#------------------------------------------------------------------------------
#$Date: 2020-11-06 13:10:01 +0100 (vie 06 de nov de 2020) $
#$Revision: 258822 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/54/7705474.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_7705474
loop_
_publ_author_name
'Arauzo, A.'
'Gasque, L.'
'Fuertes, S.'
'Tenorio, C.'
'Bernès, S'
'Bartolomé, E'
_publ_section_title
;
 Coumarin-lanthanide based compounds with SMM behavior and high quantum
 yield luminescence.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13671
_journal_page_last               13684
_journal_paper_doi               10.1039/d0dt02614j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C45 H29 N2 O12 Tb, 0.5(H2 O)'
_chemical_formula_sum            'C45 H30 N2 O12.5 Tb'
_chemical_formula_weight         957.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-27
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                104.500(5)
_cell_angle_beta                 92.593(5)
_cell_angle_gamma                98.423(5)
_cell_formula_units_Z            2
_cell_length_a                   11.0672(7)
_cell_length_b                   13.0523(8)
_cell_length_c                   14.2639(9)
_cell_measurement_reflns_used    20255
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      23.90
_cell_measurement_theta_min      2.34
_cell_volume                     1966.1(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295(1)
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1579 frames, 15-20 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            63684
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         2.336
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-AREA (Stoe & Cie, 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       prism
_exptl_crystal_F_000             958
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10452
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.789
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0210P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6372
_reflns_number_total             10452
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02614j2.cif
_cod_data_source_block           Tb-phen
_cod_depositor_comments
'Adding full bibliography for 7705471--7705478.cif.'
_cod_original_formula_sum        'C45 H30 N2 O12.50 Tb'
_cod_database_code               7705474
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.939
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 0.28848(2) 0.25259(2) 0.78545(2) 0.04432(6) Uani 1 1 d . . . . .
O1 O 0.0957(3) 0.6532(3) 0.7895(3) 0.0988(11) Uani 1 1 d . . . . .
O2 O -0.0175(4) 0.5872(3) 0.8901(3) 0.1404(17) Uani 1 1 d . . . . .
O3 O 0.2481(2) 0.38080(19) 0.70494(16) 0.0528(6) Uani 1 1 d . . . . .
O4 O 0.0898(2) 0.2904(2) 0.80845(18) 0.0623(7) Uani 1 1 d . . . . .
C2 C 0.0534(5) 0.5685(5) 0.8280(3) 0.0939(16) Uani 1 1 d . . . . .
C3 C 0.0973(4) 0.4674(4) 0.7930(3) 0.0627(11) Uani 1 1 d . . . . .
C4 C 0.1953(3) 0.4613(3) 0.7315(2) 0.0534(9) Uani 1 1 d . . . . .
C5 C 0.2366(4) 0.5561(3) 0.6969(3) 0.0599(10) Uani 1 1 d . . . . .
C6 C 0.3295(4) 0.5582(4) 0.6359(3) 0.0784(13) Uani 1 1 d . . . . .
H6A H 0.366673 0.497917 0.615078 0.094 Uiso 1 1 calc R U . . .
C7 C 0.3673(5) 0.6483(5) 0.6057(4) 0.1060(17) Uani 1 1 d . . . . .
H7A H 0.431636 0.649441 0.566021 0.127 Uiso 1 1 calc R U . . .
C8 C 0.3116(6) 0.7371(5) 0.6330(5) 0.120(2) Uani 1 1 d . . . . .
H8A H 0.336387 0.796735 0.609863 0.143 Uiso 1 1 calc R U . . .
C9 C 0.2213(6) 0.7384(4) 0.6932(4) 0.1036(19) Uani 1 1 d . . . . .
H9A H 0.184141 0.798906 0.712889 0.124 Uiso 1 1 calc R U . . .
C10 C 0.1845(5) 0.6470(4) 0.7256(3) 0.0794(13) Uani 1 1 d . . . . .
C11 C 0.0424(4) 0.3737(4) 0.8206(3) 0.0690(12) Uani 1 1 d . . . . .
C12 C -0.0799(4) 0.3667(5) 0.8625(4) 0.129(2) Uani 1 1 d . . . . .
H12A H -0.121697 0.293921 0.842894 0.194 Uiso 1 1 calc DR U . . .
