#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316439.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_4316439
loop_
_publ_author_name
'Ghulam Abbas'
'Yanhua Lan'
'George E. Kostakis'
'Wolfgang Wernsdorfer'
'Christopher E. Anson'
'Annie K. Powell'
_publ_contact_author
; 
Annie K. Powell
;
_publ_contact_author_email       annie.powell@kit.edu
_publ_contact_author_phone       '+49 721 608 2135'
_publ_section_title
;
 Series of Isostructural Planar Lanthanide Complexes
 [LnIII4(μ3-OH)2(mdeaH)2(piv)8] with Single Molecule Magnet Behavior for
 the Dy4 Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8067
_journal_page_last               8072
_journal_paper_doi               10.1021/ic1011605
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C50 H98 N2 O22 Tb4'
_chemical_formula_weight         1714.98
_chemical_name_systematic
; 
 ? 
;
_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                109.679(19)
_cell_angle_beta                 98.642(19)
_cell_angle_gamma                102.994(17)
_cell_formula_units_Z            1
_cell_length_a                   11.690(2)
_cell_length_b                   12.590(3)
_cell_length_c                   12.785(4)
_cell_measurement_reflns_used    4764
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      1.74
_cell_volume                     1673.2(8)
_computing_cell_refinement       'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_data_collection       'WinXpose 1.05 (Stoe & Cie GmbH, 2000)'
_computing_data_reduction        'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1824
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9504
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    4.243
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.954
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5913
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1605
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0486P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                3005
_reflns_number_total             5913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011605_si_002_1.cif
_cod_data_source_block           ga18
_cod_original_cell_volume        1673.2(7)
_cod_database_code               4316439
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.39738(7) 0.33324(7) 0.39457(8) 0.0397(3) Uani 1 1 d . . .
Tb2 Tb 0.72801(7) 0.42041(7) 0.43672(8) 0.0383(3) Uani 1 1 d . . .
O1 O 0.5638(9) 0.4984(9) 0.4232(10) 0.036(3) Uani 1 1 d D . .
H1 H 0.556(15) 0.517(14) 0.363(9) 0.044 Uiso 1 1 d D . .
N1 N 0.7490(12) 0.2106(11) 0.3984(12) 0.043(3) Uani 1 1 d . . .
C1 C 0.7038(18) 0.1864(17) 0.4947(18) 0.064(6) Uani 1 1 d . . .
H1A H 0.7592 0.2426 0.5691 0.076 Uiso 1 1 calc R . .
H1B H 0.7025 0.1054 0.4879 0.076 Uiso 1 1 calc R . .
C2 C 0.5772(16) 0.1989(18) 0.491(2) 0.073(7) Uani 1 1 d . . .
H2A H 0.5174 0.1283 0.4294 0.088 Uiso 1 1 calc R . .
H2B H 0.5570 0.2053 0.5647 0.088 Uiso 1 1 calc R . .
O2 O 0.5722(10) 0.3026(9) 0.4690(10) 0.045(3) Uani 1 1 d . . .
C3 C 0.8761(17) 0.2161(16) 0.406(2) 0.068(6) Uani 1 1 d . . .
H3A H 0.8824 0.1347 0.3788 0.081 Uiso 1 1 calc R . .
H3B H 0.9212 0.2563 0.4880 0.081 Uiso 1 1 calc R . .
C4 C 0.9344(17) 0.2797(14) 0.3392(18) 0.055(5) Uani 1 1 d . . .
H4A H 0.8978 0.2358 0.2560 0.066 Uiso 1 1 calc R . .
H4B H 1.0224 0.2889 0.3542 0.066 Uiso 1 1 calc R . .
O3 O 0.9119(9) 0.3979(10) 0.3791(11) 0.050(3) Uani 1 1 d D . .
H3 H 0.964(13) 0.451(12) 0.366(16) 0.060 Uiso 1 1 d D . .
C5 C 0.6690(18) 0.1177(16) 0.292(2) 0.073(7) Uani 1 1 d . . .
