# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a
_audit_block_doi                 10.5517/ccdc.csd.cc201xss
_database_code_depnum_ccdc_archive 'CCDC 1848895'
_audit_update_record             
;
2018-06-12 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H84 N6 O7 Tb2'
_chemical_formula_weight         1391.23

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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.4450(18)
_cell_length_b                   13.4450(18)
_cell_length_c                   29.702(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4649.8(15)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7079
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      29.57

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2124
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7086
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         24.94
_reflns_number_total             1756
_reflns_number_gt                1502
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+280.1074P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1756
_refine_ls_number_parameters     125
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.2153
_refine_ls_wR_factor_gt          0.1906
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

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 0.0000 0.0000 0.08087(3) 0.0364(4) Uani 1 3 d SU . .
O1 O 0.1764(7) 0.1241(7) 0.0645(3) 0.0439(19) Uani 1 1 d U . .
N4 N 0.0610(8) 0.1438(7) 0.1434(3) 0.033(2) Uani 1 1 d . . .
C1 C -0.0482(10) 0.1256(10) 0.1636(4) 0.035(2) Uani 1 1 d . . .
H1A H -0.0870 0.1478 0.1416 0.042 Uiso 1 1 calc R . .
H1B H -0.0297 0.1763 0.1893 0.042 Uiso 1 1 calc R . .
C3 C 0.1185(10) 0.2571(9) 0.1227(4) 0.038(3) Uani 1 1 d . . .
H3A H 0.1252 0.3122 0.1452 0.045 Uiso 1 1 calc R . .
H3B H 0.0688 0.2576 0.0991 0.045 Uiso 1 1 calc R . .
C11 C 0.2573(9) 0.2315(9) 0.0729(4) 0.033(2) Uani 1 1 d . . .
C4 C 0.2360(9) 0.2995(9) 0.1025(4) 0.036(3) Uani 1 1 d . . .
C5 C 0.3168(10) 0.4130(10) 0.1070(5) 0.042(3) Uani 1 1 d . . .
H5 H 0.3012 0.4590 0.1258 0.051 Uiso 1 1 calc R . .
C8 C 0.4412(11) 0.3919(11) 0.0564(5) 0.050(3) Uani 1 1 d . . .
H8 H 0.5101 0.4237 0.0406 0.060 Uiso 1 1 calc R . .
C9 C 0.3632(10) 0.2766(11) 0.0507(4) 0.041(3) Uani 1 1 d . . .
C10 C 0.3848(13) 0.2027(14) 0.0197(6) 0.066(4) Uani 1 1 d . . .
H10A H 0.3251 0.1701 -0.0025 0.099 Uiso 1 1 calc R . .
H10B H 0.3856 0.1422 0.0366 0.099 Uiso 1 1 calc R . .
H10C H 0.4576 0.2481 0.0051 0.099 Uiso 1 1 calc R . .
C6 C 0.4217(10) 0.4621(10) 0.0845(5) 0.049(3) Uani 1 1 d . . .
C2 C 0.1347(10) 0.1308(10) 0.1788(4) 0.037(3) Uani 1 1 d . . .
H2A H 0.0912 0.1029 0.2065 0.045 Uiso 1 1 calc R . .
H2B H 0.2014 0.2053 0.1848 0.045 Uiso 1 1 calc R . .
O1W O 0.0000 0.0000 0.0000 0.068(4) Uani 1 6 d SU . .
C7 C 0.5074(14) 0.5888(12) 0.0884(6) 0.072(5) Uani 1 1 d . . .
H7A H 0.4697 0.6282 0.0997 0.108 Uiso 1 1 calc R . .
H7B H 0.5393 0.6187 0.0592 0.108 Uiso 1 1 calc R . .
H7C H 0.5678 0.6000 0.1086 0.108 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O1 2.166(8) 3 ?
Tb1 O1 2.166(8) . ?
Tb1 O1 2.166(8) 2 ?
Tb1 O1W 2.4019(12) . ?
Tb1 N4 2.505(9) . ?
Tb1 N4 2.505(9) 3 ?
Tb1 N4 2.505(9) 2 ?
O1 C11 1.327(13) . ?
N4 C3 1.456(14) . ?
N4 C1 1.489(13) . ?
N4 C2 1.513(14) . ?
C1 C2 1.516(16) 2 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C4 1.510(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C11 C9 1.402(15) . ?
C11 C4 1.398(17) . ?
C4 C5 1.367(15) . ?
C5 C6 1.393(19) . ?
C5 H5 0.9300 . ?
C8 C6 1.38(2) . ?
C8 C9 1.380(18) . ?
C8 H8 0.9300 . ?
C9 C10 1.48(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 C7 1.510(18) . ?
C2 C1 1.516(16) 3 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O1W Tb1 2.4019(12) 10 ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

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
O1 Tb1 O1 115.09(17) 3 . ?
O1 Tb1 O1 115.09(17) 3 2 ?
O1 Tb1 O1 115.09(17) . 2 ?
O1 Tb1 O1W 77.0(2) 3 . ?
O1 Tb1 O1W 77.0(2) . . ?
O1 Tb1 O1W 77.0(2) 2 . ?
O1 Tb1 N4 144.5(3) 3 . ?
O1 Tb1 N4 76.3(3) . . ?
O1 Tb1 N4 85.7(3) 2 . ?
O1W Tb1 N4 137.9(2) . . ?
O1 Tb1 N4 76.3(3) 3 3 ?
O1 Tb1 N4 85.7(3) . 3 ?
O1 Tb1 N4 144.5(3) 2 3 ?
O1W Tb1 N4 137.9(2) . 3 ?
N4 Tb1 N4 71.0(3) . 3 ?
O1 Tb1 N4 85.7(3) 3 2 ?
O1 Tb1 N4 144.5(3) . 2 ?
O1 Tb1 N4 76.3(3) 2 2 ?
O1W Tb1 N4 137.9(2) . 2 ?
N4 Tb1 N4 71.0(3) . 2 ?
N4 Tb1 N4 71.0(3) 3 2 ?
C11 O1 Tb1 141.4(7) . . ?
C3 N4 C1 107.8(9) . . ?
C3 N4 C2 112.2(8) . . ?
C1 N4 C2 110.5(9) . . ?
C3 N4 Tb1 106.9(7) . . ?
C1 N4 Tb1 104.9(6) . . ?
C2 N4 Tb1 114.0(6) . . ?
N4 C1 C2 115.3(9) . 2 ?
N4 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 2 . ?
N4 C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 2 . ?
H1A C1 H1B 107.5 . . ?
N4 C3 C4 118.1(9) . . ?
N4 C3 H3A 107.8 . . ?
C4 C3 H3A 107.8 . . ?
N4 C3 H3B 107.8 . . ?
C4 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
O1 C11 C9 119.0(11) . . ?
O1 C11 C4 120.4(10) . . ?
C9 C11 C4 120.6(10) . . ?
C5 C4 C11 118.9(11) . . ?
C5 C4 C3 118.7(11) . . ?
C11 C4 C3 121.3(9) . . ?
C4 C5 C6 122.2(12) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C6 C8 C9 123.0(12) . . ?
C6 C8 H8 118.5 . . ?
C9 C8 H8 118.5 . . ?
C8 C9 C11 117.7(12) . . ?
C8 C9 C10 122.3(11) . . ?
C11 C9 C10 119.9(11) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C6 C5 117.4(11) . . ?
C8 C6 C7 121.2(13) . . ?
C5 C6 C7 121.2(14) . . ?
N4 C2 C1 111.4(8) . 3 ?
N4 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 3 . ?
N4 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 3 . ?
H2A C2 H2B 108.0 . . ?
Tb1 O1W Tb1 180.0 10 . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

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
O1 Tb1 O1 C11 -164.5(11) 3 . . . ?
O1 Tb1 O1 C11 58.1(15) 2 . . . ?
O1W Tb1 O1 C11 126.8(12) . . . . ?
N4 Tb1 O1 C11 -20.3(12) . . . . ?
N4 Tb1 O1 C11 -91.9(12) 3 . . . ?
N4 Tb1 O1 C11 -43.7(15) 2 . . . ?
O1 Tb1 N4 C3 160.9(7) 3 . . . ?
O1 Tb1 N4 C3 46.8(7) . . . . ?
O1 Tb1 N4 C3 -70.3(7) 2 . . . ?
O1W Tb1 N4 C3 -5.2(8) . . . . ?
N4 Tb1 N4 C3 136.9(8) 3 . . . ?
N4 Tb1 N4 C3 -147.3(8) 2 . . . ?
O1 Tb1 N4 C1 -84.7(8) 3 . . . ?
O1 Tb1 N4 C1 161.1(7) . . . . ?
O1 Tb1 N4 C1 44.0(7) 2 . . . ?
O1W Tb1 N4 C1 109.1(6) . . . . ?
N4 Tb1 N4 C1 -108.8(6) 3 . . . ?
N4 Tb1 N4 C1 -33.0(7) 2 . . . ?
O1 Tb1 N4 C2 36.3(10) 3 . . . ?
O1 Tb1 N4 C2 -77.8(7) . . . . ?
O1 Tb1 N4 C2 165.0(7) 2 . . . ?
O1W Tb1 N4 C2 -129.9(6) . . . . ?
N4 Tb1 N4 C2 12.2(7) 3 . . . ?
N4 Tb1 N4 C2 88.0(6) 2 . . . ?
C3 N4 C1 C2 168.6(9) . . . 2 ?
C2 N4 C1 C2 -68.4(12) . . . 2 ?
Tb1 N4 C1 C2 54.9(10) . . . 2 ?
C1 N4 C3 C4 175.8(10) . . . . ?
C2 N4 C3 C4 53.9(13) . . . . ?
Tb1 N4 C3 C4 -71.9(10) . . . . ?
Tb1 O1 C11 C9 -176.7(9) . . . . ?
Tb1 O1 C11 C4 1.7(18) . . . . ?
O1 C11 C4 C5 -173.6(10) . . . . ?
C9 C11 C4 C5 4.8(17) . . . . ?
O1 C11 C4 C3 -5.3(16) . . . . ?
C9 C11 C4 C3 173.1(10) . . . . ?
N4 C3 C4 C5 -142.0(11) . . . . ?
N4 C3 C4 C11 49.7(15) . . . . ?
C11 C4 C5 C6 -2.7(18) . . . . ?
C3 C4 C5 C6 -171.3(11) . . . . ?
C6 C8 C9 C11 3(2) . . . . ?
C6 C8 C9 C10 178.9(13) . . . . ?
O1 C11 C9 C8 173.4(11) . . . . ?
C4 C11 C9 C8 -5.1(17) . . . . ?
O1 C11 C9 C10 -2.3(18) . . . . ?
C4 C11 C9 C10 179.3(12) . . . . ?
C9 C8 C6 C5 -1.4(19) . . . . ?
C9 C8 C6 C7 -177.6(13) . . . . ?
C4 C5 C6 C8 1.0(18) . . . . ?
C4 C5 C6 C7 177.2(12) . . . . ?
C3 N4 C2 C1 -110.8(10) . . . 3 ?
C1 N4 C2 C1 128.8(10) . . . 3 ?
Tb1 N4 C2 C1 11.0(11) . . . 3 ?
O1 Tb1 O1W Tb1 0(6) 3 . . 10 ?
O1 Tb1 O1W Tb1 0(23) . . . 10 ?
O1 Tb1 O1W Tb1 0(11) 2 . . 10 ?
N4 Tb1 O1W Tb1 0(20) . . . 10 ?
N4 Tb1 O1W Tb1 0(13) 3 . . 10 ?
N4 Tb1 O1W Tb1 0(3) 2 . . 10 ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        24.94
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         3.540
_refine_diff_density_min         -6.350
_refine_diff_density_rms         0.221
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc201xww
_database_code_depnum_ccdc_archive 'CCDC 1848898'
_audit_update_record             
;
2018-06-12 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H84 Cl N6 Ni2 O10 Tb'
_chemical_formula_weight         1433.18