H12B H -0.128272 0.412051 0.839284 0.194 Uiso 1 1 calc R U . . .
H12C H -0.067808 0.389775 0.932175 0.194 Uiso 1 1 calc R U . . .
O21 O 0.1309(2) -0.1405(2) 0.44275(17) 0.0681(7) Uani 1 1 d . . . . .
O22 O 0.2980(3) -0.0713(2) 0.3920(2) 0.1004(11) Uani 1 1 d . . . . .
O23 O 0.1666(2) 0.09389(18) 0.69861(15) 0.0539(6) Uani 1 1 d . . . . .
O24 O 0.3579(2) 0.19113(18) 0.63262(16) 0.0562(7) Uani 1 1 d . . . . .
C22 C 0.2314(4) -0.0601(3) 0.4578(3) 0.0649(11) Uani 1 1 d . . . . .
C23 C 0.2459(3) 0.0255(3) 0.5456(2) 0.0477(8) Uani 1 1 d . . . . .
C24 C 0.1613(3) 0.0238(3) 0.6181(2) 0.0452(8) Uani 1 1 d . . . . .
C25 C 0.0575(3) -0.0653(2) 0.5967(2) 0.0451(8) Uani 1 1 d . . . . .
C26 C -0.0309(3) -0.0721(3) 0.6610(3) 0.0601(10) Uani 1 1 d . . . . .
H26A H -0.025120 -0.019943 0.719655 0.072 Uiso 1 1 calc R U . . .
C27 C -0.1283(4) -0.1563(3) 0.6382(3) 0.0781(13) Uani 1 1 d . . . . .
H27A H -0.187517 -0.161562 0.681736 0.094 Uiso 1 1 calc R U . . .
C28 C -0.1366(4) -0.2329(3) 0.5499(3) 0.0786(13) Uani 1 1 d . . . . .
H28A H -0.202485 -0.288997 0.534108 0.094 Uiso 1 1 calc R U . . .
C29 C -0.0502(4) -0.2271(3) 0.4864(3) 0.0704(12) Uani 1 1 d . . . . .
H29A H -0.056073 -0.278906 0.427539 0.084 Uiso 1 1 calc R U . . .
C30 C 0.0472(3) -0.1427(3) 0.5104(3) 0.0548(9) Uani 1 1 d . . . . .
C31 C 0.3424(3) 0.1157(3) 0.5588(3) 0.0545(9) Uani 1 1 d . . . . .
C32 C 0.4306(4) 0.1275(3) 0.4826(3) 0.0811(14) Uani 1 1 d . . . . .
H32A H 0.494120 0.187722 0.509112 0.122 Uiso 1 1 calc R U . . .
H32B H 0.387106 0.138673 0.427132 0.122 Uiso 1 1 calc R U . . .
H32C H 0.466303 0.063487 0.463084 0.122 Uiso 1 1 calc R U . . .
O41 O 0.6449(3) 0.6445(2) 0.8147(2) 0.0744(8) Uani 1 1 d . . . . .
O42 O 0.5188(3) 0.7118(2) 0.9167(2) 0.0876(9) Uani 1 1 d . . . . .
O43 O 0.4870(2) 0.33540(17) 0.79156(16) 0.0521(6) Uani 1 1 d . . . . .
O44 O 0.3265(2) 0.41158(17) 0.91123(15) 0.0489(6) Uani 1 1 d . . . . .
C42 C 0.5459(4) 0.6296(3) 0.8686(3) 0.0626(10) Uani 1 1 d . . . . .
C43 C 0.4862(3) 0.5209(3) 0.8614(2) 0.0468(8) Uani 1 1 d . . . . .
C44 C 0.5304(3) 0.4328(3) 0.8007(2) 0.0472(8) Uani 1 1 d . . . . .
C45 C 0.6345(3) 0.4553(3) 0.7455(3) 0.0528(9) Uani 1 1 d . . . . .
C46 C 0.6819(3) 0.3736(3) 0.6814(3) 0.0666(11) Uani 1 1 d . . . . .
H46A H 0.647134 0.302279 0.673379 0.080 Uiso 1 1 calc R U . . .
C47 C 0.7792(4) 0.3984(4) 0.6306(3) 0.0851(14) Uani 1 1 d . . . . .
H47A H 0.810222 0.343667 0.588559 0.102 Uiso 1 1 calc R U . . .
