#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/53/2215343.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_2215343
loop_
_publ_author_name
'Xia, Hai-Tao'
'Liu, Yu-Fen'
'Wang, Da-Qi'
'Yang, Shu-Ping'
_publ_section_title
;
 Hexakis(μ-naphthalene-1-acetato)bis[(1,10-phenanthroline)terbium(III)]
 N,N-dimethylformamide disolvate
;
_journal_coeditor_code           AT2407
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2624
_journal_page_last               m2624
_journal_paper_doi               10.1107/S1600536807047095
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Tb2 (C12 H9 O2)6 (C12 H8 N2)2] , 2C3 H7 N O'
_chemical_formula_moiety         'C96 H70 Tb2 N4 O12 , 2C3 H7 N O'
_chemical_formula_sum            'C102 H84 N6 O14 Tb2'
_chemical_formula_weight         1935.59
_chemical_name_systematic
;
Hexakis(μ-naphthalene-1-acetato)bis[(1,10-phenanthroline)terbium(III)]
N,N-dimethylformamide disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.584(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4619(16)
_cell_length_b                   15.086(2)
_cell_length_c                   22.166(2)
_cell_measurement_reflns_used    6504
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.308
_cell_measurement_theta_min      2.419
_cell_volume                     4375.7(9)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_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  0.1927
_diffrn_reflns_av_sigmaI/netI    0.1529
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21422
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.8245
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.202
_refine_diff_density_min         -2.724
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0648P)²+17.4888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1965
_reflns_number_gt                4674
_reflns_number_total             7389
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2407.cif
_cod_data_source_block           I
_cod_original_cell_volume        4375.6(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215343
_cod_database_fobs_code          2215343
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Tb Tb1 0.38253(3) 0.43006(3) 1.01126(2) 0.03377(19) Uani d . 1
N N1 0.2316(6) 0.4439(6) 1.0645(4) 0.043(2) Uani d . 1
N N2 0.2134(6) 0.3634(6) 0.9529(4) 0.045(2) Uani d . 1
N N3 0.3685(12) 0.3365(11) 0.2523(6) 0.089(4) Uani d . 1
O O1 0.4406(4) 0.5791(5) 0.9788(3) 0.0361(15) Uani d . 1
O O2 0.2766(5) 0.5556(5) 0.9603(3) 0.0419(17) Uani d . 1
O O3 0.4044(5) 0.4251(5) 0.9092(3) 0.0405(16) Uani d . 1
O O4 0.5497(5) 0.4868(5) 0.8977(3) 0.0426(18) Uani d . 1
O O5 0.4125(6) 0.2737(5) 0.9880(4) 0.052(2) Uani d . 1
O O6 0.4021(6) 0.3048(5) 1.0822(4) 0.055(2) Uani d . 1
O O7 0.2327(12) 0.2428(11) 0.2366(8) 0.141(5) Uani d . 1
C C1 0.3510(7) 0.5982(7) 0.9521(5) 0.041(3) Uani d . 1
C C2 0.3350(8) 0.6742(9) 0.9067(6) 0.058(3) Uani d . 1
H H2A 0.3780 0.6646 0.8778 0.070 Uiso calc R 1
H H2B 0.3583 0.7282 0.9295 0.070 Uiso calc R 1
C C3 0.2269(9) 0.6888(9) 0.8697(6) 0.056(3) Uani d . 1