H5A H 0.6824 0.0417 0.2849 0.109 Uiso 1 1 calc R . .
H5B H 0.6869 0.1362 0.2263 0.109 Uiso 1 1 calc R . .
H5C H 0.5844 0.1130 0.2928 0.109 Uiso 1 1 calc R . .
O4 O 0.7155(9) 0.5415(9) 0.6367(10) 0.040(3) Uani 1 1 d . . .
O5 O 0.8676(9) 0.4668(9) 0.6202(9) 0.040(3) Uani 1 1 d . . .
C6 C 0.8055(14) 0.5162(13) 0.6831(15) 0.036(4) Uani 1 1 d . A .
C7 C 0.8275(14) 0.5297(13) 0.8075(17) 0.052(5) Uani 1 1 d D . .
C8A C 0.958(2) 0.617(2) 0.868(3) 0.101(13) Uiso 0.64 1 d PD A 1
H8A1 H 1.0166 0.5835 0.8310 0.151 Uiso 0.64 1 calc PR A 1
H8A2 H 0.9768 0.6288 0.9488 0.151 Uiso 0.64 1 calc PR A 1
H8A3 H 0.9617 0.6926 0.8607 0.151 Uiso 0.64 1 calc PR A 1
C9A C 0.829(2) 0.4131(19) 0.824(3) 0.055(7) Uiso 0.64 1 d PD A 1
H9A1 H 0.8855 0.3793 0.7850 0.083 Uiso 0.64 1 calc PR A 1
H9A2 H 0.7471 0.3568 0.7922 0.083 Uiso 0.64 1 calc PR A 1
H9A3 H 0.8537 0.4298 0.9063 0.083 Uiso 0.64 1 calc PR A 1
C10A C 0.739(3) 0.582(3) 0.872(3) 0.100(13) Uiso 0.64 1 d PD A 1
H10A H 0.7612 0.5899 0.9523 0.150 Uiso 0.64 1 calc PR A 1
H10B H 0.6563 0.5291 0.8361 0.150 Uiso 0.64 1 calc PR A 1
H10C H 0.7435 0.6596 0.8700 0.150 Uiso 0.64 1 calc PR A 1
C8B C 0.868(4) 0.663(2) 0.883(4) 0.082(18) Uiso 0.36 1 d PD A 2
H8B1 H 0.8148 0.7010 0.8527 0.123 Uiso 0.36 1 calc PR A 2
H8B2 H 0.9517 0.6977 0.8817 0.123 Uiso 0.36 1 calc PR A 2
H8B3 H 0.8642 0.6735 0.9615 0.123 Uiso 0.36 1 calc PR A 2
C9B C 0.918(4) 0.471(4) 0.846(5) 0.09(2) Uiso 0.36 1 d PD A 2
H9B1 H 0.8929 0.3869 0.7957 0.130 Uiso 0.36 1 calc PR A 2
H9B2 H 0.9187 0.4780 0.9251 0.130 Uiso 0.36 1 calc PR A 2
H9B3 H 0.9987 0.5092 0.8424 0.130 Uiso 0.36 1 calc PR A 2
C10B C 0.701(3) 0.473(4) 0.821(6) 0.10(2) Uiso 0.36 1 d PD A 2
H10D H 0.6446 0.5153 0.8028 0.149 Uiso 0.36 1 calc PR A 2
H10E H 0.7072 0.4783 0.8997 0.149 Uiso 0.36 1 calc PR A 2
H10F H 0.6705 0.3900 0.7680 0.149 Uiso 0.36 1 calc PR A 2
O6 O 0.7131(13) 0.7301(10) 0.4868(13) 0.069(4) Uani 1 1 d . . .
O7 O 0.8210(10) 0.6023(10) 0.4343(11) 0.051(3) Uani 1 1 d . . .
C11 C 0.7766(15) 0.6839(16) 0.4254(16) 0.050(5) Uani 1 1 d . B .
