) ?
O3 Tb1 2_676 2.377(3) ?
O4 C6 . 1.239(5) ?
O5 C20 . 1.248(5) ?
O6 C20 . 1.252(5) ?
O6 Tb1 2_676 2.364(3) ?
N1 C27 . 1.325(7) ?
N1 C31 . 1.347(6) ?
N2 C1 . 1.315(7) ?
N2 C5 . 1.345(6) ?
C1 C2 . 1.394(7) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.342(9) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.354(9) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.385(7) ?
C4 H4 . 0.9300 ?
C5 C31 . 1.463(8) ?
C6 C7 . 1.501(6) ?
C7 C8 . 1.377(7) ?
C7 C12 . 1.377(7) ?
C8 C9 . 1.382(8) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.347(10) ?
C10 C11 . 1.367(10) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.373(8) ?
C11 H11 . 0.9300 ?
C13 C14 . 1.508(6) ?
C14 C19 . 1.363(7) ?
C14 C15 . 1.374(7) ?
C15 C16 . 1.362(7) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.346(9) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.354(9) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.362(8) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
C20 C21 . 1.495(6) ?
C21 C22 . 1.372(6) ?
C21 C26 . 1.393(7) ?
C22 C23 . 1.375(7) ?
C23 C24 . 1.373(9) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.351(8) ?
C24 H24 . 0.9300 ?
C25 C26 . 1.364(7) ?
C26 H26 . 0.9300 ?
C27 C28 . 1.371(7) ?
C27 H27 . 0.9300 ?
C28 C29 . 1.332(10) ?
C28 H28 . 0.9300 ?
C29 C30 . 1.378(10) ?
C29 H29 . 0.9300 ?
C30 C31 . 1.394(7) ?
C30 H30 . 0.9300 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O6 Tb1 O1 C13 2_676 . . . 153.0(3) ?
O3 Tb1 O1 C13 2_676 . . . 76.4(2) ?
O5 Tb1 O1 C13 . . . . 12.8(3) ?
O2 Tb1 O1 C13 . . . . -5.5(2) ?
O4 Tb1 O1 C13 . . . . -137.2(3) ?
N1 Tb1 O1 C13 . . . . -126.3(3) ?
N2 Tb1 O1 C13 . . . . -68.6(3) ?
O3 Tb1 O1 C13 . . . . 114.7(3) ?
C6 Tb1 O1 C13 . . . . 167.7(3) ?
O6 Tb1 O2 C13 2_676 . . . -24.4(3) ?
O3 Tb1 O2 C13 2_676 . . . -82.2(3) ?
O5 Tb1 O2 C13 . . . . -159.0(3) ?
O4 Tb1 O2 C13 . . . . 147.7(2) ?
O1 Tb1 O2 C13 . . . . 5.5(2) ?
N1 Tb1 O2 C13 . . . . 62.0(3) ?
N2 Tb1 O2 C13 . . . . 119.1(3) ?
O3 Tb1 O2 C13 . . . . -133.1(2) ?
C6 Tb1 O2 C13 . . . . -171.4(2) ?
O6 Tb1 O3 C6 2_676 . . . 108.2(3) ?
O3 Tb1 O3 C6 2_676 . . . -171.4(3) ?
O5 Tb1 O3 C6 . . . . -91.8(3) ?
O2 Tb1 O3 C6 . . . . -119.2(3) ?
O4 Tb1 O3 C6 . . . . 8.2(2) ?
O1 Tb1 O3 C6 . . . . 149.0(2) ?
N1 Tb1 O3 C6 . . . . 43.6(3) ?
N2 Tb1 O3 C6 . . . . -27.5(3) ?
C13 Tb1 O3 C6 . . . . -158.5(3) ?
O6 Tb1 O3 Tb1 2_676 . . 2_676 -80.42(12) ?
O3 Tb1 O3 Tb1 2_676 . . 2_676 0.0 ?
O5 Tb1 O3 Tb1 . . . 2_676 79.59(12) ?