C C4 0.1766(10) 0.7654(9) 0.8805(6) 0.067(4) Uani d . 1
H H4 0.2098 0.8065 0.9096 0.080 Uiso calc R 1
C C5 0.0754(11) 0.7809(11) 0.8473(7) 0.076(4) Uani d . 1
H H5 0.0416 0.8312 0.8563 0.091 Uiso calc R 1
C C6 0.0274(10) 0.7262(11) 0.8041(7) 0.073(4) Uani d . 1
H H6 -0.0388 0.7391 0.7822 0.088 Uiso calc R 1
C C7 0.0743(10) 0.6496(11) 0.7907(7) 0.069(4) Uani d . 1
C C8 0.1752(9) 0.6298(9) 0.8235(6) 0.059(3) Uani d . 1
C C9 0.2205(12) 0.5507(11) 0.8086(7) 0.076(4) Uani d . 1
H H9 0.2872 0.5378 0.8297 0.092 Uiso calc R 1
C C10 0.1713(13) 0.4931(13) 0.7650(8) 0.095(5) Uani d . 1
H H10 0.2021 0.4410 0.7563 0.114 Uiso calc R 1
C C11 0.0680(13) 0.5166(14) 0.7324(8) 0.097(5) Uani d . 1
H H11 0.0321 0.4781 0.7023 0.116 Uiso calc R 1
C C12 0.0236(13) 0.5897(13) 0.7436(8) 0.086(5) Uani d . 1
H H12 -0.0419 0.6029 0.7207 0.103 Uiso calc R 1
C C13 0.4733(7) 0.4365(7) 0.8814(5) 0.041(2) Uani d . 1
C C14 0.4627(9) 0.3853(9) 0.8215(6) 0.055(3) Uani d . 1
H H14A 0.4148 0.3372 0.8213 0.066 Uiso calc R 1
H H14B 0.4328 0.4244 0.7873 0.066 Uiso calc R 1
C C15 0.5584(10) 0.3469(9) 0.8091(6) 0.061(3) Uani d . 1
C C16 0.5901(10) 0.3733(10) 0.7564(6) 0.069(4) Uani d . 1
H H16 0.5521 0.4155 0.7303 0.082 Uiso calc R 1
C C17 0.6774(11) 0.3380(11) 0.7418(7) 0.077(4) Uani d . 1
H H17 0.6988 0.3583 0.7073 0.092 Uiso calc R 1
C C18 0.7313(11) 0.2728(11) 0.7791(7) 0.075(4) Uani d . 1
H H18 0.7897 0.2494 0.7696 0.090 Uiso calc R 1
C C19 0.7003(10) 0.2412(10) 0.8305(7) 0.070(4) Uani d . 1
C C20 0.6141(9) 0.2793(9) 0.8467(6) 0.061(3) Uani d . 1
C C21 0.5847(11) 0.2480(10) 0.8994(7) 0.067(4) Uani d . 1
H H21 0.5300 0.2742 0.9117 0.081 Uiso calc R 1
C C22 0.6357(12) 0.1798(11) 0.9324(8) 0.083(4) Uani d . 1
H H22 0.6131 0.1582 0.9662 0.100 Uiso calc R 1
C C23 0.7221(13) 0.1400(12) 0.9176(9) 0.091(5) Uani d . 1
H H23 0.7569 0.0941 0.9415 0.110 Uiso calc R 1
C C24 0.7519(12) 0.1707(11) 0.8680(8) 0.081(5) Uani d . 1
H H24 0.8085 0.1451 0.8576 0.098 Uiso calc R 1
C C25 0.4093(9) 0.2508(8) 1.0418(7) 0.054(3) Uani d . 1
C C26 0.4137(11) 0.1524(9) 1.0563(7) 0.073(4) Uani d . 1
H H26A 0.4806 0.1296 1.0550 0.088 Uiso calc R 1
H H26B 0.4041 0.1433 1.0978 0.088 Uiso calc R 1
C C27 0.3350(13) 0.1034(11) 1.0117(8) 0.079(4) Uani d . 1
C C28 0.3615(15) 0.0497(11) 0.9671(9) 0.089(5) Uani d . 1
H H28 0.4296 0.0429 0.9659 0.107 Uiso calc R 1
C C29 0.2822(17) 0.0045(12) 0.9227(9) 0.101(6) Uani d . 1
H H29 0.3005 -0.0333 0.8939 0.121 Uiso calc R 1
C C30 0.1862(18) 0.0149(13) 0.9216(10) 0.106(6) Uani d . 1
H H30 0.1374 -0.0131 0.8908 0.127 Uiso calc R 1
C C31 0.1539(15) 0.0682(12) 0.9665(10) 0.096(5) Uani d . 1
C C32 0.2307(13) 0.1116(11) 1.0113(8) 0.080(4) Uani d . 1
C C33 0.1998(12) 0.1637(10) 1.0553(9) 0.084(5) Uani d . 1
H H33 0.2489 0.1919 1.0857 0.100 Uiso calc R 1
C C34 0.0975(12) 0.1744(11) 1.0547(9) 0.088(5) Uani d . 1
H H34 0.0774 0.2093 1.0843 0.106 Uiso calc R 1
C C35 0.0270(15) 0.1323(13) 1.0095(11) 0.100(6) Uani d . 1
H H35 -0.0414 0.1387 1.0103 0.120 Uiso calc R 1