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.2418(5)
_cell_length_b                   14.0078(6)
_cell_length_c                   20.9681(5)
_cell_angle_alpha                90.264(3)
_cell_angle_beta                 104.938(3)
_cell_angle_gamma                117.541(4)
_cell_volume                     3297.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10815
_cell_measurement_theta_min      3.9320
_cell_measurement_theta_max      28.5400

_exptl_crystal_description       strip
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36076
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         25.01
_reflns_number_total             11607
_reflns_number_gt                8395
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0422P)²+14.5745P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11607
_refine_ls_number_parameters     790
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1420
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001

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 0.0000 0.5000 0.0000 0.02636(13) Uani 1 2 d S . .
Ni1 Ni -0.06273(7) 0.28174(6) 0.04601(4) 0.02650(19) Uani 1 1 d . . .
C16 C 0.1855(5) 0.3794(6) 0.0290(3) 0.0323(15) Uani 1 1 d . . .
C20 C -0.1525(6) 0.4606(5) 0.1607(3) 0.0336(15) Uani 1 1 d . . .
C19 C -0.0758(5) 0.4248(5) 0.1488(3) 0.0263(14) Uani 1 1 d . . .
C28 C 0.2407(5) 0.7511(5) 0.0878(3) 0.0300(15) Uani 1 1 d . . .
C25 C -0.0415(6) 0.3830(6) 0.2617(3) 0.0405(17) Uani 1 1 d . . .
H25 H -0.0032 0.3579 0.2955 0.049 Uiso 1 1 calc R . .
C9 C 0.1592(6) 0.2800(6) -0.0031(3) 0.0362(16) Uani 1 1 d . . .
C14 C 0.3065(6) 0.4572(6) 0.0603(3) 0.0389(17) Uani 1 1 d . . .
C18 C -0.0181(6) 0.3883(5) 0.2005(3) 0.0298(14) Uani 1 1 d . . .
C30 C 0.4375(6) 0.9027(6) 0.1109(4) 0.0448(18) Uani 1 1 d . . .
H30 H 0.5003 0.9499 0.0955 0.054 Uiso 1 1 calc R . .
C29 C 0.3347(6) 0.8228(5) 0.0648(3) 0.0343(15) Uani 1 1 d . . .
C31 C 0.4501(6) 0.9150(6) 0.1779(4) 0.0464(19) Uani 1 1 d . . .
C27 C 0.2517(6) 0.7602(5) 0.1564(3) 0.0366(16) Uani 1 1 d . . .
C33 C 0.3562(6) 0.8428(6) 0.1989(4) 0.0443(18) Uani 1 1 d . . .
H33 H 0.3632 0.8497 0.2442 0.053 Uiso 1 1 calc R . .
C23 C -0.1209(7) 0.4146(7) 0.2731(3) 0.0479(19) Uani 1 1 d . . .
C10 C 0.2501(7) 0.2588(6) -0.0058(4) 0.0457(18) Uani 1 1 d . . .
H10 H 0.2311 0.1927 -0.0284 0.055 Uiso 1 1 calc R . .
C22 C -0.1749(7) 0.4524(7) 0.2222(4) 0.049(2) Uani 1 1 d . . .
H22 H -0.2287 0.4735 0.2292 0.058 Uiso 1 1 calc R . .
C13 C 0.3943(6) 0.4311(7) 0.0567(4) 0.0479(19) Uani 1 1 d . . .
H13 H 0.4736 0.4816 0.0772 0.057 Uiso 1 1 calc R . .
C11 C 0.3688(7) 0.3333(7) 0.0240(4) 0.055(2) Uani 1 1 d . . .
C21 C -0.2063(7) 0.5086(7) 0.1078(4) 0.053(2) Uani 1 1 d . . .
H21A H -0.1458 0.5788 0.1038 0.079 Uiso 1 1 calc R . .
H21B H -0.2678 0.5163 0.1196 0.079 Uiso 1 1 calc R . .
H21C H -0.2398 0.4617 0.0660 0.079 Uiso 1 1 calc R . .
C24 C -0.1465(10) 0.4076(9) 0.3401(4) 0.078(3) Uani 1 1 d . . .
H24A H -0.1051 0.4790 0.3655 0.117 Uiso 1 1 calc R . .
H24B H -0.1199 0.3612 0.3641 0.117 Uiso 1 1 calc R . .
H24C H -0.2306 0.3781 0.3330 0.117 Uiso 1 1 calc R . .
C12 C 0.4673(8) 0.3077(9) 0.0199(6) 0.091(4) Uani 1 1 d . . .
H12A H 0.5151 0.3126 0.0641 0.136 Uiso 1 1 calc R . .
H12B H 0.5164 0.3590 -0.0038 0.136 Uiso 1 1 calc R . .
H12C H 0.4325 0.2354 -0.0033 0.136 Uiso 1 1 calc R . .
Tb2 Tb 0.5000 0.5000 0.5000 0.03797(15) Uani 1 2 d S . .
Ni2 Ni 0.61754(8) 0.64068(7) 0.40558(4) 0.0414(2) Uani 1 1 d . . .
O6 O 0.3143(4) 0.3616(4) 0.4913(2) 0.0458(13) Uani 1 1 d . . .
O4 O 0.5381(4) 0.4693(4) 0.4037(2) 0.0451(13) Uani 1 1 d . . .
O5 O 0.4705(4) 0.6229(4) 0.4362(2) 0.0423(12) Uani 1 1 d . . .
N6 N 0.6773(6) 0.8056(5) 0.4027(3) 0.0481(16) Uani 1 1 d . . .
N5 N 0.5472(6) 0.6210(5) 0.3028(3) 0.0448(15) Uani 1 1 d . . .
C52 C 0.4283(7) 0.6942(6) 0.4240(3) 0.0444(18) Uani 1 1 d . . .
C41 C 0.5044(6) 0.3990(6) 0.3480(3) 0.0433(18) Uani 1 1 d . . .
C59 C 0.1954(7) 0.3066(6) 0.4620(4) 0.0457(19) Uani 1 1 d . . .
N4 N 0.7736(6) 0.6703(5) 0.3865(3) 0.0496(16) Uani 1 1 d . . .
C49 C 0.4355(7) 0.5173(6) 0.2797(4) 0.051(2) Uani 1 1 d . . .
H49A H 0.3967 0.5160 0.2334 0.061 Uiso 1 1 calc R . .
H49B H 0.3830 0.5138 0.3055 0.061 Uiso 1 1 calc R . .
C42 C 0.5194(7) 0.3074(6) 0.3521(3) 0.0476(19) Uani 1 1 d . . .
C65 C -0.0060(7) 0.2505(7) 0.4619(4) 0.060(2) Uani 1 1 d . . .
H65 H -0.0582 0.2524 0.4836 0.072 Uiso 1 1 calc R . .
C60 C 0.1509(7) 0.2416(6) 0.3992(4) 0.050(2) Uani 1 1 d . . .
C48 C 0.4521(7) 0.4187(6) 0.2854(3) 0.0448(18) Uani 1 1 d . . .
C66 C 0.1155(7) 0.3083(6) 0.4932(4) 0.052(2) Uani 1 1 d . . .
C50 C 0.6373(8) 0.8481(6) 0.4503(4) 0.056(2) Uani 1 1 d . . .
H50A H 0.6765 0.9268 0.4543 0.067 Uiso 1 1 calc R . .
H50B H 0.6619 0.8290 0.4939 0.067 Uiso 1 1 calc R . .
C51 C 0.5048(8) 0.8054(7) 0.4303(4) 0.050(2) Uani 1 1 d . . .
C37 C 0.5237(8) 0.7148(6) 0.2922(4) 0.054(2) Uani 1 1 d . . .
H37A H 0.4537 0.7011 0.3055 0.065 Uiso 1 1 calc R . .
H37B H 0.5074 0.7219 0.2452 0.065 Uiso 1 1 calc R . .
C38 C 0.6297(8) 0.8209(6) 0.3324(4) 0.052(2) Uani 1 1 d . . .
H38A H 0.6923 0.8459 0.3108 0.063 Uiso 1 1 calc R . .
H38B H 0.6052 0.8762 0.3333 0.063 Uiso 1 1 calc R . .
C53 C 0.3049(8) 0.6563(7) 0.4053(4) 0.056(2) Uani 1 1 d . . .
C43 C 0.5773(9) 0.2855(7) 0.4186(4) 0.068(3) Uani 1 1 d . . .
H43A H 0.5223 0.2608 0.4446 0.101 Uiso 1 1 calc R . .
H43B H 0.6474 0.3512 0.4421 0.101 Uiso 1 1 calc R . .
H43C H 0.5988 0.2306 0.4112 0.101 Uiso 1 1 calc R . .
C40 C 0.8478(7) 0.7908(6) 0.3878(4) 0.057(2) Uani 1 1 d . . .
H40A H 0.9307 0.8126 0.4100 0.069 Uiso 1 1 calc R . .
H40B H 0.8414 0.8067 0.3424 0.069 Uiso 1 1 calc R . .
C62 C 0.0281(8) 0.1849(7) 0.3699(4) 0.062(2) Uani 1 1 d . . .
H62 H -0.0016 0.1417 0.3287 0.074 Uiso 1 1 calc R . .
C45 C 0.4238(9) 0.2503(7) 0.2330(4) 0.065(2) Uani 1 1 d . . .
C47 C 0.4142(8) 0.3435(7) 0.2295(4) 0.058(2) Uani 1 1 d . . .
H47 H 0.3810 0.3570 0.1881 0.069 Uiso 1 1 calc R . .
C58 C 0.4595(10) 0.8774(7) 0.4179(4) 0.066(3) Uani 1 1 d . . .
H58 H 0.5120 0.9514 0.4223 0.079 Uiso 1 1 calc R . .
C44 C 0.4782(8) 0.2344(7) 0.2948(4) 0.060(2) Uani 1 1 d . . .
H44 H 0.4875 0.1726 0.2980 0.072 Uiso 1 1 calc R . .
C39 C 0.8087(7) 0.8552(7) 0.4232(4) 0.055(2) Uani 1 1 d . . .
H39A H 0.8378 0.8580 0.4710 0.066 Uiso 1 1 calc R . .
H39B H 0.8427 0.9291 0.4131 0.066 Uiso 1 1 calc R . .
C63 C -0.0516(8) 0.1902(7) 0.3995(5) 0.066(3) Uani 1 1 d . . .
C34 C 0.8386(7) 0.6287(7) 0.4378(4) 0.053(2) Uani 1 1 d . . .
H34A H 0.9053 0.6322 0.4247 0.064 Uiso 1 1 calc R . .
H34B H 0.7856 0.5529 0.4391 0.064 Uiso 1 1 calc R . .
C35 C 0.7350(8) 0.6090(7) 0.3197(4) 0.057(2) Uani 1 1 d . . .
H35A H 0.7031 0.5319 0.3228 0.068 Uiso 1 1 calc R . .
H35B H 0.8028 0.6318 0.3026 0.068 Uiso 1 1 calc R . .
C54 C 0.2211(8) 0.5379(7) 0.4005(5) 0.078(3) Uani 1 1 d . . .
H54A H 0.2371 0.4967 0.3716 0.117 Uiso 1 1 calc R . .