O2 Tb1 O3 Tb1 . . . 2_676 52.25(19) ?
O4 Tb1 O3 Tb1 . . . 2_676 179.60(19) ?
O1 Tb1 O3 Tb1 . . . 2_676 -39.5(2) ?
N1 Tb1 O3 Tb1 . . . 2_676 -144.96(13) ?
N2 Tb1 O3 Tb1 . . . 2_676 143.93(13) ?
C13 Tb1 O3 Tb1 . . . 2_676 12.9(3) ?
C6 Tb1 O3 Tb1 . . . 2_676 171.4(3) ?
O6 Tb1 O4 C6 2_676 . . . -77.4(3) ?
O3 Tb1 O4 C6 2_676 . . . -8.0(3) ?
O5 Tb1 O4 C6 . . . . 57.3(3) ?
O2 Tb1 O4 C6 . . . . 108.4(3) ?
O1 Tb1 O4 C6 . . . . -147.1(3) ?
N1 Tb1 O4 C6 . . . . -157.7(3) ?
N2 Tb1 O4 C6 . . . . 137.4(3) ?
O3 Tb1 O4 C6 . . . . -8.4(3) ?
C13 Tb1 O4 C6 . . . . 151.6(4) ?
O6 Tb1 O5 C20 2_676 . . . -43.3(5) ?
O3 Tb1 O5 C20 2_676 . . . 9.4(4) ?
O2 Tb1 O5 C20 . . . . 91.3(4) ?
O4 Tb1 O5 C20 . . . . -118.5(4) ?
O1 Tb1 O5 C20 . . . . 76.2(4) ?
N1 Tb1 O5 C20 . . . . -179.2(4) ?
N2 Tb1 O5 C20 . . . . 168.2(4) ?
O3 Tb1 O5 C20 . . . . -69.5(4) ?
C13 Tb1 O5 C20 . . . . 82.0(4) ?
C6 Tb1 O5 C20 . . . . -96.6(4) ?
O6 Tb1 N1 C27 2_676 . . . 18.5(4) ?
O3 Tb1 N1 C27 2_676 . . . -27.2(5) ?
O5 Tb1 N1 C27 . . . . 167.3(3) ?
O2 Tb1 N1 C27 . . . . -113.4(4) ?
O4 Tb1 N1 C27 . . . . 105.4(4) ?
O1 Tb1 N1 C27 . . . . -69.0(4) ?
N2 Tb1 N1 C27 . . . . -178.8(4) ?
O3 Tb1 N1 C27 . . . . 78.6(4) ?
C13 Tb1 N1 C27 . . . . -90.2(4) ?
C6 Tb1 N1 C27 . . . . 96.1(4) ?
O6 Tb1 N1 C31 2_676 . . . -173.7(4) ?
O3 Tb1 N1 C31 2_676 . . . 140.5(3) ?
O5 Tb1 N1 C31 . . . . -24.9(4) ?
O2 Tb1 N1 C31 . . . . 54.3(3) ?
O4 Tb1 N1 C31 . . . . -86.9(3) ?
O1 Tb1 N1 C31 . . . . 98.7(3) ?
N2 Tb1 N1 C31 . . . . -11.0(3) ?
O3 Tb1 N1 C31 . . . . -113.6(3) ?
C13 Tb1 N1 C31 . . . . 77.5(3) ?
C6 Tb1 N1 C31 . . . . -96.1(3) ?
O6 Tb1 N2 C1 2_676 . . . -147.6(3) ?
O3 Tb1 N2 C1 2_676 . . . 34.8(4) ?
O5 Tb1 N2 C1 . . . . -3.0(4) ?
O2 Tb1 N2 C1 . . . . 73.6(4) ?
O4 Tb1 N2 C1 . . . . -88.3(4) ?
O1 Tb1 N2 C1 . . . . 121.2(4) ?
N1 Tb1 N2 C1 . . . . -173.9(4) ?