C48 C 0.8317(4) 0.5038(5) 0.6411(4) 0.0918(15) Uani 1 1 d . . . . .
H48A H 0.897873 0.519826 0.606475 0.110 Uiso 1 1 calc R U . . .
C49 C 0.7857(4) 0.5847(4) 0.7030(4) 0.0853(14) Uani 1 1 d . . . . .
H49A H 0.820456 0.655867 0.710466 0.102 Uiso 1 1 calc R U . . .
C50 C 0.6874(4) 0.5597(3) 0.7541(3) 0.0638(10) Uani 1 1 d . . . . .
C51 C 0.3851(3) 0.5033(3) 0.9187(2) 0.0476(9) Uani 1 1 d . . . . .
C52 C 0.3408(3) 0.5933(3) 0.9902(3) 0.0633(10) Uani 1 1 d . . . . .
H52A H 0.280886 0.563962 1.027057 0.095 Uiso 1 1 calc R U . . .
H52B H 0.304460 0.637079 0.955555 0.095 Uiso 1 1 calc R U . . .
H52C H 0.408795 0.636276 1.033329 0.095 Uiso 1 1 calc R U . . .
N61 N 0.4080(3) 0.1131(2) 0.82127(19) 0.0494(7) Uani 1 1 d . . . . .
C62 C 0.5038(3) 0.0830(3) 0.7745(3) 0.0582(10) Uani 1 1 d . . . . .
H62A H 0.539563 0.125194 0.736171 0.070 Uiso 1 1 calc R U . . .
C63 C 0.5537(4) -0.0075(3) 0.7794(3) 0.0661(11) Uani 1 1 d . . . . .
H63A H 0.621611 -0.024132 0.746170 0.079 Uiso 1 1 calc R U . . .
C64 C 0.5014(4) -0.0713(3) 0.8335(3) 0.0697(11) Uani 1 1 d . . . . .
H64A H 0.531903 -0.133330 0.836108 0.084 Uiso 1 1 calc R U . . .
C65 C 0.4005(4) -0.0432(3) 0.8859(3) 0.0562(10) Uani 1 1 d . . . . .
C66 C 0.3440(4) -0.1042(3) 0.9465(3) 0.0712(12) Uani 1 1 d . . . . .
H66A H 0.368949 -0.168707 0.948489 0.085 Uiso 1 1 calc R U . . .
C67 C 0.2553(4) -0.0699(3) 1.0006(3) 0.0682(11) Uani 1 1 d . . . . .
H67A H 0.219127 -0.111295 1.039385 0.082 Uiso 1 1 calc R U . . .
C68 C 0.2146(3) 0.0291(3) 1.0003(3) 0.0549(9) Uani 1 1 d . . . . .
C69 C 0.1293(4) 0.0732(3) 1.0622(3) 0.0651(11) Uani 1 1 d . . . . .
H69A H 0.094249 0.036622 1.105044 0.078 Uiso 1 1 calc R U . . .
C70 C 0.0982(4) 0.1695(3) 1.0593(3) 0.0666(11) Uani 1 1 d . . . . .
H70A H 0.044398 0.200766 1.101525 0.080 Uiso 1 1 calc R U . . .
C71 C 0.1490(3) 0.2204(3) 0.9914(3) 0.0598(10) Uani 1 1 d . . . . .
H71A H 0.126006 0.285525 0.989079 0.072 Uiso 1 1 calc R U . . .
N72 N 0.2277(3) 0.1817(2) 0.93025(19) 0.0491(7) Uani 1 1 d . . . . .
C73 C 0.2639(3) 0.0883(3) 0.9372(2) 0.0493(9) Uani 1 1 d . . . . .
C74 C 0.3595(3) 0.0513(3) 0.8784(2) 0.0471(8) Uani 1 1 d . . . . .
O81 O -0.1265(8) 0.1303(8) 0.8005(6) 0.158(3) Uani 0.5 1 d D . P . .
H81A H -0.145(5) 0.097(11) 0.739(3) 0.190 Uiso 0.5 1 d D U P . .