C C36 0.0473(16) 0.0840(13) 0.9654(11) 0.104(6) Uani d . 1
H H36 -0.0046 0.0604 0.9342 0.125 Uiso calc R 1
C C37 0.2364(8) 0.4819(9) 1.1177(6) 0.056(3) Uani d . 1
H H37 0.2998 0.5037 1.1386 0.067 Uiso calc R 1
C C38 0.1546(10) 0.4932(9) 1.1467(7) 0.066(4) Uani d . 1
H H38 0.1633 0.5215 1.1848 0.080 Uiso calc R 1
C C39 0.0600(9) 0.4596(9) 1.1153(7) 0.065(4) Uani d . 1
H H39 0.0040 0.4647 1.1330 0.078 Uiso calc R 1
C C40 0.0490(8) 0.4191(8) 1.0584(6) 0.055(3) Uani d . 1
C C41 0.1391(8) 0.4124(8) 1.0345(6) 0.050(3) Uani d . 1
C C42 0.1272(8) 0.3709(9) 0.9741(6) 0.056(3) Uani d . 1
C C43 0.0315(8) 0.3372(9) 0.9417(7) 0.064(4) Uani d . 1
C C44 0.0268(10) 0.2992(10) 0.8847(8) 0.077(4) Uani d . 1
H H44 -0.0352 0.2787 0.8608 0.092 Uiso calc R 1
C C45 0.1130(10) 0.2920(11) 0.8639(7) 0.080(4) Uani d . 1
H H45 0.1106 0.2662 0.8255 0.095 Uiso calc R 1
C C46 0.2051(9) 0.3232(9) 0.8997(7) 0.063(4) Uani d . 1
H H46 0.2638 0.3151 0.8851 0.075 Uiso calc R 1
C C47 -0.0462(9) 0.3862(10) 1.0248(8) 0.065(4) Uani d . 1
H H47 -0.1035 0.3925 1.0410 0.078 Uiso calc R 1
C C48 -0.0549(9) 0.3465(10) 0.9703(7) 0.068(4) Uani d . 1
H H48 -0.1181 0.3238 0.9498 0.082 Uiso calc R 1
C C49 0.3092(17) 0.2712(17) 0.2221(10) 0.108(6) Uani d . 1
H H49 0.3275 0.2459 0.1880 0.129 Uiso calc R 1
C C50 0.4600(14) 0.3654(13) 0.2341(8) 0.100(6) Uani d . 1
H H50A 0.4724 0.3271 0.2020 0.151 Uiso calc R 1
H H50B 0.5172 0.3631 0.2693 0.151 Uiso calc R 1
H H50C 0.4508 0.4251 0.2187 0.151 Uiso calc R 1
C C51 0.3405(18) 0.3704(16) 0.3046(10) 0.136(8) Uani d . 1
H H51A 0.2707 0.3550 0.3030 0.205 Uiso calc R 1
H H51B 0.3475 0.4337 0.3054 0.205 Uiso calc R 1
H H51C 0.3839 0.3457 0.3414 0.205 Uiso calc R 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'
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
O1 Tb1 O3 3_667 . 74.6(2)
O1 Tb1 O4 3_667 3_667 76.8(2)
O3 Tb1 O4 . 3_667 136.6(2)
O1 Tb1 O6 3_667 . 86.6(2)
O3 Tb1 O6 . . 125.4(3)
O4 Tb1 O6 3_667 . 84.2(3)
O1 Tb1 O5 3_667 . 75.6(2)
O3 Tb1 O5 . . 72.9(2)
O4 Tb1 O5 3_667 . 129.4(3)
O6 Tb1 O5 . . 52.7(3)
O1 Tb1 O2 3_667 . 123.5(2)
O3 Tb1 O2 . . 77.0(2)
O4 Tb1 O2 3_667 . 92.8(2)
O6 Tb1 O2 . . 148.4(2)
O5 Tb1 O2 . . 137.8(3)
O1 Tb1 O1 3_667 . 72.8(3)
O3 Tb1 O1 . . 68.8(2)
O4 Tb1 O1 3_667 . 72.0(2)
O6 Tb1 O1 . . 151.3(3)
O5 Tb1 O1 . . 135.3(2)
O2 Tb1 O1 . . 51.5(2)
O1 Tb1 N2 3_667 . 142.4(2)
O3 Tb1 N2 . . 78.3(2)
O4 Tb1 N2 3_667 . 139.6(2)
O6 Tb1 N2 . . 88.3(3)
O5 Tb1 N2 . . 71.7(3)
O2 Tb1 N2 . . 73.8(3)
O1 Tb1 N2 . . 120.3(3)
O1 Tb1 N1 3_667 . 148.4(3)
O3 Tb1 N1 . . 137.0(3)
O4 Tb1 N1 3_667 . 75.8(3)
O6 Tb1 N1 . . 75.2(3)
O5 Tb1 N1 . . 110.9(3)
O2 Tb1 N1 . . 73.5(2)
O1 Tb1 N1 . . 112.7(2)
N2 Tb1 N1 . . 63.9(3)
O1 Tb1 Tb1 3_667 3_667 38.12(17)
O3 Tb1 Tb1 . 3_667 66.94(16)
O4 Tb1 Tb1 3_667 3_667 70.35(15)
O6 Tb1 Tb1 . 3_667 122.06(18)
O5 Tb1 Tb1 . 3_667 108.12(16)
O2 Tb1 Tb1 . 3_667 85.76(15)
O1 Tb1 Tb1 . 3_667 34.72(13)
N2 Tb1 Tb1 . 3_667 142.9(2)
N1 Tb1 Tb1 . 3_667 139.2(2)
C37 N1 C41 . . 116.4(8)
C37 N1 Tb1 . . 124.9(7)
C41 N1 Tb1 . . 118.6(7)
C46 N2 C42 . . 116.9(10)
C46 N2 Tb1 . . 121.3(6)