C12 C 0.8033(15) 0.7331(14) 0.3361(17) 0.066(6) Uani 1 1 d D . .
C13A C 0.871(2) 0.8652(19) 0.402(3) 0.069(9) Uiso 0.64 1 d PD B 1
H13A H 0.8906 0.9014 0.3471 0.104 Uiso 0.64 1 calc PR B 1
H13B H 0.9465 0.8743 0.4541 0.104 Uiso 0.64 1 calc PR B 1
H13C H 0.8202 0.9042 0.4456 0.104 Uiso 0.64 1 calc PR B 1
C14A C 0.678(2) 0.715(3) 0.263(3) 0.097(12) Uiso 0.64 1 d PD B 1
H14A H 0.6886 0.7436 0.2016 0.145 Uiso 0.64 1 calc PR B 1
H14B H 0.6332 0.7582 0.3110 0.145 Uiso 0.64 1 calc PR B 1
H14C H 0.6338 0.6303 0.2289 0.145 Uiso 0.64 1 calc PR B 1
C15A C 0.878(2) 0.670(2) 0.262(2) 0.048(7) Uiso 0.64 1 d PD B 1
H15A H 0.8916 0.7043 0.2043 0.071 Uiso 0.64 1 calc PR B 1
H15B H 0.8348 0.5860 0.2232 0.071 Uiso 0.64 1 calc PR B 1
H15C H 0.9567 0.6810 0.3103 0.071 Uiso 0.64 1 calc PR B 1
C13B C 0.793(5) 0.856(3) 0.353(5) 0.069(16) Uiso 0.36 1 d PD B 2
H13D H 0.8084 0.8747 0.2871 0.104 Uiso 0.36 1 calc PR B 2
H13E H 0.8528 0.9145 0.4229 0.104 Uiso 0.36 1 calc PR B 2
H13F H 0.7114 0.8588 0.3609 0.104 Uiso 0.36 1 calc PR B 2
C14B C 0.703(6) 0.637(5) 0.235(8) 0.35(11) Uiso 0.36 1 d PD B 2
H14D H 0.7011 0.6582 0.1674 0.527 Uiso 0.36 1 calc PR B 2
H14E H 0.6250 0.6317 0.2546 0.527 Uiso 0.36 1 calc PR B 2
H14F H 0.7201 0.5613 0.2179 0.527 Uiso 0.36 1 calc PR B 2
C15B C 0.929(4) 0.724(6) 0.322(8) 0.14(4) Uiso 0.36 1 d PD B 2
H15D H 0.9505 0.7556 0.2642 0.211 Uiso 0.36 1 calc PR B 2
H15E H 0.9284 0.6415 0.2962 0.211 Uiso 0.36 1 calc PR B 2
H15F H 0.9891 0.7702 0.3950 0.211 Uiso 0.36 1 calc PR B 2
O8 O 0.4507(11) 0.2938(11) 0.2153(10) 0.056(3) Uani 1 1 d . . .
O9 O 0.6524(11) 0.3400(11) 0.2437(11) 0.056(3) Uani 1 1 d . . .
C16 C 0.5466(18) 0.3011(15) 0.1811(16) 0.050(5) Uani 1 1 d . C .
C17 C 0.5314(15) 0.2601(15) 0.0493(17) 0.062(5) Uani 1 1 d D . .