H81B H -0.199(2) 0.1323(19) 0.8208(17) 0.190 Uiso 0.5 1 d D U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.3496 2.7654 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -5 -1 0.0340
-3 5 1 0.0300
-3 -1 0 0.1120
2 1 0 0.1440
1 1 -6 0.0690
0 -1 6 0.0970
-2 -1 1 0.1260
-3 -1 -5 0.1000
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
_geom_angle_publ_flag
O43 Tb1 O23 137.55(8) . . ?
O43 Tb1 O24 72.70(8) . . ?
O23 Tb1 O24 69.12(7) . . ?
O43 Tb1 O3 83.02(8) . . ?
O23 Tb1 O3 105.15(8) . . ?
O24 Tb1 O3 76.68(8) . . ?
O43 Tb1 O4 141.59(9) . . ?
O23 Tb1 O4 77.37(9) . . ?
O24 Tb1 O4 123.39(9) . . ?
O3 Tb1 O4 69.69(9) . . ?
O43 Tb1 O44 69.55(8) . . ?
O23 Tb1 O44 152.67(8) . . ?
O24 Tb1 O44 136.37(8) . . ?
O3 Tb1 O44 77.78(8) . . ?
O4 Tb1 O44 78.41(8) . . ?
O43 Tb1 N61 78.04(8) . . ?
O23 Tb1 N61 78.23(9) . . ?
O24 Tb1 N61 80.81(9) . . ?
O3 Tb1 N61 154.05(8) . . ?
O4 Tb1 N61 135.00(9) . . ?
O44 Tb1 N61 111.26(8) . . ?
O43 Tb1 N72 116.88(9) . . ?
O23 Tb1 N72 82.70(8) . . ?
O24 Tb1 N72 139.01(9) . . ?
O3 Tb1 N72 141.33(9) . . ?
O4 Tb1 N72 75.55(9) . . ?
O44 Tb1 N72 79.17(8) . . ?
N61 Tb1 N72 64.27(9) . . ?
C10 O1 C2 121.9(4) . . ?
C4 O3 Tb1 130.6(2) . . ?
C11 O4 Tb1 134.3(3) . . ?
O2 C2 O1 115.5(5) . . ?
O2 C2 C3 125.8(6) . . ?
O1 C2 C3 118.8(4) . . ?
C4 C3 C11 120.0(4) . . ?
C4 C3 C2 119.8(4) . . ?
C11 C3 C2 120.1(4) . . ?
O3 C4 C3 124.9(4) . . ?
O3 C4 C5 118.2(4) . . ?
C3 C4 C5 116.9(4) . . ?
C10 C5 C6 117.7(4) . . ?
C10 C5 C4 120.7(4) . . ?
C6 C5 C4 121.6(4) . . ?
C7 C6 C5 120.4(5) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C6 C7 C8 120.9(6) . . ?
C6 C7 H7A 119.5 . . ?
C8 C7 H7A 119.5 . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 H8A 119.8 . . ?
C7 C8 H8A 119.8 . . ?
C8 C9 C10 118.5(6) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
O1 C10 C5 121.4(5) . . ?
O1 C10 C9 116.6(5) . . ?
C5 C10 C9 122.1(5) . . ?
O4 C11 C3 123.0(4) . . ?
O4 C11 C12 114.8(4) . . ?
C3 C11 C12 122.2(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 121.8(3) . . ?
C24 O23 Tb1 139.6(2) . . ?
C31 O24 Tb1 143.5(2) . . ?
O22 C22 O21 113.5(3) . . ?
O22 C22 C23 127.5(4) . . ?
O21 C22 C23 118.9(3) . . ?
C24 C23 C31 119.5(3) . . ?
C24 C23 C22 120.3(3) . . ?
C31 C23 C22 120.1(3) . . ?
O23 C24 C23 125.5(3) . . ?
O23 C24 C25 117.2(3) . . ?
C23 C24 C25 117.3(3) . . ?
C30 C25 C26 119.1(3) . . ?
C30 C25 C24 119.4(3) . . ?
C26 C25 C24 121.5(3) . . ?
C25 C26 C27 120.1(4) . . ?
C25 C26 H26A 120.0 . . ?
C27 C26 H26A 120.0 . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
C29 C28 C27 120.9(4) . . ?
C29 C28 H28A 119.5 . . ?
C27 C28 H28A 119.5 . . ?
C28 C29 C30 119.0(4) . . ?
C28 C29 H29A 120.5 . . ?
C30 C29 H29A 120.5 . . ?