C42 N2 Tb1 . . 121.8(8)
C49 N3 C51 . . 115.9(18)
C49 N3 C50 . . 121.6(16)
C51 N3 C50 . . 122(2)
C1 O1 Tb1 . 3_667 155.2(6)
C1 O1 Tb1 . . 90.6(6)
Tb1 O1 Tb1 3_667 . 107.2(2)
C1 O2 Tb1 . . 93.7(6)
C13 O3 Tb1 . . 138.8(7)
C13 O4 Tb1 . 3_667 133.5(6)
C25 O5 Tb1 . . 91.2(7)
C25 O6 Tb1 . . 93.3(7)
O2 C1 O1 . . 122.4(10)
O2 C1 C2 . . 119.9(9)
O1 C1 C2 . . 117.6(8)
C1 C2 C3 . . 116.3(9)
C1 C2 H2A . . 108.2
C3 C2 H2A . . 108.2
C1 C2 H2B . . 108.2
C3 C2 H2B . . 108.2
H2A C2 H2B . . 107.4
C4 C3 C8 . . 118.2(12)
C4 C3 C2 . . 118.4(13)
C8 C3 C2 . . 123.4(11)
C3 C4 C5 . . 120.0(15)
C3 C4 H4 . . 120.0
C5 C4 H4 . . 120.0
C6 C5 C4 . . 121.8(14)
C6 C5 H5 . . 119.1
C4 C5 H5 . . 119.1
C5 C6 C7 . . 120.7(14)
C5 C6 H6 . . 119.7
C7 C6 H6 . . 119.7
C6 C7 C8 . . 119.9(15)
C6 C7 C12 . . 121.4(15)
C8 C7 C12 . . 118.7(14)
C3 C8 C7 . . 119.4(13)
C3 C8 C9 . . 122.4(13)
C7 C8 C9 . . 118.2(14)
C10 C9 C8 . . 122.9(15)
C10 C9 H9 . . 118.5
C8 C9 H9 . . 118.5
C9 C10 C11 . . 116.7(17)
C9 C10 H10 . . 121.6
C11 C10 H10 . . 121.6
C12 C11 C10 . . 122.6(19)
C12 C11 H11 . . 118.7
C10 C11 H11 . . 118.7
C11 C12 C7 . . 120.8(17)
C11 C12 H12 . . 119.6
C7 C12 H12 . . 119.6
O3 C13 O4 . . 126.5(9)
O3 C13 C14 . . 116.1(9)
O4 C13 C14 . . 117.4(8)
C15 C14 C13 . . 116.8(10)
C15 C14 H14A . . 108.1
C13 C14 H14A . . 108.1
C15 C14 H14B . . 108.1
C13 C14 H14B . . 108.1
H14A C14 H14B . . 107.3
C16 C15 C20 . . 118.4(11)
C16 C15 C14 . . 119.3(13)
C20 C15 C14 . . 122.1(10)
C15 C16 C17 . . 121.8(15)
C15 C16 H16 . . 119.1
C17 C16 H16 . . 119.1
C18 C17 C16 . . 119.0(13)
C18 C17 H17 . . 120.5
C16 C17 H17 . . 120.5
C17 C18 C19 . . 121.4(13)
C17 C18 H18 . . 119.3
C19 C18 H18 . . 119.3
C18 C19 C20 . . 119.5(15)
C18 C19 C24 . . 122.4(13)
C20 C19 C24 . . 118.2(13)
C21 C20 C19 . . 119.0(14)
C21 C20 C15 . . 121.3(11)
C19 C20 C15 . . 119.7(12)
C22 C21 C20 . . 120.0(13)
C22 C21 H21 . . 120.0
C20 C21 H21 . . 120.0
C21 C22 C23 . . 122.5(16)
C21 C22 H22 . . 118.7
C23 C22 H22 . . 118.7
C24 C23 C22 . . 117.8(18)
C24 C23 H23 . . 121.1
C22 C23 H23 . . 121.1
C23 C24 C19 . . 122.5(14)
C23 C24 H24 . . 118.8
C19 C24 H24 . . 118.8
O6 C25 O5 . . 122.5(11)
O6 C25 C26 . . 120.0(12)
O5 C25 C26 . . 117.5(13)
C27 C26 C25 . . 111.4(13)
C27 C26 H26A . . 109.4
C25 C26 H26A . . 109.4
C27 C26 H26B . . 109.4
C25 C26 H26B . . 109.4
H26A C26 H26B . . 108.0
C28 C27 C32 . . 118.1(17)
C28 C27 C26 . . 120.5(15)
C32 C27 C26 . . 121.4(16)
C27 C28 C29 . . 119.3(18)
C27 C28 H28 . . 120.3
C29 C28 H28 . . 120.3
C30 C29 C28 . . 122(2)
C30 C29 H29 . . 119.0
C28 C29 H29 . . 119.0
C29 C30 C31 . . 121(2)
C29 C30 H30 . . 119.3
C31 C30 H30 . . 119.3
C32 C31 C30 . . 117.4(19)
C32 C31 C36 . . 120(2)
C30 C31 C36 . . 123(2)
C33 C32 C27 . . 120.6(16)
C33 C32 C31 . . 117.7(17)
C27 C32 C31 . . 121.8(18)
C34 C33 C32 . . 121.4(17)
C34 C33 H33 . . 119.3
C32 C33 H33 . . 119.3
C35 C34 C33 . . 118.1(19)
C35 C34 H34 . . 120.9
C33 C34 H34 . . 120.9
C36 C35 C34 . . 125(2)
C36 C35 H35 . . 117.3
C34 C35 H35 . . 117.3
C35 C36 C31 . . 118(2)
C35 C36 H36 . . 121.2
C31 C36 H36 . . 121.2
N1 C37 C38 . . 126.1(12)