C18A C 0.629(2) 0.201(3) 0.012(3) 0.104(11) Uiso 0.76 1 d PD C 1
H18A H 0.6179 0.1760 -0.0712 0.155 Uiso 0.76 1 calc PR C 1
H18B H 0.6218 0.1319 0.0326 0.155 Uiso 0.76 1 calc PR C 1
H18C H 0.7098 0.2575 0.0508 0.155 Uiso 0.76 1 calc PR C 1
C19A C 0.549(2) 0.373(2) 0.020(3) 0.086(9) Uiso 0.76 1 d PD C 1
H19A H 0.5407 0.3502 -0.0622 0.129 Uiso 0.76 1 calc PR C 1
H19B H 0.6300 0.4273 0.0620 0.129 Uiso 0.76 1 calc PR C 1
H19C H 0.4877 0.4113 0.0433 0.129 Uiso 0.76 1 calc PR C 1
C20A C 0.4034(19) 0.175(2) -0.018(2) 0.064(7) Uiso 0.76 1 d PD C 1
H20A H 0.3971 0.1506 -0.1001 0.097 Uiso 0.76 1 calc PR C 1
H20B H 0.3425 0.2151 0.0028 0.097 Uiso 0.76 1 calc PR C 1
H20C H 0.3898 0.1051 0.0022 0.097 Uiso 0.76 1 calc PR C 1
C18B C 0.526(10) 0.127(4) 0.014(10) 0.12(4) Uiso 0.24 1 d PD C 2
H18D H 0.5184 0.0920 -0.0688 0.186 Uiso 0.24 1 calc PR C 2
H18E H 0.4556 0.0855 0.0327 0.186 Uiso 0.24 1 calc PR C 2
H18F H 0.6001 0.1211 0.0553 0.186 Uiso 0.24 1 calc PR C 2
C19B C 0.643(9) 0.324(9) 0.017(13) 0.17(6) Uiso 0.24 1 d PD C 2
H19D H 0.6362 0.2842 -0.0649 0.252 Uiso 0.24 1 calc PR C 2
H19E H 0.7171 0.3207 0.0615 0.252 Uiso 0.24 1 calc PR C 2
H19F H 0.6449 0.4062 0.0345 0.252 Uiso 0.24 1 calc PR C 2
C20B C 0.416(8) 0.273(10) -0.008(15) 0.17(7) Uiso 0.24 1 d PD C 2
H20D H 0.4086 0.2469 -0.0906 0.259 Uiso 0.24 1 calc PR C 2
H20E H 0.4167 0.3555 0.0234 0.259 Uiso 0.24 1 calc PR C 2
H20F H 0.3466 0.2238 0.0063 0.259 Uiso 0.24 1 calc PR C 2
O10 O 0.3421(11) 0.1193(9) 0.3091(11) 0.053(3) Uani 1 1 d . . .
O11 O 0.2068(10) 0.2051(10) 0.2674(12) 0.060(4) Uani 1 1 d . . .
C21 C 0.2389(16) 0.1109(15) 0.2607(16) 0.049(5) Uani 1 1 d . . .
C22 C 0.1474(16) -0.0097(17) 0.185(2) 0.067(6) Uani 1 1 d . . .
C23 C 0.181(2) -0.1037(19) 0.225(3) 0.112(10) Uani 1 1 d . . .
H23A H 0.1763 -0.0851 0.3049 0.167 Uiso 1 1 calc R . .
H23B H 0.2633 -0.1042 0.2192 0.167 Uiso 1 1 calc R . .
H23C H 0.1240 -0.1816 0.1767 0.167 Uiso 1 1 calc R . .
C24 C 0.0193(17) -0.0036(17) 0.197(2) 0.081(8) Uani 1 1 d . . .
H24A H 0.0151 0.0114 0.2764 0.121 Uiso 1 1 calc R . .
H24B H -0.0406 -0.0787 0.1459 0.121 Uiso 1 1 calc R . .
H24C H 0.0022 0.0605 0.1763 0.121 Uiso 1 1 calc R . .
C25 C 0.154(2) -0.0328(18) 0.0617(19) 0.086(8) Uani 1 1 d . . .
H25A H 0.2365 -0.0340 0.0548 0.129 Uiso 1 1 calc R . .
H25B H 0.1347 0.0298 0.0401 0.129 Uiso 1 1 calc R . .
H25C H 0.0964 -0.1092 0.0108 0.129 Uiso 1 1 calc R . .
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
_geom_angle_publ_flag
O2 Tb1 O6 94.9(5) . 2_666 ?
O2 Tb1 O4 151.7(4) . 2_666 ?