O21 C30 C25 122.2(3) . . ?
O21 C30 C29 116.4(3) . . ?
C25 C30 C29 121.4(4) . . ?
O24 C31 C23 122.3(3) . . ?
O24 C31 C32 114.7(3) . . ?
C23 C31 C32 122.9(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.2(3) . . ?
C44 O43 Tb1 130.5(2) . . ?
C51 O44 Tb1 133.7(2) . . ?
O42 C42 O41 114.1(3) . . ?
O42 C42 C43 127.3(4) . . ?
O41 C42 C43 118.6(3) . . ?
C44 C43 C51 120.5(3) . . ?
C44 C43 C42 119.8(3) . . ?
C51 C43 C42 119.6(3) . . ?
O43 C44 C43 124.7(3) . . ?
O43 C44 C45 117.1(3) . . ?
C43 C44 C45 118.2(3) . . ?
C50 C45 C46 118.0(4) . . ?
C50 C45 C44 119.8(3) . . ?
C46 C45 C44 122.2(3) . . ?
C47 C46 C45 120.2(4) . . ?
C47 C46 H46A 119.9 . . ?
C45 C46 H46A 119.9 . . ?
C46 C47 C48 120.8(4) . . ?
C46 C47 H47A 119.6 . . ?
C48 C47 H47A 119.6 . . ?
C49 C48 C47 119.7(4) . . ?
C49 C48 H48A 120.2 . . ?
C47 C48 H48A 120.2 . . ?
C48 C49 C50 119.6(4) . . ?
C48 C49 H49A 120.2 . . ?
C50 C49 H49A 120.2 . . ?
C45 C50 O41 121.4(4) . . ?
C45 C50 C49 121.7(4) . . ?
O41 C50 C49 116.9(4) . . ?
O44 C51 C43 121.9(3) . . ?
O44 C51 C52 115.3(3) . . ?
C43 C51 C52 122.7(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C62 N61 C74 116.6(3) . . ?
C62 N61 Tb1 124.1(2) . . ?
C74 N61 Tb1 118.2(2) . . ?
N61 C62 C63 124.1(4) . . ?
N61 C62 H62A 117.9 . . ?
C63 C62 H62A 117.9 . . ?
C64 C63 C62 118.8(4) . . ?
C64 C63 H63A 120.6 . . ?
C62 C63 H63A 120.6 . . ?
C63 C64 C65 119.9(4) . . ?
C63 C64 H64A 120.1 . . ?
C65 C64 H64A 120.1 . . ?
C74 C65 C64 116.8(4) . . ?
C74 C65 C66 120.3(4) . . ?
C64 C65 C66 122.9(4) . . ?
C67 C66 C65 120.6(4) . . ?
C67 C66 H66A 119.7 . . ?
C65 C66 H66A 119.7 . . ?
C66 C67 C68 121.6(4) . . ?
C66 C67 H67A 119.2 . . ?
C68 C67 H67A 119.2 . . ?
C73 C68 C69 117.2(4) . . ?
C73 C68 C67 119.1(3) . . ?
C69 C68 C67 123.6(4) . . ?
C70 C69 C68 119.9(4) . . ?
C70 C69 H69A 120.1 . . ?
C68 C69 H69A 120.1 . . ?
C69 C70 C71 118.6(4) . . ?
C69 C70 H70A 120.7 . . ?
C71 C70 H70A 120.7 . . ?
N72 C71 C70 124.1(4) . . ?
N72 C71 H71A 117.9 . . ?
C70 C71 H71A 117.9 . . ?
C71 N72 C73 117.1(3) . . ?
C71 N72 Tb1 124.4(2) . . ?
C73 N72 Tb1 117.8(2) . . ?
N72 C73 C68 122.9(3) . . ?
N72 C73 C74 117.6(3) . . ?
C68 C73 C74 119.4(3) . . ?
N61 C74 C65 123.7(3) . . ?
N61 C74 C73 117.5(3) . . ?
C65 C74 C73 118.8(3) . . ?
H81A O81 H81B 100(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O43 2.289(2) . ?
Tb1 O23 2.322(2) . ?
Tb1 O24 2.333(2) . ?
Tb1 O3 2.335(2) . ?
Tb1 O4 2.342(3) . ?
Tb1 O44 2.348(2) . ?