N1 C37 H37 . . 116.9
C38 C37 H37 . . 116.9
C39 C38 C37 . . 116.7(13)
C39 C38 H38 . . 121.7
C37 C38 H38 . . 121.7
C40 C39 C38 . . 120.4(10)
C40 C39 H39 . . 119.8
C38 C39 H39 . . 119.8
C39 C40 C47 . . 121.9(10)
C39 C40 C41 . . 116.7(11)
C47 C40 C41 . . 121.3(13)
N1 C41 C40 . . 123.7(11)
N1 C41 C42 . . 119.6(8)
C40 C41 C42 . . 116.7(11)
N2 C42 C43 . . 123.1(12)
N2 C42 C41 . . 116.0(10)
C43 C42 C41 . . 120.9(10)
C44 C43 C42 . . 117.2(10)
C44 C43 C48 . . 124.8(12)
C42 C43 C48 . . 118.0(13)
C45 C44 C43 . . 119.3(13)
C45 C44 H44 . . 120.3
C43 C44 H44 . . 120.3
C44 C45 C46 . . 120.0(15)
C44 C45 H45 . . 120.0
C46 C45 H45 . . 120.0
N2 C46 C45 . . 123.3(11)
N2 C46 H46 . . 118.3
C45 C46 H46 . . 118.3
C48 C47 C40 . . 121.0(10)
C48 C47 H47 . . 119.5
C40 C47 H47 . . 119.5
C47 C48 C43 . . 122.0(12)
C47 C48 H48 . . 119.0
C43 C48 H48 . . 119.0
O7 C49 N3 . . 124(2)
O7 C49 H49 . . 117.9
N3 C49 H49 . . 117.9
N3 C50 H50A . . 109.5
N3 C50 H50B . . 109.5
H50A C50 H50B . . 109.5
N3 C50 H50C . . 109.5
H50A C50 H50C . . 109.5
H50B C50 H50C . . 109.5
N3 C51 H51A . . 109.5
N3 C51 H51B . . 109.5
H51A C51 H51B . . 109.5
N3 C51 H51C . . 109.5
H51A C51 H51C . . 109.5
H51B C51 H51C . . 109.5
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 O1 3_667 2.343(5) y
Tb1 O3 . 2.349(6) y
Tb1 O4 3_667 2.369(7) y
Tb1 O6 . 2.433(8) y
Tb1 O5 . 2.468(8) y
Tb1 O2 . 2.478(7) y
Tb1 O1 . 2.539(7) y
Tb1 N2 . 2.547(9) y
Tb1 N1 . 2.587(7) y
Tb1 Tb1 3_667 3.9302(9) n
N1 C37 . 1.299(14) ?
N1 C41 . 1.352(15) ?
N2 C46 . 1.306(15) ?
N2 C42 . 1.356(12) ?
N3 C49 . 1.34(2) ?
N3 C51 . 1.40(2) ?
N3 C50 . 1.45(2) ?
O1 C1 . 1.247(12) ?
O1 Tb1 3_667 2.343(5) ?
O2 C1 . 1.239(11) ?
O3 C13 . 1.241(10) ?
O4 C13 . 1.262(11) ?
O4 Tb1 3_667 2.369(7) ?
O5 C25 . 1.252(15) ?
O6 C25 . 1.231(14) ?
O7 C49 . 1.23(2) ?
C1 C2 . 1.507(16) ?
C2 C3 . 1.509(16) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.388(18) ?
C3 C8 . 1.411(18) ?
C4 C5 . 1.407(19) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.31(2) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.38(2) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.413(18) ?
C7 C12 . 1.43(2) ?
C8 C9 . 1.41(2) ?
C9 C10 . 1.35(2) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.45(2) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.31(2) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.513(15) ?
C14 C15 . 1.495(15) ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C15 C16 . 1.393(17) ?
C15 C20 . 1.416(19) ?
C16 C17 . 1.395(17) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.38(2) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.39(2) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.415(16) ?
C19 C24 . 1.43(2) ?
C20 C21 . 1.400(18) ?
C21 C22 . 1.35(2) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.41(2) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.34(2) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
C25 C26 . 1.518(18) ?
C26 C27 . 1.47(2) ?
C26 H26A . 0.9700 ?
C26 H26B . 0.9700 ?
C27 C28 . 1.39(2) ?
C27 C32 . 1.41(2) ?
C28 C29 . 1.44(2) ?
C28 H28 . 0.9300 ?