O3 Tb1 N2 C1 . . . . -60.6(4) ?
C13 Tb1 N2 C1 . . . . 96.6(4) ?
C6 Tb1 N2 C1 . . . . -72.0(4) ?
O6 Tb1 N2 C5 2_676 . . . 31.1(4) ?
O3 Tb1 N2 C5 2_676 . . . -146.5(3) ?
O5 Tb1 N2 C5 . . . . 175.7(3) ?
O2 Tb1 N2 C5 . . . . -107.7(3) ?
O4 Tb1 N2 C5 . . . . 90.3(3) ?
O1 Tb1 N2 C5 . . . . -60.1(3) ?
N1 Tb1 N2 C5 . . . . 4.8(3) ?
O3 Tb1 N2 C5 . . . . 118.1(3) ?
C13 Tb1 N2 C5 . . . . -84.8(3) ?
C6 Tb1 N2 C5 . . . . 106.7(3) ?
C5 N2 C1 C2 . . . . -0.7(7) ?
Tb1 N2 C1 C2 . . . . 178.1(4) ?
N2 C1 C2 C3 . . . . 0.4(9) ?
C1 C2 C3 C4 . . . . 0.0(9) ?
C2 C3 C4 C5 . . . . 0.0(9) ?
C1 N2 C5 C4 . . . . 0.7(7) ?
Tb1 N2 C5 C4 . . . . -178.1(3) ?
C1 N2 C5 C31 . . . . 179.7(4) ?
Tb1 N2 C5 C31 . . . . 1.0(5) ?
C3 C4 C5 N2 . . . . -0.4(7) ?
C3 C4 C5 C31 . . . . -179.3(5) ?
Tb1 O4 C6 O3 . . . . 16.1(5) ?
Tb1 O4 C6 C7 . . . . -160.3(3) ?
Tb1 O3 C6 O4 2_676 . . . -165.0(7) ?
Tb1 O3 C6 O4 . . . . -14.6(4) ?
Tb1 O3 C6 C7 2_676 . . . 11.5(12) ?
Tb1 O3 C6 C7 . . . . 161.8(4) ?
Tb1 O3 C6 Tb1 2_676 . . . -150.4(10) ?
O6 Tb1 C6 O4 2_676 . . . 99.4(3) ?
O3 Tb1 C6 O4 2_676 . . . 173.3(3) ?
O5 Tb1 C6 O4 . . . . -117.2(3) ?
O2 Tb1 C6 O4 . . . . -104.6(3) ?
O1 Tb1 C6 O4 . . . . 84.5(5) ?
N1 Tb1 C6 O4 . . . . 22.3(3) ?
N2 Tb1 C6 O4 . . . . -40.1(3) ?
O3 Tb1 C6 O4 . . . . 164.9(5) ?
C13 Tb1 C6 O4 . . . . -124.1(6) ?
O6 Tb1 C6 O3 2_676 . . . -65.6(2) ?
O3 Tb1 C6 O3 2_676 . . . 8.3(3) ?
O5 Tb1 C6 O3 . . . . 77.9(2) ?
O2 Tb1 C6 O3 . . . . 90.5(3) ?
O4 Tb1 C6 O3 . . . . -164.9(5) ?
O1 Tb1 C6 O3 . . . . -80.4(4) ?
N1 Tb1 C6 O3 . . . . -142.7(2) ?
N2 Tb1 C6 O3 . . . . 155.0(3) ?
C13 Tb1 C6 O3 . . . . 70.9(7) ?
O6 Tb1 C6 C7 2_676 . . . -178.3(10) ?
O3 Tb1 C6 C7 2_676 . . . -104.4(9) ?
O5 Tb1 C6 C7 . . . . -34.8(9) ?
O2 Tb1 C6 C7 . . . . -22.2(10) ?
O4 Tb1 C6 C7 . . . . 82.4(10) ?
O1 Tb1 C6 C7 . . . . 166.9(8) ?
N1 Tb1 C6 C7 . . . . 104.6(9) ?