H54B H 0.1406 0.5246 0.3827 0.117 Uiso 1 1 calc R . .
H54C H 0.2319 0.5163 0.4440 0.117 Uiso 1 1 calc R . .
C61 C 0.2336(8) 0.2346(8) 0.3645(4) 0.074(3) Uani 1 1 d . . .
H61A H 0.1882 0.1801 0.3258 0.110 Uiso 1 1 calc R . .
H61B H 0.2876 0.2155 0.3943 0.110 Uiso 1 1 calc R . .
H61C H 0.2780 0.3038 0.3512 0.110 Uiso 1 1 calc R . .
C36 C 0.6398(8) 0.6285(7) 0.2719(4) 0.059(2) Uani 1 1 d . . .
H36A H 0.6774 0.7000 0.2588 0.071 Uiso 1 1 calc R . .
H36B H 0.6019 0.5751 0.2321 0.071 Uiso 1 1 calc R . .
C64 C -0.1845(8) 0.1295(8) 0.3646(5) 0.090(4) Uani 1 1 d . . .
H64A H -0.2273 0.1137 0.3972 0.136 Uiso 1 1 calc R . .
H64B H -0.2044 0.0628 0.3393 0.136 Uiso 1 1 calc R . .
H64C H -0.2061 0.1738 0.3352 0.136 Uiso 1 1 calc R . .
C56 C 0.3374(11) 0.8415(9) 0.3990(5) 0.076(3) Uani 1 1 d . . .
C46 C 0.3750(12) 0.1661(9) 0.1711(5) 0.117(5) Uani 1 1 d . . .
H46A H 0.3288 0.1842 0.1349 0.175 Uiso 1 1 calc R . .
H46B H 0.3256 0.0953 0.1807 0.175 Uiso 1 1 calc R . .
H46C H 0.4401 0.1661 0.1590 0.175 Uiso 1 1 calc R . .
C55 C 0.2638(9) 0.7311(9) 0.3934(4) 0.074(3) Uani 1 1 d . . .
H55 H 0.1819 0.7055 0.3809 0.088 Uiso 1 1 calc R . .
C57 C 0.2898(13) 0.9224(11) 0.3850(7) 0.134(5) Uani 1 1 d . . .
H57A H 0.2401 0.9049 0.3397 0.202 Uiso 1 1 calc R . .
H57B H 0.3554 0.9948 0.3917 0.202 Uiso 1 1 calc R . .
H57C H 0.2441 0.9185 0.4147 0.202 Uiso 1 1 calc R . .
O1 O 0.0972(4) 0.4016(3) 0.0319(2) 0.0308(10) Uani 1 1 d . . .
Cl1 Cl 0.1342(7) 0.1129(3) 0.7983(2) 0.178(3) Uani 1 1 d . . .
O2 O -0.0598(4) 0.4229(3) 0.0878(2) 0.0309(10) Uani 1 1 d . . .
O3 O 0.1375(3) 0.6746(3) 0.0441(2) 0.0306(10) Uani 1 1 d . . .
N2 N -0.0405(5) 0.1570(4) 0.0101(3) 0.0325(12) Uani 1 1 d . . .
N3 N -0.0027(4) 0.2460(4) 0.1395(3) 0.0301(12) Uani 1 1 d . . .
N1 N -0.2295(4) 0.1577(4) 0.0459(3) 0.0308(12) Uani 1 1 d . . .
C17 C 0.0632(6) 0.3471(5) 0.1890(3) 0.0352(16) Uani 1 1 d . . .
H17A H 0.1247 0.4028 0.1730 0.042 Uiso 1 1 calc R . .
H17B H 0.1017 0.3326 0.2309 0.042 Uiso 1 1 calc R . .
C4 C 0.0180(6) 0.1197(5) 0.0683(4) 0.0387(17) Uani 1 1 d . . .
H4A H 0.0780 0.1071 0.0574 0.046 Uiso 1 1 calc R . .
H4B H -0.0412 0.0514 0.0768 0.046 Uiso 1 1 calc R . .
C15 C 0.3363(6) 0.5655(6) 0.0939(4) 0.0451(18) Uani 1 1 d . . .
H15A H 0.4202 0.6051 0.1164 0.068 Uiso 1 1 calc R . .
H15B H 0.2926 0.5547 0.1257 0.068 Uiso 1 1 calc R . .
H15C H 0.3153 0.6059 0.0611 0.068 Uiso 1 1 calc R . .
C5 C 0.0762(6) 0.2036(6) 0.1315(3) 0.0376(16) Uani 1 1 d . . .
H5A H 0.0938 0.1698 0.1701 0.045 Uiso 1 1 calc R . .
H5B H 0.1507 0.2630 0.1286 0.045 Uiso 1 1 calc R . .
C8 C 0.0320(6) 0.1966(5) -0.0374(3) 0.0380(16) Uani 1 1 d . . .
H8A H -0.0036 0.2283 -0.0710 0.046 Uiso 1 1 calc R . .
H8B H 0.0309 0.1353 -0.0599 0.046 Uiso 1 1 calc R . .
C7 C -0.2242(6) 0.1563(6) 0.1176(3) 0.0353(16) Uani 1 1 d . . .
H7A H -0.2906 0.0899 0.1226 0.042 Uiso 1 1 calc R . .
H7B H -0.2309 0.2174 0.1338 0.042 Uiso 1 1 calc R . .
C6 C -0.1083(6) 0.1627(6) 0.1584(3) 0.0386(16) Uani 1 1 d . . .
H6A H -0.0973 0.1806 0.2053 0.046 Uiso 1 1 calc R . .
H6B H -0.1129 0.0919 0.1521 0.046 Uiso 1 1 calc R . .
C2 C -0.2457(6) 0.0525(5) 0.0165(3) 0.0395(17) Uani 1 1 d . . .
H2A H -0.3274 0.0092 -0.0110 0.047 Uiso 1 1 calc R . .
H2B H -0.2311 0.0125 0.0522 0.047 Uiso 1 1 calc R . .
C3 C -0.1621(6) 0.0698(5) -0.0254(4) 0.0409(17) Uani 1 1 d . . .
H3A H -0.1602 0.0027 -0.0342 0.049 Uiso 1 1 calc R . .
H3B H -0.1910 0.0897 -0.0679 0.049 Uiso 1 1 calc R . .
C26 C 0.1532(7) 0.6828(7) 0.1825(4) 0.059(2) Uani 1 1 d . . .
H26A H 0.1759 0.7010 0.2301 0.089 Uiso 1 1 calc R . .
H26B H 0.1382 0.6099 0.1717 0.089 Uiso 1 1 calc R . .
H26C H 0.0823 0.6879 0.1626 0.089 Uiso 1 1 calc R . .
O9 O 0.064(2) 0.0623(11) 0.8334(10) 0.264(11) Uani 1 1 d . . .
C32 C 0.5630(7) 1.0044(7) 0.2259(4) 0.064(3) Uani 1 1 d . . .
H32A H 0.5518 1.0075 0.2692 0.096 Uiso 1 1 calc R . .
H32B H 0.5809 1.0729 0.2100 0.096 Uiso 1 1 calc R . .
H32C H 0.6277 0.9894 0.2289 0.096 Uiso 1 1 calc R . .
O8 O 0.244(3) 0.126(2) 0.8508(10) 0.43(2) Uani 1 1 d . . .
O7 O 0.1438(14) 0.0676(9) 0.7484(5) 0.198(6) Uani 1 1 d . . .
O10 O 0.1438(15) 0.2141(9) 0.7916(7) 0.216(7) Uani 1 1 d . . .
C1 C -0.3232(6) 0.1833(6) 0.0082(3) 0.0364(16) Uani 1 1 d . . .
H1A H -0.3041 0.2558 0.0255 0.044 Uiso 1 1 calc R . .
H1B H -0.3989 0.1323 0.0146 0.044 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O3 2.268(4) 2_565 ?
Tb1 O3 2.268(4) . ?
Tb1 O2 2.272(4) . ?
Tb1 O2 2.272(4) 2_565 ?
Tb1 O1 2.282(4) . ?
Tb1 O1 2.282(4) 2_565 ?
Tb1 Ni1 3.0099(8) 2_565 ?
Ni1 N2 2.070(5) . ?
Ni1 N3 2.074(5) . ?
Ni1 N1 2.084(5) . ?
Ni1 O1 2.105(4) . ?
Ni1 O3 2.128(4) 2_565 ?
Ni1 O2 2.138(4) . ?
C16 O1 1.357(7) . ?
C16 C9 1.391(9) . ?
C16 C14 1.422(9) . ?
C20 C22 1.388(9) . ?
C20 C19 1.396(9) . ?
C20 C21 1.495(9) . ?
C19 O2 1.351(7) . ?
C19 C18 1.400(9) . ?
C28 O3 1.359(7) . ?
C28 C29 1.396(9) . ?
C28 C27 1.407(9) . ?
C25 C23 1.385(10) . ?
C25 C18 1.391(9) . ?
C9 C10 1.380(9) . ?
C9 C8 1.505(9) . ?
C14 C13 1.389(9) . ?
C14 C15 1.499(10) . ?
C18 C17 1.502(9) . ?
C30 C31 1.373(10) . ?
C30 C29 1.393(9) . ?
C29 C1 1.496(9) 2_565 ?
C31 C33 1.373(10) . ?
C31 C32 1.516(9) . ?
C27 C33 1.387(9) . ?
C27 C26 1.498(10) . ?
C23 C22 1.377(10) . ?
C23 C24 1.520(10) . ?
C10 C11 1.386(11) . ?
C13 C11 1.380(11) . ?
C11 C12 1.525(10) . ?
Tb2 O6 2.279(5) . ?
Tb2 O6 2.279(5) 2_666 ?
Tb2 O4 2.288(5) 2_666 ?
Tb2 O4 2.288(5) . ?
Tb2 O5 2.297(5) 2_666 ?
Tb2 O5 2.297(5) . ?
Tb2 Ni2 3.0023(10) 2_666 ?
Ni2 N4 2.059(7) . ?
Ni2 N6 2.074(6) . ?
Ni2 N5 2.075(5) . ?
Ni2 O5 2.113(5) . ?
Ni2 O6 2.124(4) 2_666 ?
Ni2 O4 2.125(5) . ?
O6 C59 1.351(8) . ?
O6 Ni2 2.124(4) 2_666 ?
O4 C41 1.359(8) . ?
O5 C52 1.348(8) . ?
N6 C50 1.480(10) . ?
N6 C39 1.480(10) . ?
N6 C38 1.506(9) . ?
N5 C49 1.472(9) . ?
N5 C37 1.489(9) . ?
N5 C36 1.492(10) . ?
C52 C51 1.392(10) . ?
C52 C53 1.405(11) . ?
C41 C42 1.385(10) . ?
C41 C48 1.411(10) . ?
C59 C66 1.390(11) . ?
C59 C60 1.415(10) . ?
N4 C35 1.475(9) . ?
N4 C34 1.493(9) . ?
N4 C40 1.506(9) . ?
C49 C48 1.496(10) . ?
C42 C44 1.387(10) . ?
C42 C43 1.515(10) . ?
C65 C63 1.378(12) . ?
C65 C66 1.386(11) . ?
C60 C62 1.392(11) . ?
C60 C61 1.499(12) . ?
C48 C47 1.390(10) . ?
C66 C34 1.509(11) 2_666 ?
C50 C51 1.502(11) . ?
C51 C58 1.389(11) . ?
C37 C38 1.530(10) . ?
C53 C55 1.384(11) . ?
C53 C54 1.494(11) . ?
C40 C39 1.503(11) . ?
C62 C63 1.385(13) . ?
C45 C47 1.369(11) . ?
C45 C44 1.384(11) . ?
C45 C46 1.530(11) . ?
C58 C56 1.393(13) . ?
C63 C64 1.518(11) . ?
C34 C66 1.509(11) 2_666 ?
C35 C36 1.528(11) . ?
C56 C55 1.379(13) . ?
C56 C57 1.529(13) . ?
Cl1 O9 1.284(11) . ?
Cl1 O7 1.285(9) . ?
Cl1 O10 1.374(10) . ?
Cl1 O8 1.52(3) . ?
O3 Ni1 2.128(4) 2_565 ?
N2 C3 1.481(8) . ?
N2 C8 1.493(8) . ?
N2 C4 1.502(8) . ?
N3 C5 1.463(8) . ?
N3 C17 1.490(8) . ?
N3 C6 1.501(8) . ?
N1 C1 1.484(8) . ?
N1 C7 1.487(8) . ?
N1 C2 1.492(8) . ?
C4 C5 1.533(9) . ?
C7 C6 1.514(9) . ?
C2 C3 1.522(9) . ?
C1 C29 1.496(9) 2_565 ?