O6 Tb1 O4 96.5(4) 2_666 2_666 ?
O2 Tb1 O8 89.6(4) . . ?
O6 Tb1 O8 150.0(4) 2_666 . ?
O4 Tb1 O8 93.3(4) 2_666 . ?
O2 Tb1 O1 71.6(4) . . ?
O6 Tb1 O1 135.4(4) 2_666 . ?
O4 Tb1 O1 82.2(3) 2_666 . ?
O8 Tb1 O1 74.0(4) . . ?
O2 Tb1 O11 133.9(4) . . ?
O6 Tb1 O11 75.5(5) 2_666 . ?
O4 Tb1 O11 74.2(4) 2_666 . ?
O8 Tb1 O11 80.1(4) . . ?
O1 Tb1 O11 143.6(4) . . ?
O2 Tb1 O10 79.5(4) . . ?
O6 Tb1 O10 75.4(4) 2_666 . ?
O4 Tb1 O10 128.4(4) 2_666 . ?
O8 Tb1 O10 76.4(4) . . ?
O1 Tb1 O10 138.3(4) . . ?
O11 Tb1 O10 54.4(4) . . ?
O2 Tb1 O1 87.6(4) . 2_666 ?
O6 Tb1 O1 71.4(4) 2_666 2_666 ?
O4 Tb1 O1 71.8(4) 2_666 2_666 ?
O8 Tb1 O1 138.5(4) . 2_666 ?
O1 Tb1 O1 65.8(4) . 2_666 ?
O11 Tb1 O1 128.6(4) . 2_666 ?
O10 Tb1 O1 143.1(4) . 2_666 ?
O2 Tb2 O9 93.7(4) . . ?
O2 Tb2 O7 149.2(4) . . ?
O9 Tb2 O7 92.3(5) . . ?
O2 Tb2 O1 72.7(4) . . ?
O9 Tb2 O1 80.2(4) . . ?
O7 Tb2 O1 78.6(4) . . ?
O2 Tb2 O3 134.9(4) . . ?
O9 Tb2 O3 81.1(4) . . ?
O7 Tb2 O3 75.9(4) . . ?
O1 Tb2 O3 147.5(4) . . ?
O2 Tb2 O5 94.7(4) . . ?
O9 Tb2 O5 157.3(3) . . ?
O7 Tb2 O5 91.2(4) . . ?
O1 Tb2 O5 122.5(4) . . ?
O3 Tb2 O5 78.0(4) . . ?
O2 Tb2 O4 75.8(4) . . ?
O9 Tb2 O4 150.6(4) . . ?
O7 Tb2 O4 84.3(4) . . ?
O1 Tb2 O4 70.5(3) . . ?
O3 Tb2 O4 125.8(4) . . ?
O5 Tb2 O4 52.1(3) . . ?
O2 Tb2 N1 67.5(4) . . ?
O9 Tb2 N1 81.6(4) . . ?
O7 Tb2 N1 143.3(4) . . ?
O1 Tb2 N1 134.7(4) . . ?
O3 Tb2 N1 67.4(4) . . ?
O5 Tb2 N1 82.2(4) . . ?
O4 Tb2 N1 117.7(4) . . ?
Tb2 O1 Tb1 101.6(4) . . ?
Tb2 O1 Tb1 106.6(4) . 2_666 ?
Tb1 O1 Tb1 114.2(4) . 2_666 ?
Tb2 O1 H1 110(10) . . ?
Tb1 O1 H1 110(10) . . ?
Tb1 O1 H1 114(10) 2_666 . ?
C3 N1 C5 112.3(14) . . ?
C3 N1 C1 112.9(15) . . ?
C5 N1 C1 106.3(15) . . ?
C3 N1 Tb2 108.8(10) . . ?
C5 N1 Tb2 115.1(11) . . ?
C1 N1 Tb2 100.9(9) . . ?
N1 C1 C2 110.2(16) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
O2 C2 C1 109.2(16) . . ?