N2 Tb1 C6 C7 . . . . 42.3(9) ?
O3 Tb1 C6 C7 . . . . -112.7(10) ?
C13 Tb1 C6 C7 . . . . -41.8(13) ?
O4 C6 C7 C8 . . . . 119.8(5) ?
O3 C6 C7 C8 . . . . -56.7(6) ?
Tb1 C6 C7 C8 . . . . 47.9(11) ?
O4 C6 C7 C12 . . . . -57.6(6) ?
O3 C6 C7 C12 . . . . 126.0(5) ?
Tb1 C6 C7 C12 . . . . -129.5(9) ?
C12 C7 C8 C9 . . . . 0.5(8) ?
C6 C7 C8 C9 . . . . -176.9(5) ?
C7 C8 C9 F4 . . . . 178.5(5) ?
C7 C8 C9 C10 . . . . -2.2(10) ?
F4 C9 C10 C11 . . . . -178.5(6) ?
C8 C9 C10 C11 . . . . 2.2(11) ?
C9 C10 C11 C12 . . . . -0.4(10) ?
C10 C11 C12 F3 . . . . 178.8(6) ?
C10 C11 C12 C7 . . . . -1.2(10) ?
C8 C7 C12 F3 . . . . -178.9(5) ?
C6 C7 C12 F3 . . . . -1.5(7) ?
C8 C7 C12 C11 . . . . 1.1(8) ?
C6 C7 C12 C11 . . . . 178.6(5) ?
Tb1 O2 C13 O1 . . . . -10.3(4) ?
Tb1 O2 C13 C14 . . . . 166.2(3) ?
Tb1 O1 C13 O2 . . . . 9.9(4) ?
Tb1 O1 C13 C14 . . . . -166.5(3) ?
O6 Tb1 C13 O2 2_676 . . . 161.4(2) ?
O3 Tb1 C13 O2 2_676 . . . 91.6(3) ?
O5 Tb1 C13 O2 . . . . 20.4(3) ?
O4 Tb1 C13 O2 . . . . -70.9(5) ?
O1 Tb1 C13 O2 . . . . -170.2(4) ?
N1 Tb1 C13 O2 . . . . -120.1(3) ?
N2 Tb1 C13 O2 . . . . -57.3(3) ?
O3 Tb1 C13 O2 . . . . 78.8(3) ?
C6 Tb1 C13 O2 . . . . 27.0(7) ?
O6 Tb1 C13 O1 2_676 . . . -28.4(3) ?
O3 Tb1 C13 O1 2_676 . . . -98.2(3) ?
O5 Tb1 C13 O1 . . . . -169.4(2) ?
O2 Tb1 C13 O1 . . . . 170.2(4) ?
O4 Tb1 C13 O1 . . . . 99.3(4) ?
N1 Tb1 C13 O1 . . . . 50.1(3) ?
N2 Tb1 C13 O1 . . . . 112.8(3) ?
O3 Tb1 C13 O1 . . . . -111.0(3) ?
C6 Tb1 C13 O1 . . . . -162.9(5) ?
O6 Tb1 C13 C14 2_676 . . . 77.8(17) ?
O3 Tb1 C13 C14 2_676 . . . 8.0(17) ?
O5 Tb1 C13 C14 . . . . -63.2(17) ?
O2 Tb1 C13 C14 . . . . -83.6(17) ?
O4 Tb1 C13 C14 . . . . -154.5(15) ?
O1 Tb1 C13 C14 . . . . 106.2(17) ?
N1 Tb1 C13 C14 . . . . 156.3(17) ?
N2 Tb1 C13 C14 . . . . -140.9(17) ?
O3 Tb1 C13 C14 . . . . -4.8(18) ?
C6 Tb1 C13 C14 . . . . -57(2) ?
O2 C13 C14 C19 . . . . -14.5(6) ?
O1 C13 C14 C19 . . . . 162.0(4) ?
Tb1 C13 C14 C19 . . . . 62.3(18) ?