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
O3 Tb1 O3 180.00(17) 2_565 . ?
O3 Tb1 O2 75.74(15) 2_565 . ?
O3 Tb1 O2 104.26(15) . . ?
O3 Tb1 O2 104.26(15) 2_565 2_565 ?
O3 Tb1 O2 75.74(15) . 2_565 ?
O2 Tb1 O2 180.0(2) . 2_565 ?
O3 Tb1 O1 75.15(15) 2_565 . ?
O3 Tb1 O1 104.85(15) . . ?
O2 Tb1 O1 74.53(15) . . ?
O2 Tb1 O1 105.47(15) 2_565 . ?
O3 Tb1 O1 104.85(15) 2_565 2_565 ?
O3 Tb1 O1 75.15(15) . 2_565 ?
O2 Tb1 O1 105.47(15) . 2_565 ?
O2 Tb1 O1 74.53(15) 2_565 2_565 ?
O1 Tb1 O1 180.0 . 2_565 ?
O3 Tb1 Ni1 135.13(11) 2_565 2_565 ?
O3 Tb1 Ni1 44.87(11) . 2_565 ?
O2 Tb1 Ni1 134.87(10) . 2_565 ?
O2 Tb1 Ni1 45.13(10) 2_565 2_565 ?
O1 Tb1 Ni1 135.74(10) . 2_565 ?
O1 Tb1 Ni1 44.26(10) 2_565 2_565 ?
N2 Ni1 N3 85.2(2) . . ?
N2 Ni1 N1 84.6(2) . . ?
N3 Ni1 N1 85.1(2) . . ?
N2 Ni1 O1 92.23(19) . . ?
N3 Ni1 O1 101.75(18) . . ?
N1 Ni1 O1 172.22(19) . . ?
N2 Ni1 O3 101.57(19) . 2_565 ?
N3 Ni1 O3 172.27(19) . 2_565 ?
N1 Ni1 O3 91.73(18) . 2_565 ?
O1 Ni1 O3 81.93(16) . 2_565 ?
N2 Ni1 O2 172.18(19) . . ?
N3 Ni1 O2 92.23(18) . . ?
N1 Ni1 O2 102.55(18) . . ?
O1 Ni1 O2 81.07(16) . . ?
O3 Ni1 O2 81.57(16) 2_565 . ?
O1 C16 C9 120.8(6) . . ?
O1 C16 C14 120.0(6) . . ?
C9 C16 C14 119.2(6) . . ?
C22 C20 C19 118.8(6) . . ?
C22 C20 C21 121.8(6) . . ?
C19 C20 C21 119.3(6) . . ?
O2 C19 C20 120.5(5) . . ?
O2 C19 C18 120.6(6) . . ?
C20 C19 C18 118.9(6) . . ?
O3 C28 C29 120.3(6) . . ?
O3 C28 C27 119.9(6) . . ?
C29 C28 C27 119.8(5) . . ?
C23 C25 C18 121.0(6) . . ?
C10 C9 C16 120.0(7) . . ?
C10 C9 C8 119.5(6) . . ?
C16 C9 C8 120.4(6) . . ?
C13 C14 C16 118.3(7) . . ?
C13 C14 C15 121.9(7) . . ?
C16 C14 C15 119.8(6) . . ?
C25 C18 C19 120.4(6) . . ?
C25 C18 C17 119.2(6) . . ?
C19 C18 C17 120.3(6) . . ?
C31 C30 C29 123.0(7) . . ?
C30 C29 C28 118.7(6) . . ?
C30 C29 C1 120.7(6) . 2_565 ?
C28 C29 C1 120.6(6) . 2_565 ?
C30 C31 C33 116.9(6) . . ?
C30 C31 C32 121.0(7) . . ?
C33 C31 C32 122.1(7) . . ?
C33 C27 C28 118.1(6) . . ?
C33 C27 C26 121.1(6) . . ?
C28 C27 C26 120.8(6) . . ?
C31 C33 C27 123.7(7) . . ?
C22 C23 C25 117.9(6) . . ?
C22 C23 C24 121.7(7) . . ?
C25 C23 C24 120.5(7) . . ?
C9 C10 C11 122.0(7) . . ?
C23 C22 C20 122.9(7) . . ?
C11 C13 C14 122.7(7) . . ?
C13 C11 C10 117.7(7) . . ?
C13 C11 C12 121.5(8) . . ?
C10 C11 C12 120.7(8) . . ?
O6 Tb2 O6 180.0(2) . 2_666 ?
O6 Tb2 O4 75.01(17) . 2_666 ?
O6 Tb2 O4 104.99(17) 2_666 2_666 ?
O6 Tb2 O4 104.99(17) . . ?
O6 Tb2 O4 75.01(17) 2_666 . ?
O4 Tb2 O4 180.00(8) 2_666 . ?
O6 Tb2 O5 74.45(17) . 2_666 ?
O6 Tb2 O5 105.55(17) 2_666 2_666 ?
O4 Tb2 O5 76.06(17) 2_666 2_666 ?
O4 Tb2 O5 103.94(17) . 2_666 ?
O6 Tb2 O5 105.55(17) . . ?
O6 Tb2 O5 74.45(17) 2_666 . ?
O4 Tb2 O5 103.94(17) 2_666 . ?
O4 Tb2 O5 76.06(17) . . ?
O5 Tb2 O5 180.0(2) 2_666 . ?
O6 Tb2 Ni2 44.88(11) . 2_666 ?
O6 Tb2 Ni2 135.12(11) 2_666 2_666 ?
O4 Tb2 Ni2 44.89(12) 2_666 2_666 ?
O4 Tb2 Ni2 135.11(12) . 2_666 ?
O5 Tb2 Ni2 44.57(13) 2_666 2_666 ?
O5 Tb2 Ni2 135.43(13) . 2_666 ?
N4 Ni2 N6 85.0(3) . . ?
N4 Ni2 N5 85.7(2) . . ?
N6 Ni2 N5 86.0(2) . . ?
N4 Ni2 O5 173.0(2) . . ?
N6 Ni2 O5 92.0(2) . . ?
N5 Ni2 O5 100.3(2) . . ?
N4 Ni2 O6 92.9(2) . 2_666 ?
N6 Ni2 O6 101.7(2) . 2_666 ?
N5 Ni2 O6 172.0(2) . 2_666 ?
O5 Ni2 O6 81.61(18) . 2_666 ?
N4 Ni2 O4 99.9(2) . . ?
N6 Ni2 O4 174.0(2) . . ?
N5 Ni2 O4 90.8(2) . . ?
O5 Ni2 O4 83.61(19) . . ?
O6 Ni2 O4 81.76(18) 2_666 . ?
C59 O6 Ni2 119.2(4) . 2_666 ?
C59 O6 Tb2 152.0(4) . . ?
Ni2 O6 Tb2 85.90(15) 2_666 . ?
C41 O4 Ni2 123.0(4) . . ?
C41 O4 Tb2 146.9(5) . . ?
Ni2 O4 Tb2 85.66(16) . . ?
C52 O5 Ni2 121.0(5) . . ?
C52 O5 Tb2 150.5(5) . . ?
Ni2 O5 Tb2 85.69(17) . . ?
C50 N6 C39 110.9(6) . . ?
C50 N6 C38 111.6(6) . . ?
C39 N6 C38 111.5(6) . . ?
C50 N6 Ni2 109.5(5) . . ?
C39 N6 Ni2 104.7(5) . . ?
C38 N6 Ni2 108.4(4) . . ?
C49 N5 C37 110.7(6) . . ?
C49 N5 C36 112.9(6) . . ?
C37 N5 C36 111.3(6) . . ?
C49 N5 Ni2 110.2(4) . . ?
C37 N5 Ni2 103.5(4) . . ?
C36 N5 Ni2 107.9(4) . . ?
O5 C52 C51 121.4(7) . . ?
O5 C52 C53 119.7(7) . . ?
C51 C52 C53 118.9(7) . . ?
O4 C41 C42 120.8(6) . . ?
O4 C41 C48 119.6(7) . . ?
C42 C41 C48 119.6(6) . . ?
O6 C59 C66 121.7(7) . . ?
O6 C59 C60 119.1(7) . . ?
C66 C59 C60 119.1(7) . . ?
C35 N4 C34 111.0(6) . . ?
C35 N4 C40 111.9(6) . . ?
C34 N4 C40 110.9(6) . . ?
C35 N4 Ni2 104.5(5) . . ?
C34 N4 Ni2 109.2(5) . . ?
C40 N4 Ni2 109.0(5) . . ?
N5 C49 C48 114.1(6) . . ?
C41 C42 C44 119.2(7) . . ?
C41 C42 C43 120.6(7) . . ?
C44 C42 C43 120.2(7) . . ?
C63 C65 C66 121.9(9) . . ?
C62 C60 C59 118.4(8) . . ?
C62 C60 C61 120.6(7) . . ?
C59 C60 C61 121.0(7) . . ?
C47 C48 C41 118.6(7) . . ?
C47 C48 C49 120.9(7) . . ?
C41 C48 C49 120.6(6) . . ?
C65 C66 C59 120.2(8) . . ?
C65 C66 C34 120.1(8) . 2_666 ?
C59 C66 C34 119.7(7) . 2_666 ?
N6 C50 C51 113.5(6) . . ?
C58 C51 C52 120.4(8) . . ?
C58 C51 C50 119.5(8) . . ?
C52 C51 C50 120.1(7) . . ?
N5 C37 C38 111.5(6) . . ?
N6 C38 C37 111.2(6) . . ?
C55 C53 C52 118.6(8) . . ?
C55 C53 C54 121.4(8) . . ?
C52 C53 C54 119.9(7) . . ?
C39 C40 N4 111.7(7) . . ?
C63 C62 C60 122.6(8) . . ?
C47 C45 C44 117.6(7) . . ?
C47 C45 C46 121.3(8) . . ?
C44 C45 C46 121.1(8) . . ?
C45 C47 C48 122.6(7) . . ?
C51 C58 C56 121.6(9) . . ?
C45 C44 C42 122.3(8) . . ?
N6 C39 C40 110.9(6) . . ?
C65 C63 C62 117.6(8) . . ?
C65 C63 C64 121.7(10) . . ?
C62 C63 C64 120.6(9) . . ?
N4 C34 C66 113.2(6) . 2_666 ?
N4 C35 C36 110.5(7) . . ?
N5 C36 C35 112.0(6) . . ?
C55 C56 C58 116.8(8) . . ?
C55 C56 C57 122.7(11) . . ?
C58 C56 C57 120.5(11) . . ?
C56 C55 C53 123.6(9) . . ?
C16 O1 Ni1 121.5(4) . . ?
C16 O1 Tb1 148.6(4) . . ?
Ni1 O1 Tb1 86.55(14) . . ?
O9 Cl1 O7 124.8(10) . . ?
O9 Cl1 O10 111.3(8) . . ?
O7 Cl1 O10 114.8(7) . . ?
O9 Cl1 O8 93.7(13) . . ?
O7 Cl1 O8 98.9(14) . . ?
O10 Cl1 O8 108.6(13) . . ?
C19 O2 Ni1 118.6(4) . . ?
C19 O2 Tb1 154.2(4) . . ?
Ni1 O2 Tb1 86.02(15) . . ?
C28 O3 Ni1 119.4(4) . 2_565 ?
C28 O3 Tb1 152.7(4) . . ?
Ni1 O3 Tb1 86.36(14) 2_565 . ?
C3 N2 C8 110.1(5) . . ?
C3 N2 C4 111.4(5) . . ?
C8 N2 C4 111.9(5) . . ?
C3 N2 Ni1 105.5(4) . . ?
C8 N2 Ni1 109.3(4) . . ?
C4 N2 Ni1 108.4(4) . . ?
C5 N3 C17 111.2(5) . . ?
C5 N3 C6 112.0(5) . . ?
C17 N3 C6 110.7(5) . . ?
C5 N3 Ni1 104.7(4) . . ?
C17 N3 Ni1 109.5(4) . . ?
C6 N3 Ni1 108.6(4) . . ?
C1 N1 C7 111.6(5) . . ?
C1 N1 C2 112.0(5) . . ?
C7 N1 C2 110.1(5) . . ?
C1 N1 Ni1 109.5(4) . . ?
C7 N1 Ni1 104.6(4) . . ?
C2 N1 Ni1 108.8(4) . . ?
N3 C17 C18 111.8(5) . . ?
N2 C4 C5 111.9(5) . . ?
N3 C5 C4 110.6(5) . . ?
N2 C8 C9 112.4(5) . . ?
N1 C7 C6 110.6(5) . . ?
N3 C6 C7 112.5(5) . . ?
N1 C2 C3 111.9(5) . . ?
N2 C3 C2 110.1(5) . . ?
N1 C1 C29 111.9(5) . 2_565 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.195
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.121
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a_CCDC2
_audit_block_doi                 10.5517/ccdc.csd.cc201xtt
_database_code_depnum_ccdc_archive 'CCDC 1848896'
_audit_update_record             
;
2018-06-12 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 N3 O4 Tb'
_chemical_formula_weight         745.69