Tb1 N61 2.537(3) . ?
Tb1 N72 2.544(3) . ?
O1 C10 1.368(5) . ?
O1 C2 1.386(6) . ?
O2 C2 1.212(5) . ?
O3 C4 1.261(4) . ?
O4 C11 1.252(5) . ?
C2 C3 1.451(6) . ?
C3 C4 1.424(5) . ?
C3 C11 1.438(6) . ?
C4 C5 1.464(5) . ?
C5 C10 1.372(6) . ?
C5 C6 1.379(5) . ?
C6 C7 1.368(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.370(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.346(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.398(6) . ?
C9 H9A 0.9300 . ?
C11 C12 1.504(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.370(4) . ?
O21 C22 1.381(4) . ?
O22 C22 1.214(4) . ?
O23 C24 1.270(3) . ?
O24 C31 1.234(4) . ?
C22 C23 1.438(4) . ?
C23 C24 1.429(4) . ?
C23 C31 1.436(4) . ?
C24 C25 1.471(4) . ?
C25 C30 1.371(4) . ?
C25 C26 1.378(4) . ?
C26 C27 1.385(5) . ?
C26 H26A 0.9300 . ?
C27 C28 1.388(6) . ?
C27 H27A 0.9300 . ?
C28 C29 1.353(5) . ?
C28 H28A 0.9300 . ?
C29 C30 1.386(5) . ?
C29 H29A 0.9300 . ?
C31 C32 1.515(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.379(4) . ?
O41 C42 1.385(4) . ?
O42 C42 1.207(4) . ?
O43 C44 1.264(4) . ?
O44 C51 1.252(4) . ?
C42 C43 1.451(5) . ?
C43 C44 1.420(4) . ?
C43 C51 1.440(5) . ?
C44 C45 1.460(5) . ?
C45 C50 1.375(5) . ?
C45 C46 1.403(5) . ?
C46 C47 1.369(5) . ?
C46 H46A 0.9300 . ?
C47 C48 1.380(6) . ?
C47 H47A 0.9300 . ?
C48 C49 1.373(6) . ?
C48 H48A 0.9300 . ?
C49 C50 1.380(5) . ?
C49 H49A 0.9300 . ?
C51 C52 1.508(4) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N61 C62 1.334(4) . ?
N61 C74 1.357(4) . ?
C62 C63 1.391(5) . ?
C62 H62A 0.9300 . ?
C63 C64 1.358(5) . ?
C63 H63A 0.9300 . ?
C64 C65 1.413(5) . ?
C64 H64A 0.9300 . ?
C65 C74 1.402(5) . ?
C65 C66 1.421(5) . ?
C66 C67 1.336(5) . ?
C66 H66A 0.9300 . ?
C67 C68 1.430(5) . ?
C67 H67A 0.9300 . ?
C68 C73 1.405(5) . ?
C68 C69 1.408(5) . ?
C69 C70 1.360(5) . ?
C69 H69A 0.9300 . ?
C70 C71 1.400(5) . ?
C70 H70A 0.9300 . ?
C71 N72 1.323(4) . ?
C71 H71A 0.9300 . ?
N72 C73 1.363(4) . ?
C73 C74 1.444(5) . ?
O81 H81A 0.88(2) . ?
O81 H81B 0.87(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C12 H12A O81 0.96 2.06 2.949(12) 153.1 . no
C12 H12C O2 0.96 2.59 3.518(7) 161.7 2_567 no
C52 H52C O43 0.96 2.62 3.419(4) 141.0 2_667 no
C71 H71A O2 0.93 2.55 3.233(5) 130.4 2_567 no
O81 H81A O22 0.88(2) 2.39(6) 3.127(10) 142(8) 2_556 no
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 173.8(4) . . . . ?
C10 O1 C2 C3 -5.4(7) . . . . ?
O2 C2 C3 C4 -169.8(5) . . . . ?
O1 C2 C3 C4 9.3(6) . . . . ?
O2 C2 C3 C11 10.0(7) . . . . ?
O1 C2 C3 C11 -170.9(4) . . . . ?
Tb1 O3 C4 C3 -32.9(5) . . . . ?
Tb1 O3 C4 C5 147.4(2) . . . . ?
C11 C3 C4 O3 -7.0(6) . . . . ?