C29 C30 . 1.30(2) ?
C29 H29 . 0.9300 ?
C30 C31 . 1.43(3) ?
C30 H30 . 0.9300 ?
C31 C32 . 1.41(3) ?
C31 C36 . 1.45(3) ?
C32 C33 . 1.39(2) ?
C33 C34 . 1.38(2) ?
C33 H33 . 0.9300 ?
C34 C35 . 1.37(3) ?
C34 H34 . 0.9300 ?
C35 C36 . 1.30(3) ?
C35 H35 . 0.9300 ?
C36 H36 . 0.9300 ?
C37 C38 . 1.410(13) ?
C37 H37 . 0.9300 ?
C38 C39 . 1.395(19) ?
C38 H38 . 0.9300 ?
C39 C40 . 1.378(19) ?
C39 H39 . 0.9300 ?
C40 C47 . 1.412(19) ?
C40 C41 . 1.437(12) ?
C41 C42 . 1.453(17) ?
C42 C43 . 1.413(17) ?
C43 C44 . 1.375(19) ?
C43 C48 . 1.456(16) ?
C44 C45 . 1.351(17) ?
C44 H44 . 0.9300 ?
C45 C46 . 1.388(18) ?
C45 H45 . 0.9300 ?
C46 H46 . 0.9300 ?
C47 C48 . 1.328(19) ?
C47 H47 . 0.9300 ?
C48 H48 . 0.9300 ?
C49 H49 . 0.9300 ?
C50 H50A . 0.9600 ?
C50 H50B . 0.9600 ?
C50 H50C . 0.9600 ?
C51 H51A . 0.9600 ?
C51 H51B . 0.9600 ?
C51 H51C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C6 H6 O7 3_566 0.93 2.56 3.44(2) 157.4
C37 H37 O4 3_667 0.93 2.35 3.015(11) 127.9
C46 H46 O3 . 0.93 2.48 3.056(13) 120.4
C47 H47 O2 3_567 0.93 2.45 3.314(13) 154.3
C50 H50A O6 1_554 0.96 2.62 3.40(2) 137.8
C18 H18 Cg1 2_655 0.93 2.90 3.673(16) 141
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_4
_geom_torsion
O1 Tb1 N1 C37 3_667 . 27.9(11)
O3 Tb1 N1 C37 . . -148.8(8)
O4 Tb1 N1 C37 3_667 . -2.9(9)
O6 Tb1 N1 C37 . . 84.7(9)
O5 Tb1 N1 C37 . . 124.3(9)
O2 Tb1 N1 C37 . . -100.2(9)
O1 Tb1 N1 C37 . . -66.0(9)
N2 Tb1 N1 C37 . . -179.8(10)
Tb1 Tb1 N1 C37 3_667 . -37.6(10)
O1 Tb1 N1 C41 3_667 . -154.6(7)
O3 Tb1 N1 C41 . . 28.7(10)
O4 Tb1 N1 C41 3_667 . 174.6(8)
O6 Tb1 N1 C41 . . -97.8(8)
O5 Tb1 N1 C41 . . -58.2(8)
O2 Tb1 N1 C41 . . 77.3(8)
O1 Tb1 N1 C41 . . 111.4(8)
N2 Tb1 N1 C41 . . -2.3(8)
Tb1 Tb1 N1 C41 3_667 . 139.9(7)
O1 Tb1 N2 C46 3_667 . -22.3(11)
O3 Tb1 N2 C46 . . 22.3(9)
O4 Tb1 N2 C46 3_667 . 176.7(8)
O6 Tb1 N2 C46 . . -104.4(9)
O5 Tb1 N2 C46 . . -53.3(9)
O2 Tb1 N2 C46 . . 102.0(9)
O1 Tb1 N2 C46 . . 79.1(10)
N1 Tb1 N2 C46 . . -178.7(10)
Tb1 Tb1 N2 C46 3_667 . 42.8(11)
O1 Tb1 N2 C42 3_667 . 160.4(8)
O3 Tb1 N2 C42 . . -155.0(9)
O4 Tb1 N2 C42 3_667 . -0.6(11)
O6 Tb1 N2 C42 . . 78.3(9)
O5 Tb1 N2 C42 . . 129.4(9)
O2 Tb1 N2 C42 . . -75.3(9)
O1 Tb1 N2 C42 . . -98.2(9)
N1 Tb1 N2 C42 . . 3.9(8)
Tb1 Tb1 N2 C42 3_667 . -134.5(8)
O1 Tb1 O1 C1 3_667 . 162.4(7)
O3 Tb1 O1 C1 . . 82.7(6)
O4 Tb1 O1 C1 3_667 . -116.3(6)
O6 Tb1 O1 C1 . . -151.6(6)
O5 Tb1 O1 C1 . . 115.4(6)
O2 Tb1 O1 C1 . . -7.3(5)
N2 Tb1 O1 C1 . . 21.2(6)