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9040(3)
_cell_length_b                   14.7738(6)
_cell_length_c                   16.2199(7)
_cell_angle_alpha                109.1650(10)
_cell_angle_beta                 99.7760(10)
_cell_angle_gamma                100.7120(10)
_cell_volume                     1702.65(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9334
_cell_measurement_theta_min      3.012
_cell_measurement_theta_max      24.283

_exptl_crystal_description       needle-like
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19018
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5971
_reflns_number_gt                5113
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0339P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5971
_refine_ls_number_parameters     405
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0579
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000

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 0.53493(2) 0.327313(11) 0.180533(10) 0.02776(7) Uani 1 1 d . . .
O1 O 0.3316(3) 0.4324(2) 0.1651(2) 0.0703(9) Uani 1 1 d . . .
O2 O 0.7033(3) 0.47275(16) 0.20244(15) 0.0398(6) Uani 1 1 d . . .
O3 O 0.3741(3) 0.23819(17) 0.04489(14) 0.0394(6) Uani 1 1 d . . .
O4 O 0.4016(3) 0.31147(15) 0.28409(15) 0.0366(6) Uani 1 1 d . . .
N1 N 0.5598(3) 0.15861(18) 0.18585(16) 0.0280(6) Uani 1 1 d . . .
N2 N 0.8237(3) 0.34490(17) 0.28838(16) 0.0273(6) Uani 1 1 d . . .
N3 N 0.7559(3) 0.26156(19) 0.09433(17) 0.0303(6) Uani 1 1 d . . .
C1 C 0.3361(5) 0.5173(3) 0.1885(3) 0.0595(12) Uani 1 1 d . . .
C2 C 0.2503(8) 0.5585(4) 0.1276(5) 0.129(3) Uani 1 1 d . . .
H2A H 0.3389 0.6043 0.1169 0.193 Uiso 1 1 calc R . .
H2B H 0.1691 0.5924 0.1543 0.193 Uiso 1 1 calc R . .
H2C H 0.1863 0.5057 0.0716 0.193 Uiso 1 1 calc R . .
C3 C 0.4243(8) 0.5867(5) 0.2821(4) 0.128(3) Uani 1 1 d . . .
H3A H 0.5037 0.5576 0.3104 0.192 Uiso 1 1 calc R . .
H3B H 0.3360 0.5996 0.3152 0.192 Uiso 1 1 calc R . .
H3C H 0.4902 0.6478 0.2813 0.192 Uiso 1 1 calc R . .
C4 C 0.5581(5) 0.1733(3) -0.1508(2) 0.0414(9) Uani 1 1 d . . .
H4 H 0.6668 0.1853 -0.1653 0.050 Uiso 1 1 calc R . .
C5 C 0.5515(5) 0.2132(2) -0.0610(2) 0.0345(8) Uani 1 1 d . . .
C6 C 0.2518(5) 0.0956(3) -0.1942(2) 0.0448(10) Uani 1 1 d . . .
H6 H 0.1506 0.0548 -0.2389 0.054 Uiso 1 1 calc R . .
C7 C 0.4077(5) 0.1164(3) -0.2188(2) 0.0430(9) Uani 1 1 d . . .
C8 C 0.4150(6) 0.0826(3) -0.3166(2) 0.0658(13) Uani 1 1 d . . .
H8A H 0.5367 0.0956 -0.3199 0.099 Uiso 1 1 calc R . .
H8B H 0.3531 0.1180 -0.3460 0.099 Uiso 1 1 calc R . .
H8C H 0.3598 0.0127 -0.3458 0.099 Uiso 1 1 calc R . .
C9 C 0.2377(5) 0.1324(2) -0.1060(2) 0.0385(9) Uani 1 1 d . . .
C10 C 0.0658(5) 0.1094(3) -0.0819(3) 0.0633(12) Uani 1 1 d . . .
H10A H 0.0787 0.0782 -0.0385 0.095 Uiso 1 1 calc R . .
H10B H -0.0241 0.0654 -0.1349 0.095 Uiso 1 1 calc R . .
H10C H 0.0318 0.1697 -0.0565 0.095 Uiso 1 1 calc R . .
C11 C 0.3876(4) 0.1960(2) -0.0387(2) 0.0335(8) Uani 1 1 d . . .
C12 C 0.2678(5) 0.0787(3) 0.3146(2) 0.0432(9) Uani 1 1 d . . .
H12 H 0.2580 0.0117 0.2847 0.052 Uiso 1 1 calc R . .
C13 C 0.3003(4) 0.2779(3) 0.4034(2) 0.0378(8) Uani 1 1 d . . .
C14 C 0.2178(5) 0.1078(3) 0.3943(3) 0.0501(10) Uani 1 1 d . . .
C15 C 0.2358(5) 0.2076(3) 0.4370(2) 0.0489(10) Uani 1 1 d . . .
H15 H 0.2029 0.2287 0.4912 0.059 Uiso 1 1 calc R . .
C16 C 0.3265(5) 0.3861(3) 0.4543(2) 0.0559(11) Uani 1 1 d . . .
H16A H 0.2520 0.3947 0.4958 0.084 Uiso 1 1 calc R . .
H16B H 0.2956 0.4176 0.4128 0.084 Uiso 1 1 calc R . .
H16C H 0.4487 0.4155 0.4870 0.084 Uiso 1 1 calc R . .
C17 C 0.1487(7) 0.0342(3) 0.4350(3) 0.0819(16) Uani 1 1 d . . .
H17A H 0.0715 -0.0249 0.3881 0.123 Uiso 1 1 calc R . .
H17B H 0.0840 0.0629 0.4773 0.123 Uiso 1 1 calc R . .
H17C H 0.2469 0.0178 0.4654 0.123 Uiso 1 1 calc R . .
C18 C 0.3449(4) 0.2465(2) 0.3205(2) 0.0320(8) Uani 1 1 d . . .
C19 C 0.3321(4) 0.1453(2) 0.2771(2) 0.0334(8) Uani 1 1 d . . .
C20 C 0.3797(4) 0.1079(2) 0.1883(2) 0.0345(8) Uani 1 1 d . . .
H20A H 0.3719 0.0376 0.1721 0.041 Uiso 1 1 calc R . .
H20B H 0.2917 0.1147 0.1427 0.041 Uiso 1 1 calc R . .
C21 C 0.9283(4) 0.5340(2) 0.3388(2) 0.0338(8) Uani 1 1 d . . .
C22 C 0.8408(4) 0.5445(2) 0.2615(2) 0.0352(8) Uani 1 1 d . . .
C23 C 0.8979(5) 0.6329(3) 0.2473(3) 0.0437(9) Uani 1 1 d . . .
C24 C 1.0661(5) 0.6116(2) 0.4007(2) 0.0404(9) Uani 1 1 d . . .
H24 H 1.1245 0.6035 0.4516 0.048 Uiso 1 1 calc R . .
C25 C 1.1204(5) 0.7003(2) 0.3901(3) 0.0478(10) Uani 1 1 d . . .
C26 C 1.0343(5) 0.7084(3) 0.3127(3) 0.0487(10) Uani 1 1 d . . .
H26 H 1.0695 0.7674 0.3039 0.058 Uiso 1 1 calc R . .
C27 C 0.8090(6) 0.6440(3) 0.1624(3) 0.0650(12) Uani 1 1 d . . .
H27A H 0.6979 0.6596 0.1684 0.098 Uiso 1 1 calc R . .
H27B H 0.7877 0.5830 0.1120 0.098 Uiso 1 1 calc R . .
H27C H 0.8847 0.6965 0.1529 0.098 Uiso 1 1 calc R . .
C28 C 0.8629(5) 0.4451(2) 0.3616(2) 0.0352(8) Uani 1 1 d . . .
H28A H 0.7554 0.4513 0.3817 0.042 Uiso 1 1 calc R . .
H28B H 0.9513 0.4473 0.4121 0.042 Uiso 1 1 calc R . .
C29 C 0.7805(4) 0.2709(2) 0.3300(2) 0.0314(8) Uani 1 1 d . . .
H29A H 0.6963 0.2889 0.3655 0.038 Uiso 1 1 calc R . .
H29B H 0.8878 0.2731 0.3706 0.038 Uiso 1 1 calc R . .
C30 C 0.5914(4) 0.1026(2) 0.0983(2) 0.0339(8) Uani 1 1 d . . .
H30A H 0.4866 0.0893 0.0508 0.041 Uiso 1 1 calc R . .
H30B H 0.6081 0.0393 0.0984 0.041 Uiso 1 1 calc R . .
C31 C 0.7497(4) 0.1556(2) 0.0772(2) 0.0340(8) Uani 1 1 d . . .
H31A H 0.8572 0.1519 0.1135 0.041 Uiso 1 1 calc R . .
H31B H 0.7469 0.1221 0.0143 0.041 Uiso 1 1 calc R . .
C32 C 0.9332(4) 0.3274(2) 0.1494(2) 0.0349(8) Uani 1 1 d . . .
H32A H 0.9392 0.3939 0.1504 0.042 Uiso 1 1 calc R . .
H32B H 1.0238 0.3041 0.1211 0.042 Uiso 1 1 calc R . .
C33 C 0.9728(4) 0.3312(2) 0.2453(2) 0.0334(8) Uani 1 1 d . . .
H33A H 1.0007 0.2701 0.2455 0.040 Uiso 1 1 calc R . .
H33B H 1.0769 0.3854 0.2808 0.040 Uiso 1 1 calc R . .
C70 C 1.2709(6) 0.7841(3) 0.4598(3) 0.0728(14) Uani 1 1 d . . .
H70A H 1.2229 0.8280 0.5021 0.109 Uiso 1 1 calc R . .
H70B H 1.3351 0.8203 0.4303 0.109 Uiso 1 1 calc R . .
H70C H 1.3498 0.7572 0.4910 0.109 Uiso 1 1 calc R . .
C71 C 0.7026(4) 0.1656(2) 0.2617(2) 0.0337(8) Uani 1 1 d . . .
H71A H 0.7967 0.1408 0.2379 0.040 Uiso 1 1 calc R . .
H71B H 0.6549 0.1236 0.2918 0.040 Uiso 1 1 calc R . .
C72 C 0.7164(5) 0.2815(3) 0.0096(2) 0.0389(9) Uani 1 1 d . . .
H72A H 0.8174 0.2776 -0.0168 0.047 Uiso 1 1 calc R . .
H72B H 0.7053 0.3490 0.0253 0.047 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O3 2.172(2) . ?
Tb1 O4 2.181(2) . ?
Tb1 O2 2.188(2) . ?
Tb1 O1 2.470(3) . ?
Tb1 N2 2.542(3) . ?
Tb1 N3 2.553(3) . ?
Tb1 N1 2.564(2) . ?
O1 C1 1.178(4) . ?
O2 C22 1.332(4) . ?
O3 C11 1.326(4) . ?
O4 C18 1.331(4) . ?
N1 C30 1.480(4) . ?
N1 C71 1.483(4) . ?
N1 C20 1.494(4) . ?
N2 C33 1.481(4) . ?
N2 C29 1.480(4) . ?
N2 C28 1.499(4) . ?
N3 C32 1.485(4) . ?
N3 C31 1.487(4) . ?
N3 C72 1.492(4) . ?
C1 C2 1.457(7) . ?
C1 C3 1.480(7) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C7 1.382(5) . ?
C4 C5 1.395(4) . ?
C4 H4 0.9300 . ?
C5 C11 1.403(5) . ?
C5 C72 1.508(4) . ?
C6 C7 1.371(5) . ?
C6 C9 1.385(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.513(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C11 1.397(4) . ?
C9 C10 1.488(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 C14 1.373(5) . ?
C12 C19 1.381(5) . ?
C12 H12 0.9300 . ?
C13 C15 1.380(5) . ?
C13 C18 1.400(4) . ?
C13 C16 1.495(5) . ?
C14 C15 1.376(5) . ?
C14 C17 1.512(5) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.403(4) . ?
C19 C20 1.503(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C24 1.385(4) . ?
C21 C22 1.395(5) . ?
C21 C28 1.503(4) . ?
C22 C23 1.406(5) . ?
C23 C26 1.386(5) . ?
C23 C27 1.509(5) . ?
C24 C25 1.376(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.375(5) . ?
C25 C70 1.518(5) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C71 1.519(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.501(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.514(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?