C2 C3 C4 O3 172.7(3) . . . . ?
C11 C3 C4 C5 172.8(3) . . . . ?
C2 C3 C4 C5 -7.5(5) . . . . ?
O3 C4 C5 C10 -178.3(3) . . . . ?
C3 C4 C5 C10 1.9(5) . . . . ?
O3 C4 C5 C6 0.8(5) . . . . ?
C3 C4 C5 C6 -179.0(3) . . . . ?
C10 C5 C6 C7 0.0(6) . . . . ?
C4 C5 C6 C7 -179.1(4) . . . . ?
C5 C6 C7 C8 -1.9(8) . . . . ?
C6 C7 C8 C9 2.4(9) . . . . ?
C7 C8 C9 C10 -1.1(9) . . . . ?
C2 O1 C10 C5 -0.3(6) . . . . ?
C2 O1 C10 C9 -178.7(4) . . . . ?
C6 C5 C10 O1 -177.1(4) . . . . ?
C4 C5 C10 O1 2.1(6) . . . . ?
C6 C5 C10 C9 1.3(6) . . . . ?
C4 C5 C10 C9 -179.5(4) . . . . ?
C8 C9 C10 O1 177.6(5) . . . . ?
C8 C9 C10 C5 -0.8(8) . . . . ?
Tb1 O4 C11 C3 20.6(6) . . . . ?
Tb1 O4 C11 C12 -162.0(3) . . . . ?
C4 C3 C11 O4 13.5(6) . . . . ?
C2 C3 C11 O4 -166.3(4) . . . . ?
C4 C3 C11 C12 -163.7(4) . . . . ?
C2 C3 C11 C12 16.5(6) . . . . ?
C30 O21 C22 O22 178.3(4) . . . . ?
C30 O21 C22 C23 -2.2(6) . . . . ?
O22 C22 C23 C24 -177.1(4) . . . . ?
O21 C22 C23 C24 3.4(6) . . . . ?
O22 C22 C23 C31 5.7(7) . . . . ?
O21 C22 C23 C31 -173.7(3) . . . . ?
Tb1 O23 C24 C23 -0.4(6) . . . . ?
Tb1 O23 C24 C25 -178.9(2) . . . . ?
C31 C23 C24 O23 -4.1(5) . . . . ?
C22 C23 C24 O23 178.7(4) . . . . ?
C31 C23 C24 C25 174.3(3) . . . . ?
C22 C23 C24 C25 -2.8(5) . . . . ?
O23 C24 C25 C30 179.6(3) . . . . ?
C23 C24 C25 C30 1.0(5) . . . . ?
O23 C24 C25 C26 0.5(5) . . . . ?
C23 C24 C25 C26 -178.0(3) . . . . ?
C30 C25 C26 C27 0.2(6) . . . . ?
C24 C25 C26 C27 179.2(3) . . . . ?
C25 C26 C27 C28 -0.8(6) . . . . ?
C26 C27 C28 C29 0.9(7) . . . . ?
C27 C28 C29 C30 -0.4(7) . . . . ?
C22 O21 C30 C25 0.4(5) . . . . ?
C22 O21 C30 C29 179.5(4) . . . . ?
C26 C25 C30 O21 179.3(3) . . . . ?
C24 C25 C30 O21 0.3(5) . . . . ?
C26 C25 C30 C29 0.2(6) . . . . ?
C24 C25 C30 C29 -178.8(3) . . . . ?
C28 C29 C30 O21 -179.3(4) . . . . ?
C28 C29 C30 C25 -0.1(6) . . . . ?
Tb1 O24 C31 C23 4.4(7) . . . . ?
Tb1 O24 C31 C32 -177.3(3) . . . . ?
C24 C23 C31 O24 2.5(6) . . . . ?
C22 C23 C31 O24 179.6(4) . . . . ?
C24 C23 C31 C32 -175.7(4) . . . . ?
C22 C23 C31 C32 1.5(6) . . . . ?
C50 O41 C42 O42 -178.8(3) . . . . ?
C50 O41 C42 C43 0.6(5) . . . . ?
O42 C42 C43 C44 179.9(4) . . . . ?
O41 C42 C43 C44 0.5(5) . . . . ?
O42 C42 C43 C51 -2.2(6) . . . . ?
O41 C42 C43 C51 178.4(3) . . . . ?