N1 Tb1 O1 C1 . . -50.8(6)
Tb1 Tb1 O1 C1 3_667 . 162.4(7)
O1 Tb1 O1 Tb1 3_667 3_667 0.0
O3 Tb1 O1 Tb1 . 3_667 -79.7(3)
O4 Tb1 O1 Tb1 3_667 3_667 81.3(3)
O6 Tb1 O1 Tb1 . 3_667 46.0(6)
O5 Tb1 O1 Tb1 . 3_667 -47.0(4)
O2 Tb1 O1 Tb1 . 3_667 -169.7(4)
N2 Tb1 O1 Tb1 . 3_667 -141.2(3)
N1 Tb1 O1 Tb1 . 3_667 146.8(3)
O1 Tb1 O2 C1 3_667 . -4.4(7)
O3 Tb1 O2 C1 . . -65.8(6)
O4 Tb1 O2 C1 3_667 . 71.5(6)
O6 Tb1 O2 C1 . . 155.0(6)
O5 Tb1 O2 C1 . . -111.0(6)
O1 Tb1 O2 C1 . . 7.4(6)
N2 Tb1 O2 C1 . . -147.2(6)
N1 Tb1 O2 C1 . . 145.9(7)
Tb1 Tb1 O2 C1 3_667 . 1.5(6)
O1 Tb1 O3 C13 3_667 . -17.2(10)
O4 Tb1 O3 C13 3_667 . 33.3(11)
O6 Tb1 O3 C13 . . -91.4(10)
O5 Tb1 O3 C13 . . -96.6(10)
O2 Tb1 O3 C13 . . 113.4(10)
O1 Tb1 O3 C13 . . 60.0(10)
N2 Tb1 O3 C13 . . -170.8(11)
N1 Tb1 O3 C13 . . 161.0(9)
Tb1 Tb1 O3 C13 3_667 . 22.5(10)
O1 Tb1 O5 C25 3_667 . 99.6(7)
O3 Tb1 O5 C25 . . 177.6(7)
O4 Tb1 O5 C25 3_667 . 40.6(7)
O6 Tb1 O5 C25 . . 2.8(6)
O2 Tb1 O5 C25 . . -136.1(6)
O1 Tb1 O5 C25 . . 145.7(6)
N2 Tb1 O5 C25 . . -99.4(7)
N1 Tb1 O5 C25 . . -47.9(7)
Tb1 Tb1 O5 C25 3_667 . 119.7(6)
O1 Tb1 O6 C25 3_667 . -77.4(6)
O3 Tb1 O6 C25 . . -9.0(7)
O4 Tb1 O6 C25 3_667 . -154.4(7)
O5 Tb1 O6 C25 . . -2.9(6)
O2 Tb1 O6 C25 . . 119.7(7)
O1 Tb1 O6 C25 . . -120.9(7)
N2 Tb1 O6 C25 . . 65.4(7)
N1 Tb1 O6 C25 . . 128.7(7)
Tb1 Tb1 O6 C25 3_667 . -92.0(7)
Tb1 O2 C1 O1 . . -14.0(10)
Tb1 O2 C1 C2 . . 163.7(9)
Tb1 O1 C1 O2 3_667 . 150.2(11)
Tb1 O1 C1 O2 . . 13.6(10)
Tb1 O1 C1 C2 3_667 . -28(2)
Tb1 O1 C1 C2 . . -164.1(9)
O2 C1 C2 C3 . . -4.7(16)
O1 C1 C2 C3 . . 173.1(10)
C1 C2 C3 C4 . . 112.9(13)
C1 C2 C3 C8 . . -68.9(15)
C8 C3 C4 C5 . . 2.3(18)
C2 C3 C4 C5 . . -179.4(11)
C3 C4 C5 C6 . . -3(2)
C4 C5 C6 C7 . . 2(2)
C5 C6 C7 C8 . . 0(2)
C5 C6 C7 C12 . . -179.6(13)
C4 C3 C8 C7 . . -1.0(17)
C2 C3 C8 C7 . . -179.3(11)
C4 C3 C8 C9 . . 179.1(12)
C2 C3 C8 C9 . . 0.9(18)
C6 C7 C8 C3 . . 0.1(18)
C12 C7 C8 C3 . . 179.2(11)
C6 C7 C8 C9 . . 179.9(12)
C12 C7 C8 C9 . . -0.9(18)
C3 C8 C9 C10 . . 179.2(14)
C7 C8 C9 C10 . . -1(2)
C8 C9 C10 C11 . . 1(2)
C9 C10 C11 C12 . . 0(3)
C10 C11 C12 C7 . . -2(3)
C6 C7 C12 C11 . . -178.6(16)
C8 C7 C12 C11 . . 2(2)
Tb1 O3 C13 O4 . . -28.8(18)
Tb1 O3 C13 C14 . . 152.1(8)
Tb1 O4 C13 O3 3_667 . 8.6(17)
Tb1 O4 C13 C14 3_667 . -172.3(7)
O3 C13 C14 C15 . . -140.2(12)
O4 C13 C14 C15 . . 40.6(16)
C13 C14 C15 C16 . . -119.7(13)
C13 C14 C15 C20 . . 65.3(16)
C20 C15 C16 C17 . . -3(2)
C14 C15 C16 C17 . . -178.4(13)
C15 C16 C17 C18 . . 3(2)