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
O3 Tb1 O4 112.80(8) . . ?
O3 Tb1 O2 117.44(9) . . ?
O4 Tb1 O2 118.86(8) . . ?
O3 Tb1 O1 80.55(10) . . ?
O4 Tb1 O1 82.71(9) . . ?
O2 Tb1 O1 73.73(9) . . ?
O3 Tb1 N2 141.13(8) . . ?
O4 Tb1 N2 87.16(8) . . ?
O2 Tb1 N2 74.95(8) . . ?
O1 Tb1 N2 136.82(9) . . ?
O3 Tb1 N3 75.62(8) . . ?
O4 Tb1 N3 142.17(8) . . ?
O2 Tb1 N3 83.90(8) . . ?
O1 Tb1 N3 134.69(10) . . ?
N2 Tb1 N3 69.09(8) . . ?
O3 Tb1 N1 83.50(8) . . ?
O4 Tb1 N1 75.70(8) . . ?
O2 Tb1 N1 140.44(8) . . ?
O1 Tb1 N1 145.58(9) . . ?
N2 Tb1 N1 69.04(8) . . ?
N3 Tb1 N1 68.56(8) . . ?
C1 O1 Tb1 138.4(3) . . ?
C22 O2 Tb1 141.7(2) . . ?
C11 O3 Tb1 141.7(2) . . ?
C18 O4 Tb1 142.0(2) . . ?
C30 N1 C71 110.8(3) . . ?
C30 N1 C20 107.4(2) . . ?
C71 N1 C20 112.8(2) . . ?
C30 N1 Tb1 105.89(18) . . ?
C71 N1 Tb1 113.83(17) . . ?
C20 N1 Tb1 105.65(19) . . ?
C33 N2 C29 111.6(2) . . ?
C33 N2 C28 112.8(2) . . ?
C29 N2 C28 106.6(2) . . ?
C33 N2 Tb1 114.16(18) . . ?
C29 N2 Tb1 105.53(18) . . ?
C28 N2 Tb1 105.56(19) . . ?
C32 N3 C31 111.3(3) . . ?
C32 N3 C72 107.7(2) . . ?
C31 N3 C72 112.7(2) . . ?
C32 N3 Tb1 105.16(17) . . ?
C31 N3 Tb1 114.70(18) . . ?
C72 N3 Tb1 104.72(19) . . ?
O1 C1 C2 121.6(5) . . ?
O1 C1 C3 121.5(5) . . ?
C2 C1 C3 116.9(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C7 C4 C5 121.9(4) . . ?
C7 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C11 119.3(3) . . ?
C4 C5 C72 119.8(3) . . ?
C11 C5 C72 120.7(3) . . ?
C7 C6 C9 123.1(3) . . ?
C7 C6 H6 118.4 . . ?
C9 C6 H6 118.4 . . ?
C6 C7 C4 117.4(3) . . ?
C6 C7 C8 121.7(3) . . ?
C4 C7 C8 120.8(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 C11 119.0(3) . . ?
C6 C9 C10 121.7(3) . . ?
C11 C9 C10 119.2(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C11 C9 120.0(3) . . ?
O3 C11 C5 121.0(3) . . ?
C9 C11 C5 119.0(3) . . ?
C14 C12 C19 122.5(3) . . ?
C14 C12 H12 118.8 . . ?
C19 C12 H12 118.8 . . ?
C15 C13 C18 118.9(3) . . ?
C15 C13 C16 121.5(3) . . ?
C18 C13 C16 119.7(3) . . ?
C12 C14 C15 117.1(3) . . ?
C12 C14 C17 122.0(4) . . ?
C15 C14 C17 120.9(4) . . ?
C13 C15 C14 123.2(3) . . ?
C13 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 C18 C19 120.5(3) . . ?
O4 C18 C13 120.8(3) . . ?
C19 C18 C13 118.7(3) . . ?
C12 C19 C18 119.5(3) . . ?
C12 C19 C20 119.5(3) . . ?
C18 C19 C20 120.8(3) . . ?
N1 C20 C19 115.6(3) . . ?
N1 C20 H20A 108.4 . . ?
C19 C20 H20A 108.4 . . ?
N1 C20 H20B 108.4 . . ?
C19 C20 H20B 108.4 . . ?
H20A C20 H20B 107.4 . . ?
C24 C21 C22 119.3(3) . . ?
C24 C21 C28 119.0(3) . . ?
C22 C21 C28 121.3(3) . . ?
O2 C22 C21 120.8(3) . . ?
O2 C22 C23 120.1(3) . . ?
C21 C22 C23 119.1(3) . . ?
C26 C23 C22 118.6(3) . . ?
C26 C23 C27 121.6(3) . . ?
C22 C23 C27 119.7(3) . . ?
C25 C24 C21 122.8(4) . . ?
C25 C24 H24 118.6 . . ?
C21 C24 H24 118.6 . . ?
C26 C25 C24 116.9(3) . . ?
C26 C25 C70 121.8(4) . . ?
C24 C25 C70 121.3(4) . . ?
C25 C26 C23 123.2(3) . . ?
C25 C26 H26 118.4 . . ?
C23 C26 H26 118.4 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C21 C28 N2 117.2(3) . . ?
C21 C28 H28A 108.0 . . ?
N2 C28 H28A 108.0 . . ?
C21 C28 H28B 108.0 . . ?
N2 C28 H28B 108.0 . . ?
H28A C28 H28B 107.2 . . ?
N2 C29 C71 113.4(3) . . ?
N2 C29 H29A 108.9 . . ?
C71 C29 H29A 108.9 . . ?
N2 C29 H29B 108.9 . . ?
C71 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
N1 C30 C31 113.8(2) . . ?
N1 C30 H30A 108.8 . . ?
C31 C30 H30A 108.8 . . ?
N1 C30 H30B 108.8 . . ?
C31 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
N3 C31 C30 112.9(3) . . ?
N3 C31 H31A 109.0 . . ?
C30 C31 H31A 109.0 . . ?
N3 C31 H31B 109.0 . . ?
C30 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
N3 C32 C33 113.1(3) . . ?
N3 C32 H32A 109.0 . . ?
C33 C32 H32A 109.0 . . ?
N3 C32 H32B 109.0 . . ?
C33 C32 H32B 109.0 . . ?
H32A C32 H32B 107.8 . . ?
N2 C33 C32 113.3(3) . . ?
N2 C33 H33A 108.9 . . ?
C32 C33 H33A 108.9 . . ?
N2 C33 H33B 108.9 . . ?
C32 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
C25 C70 H70A 109.5 . . ?
C25 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C25 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
N1 C71 C29 112.8(3) . . ?
N1 C71 H71A 109.0 . . ?
C29 C71 H71A 109.0 . . ?
N1 C71 H71B 109.0 . . ?
C29 C71 H71B 109.0 . . ?
H71A C71 H71B 107.8 . . ?
N3 C72 C5 116.0(3) . . ?
N3 C72 H72A 108.3 . . ?
C5 C72 H72A 108.3 . . ?
N3 C72 H72B 108.3 . . ?
C5 C72 H72B 108.3 . . ?
H72A C72 H72B 107.4 . . ?