O2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
C2 O2 Tb2 124.1(9) . . ?
C2 O2 Tb1 124.3(10) . . ?
Tb2 O2 Tb1 107.7(5) . . ?
N1 C3 C4 113.7(17) . . ?
N1 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 O3 105.5(14) . . ?
C3 C4 H4A 110.7 . . ?
O3 C4 H4A 110.7 . . ?
C3 C4 H4B 110.7 . . ?
O3 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
C4 O3 Tb2 121.1(9) . . ?
C4 O3 H3 112(10) . . ?
Tb2 O3 H3 125(10) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 O4 Tb1 155.9(10) . 2_666 ?
C6 O4 Tb2 91.5(9) . . ?
Tb1 O4 Tb2 103.7(4) 2_666 . ?
C6 O5 Tb2 96.3(10) . . ?
O5 C6 O4 118.8(15) . . ?
O5 C6 C7 119.8(14) . . ?
O4 C6 C7 120.9(13) . . ?
C6 C7 C9B 116(3) . . ?
C6 C7 C8B 108(2) . . ?
C9B C7 C8B 110.0(17) . . ?
C6 C7 C10A 115(2) . . ?
C6 C7 C10B 104(3) . . ?
C9B C7 C10B 109.1(16) . . ?
C8B C7 C10B 108.6(16) . . ?
C6 C7 C9A 113.5(16) . . ?
C10A C7 C9A 108.1(14) . . ?
C6 C7 C8A 106.0(19) . . ?
C10A C7 C8A 107.7(14) . . ?
C9A C7 C8A 106.1(13) . . ?
C7 C8A H8A1 109.5 . . ?
C7 C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7 C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7 C9A H9A1 109.5 . . ?
C7 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C7 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C7 C10A H10A 109.5 . . ?
C7 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C7 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C7 C8B H8B1 109.5 . . ?
C7 C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7 C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7 C9B H9B1 109.5 . . ?
C7 C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7 C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C7 C10B H10D 109.5 . . ?
C7 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C7 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C11 O6 Tb1 131.6(12) . 2_666 ?
C11 O7 Tb2 130.4(10) . . ?
O6 C11 O7 125.6(18) . . ?
O6 C11 C12 115.4(16) . . ?
O7 C11 C12 119.0(15) . . ?
C11 C12 C13B 118(3) . . ?
C11 C12 C15A 112.7(16) . . ?
C11 C12 C15B 107(3) . . ?
C13B C12 C15B 111.3(18) . . ?
C11 C12 C14A 105(2) . . ?
C15A C12 C14A 110.6(13) . . ?
C11 C12 C14B 97(5) . . ?
C13B C12 C14B 111.4(19) . . ?
C15B C12 C14B 111.1(18) . . ?
C11 C12 C13A 106.4(19) . . ?
C15A C12 C13A 110.9(13) . . ?
C14A C12 C13A 111.3(13) . . ?
C12 C13A H13A 109.5 . . ?
C12 C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C12 C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C12 C14A H14A 109.5 . . ?
C12 C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C12 C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C12 C15A H15A 109.5 . . ?
C12 C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C12 C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C12 C13B H13D 109.5 . . ?
C12 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C12 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C12 C14B H14D 109.5 . . ?
C12 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C12 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C12 C15B H15D 109.5 . . ?
C12 C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C12 C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C16 O8 Tb1 136.9(12) . . ?
C16 O9 Tb2 132.9(11) . . ?
O9 C16 O8 125.9(17) . . ?
O9 C16 C17 117.7(15) . . ?
O8 C16 C17 116.5(17) . . ?
C20A C17 C18A 110.1(13) . . ?
C20B C17 C19B 111(4) . . ?
C20B C17 C16 111(6) . . ?
C20A C17 C16 111.6(17) . . ?
C18A C17 C16 110.9(19) . . ?
C19B C17 C16 113(6) . . ?
C20A C17 C19A 108.6(13) . . ?