C16 C17 C18 C19 . . 0(2)
C17 C18 C19 C20 . . -3(2)
C17 C18 C19 C24 . . 176.8(14)
C18 C19 C20 C21 . . -178.8(12)
C24 C19 C20 C21 . . 1.6(19)
C18 C19 C20 C15 . . 2.2(19)
C24 C19 C20 C15 . . -177.4(12)
C16 C15 C20 C21 . . -178.2(13)
C14 C15 C20 C21 . . -3.2(18)
C16 C15 C20 C19 . . 0.7(18)
C14 C15 C20 C19 . . 175.7(12)
C19 C20 C21 C22 . . -3(2)
C15 C20 C21 C22 . . 176.1(13)
C20 C21 C22 C23 . . 3(2)
C21 C22 C23 C24 . . -1(2)
C22 C23 C24 C19 . . 0(2)
C18 C19 C24 C23 . . -179.9(15)
C20 C19 C24 C23 . . 0(2)
Tb1 O6 C25 O5 . . 5.3(11)
Tb1 O6 C25 C26 . . -174.2(11)
Tb1 O5 C25 O6 . . -5.3(11)
Tb1 O5 C25 C26 . . 174.3(10)
O6 C25 C26 C27 . . 125.9(14)
O5 C25 C26 C27 . . -53.6(16)
C25 C26 C27 C28 . . 107.4(16)
C25 C26 C27 C32 . . -70.4(17)
C32 C27 C28 C29 . . 0(2)
C26 C27 C28 C29 . . -178.1(14)
C27 C28 C29 C30 . . 2(3)
C28 C29 C30 C31 . . -3(3)
C29 C30 C31 C32 . . 2(2)
C29 C30 C31 C36 . . 177.6(17)
C28 C27 C32 C33 . . 179.3(14)
C26 C27 C32 C33 . . -3(2)
C28 C27 C32 C31 . . -1(2)
C26 C27 C32 C31 . . 176.6(14)
C30 C31 C32 C33 . . -180.0(14)
C36 C31 C32 C33 . . 4(2)
C30 C31 C32 C27 . . 1(2)
C36 C31 C32 C27 . . -175.5(14)
C27 C32 C33 C34 . . 178.3(14)
C31 C32 C33 C34 . . -1(2)
C32 C33 C34 C35 . . 0(2)
C33 C34 C35 C36 . . -2(3)
C34 C35 C36 C31 . . 5(3)
C32 C31 C36 C35 . . -6(2)
C30 C31 C36 C35 . . 178.6(17)
C41 N1 C37 C38 . . 0.0(18)
Tb1 N1 C37 C38 . . 177.6(10)
N1 C37 C38 C39 . . 0(2)
C37 C38 C39 C40 . . -1.0(19)
C38 C39 C40 C47 . . -178.6(12)
C38 C39 C40 C41 . . 1.0(18)
C37 N1 C41 C40 . . -0.1(16)
Tb1 N1 C41 C40 . . -177.8(8)
C37 N1 C41 C42 . . 178.6(11)
Tb1 N1 C41 C42 . . 0.9(14)
C39 C40 C41 N1 . . -0.5(17)
C47 C40 C41 N1 . . 179.1(11)
C39 C40 C41 C42 . . -179.1(11)
C47 C40 C41 C42 . . 0.4(17)
C46 N2 C42 C43 . . 0.4(18)
Tb1 N2 C42 C43 . . 177.8(10)
C46 N2 C42 C41 . . 177.5(11)
Tb1 N2 C42 C41 . . -5.1(14)
N1 C41 C42 N2 . . 2.7(16)
C40 C41 C42 N2 . . -178.6(11)
N1 C41 C42 C43 . . 179.9(12)
C40 C41 C42 C43 . . -1.4(17)
N2 C42 C43 C44 . . -3(2)
C41 C42 C43 C44 . . 179.7(12)
N2 C42 C43 C48 . . 177.8(12)
C41 C42 C43 C48 . . 0.8(19)
C42 C43 C44 C45 . . 3(2)
C48 C43 C44 C45 . . -178.0(14)
C43 C44 C45 C46 . . 0(2)
C42 N2 C46 C45 . . 2.7(19)
Tb1 N2 C46 C45 . . -174.7(11)
C44 C45 C46 N2 . . -3(2)
C39 C40 C47 C48 . . -179.2(13)
C41 C40 C47 C48 . . 1.3(19)
C40 C47 C48 C43 . . -2(2)
C44 C43 C48 C47 . . -177.9(15)
C42 C43 C48 C47 . . 1(2)
C51 N3 C49 O7 . . 2(3)
C50 N3 C49 O7 . . 178.1(19)