Tb1 O43 C44 C43 38.3(4) . . . . ?
Tb1 O43 C44 C45 -142.4(2) . . . . ?
C51 C43 C44 O43 0.2(5) . . . . ?
C42 C43 C44 O43 178.1(3) . . . . ?
C51 C43 C44 C45 -179.0(3) . . . . ?
C42 C43 C44 C45 -1.2(5) . . . . ?
O43 C44 C45 C50 -178.6(3) . . . . ?
C43 C44 C45 C50 0.7(5) . . . . ?
O43 C44 C45 C46 2.8(5) . . . . ?
C43 C44 C45 C46 -177.9(3) . . . . ?
C50 C45 C46 C47 1.0(6) . . . . ?
C44 C45 C46 C47 179.6(4) . . . . ?
C45 C46 C47 C48 -0.3(7) . . . . ?
C46 C47 C48 C49 -0.2(8) . . . . ?
C47 C48 C49 C50 0.1(7) . . . . ?
C46 C45 C50 O41 179.2(3) . . . . ?
C44 C45 C50 O41 0.5(5) . . . . ?
C46 C45 C50 C49 -1.1(6) . . . . ?
C44 C45 C50 C49 -179.8(4) . . . . ?
C42 O41 C50 C45 -1.2(6) . . . . ?
C42 O41 C50 C49 179.1(4) . . . . ?
C48 C49 C50 C45 0.6(7) . . . . ?
C48 C49 C50 O41 -179.7(4) . . . . ?
Tb1 O44 C51 C43 -26.4(5) . . . . ?
Tb1 O44 C51 C52 152.6(2) . . . . ?
C44 C43 C51 O44 -6.1(5) . . . . ?
C42 C43 C51 O44 176.1(3) . . . . ?
C44 C43 C51 C52 175.1(3) . . . . ?
C42 C43 C51 C52 -2.7(5) . . . . ?
C74 N61 C62 C63 1.5(5) . . . . ?
Tb1 N61 C62 C63 -166.3(3) . . . . ?
N61 C62 C63 C64 1.2(6) . . . . ?
C62 C63 C64 C65 -1.9(6) . . . . ?
C63 C64 C65 C74 0.0(6) . . . . ?
C63 C64 C65 C66 -177.8(4) . . . . ?
C74 C65 C66 C67 -3.2(6) . . . . ?
C64 C65 C66 C67 174.6(4) . . . . ?
C65 C66 C67 C68 -0.5(6) . . . . ?
C66 C67 C68 C73 4.0(6) . . . . ?
C66 C67 C68 C69 -174.3(4) . . . . ?
C73 C68 C69 C70 -0.2(5) . . . . ?
C67 C68 C69 C70 178.1(4) . . . . ?
C68 C69 C70 C71 2.5(6) . . . . ?
C69 C70 C71 N72 -1.2(6) . . . . ?
C70 C71 N72 C73 -2.4(5) . . . . ?
C70 C71 N72 Tb1 167.4(3) . . . . ?
C71 N72 C73 C68 4.8(5) . . . . ?
Tb1 N72 C73 C68 -165.6(3) . . . . ?
C71 N72 C73 C74 -173.4(3) . . . . ?
Tb1 N72 C73 C74 16.1(4) . . . . ?
C69 C68 C73 N72 -3.6(5) . . . . ?
C67 C68 C73 N72 178.0(3) . . . . ?
C69 C68 C73 C74 174.6(3) . . . . ?
C67 C68 C73 C74 -3.7(5) . . . . ?
C62 N61 C74 C65 -3.6(5) . . . . ?
Tb1 N61 C74 C65 164.9(3) . . . . ?
C62 N61 C74 C73 173.9(3) . . . . ?
Tb1 N61 C74 C73 -17.6(4) . . . . ?
C64 C65 C74 N61 2.8(5) . . . . ?
C66 C65 C74 N61 -179.2(3) . . . . ?
C64 C65 C74 C73 -174.6(3) . . . . ?
C66 C65 C74 C73 3.3(5) . . . . ?
N72 C73 C74 N61 0.9(5) . . . . ?
C68 C73 C74 N61 -177.4(3) . . . . ?
N72 C73 C74 C65 178.5(3) . . . . ?
C68 C73 C74 C65 0.2(5) . . . . ?