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
O3 Tb1 O1 C1 -145.3(5) . . . . ?
O4 Tb1 O1 C1 100.1(5) . . . . ?
O2 Tb1 O1 C1 -22.9(5) . . . . ?
N2 Tb1 O1 C1 22.1(5) . . . . ?
N3 Tb1 O1 C1 -86.5(5) . . . . ?
N1 Tb1 O1 C1 151.2(4) . . . . ?
O3 Tb1 O2 C22 -164.0(3) . . . . ?
O4 Tb1 O2 C22 54.3(4) . . . . ?
O1 Tb1 O2 C22 126.1(4) . . . . ?
N2 Tb1 O2 C22 -23.8(3) . . . . ?
N3 Tb1 O2 C22 -93.7(3) . . . . ?
N1 Tb1 O2 C22 -48.7(4) . . . . ?
O4 Tb1 O3 C11 -156.6(3) . . . . ?
O2 Tb1 O3 C11 59.5(4) . . . . ?
O1 Tb1 O3 C11 125.5(4) . . . . ?
N2 Tb1 O3 C11 -40.8(4) . . . . ?
N3 Tb1 O3 C11 -15.6(3) . . . . ?
N1 Tb1 O3 C11 -85.1(3) . . . . ?
O3 Tb1 O4 C18 68.4(3) . . . . ?
O2 Tb1 O4 C18 -148.2(3) . . . . ?
O1 Tb1 O4 C18 144.9(3) . . . . ?
N2 Tb1 O4 C18 -77.2(3) . . . . ?
N3 Tb1 O4 C18 -27.4(4) . . . . ?
N1 Tb1 O4 C18 -8.1(3) . . . . ?
O3 Tb1 N1 C30 43.22(19) . . . . ?
O4 Tb1 N1 C30 158.8(2) . . . . ?
O2 Tb1 N1 C30 -83.0(2) . . . . ?
O1 Tb1 N1 C30 105.9(2) . . . . ?
N2 Tb1 N1 C30 -108.8(2) . . . . ?
N3 Tb1 N1 C30 -33.85(18) . . . . ?
O3 Tb1 N1 C71 165.2(2) . . . . ?
O4 Tb1 N1 C71 -79.2(2) . . . . ?
O2 Tb1 N1 C71 39.0(3) . . . . ?
O1 Tb1 N1 C71 -132.1(2) . . . . ?
N2 Tb1 N1 C71 13.22(19) . . . . ?
N3 Tb1 N1 C71 88.1(2) . . . . ?
O3 Tb1 N1 C20 -70.48(18) . . . . ?
O4 Tb1 N1 C20 45.08(18) . . . . ?
O2 Tb1 N1 C20 163.34(17) . . . . ?
O1 Tb1 N1 C20 -7.8(3) . . . . ?
N2 Tb1 N1 C20 137.54(19) . . . . ?
N3 Tb1 N1 C20 -147.55(19) . . . . ?
O3 Tb1 N2 C33 39.9(2) . . . . ?
O4 Tb1 N2 C33 163.8(2) . . . . ?
O2 Tb1 N2 C33 -75.3(2) . . . . ?
O1 Tb1 N2 C33 -120.0(2) . . . . ?
N3 Tb1 N2 C33 13.83(18) . . . . ?
N1 Tb1 N2 C33 88.0(2) . . . . ?
O3 Tb1 N2 C29 -83.0(2) . . . . ?
O4 Tb1 N2 C29 40.83(18) . . . . ?
O2 Tb1 N2 C29 161.74(19) . . . . ?
O1 Tb1 N2 C29 117.02(19) . . . . ?
N3 Tb1 N2 C29 -109.12(19) . . . . ?
N1 Tb1 N2 C29 -34.94(17) . . . . ?
O3 Tb1 N2 C28 164.35(17) . . . . ?
O4 Tb1 N2 C28 -71.83(18) . . . . ?
O2 Tb1 N2 C28 49.08(18) . . . . ?
O1 Tb1 N2 C28 4.4(2) . . . . ?
N3 Tb1 N2 C28 138.22(19) . . . . ?
N1 Tb1 N2 C28 -147.60(19) . . . . ?
O3 Tb1 N3 C32 161.4(2) . . . . ?
O4 Tb1 N3 C32 -89.8(2) . . . . ?
O2 Tb1 N3 C32 41.06(19) . . . . ?
O1 Tb1 N3 C32 100.9(2) . . . . ?
N2 Tb1 N3 C32 -35.13(18) . . . . ?
N1 Tb1 N3 C32 -110.0(2) . . . . ?
O3 Tb1 N3 C31 -76.0(2) . . . . ?
O4 Tb1 N3 C31 32.8(3) . . . . ?
O2 Tb1 N3 C31 163.7(2) . . . . ?
O1 Tb1 N3 C31 -136.5(2) . . . . ?
N2 Tb1 N3 C31 87.5(2) . . . . ?
N1 Tb1 N3 C31 12.62(19) . . . . ?
O3 Tb1 N3 C72 48.12(18) . . . . ?
O4 Tb1 N3 C72 156.90(17) . . . . ?
O2 Tb1 N3 C72 -72.26(18) . . . . ?
O1 Tb1 N3 C72 -12.4(2) . . . . ?
N2 Tb1 N3 C72 -148.45(19) . . . . ?
N1 Tb1 N3 C72 136.70(19) . . . . ?
Tb1 O1 C1 C2 137.5(4) . . . . ?
Tb1 O1 C1 C3 -44.5(7) . . . . ?
C7 C4 C5 C11 -0.6(5) . . . . ?
C7 C4 C5 C72 -175.1(3) . . . . ?
C9 C6 C7 C4 2.9(6) . . . . ?
C9 C6 C7 C8 -174.4(4) . . . . ?
C5 C4 C7 C6 -3.6(5) . . . . ?
C5 C4 C7 C8 173.8(3) . . . . ?
C7 C6 C9 C11 1.8(6) . . . . ?
C7 C6 C9 C10 179.2(4) . . . . ?
Tb1 O3 C11 C9 172.1(2) . . . . ?
Tb1 O3 C11 C5 -7.1(5) . . . . ?
C6 C9 C11 O3 174.8(3) . . . . ?
C10 C9 C11 O3 -2.6(5) . . . . ?
C6 C9 C11 C5 -6.0(5) . . . . ?
C10 C9 C11 C5 176.6(3) . . . . ?
C4 C5 C11 O3 -175.4(3) . . . . ?
C72 C5 C11 O3 -0.9(5) . . . . ?
C4 C5 C11 C9 5.4(5) . . . . ?
C72 C5 C11 C9 179.9(3) . . . . ?
C19 C12 C14 C15 -0.6(6) . . . . ?
C19 C12 C14 C17 -179.6(4) . . . . ?
C18 C13 C15 C14 2.0(6) . . . . ?
C16 C13 C15 C14 -176.8(4) . . . . ?
C12 C14 C15 C13 0.2(6) . . . . ?
C17 C14 C15 C13 179.1(4) . . . . ?
Tb1 O4 C18 C19 -14.3(5) . . . . ?
Tb1 O4 C18 C13 164.5(2) . . . . ?
C15 C13 C18 O4 177.6(3) . . . . ?
C16 C13 C18 O4 -3.6(5) . . . . ?
C15 C13 C18 C19 -3.6(5) . . . . ?
C16 C13 C18 C19 175.2(3) . . . . ?
C14 C12 C19 C18 -1.1(5) . . . . ?
C14 C12 C19 C20 -178.4(3) . . . . ?
O4 C18 C19 C12 -178.0(3) . . . . ?
C13 C18 C19 C12 3.2(5) . . . . ?
O4 C18 C19 C20 -0.8(5) . . . . ?
C13 C18 C19 C20 -179.5(3) . . . . ?
C30 N1 C20 C19 172.1(3) . . . . ?
C71 N1 C20 C19 49.7(4) . . . . ?
Tb1 N1 C20 C19 -75.3(3) . . . . ?
C12 C19 C20 N1 -129.4(3) . . . . ?
C18 C19 C20 N1 53.4(4) . . . . ?
Tb1 O2 C22 C21 3.4(5) . . . . ?
Tb1 O2 C22 C23 -175.6(2) . . . . ?
C24 C21 C22 O2 -177.4(3) . . . . ?
C28 C21 C22 O2 -4.5(5) . . . . ?
C24 C21 C22 C23 1.6(5) . . . . ?
C28 C21 C22 C23 174.5(3) . . . . ?
O2 C22 C23 C26 176.2(3) . . . . ?
C21 C22 C23 C26 -2.8(5) . . . . ?
O2 C22 C23 C27 -3.2(5) . . . . ?
C21 C22 C23 C27 177.8(3) . . . . ?
C22 C21 C24 C25 0.8(5) . . . . ?
C28 C21 C24 C25 -172.3(3) . . . . ?
C21 C24 C25 C26 -1.9(5) . . . . ?
C21 C24 C25 C70 179.4(4) . . . . ?
C24 C25 C26 C23 0.5(6) . . . . ?
C70 C25 C26 C23 179.3(4) . . . . ?
C22 C23 C26 C25 1.8(6) . . . . ?
C27 C23 C26 C25 -178.9(4) . . . . ?
C24 C21 C28 N2 -137.7(3) . . . . ?
C22 C21 C28 N2 49.4(4) . . . . ?
C33 N2 C28 C21 51.4(4) . . . . ?
C29 N2 C28 C21 174.2(3) . . . . ?
Tb1 N2 C28 C21 -73.9(3) . . . . ?
C33 N2 C29 C71 -67.7(3) . . . . ?
C28 N2 C29 C71 168.8(3) . . . . ?
Tb1 N2 C29 C71 56.8(3) . . . . ?
C71 N1 C30 C31 -68.4(3) . . . . ?
C20 N1 C30 C31 168.0(3) . . . . ?
Tb1 N1 C30 C31 55.5(3) . . . . ?
C32 N3 C31 C30 130.2(3) . . . . ?
C72 N3 C31 C30 -108.7(3) . . . . ?
Tb1 N3 C31 C30 11.0(3) . . . . ?
N1 C30 C31 N3 -46.2(4) . . . . ?
C31 N3 C32 C33 -68.5(3) . . . . ?
C72 N3 C32 C33 167.5(3) . . . . ?
Tb1 N3 C32 C33 56.2(3) . . . . ?
C29 N2 C33 C32 129.7(3) . . . . ?
C28 N2 C33 C32 -110.4(3) . . . . ?
Tb1 N2 C33 C32 10.1(3) . . . . ?
N3 C32 C33 N2 -46.4(4) . . . . ?
C30 N1 C71 C29 130.1(3) . . . . ?
C20 N1 C71 C29 -109.5(3) . . . . ?
Tb1 N1 C71 C29 10.8(3) . . . . ?
N2 C29 C71 N1 -47.0(4) . . . . ?
C32 N3 C72 C5 172.8(3) . . . . ?
C31 N3 C72 C5 49.7(4) . . . . ?
Tb1 N3 C72 C5 -75.6(3) . . . . ?
C4 C5 C72 N3 -134.2(3) . . . . ?
C11 C5 C72 N3 51.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.085
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a_CCDC3
_audit_block_doi                 10.5517/ccdc.csd.cc201xvv
_database_code_depnum_ccdc_archive 'CCDC 1848897'
_audit_update_record             
;
2018-06-12 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H84 Cl N6 O10 Tb Zn2'
_chemical_formula_weight         1446.50

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.1186(16)
_cell_length_b                   14.1170(17)
_cell_length_c                   20.850(3)
_cell_angle_alpha                90.790(3)
_cell_angle_beta                 105.005(2)
_cell_angle_gamma                117.267(2)
_cell_volume                     3275.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6493
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      20.87

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_absorpt_coefficient_mu    1.896
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29662
_diffrn_reflns_av_R_equivalents  0.1492
_diffrn_reflns_av_sigmaI/netI    0.1581
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         21.02
_reflns_number_total             6962
_reflns_number_gt                3934
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0362P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6962
_refine_ls_number_parameters     790
_refine_ls_number_restraints     360
_refine_ls_R_factor_all          0.1478
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.001