O2 C13 C14 C15 . . . . 166.1(5) ?
O1 C13 C14 C15 . . . . -17.4(7) ?
Tb1 C13 C14 C15 . . . . -117.2(16) ?
C19 C14 C15 F5 . . . . 179.9(7) ?
C13 C14 C15 F5 . . . . -0.6(10) ?
C19 C14 C15 C16 . . . . 0.1(9) ?
C13 C14 C15 C16 . . . . 179.5(5) ?
F5 C15 C16 C17 . . . . 178.9(7) ?
C14 C15 C16 C17 . . . . -1.2(10) ?
F5 C15 C16 F8 . . . . 2.9(13) ?
C14 C15 C16 F8 . . . . -177.2(10) ?
C15 C16 C17 C18 . . . . 1.6(10) ?
F8 C16 C17 C18 . . . . 177.3(11) ?
C16 C17 C18 F6 . . . . 177.0(8) ?
C16 C17 C18 C19 . . . . -1.0(10) ?
C17 C18 C19 F7 . . . . -179.9(10) ?
F6 C18 C19 F7 . . . . 1.9(12) ?
C17 C18 C19 C14 . . . . -0.1(10) ?
F6 C18 C19 C14 . . . . -178.3(7) ?
C15 C14 C19 F7 . . . . -179.7(10) ?
C13 C14 C19 F7 . . . . 0.9(12) ?
C15 C14 C19 C18 . . . . 0.6(8) ?
C13 C14 C19 C18 . . . . -178.9(5) ?
Tb1 O5 C20 O6 . . . . 47.9(6) ?
Tb1 O5 C20 C21 . . . . -130.2(4) ?
Tb1 O6 C20 O5 2_676 . . . -24.7(7) ?
Tb1 O6 C20 C21 2_676 . . . 153.4(3) ?
O5 C20 C21 C22 . . . . -147.8(5) ?
O6 C20 C21 C22 . . . . 33.9(7) ?
O5 C20 C21 C26 . . . . 33.5(6) ?
O6 C20 C21 C26 . . . . -144.8(4) ?
C26 C21 C22 F1 . . . . -176.8(5) ?
C20 C21 C22 F1 . . . . 4.6(7) ?
C26 C21 C22 C23 . . . . 0.4(8) ?
C20 C21 C22 C23 . . . . -178.3(5) ?
F1 C22 C23 C24 . . . . 178.5(5) ?
C21 C22 C23 C24 . . . . 1.3(9) ?
C22 C23 C24 C25 . . . . -1.9(9) ?
C23 C24 C25 C26 . . . . 0.8(9) ?
C23 C24 C25 F2 . . . . 179.6(5) ?
C24 C25 C26 C21 . . . . 0.9(9) ?
F2 C25 C26 C21 . . . . -178.0(5) ?
C22 C21 C26 C25 . . . . -1.5(7) ?
C20 C21 C26 C25 . . . . 177.3(5) ?
C31 N1 C27 C28 . . . . -1.3(8) ?
Tb1 N1 C27 C28 . . . . 166.8(4) ?
N1 C27 C28 C29 . . . . -0.4(9) ?
C27 C28 C29 C30 . . . . 1.1(10) ?
C28 C29 C30 C31 . . . . -0.2(10) ?
C27 N1 C31 C30 . . . . 2.2(7) ?
Tb1 N1 C31 C30 . . . . -165.7(4) ?
C27 N1 C31 C5 . . . . -175.9(4) ?
Tb1 N1 C31 C5 . . . . 16.1(5) ?
C29 C30 C31 N1 . . . . -1.5(8) ?
C29 C30 C31 C5 . . . . 176.5(5) ?
N2 C5 C31 N1 . . . . -11.0(6) ?
C4 C5 C31 N1 . . . . 168.0(4) ?
N2 C5 C31 C30 . . . . 170.9(5) ?
C4 C5 C31 C30 . . . . -10.1(7) ?