C18A C17 C19A 108.3(13) . . ?
C16 C17 C19A 107.2(17) . . ?
C20B C17 C18B 111(4) . . ?
C19B C17 C18B 108.2(19) . . ?
C16 C17 C18B 102(5) . . ?
C17 C18A H18A 109.5 . . ?
C17 C18A H18B 109.5 . . ?
H18A C18A H18B 109.5 . . ?
C17 C18A H18C 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C17 C19A H19A 109.5 . . ?
C17 C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
C17 C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C17 C20A H20A 109.5 . . ?
C17 C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
C17 C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C17 C18B H18D 109.5 . . ?
C17 C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
C17 C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C17 C19B H19D 109.5 . . ?
C17 C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
C17 C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C17 C20B H20D 109.5 . . ?
C17 C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C17 C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C21 O10 Tb1 92.6(10) . . ?
C21 O11 Tb1 92.3(10) . . ?
O10 C21 O11 120.6(15) . . ?
O10 C21 C22 121.4(16) . . ?
O11 C21 C22 117.9(16) . . ?
C25 C22 C21 107.5(16) . . ?
C25 C22 C23 112(2) . . ?
C21 C22 C23 108.4(18) . . ?
C25 C22 C24 110(2) . . ?
C21 C22 C24 108.5(16) . . ?
C23 C22 C24 110.8(19) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
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 O2 2.291(11) . ?
Tb1 O6 2.355(13) 2_666 ?
Tb1 O4 2.364(10) 2_666 ?
Tb1 O8 2.385(12) . ?
Tb1 O1 2.386(11) . ?
Tb1 O11 2.395(11) . ?
Tb1 O10 2.427(10) . ?
Tb1 O1 2.460(11) 2_666 ?
Tb2 O2 2.261(11) . ?
Tb2 O9 2.270(13) . ?
Tb2 O7 2.317(11) . ?
Tb2 O1 2.354(10) . ?
Tb2 O3 2.419(10) . ?
Tb2 O5 2.450(11) . ?
Tb2 O4 2.544(11) . ?
Tb2 N1 2.594(13) . ?
O1 Tb1 2.460(11) 2_666 ?
O1 H1 0.87(4) . ?
N1 C3 1.46(2) . ?
N1 C5 1.47(2) . ?
N1 C1 1.50(2) . ?
C1 C2 1.52(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.44(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.50(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.501(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 H3 0.88(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O4 C6 1.285(18) . ?
O4 Tb1 2.364(10) 2_666 ?
O5 C6 1.266(17) . ?
C6 C7 1.52(2) . ?
C7 C9B 1.53(2) . ?
C7 C8B 1.54(2) . ?
C7 C10A 1.54(2) . ?
C7 C10B 1.55(2) . ?
C7 C9A 1.556(19) . ?
C7 C8A 1.56(2) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
O6 C11 1.25(2) . ?
O6 Tb1 2.355(13) 2_666 ?
O7 C11 1.28(2) . ?
C11 C12 1.51(3) . ?
C12 C13B 1.53(2) . ?
C12 C15A 1.533(19) . ?
C12 C15B 1.53(2) . ?
C12 C14A 1.53(2) . ?
C12 C14B 1.53(2) . ?
C12 C13A 1.539(19) . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
O8 C16 1.26(2) . ?
O9 C16 1.26(2) . ?
C16 C17 1.56(3) . ?
C17 C20B 1.50(8) . ?
C17 C20A 1.548(19) . ?
C17 C18A 1.55(2) . ?
C17 C19B 1.56(2) . ?
C17 C19A 1.56(2) . ?
C17 C18B 1.56(2) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
O10 C21 1.23(2) . ?
O11 C21 1.30(2) . ?
C21 C22 1.54(2) . ?
C22 C25 1.52(3) . ?
C22 C23 1.54(3) . ?
C22 C24 1.54(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
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
O3 H3 O5 0.88(4) 1.95(10) 2.749(15) 149(16) 2_766