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 0.5000 0.5000 0.0000 0.0317(2) Uani 1 2 d S . .
Zn1 Zn 0.43905(7) 0.28407(7) 0.04584(5) 0.0338(3) Uani 1 1 d . . .
N2 N 0.4622(5) 0.1576(5) 0.0089(3) 0.039(2) Uani 1 1 d . . .
O2 O 0.5981(4) 0.4012(4) 0.0260(3) 0.0377(17) Uani 1 1 d . . .
C8 C 0.4867(6) 0.3876(6) 0.2026(4) 0.033(2) Uani 1 1 d U . .
N1 N 0.5000(5) 0.2465(5) 0.1418(3) 0.031(2) Uani 1 1 d . . .
N3 N 0.2698(5) 0.1563(5) 0.0466(3) 0.036(2) Uani 1 1 d . . .
C15 C 0.4306(7) 0.4266(6) 0.1523(4) 0.040(2) Uani 1 1 d U . .
C23 C 0.3425(7) 0.3205(7) -0.1816(4) 0.063(3) Uani 1 1 d U . .
H23A H 0.3436 0.3890 -0.1797 0.095 Uiso 1 1 calc R . .
H23B H 0.3278 0.2931 -0.2273 0.095 Uiso 1 1 calc R . .
H23C H 0.4185 0.3291 -0.1548 0.095 Uiso 1 1 calc R . .
C17 C 0.1625(6) 0.1759(6) -0.0638(4) 0.037(2) Uani 1 1 d U . .
C7 C 0.5668(6) 0.3456(6) 0.1905(4) 0.035(2) Uani 1 1 d U . .
H7A H 0.6284 0.3999 0.1741 0.043 Uiso 1 1 calc R . .
H7B H 0.6063 0.3316 0.2326 0.043 Uiso 1 1 calc R . .
C22 C 0.2446(6) 0.2426(6) -0.1551(4) 0.041(2) Uani 1 1 d U . .
C19 C 0.0486(7) 0.0840(6) -0.1780(4) 0.047(2) Uani 1 1 d U . .
C24 C 0.2557(6) 0.2505(6) -0.0862(4) 0.031(2) Uani 1 1 d U . .
C18 C 0.0596(6) 0.0946(6) -0.1102(4) 0.047(3) Uani 1 1 d U . .
H18 H -0.0031 0.0464 -0.0951 0.056 Uiso 1 1 calc R . .
C6 C 0.3941(6) 0.1636(6) 0.1592(4) 0.040(3) Uani 1 1 d U . .
H6A H 0.3900 0.0937 0.1520 0.048 Uiso 1 1 calc R . .
H6B H 0.4046 0.1803 0.2065 0.048 Uiso 1 1 calc R . .
C21 C 0.1411(6) 0.1586(6) -0.1984(4) 0.046(3) Uani 1 1 d U . .
H21 H 0.1343 0.1527 -0.2440 0.056 Uiso 1 1 calc R . .
C16 C 0.1728(6) 0.1785(6) 0.0095(4) 0.045(3) Uani 1 1 d U . .
H16A H 0.1888 0.2489 0.0282 0.054 Uiso 1 1 calc R . .
H16B H 0.0972 0.1252 0.0150 0.054 Uiso 1 1 calc R . .
C5 C 0.2784(6) 0.1571(6) 0.1188(4) 0.042(3) Uani 1 1 d U . .
H5A H 0.2119 0.0920 0.1244 0.050 Uiso 1 1 calc R . .
H5B H 0.2724 0.2184 0.1352 0.050 Uiso 1 1 calc R . .
C20 C -0.0635(7) -0.0045(7) -0.2261(4) 0.068(4) Uani 1 1 d U . .
H20A H -0.0523 -0.0076 -0.2696 0.103 Uiso 1 1 calc R . .
H20B H -0.1294 0.0097 -0.2292 0.103 Uiso 1 1 calc R . .
H20C H -0.0806 -0.0721 -0.2102 0.103 Uiso 1 1 calc R . .
C1 C 0.5772(6) 0.2050(6) 0.1312(4) 0.045(3) Uani 1 1 d U . .
H1A H 0.5972 0.1722 0.1697 0.054 Uiso 1 1 calc R . .
H1B H 0.6514 0.2646 0.1282 0.054 Uiso 1 1 calc R . .
C2 C 0.5200(6) 0.1205(6) 0.0666(4) 0.046(3) Uani 1 1 d U . .
H2A H 0.5816 0.1087 0.0562 0.055 Uiso 1 1 calc R . .
H2B H 0.4605 0.0524 0.0744 0.055 Uiso 1 1 calc R . .
C3 C 0.3399(6) 0.0717(6) -0.0252(4) 0.046(3) Uani 1 1 d U . .
H3A H 0.3422 0.0053 -0.0344 0.055 Uiso 1 1 calc R . .
H3B H 0.3097 0.0906 -0.0678 0.055 Uiso 1 1 calc R . .
Tb2 Tb 0.0000 0.5000 0.5000 0.0429(2) Uani 1 2 d S . .
Zn2 Zn 0.11523(8) 0.63734(8) 0.40345(5) 0.0476(4) Uani 1 1 d . . .
C51 C -0.0709(7) 0.6942(7) 0.4257(4) 0.048(2) Uani 1 1 d U . .
C41 C -0.0005(7) 0.3968(6) 0.3443(4) 0.040(2) Uani 1 1 d U . .
C45 C -0.0742(7) 0.2511(7) 0.2305(4) 0.063(3) Uani 1 1 d U . .
C50 C 0.0038(7) 0.8024(7) 0.4298(4) 0.049(2) Uani 1 1 d U . .
C42 C 0.0159(7) 0.3078(7) 0.3495(4) 0.046(2) Uani 1 1 d U . .
C52 C -0.1963(7) 0.6555(7) 0.4054(4) 0.059(3) Uani 1 1 d U . .
C57 C -0.0431(8) 0.8708(8) 0.4151(4) 0.071(3) Uani 1 1 d U . .
H57 H 0.0089 0.9438 0.4177 0.085 Uiso 1 1 calc R . .
C43 C 0.0708(7) 0.2856(6) 0.4166(4) 0.066(3) Uani 1 1 d U . .
H43A H 0.1446 0.3488 0.4398 0.099 Uiso 1 1 calc R . .
H43B H 0.0867 0.2269 0.4098 0.099 Uiso 1 1 calc R . .
H43C H 0.0160 0.2669 0.4429 0.099 Uiso 1 1 calc R . .
C47 C -0.0848(7) 0.3437(7) 0.2268(4) 0.055(3) Uani 1 1 d U . .
H47 H -0.1163 0.3570 0.1847 0.066 Uiso 1 1 calc R . .
C54 C -0.2384(8) 0.7273(7) 0.3923(5) 0.071(3) Uani 1 1 d U . .
H54 H -0.3209 0.7021 0.3797 0.085 Uiso 1 1 calc R . .
C55 C -0.1633(8) 0.8357(8) 0.3969(5) 0.078(3) Uani 1 1 d U . .
C53 C -0.2770(7) 0.5400(7) 0.4031(5) 0.074(3) Uani 1 1 d U . .
H53A H -0.3588 0.5266 0.3904 0.111 Uiso 1 1 calc R . .
H53B H -0.2574 0.5200 0.4466 0.111 Uiso 1 1 calc R . .
H53C H -0.2674 0.4981 0.3707 0.111 Uiso 1 1 calc R . .
C49 C 0.1370(7) 0.8463(7) 0.4462(4) 0.060(3) Uani 1 1 d U . .
H49A H 0.1740 0.9240 0.4481 0.073 Uiso 1 1 calc R . .
H49B H 0.1664 0.8319 0.4907 0.073 Uiso 1 1 calc R . .
C56 C -0.2199(9) 0.9119(8) 0.3807(6) 0.123(5) Uani 1 1 d U . .
H56A H -0.2708 0.8910 0.3351 0.184 Uiso 1 1 calc R . .
H56B H -0.1571 0.9849 0.3867 0.184 Uiso 1 1 calc R . .
H56C H -0.2666 0.9066 0.4105 0.184 Uiso 1 1 calc R . .
O1 O 0.4519(4) 0.4289(4) 0.0928(3) 0.0350(16) Uani 1 1 d . . .
O3 O 0.3554(4) 0.3294(4) -0.0420(3) 0.0389(18) Uani 1 1 d . . .
O5 O -0.0292(4) 0.6248(4) 0.4393(3) 0.0503(19) Uani 1 1 d . . .
O4 O 0.0265(4) 0.4657(4) 0.4002(2) 0.0488(19) Uani 1 1 d . . .
O6 O 0.1888(4) 0.6303(4) 0.5070(3) 0.0490(19) Uani 1 1 d . . .
N6 N 0.2745(5) 0.6688(5) 0.3836(3) 0.048(2) Uani 1 1 d . . .
N4 N 0.0415(5) 0.6172(5) 0.2980(3) 0.042(2) Uani 1 1 d . . .
C33 C 0.6872(6) 0.3797(6) 0.0256(4) 0.033(2) Uani 1 1 d U . .
N5 N 0.1764(6) 0.8032(5) 0.3995(3) 0.052(2) Uani 1 1 d . . .
C4 C 0.2541(6) 0.0529(6) 0.0165(4) 0.040(3) Uani 1 1 d U . .
H4A H 0.1720 0.0100 -0.0118 0.049 Uiso 1 1 calc R . .
H4B H 0.2688 0.0129 0.0521 0.049 Uiso 1 1 calc R . .
C25 C 0.5348(6) 0.1958(6) -0.0390(4) 0.041(2) Uani 1 1 d U . .
H25A H 0.4978 0.2261 -0.0730 0.050 Uiso 1 1 calc R . .
H25B H 0.5338 0.1346 -0.0614 0.050 Uiso 1 1 calc R . .
C31 C 0.8089(6) 0.4568(6) 0.0566(4) 0.034(2) Uani 1 1 d U . .
C39 C -0.0702(7) 0.5126(6) 0.2753(4) 0.049(3) Uani 1 1 d U . .
H39A H -0.1103 0.5093 0.2285 0.059 Uiso 1 1 calc R . .
H39B H -0.1232 0.5094 0.3011 0.059 Uiso 1 1 calc R . .
C26 C 0.6627(6) 0.2791(6) -0.0053(4) 0.037(2) Uani 1 1 d U . .
C28 C 0.8724(6) 0.3332(7) 0.0226(4) 0.051(2) Uani 1 1 d U . .
C27 C 0.7539(6) 0.2584(6) -0.0065(4) 0.046(2) Uani 1 1 d U . .
H27 H 0.7356 0.1916 -0.0275 0.056 Uiso 1 1 calc R . .
C32 C 0.8338(6) 0.5621(6) 0.0884(4) 0.047(3) Uani 1 1 d U . .
H32A H 0.9183 0.6046 0.1107 0.070 Uiso 1 1 calc R . .
H32B H 0.7903 0.5513 0.1206 0.070 Uiso 1 1 calc R . .
H32C H 0.8089 0.5991 0.0546 0.070 Uiso 1 1 calc R . .
C30 C 0.8942(7) 0.4303(6) 0.0531(4) 0.046(2) Uani 1 1 d U . .
H30 H 0.9739 0.4818 0.0729 0.055 Uiso 1 1 calc R . .
C58 C 0.3412(7) 0.6268(7) 0.4343(4) 0.052(3) Uani 1 1 d U . .
H58A H 0.2881 0.5518 0.4356 0.063 Uiso 1 1 calc R . .
H58B H 0.4082 0.6303 0.4209 0.063 Uiso 1 1 calc R . .
C35 C 0.3057(7) 0.8517(7) 0.4205(5) 0.061(3) Uani 1 1 d U . .
H35A H 0.3348 0.8544 0.4686 0.073 Uiso 1 1 calc R . .
H35B H 0.3399 0.9250 0.4107 0.073 Uiso 1 1 calc R . .
C36 C 0.3450(7) 0.7880(7) 0.3846(5) 0.060(3) Uani 1 1 d U . .
H36A H 0.4294 0.8115 0.4065 0.072 Uiso 1 1 calc R . .
H36B H 0.3365 0.8026 0.3388 0.072 Uiso 1 1 calc R . .
C60 C 0.3085(7) 0.6910(6) 0.5352(4) 0.050(3) Uani 1 1 d U . .
C34 C 0.1231(7) 0.8146(6) 0.3294(4) 0.061(3) Uani 1 1 d U . .
H34A H 0.1849 0.8420 0.3070 0.074 Uiso 1 1 calc R . .
H34B H 0.0946 0.8668 0.3310 0.074 Uiso 1 1 calc R . .
C38 C 0.1359(7) 0.6232(7) 0.2679(4) 0.058(3) Uani 1 1 d U . .
H38A H 0.1723 0.6928 0.2533 0.070 Uiso 1 1 calc R . .
H38B H 0.0983 0.5681 0.2286 0.070 Uiso 1 1 calc R . .
C48 C 0.0195(7) 0.7084(6) 0.2891(4) 0.061(3) Uani 1 1 d U . .
H48A H -0.0516 0.6940 0.3019 0.073 Uiso 1 1 calc R . .
H48B H 0.0030 0.7155 0.2418 0.073 Uiso 1 1 calc R . .
C37 C 0.2342(7) 0.6078(7) 0.3171(4) 0.054(3) Uani 1 1 d U . .
H37A H 0.2039 0.5319 0.3206 0.065 Uiso 1 1 calc R . .
H37B H 0.3022 0.6304 0.2995 0.065 Uiso 1 1 calc R . .
C59 C 0.3869(7) 0.6904(7) 0.5025(4) 0.047(2) Uani 1 1 d U . .
C29 C 0.9707(7) 0.3074(7) 0.0212(5) 0.080(3) Uani 1 1 d U . .
H29A H 1.0102 0.3455 -0.0104 0.121 Uiso 1 1 calc R . .
H29B H 0.9371 0.2312 0.0080 0.121 Uiso 1 1 calc R . .
H29C H 1.0279 0.3290 0.0651 0.121 Uiso 1 1 calc R . .
C13 C 0.3512(7) 0.4596(6) 0.1621(4) 0.040(2) Uani 1 1 d U . .
C12 C 0.3234(7) 0.4472(6) 0.2208(4) 0.046(2) Uani 1 1 d U . .
H12 H 0.2658 0.4649 0.2263 0.056 Uiso 1 1 calc R . .
C40 C -0.0511(7) 0.4174(7) 0.2820(4) 0.042(2) Uani 1 1 d U . .
C9 C 0.4558(6) 0.3795(6) 0.2607(4) 0.039(2) Uani 1 1 d U . .
H9 H 0.4914 0.3518 0.2942 0.046 Uiso 1 1 calc R . .
C10 C 0.3774(7) 0.4089(7) 0.2734(4) 0.046(2) Uani 1 1 d U . .
C14 C 0.2969(7) 0.5100(6) 0.1101(4) 0.057(3) Uani 1 1 d U . .
H14A H 0.2483 0.4585 0.0698 0.085 Uiso 1 1 calc R . .
H14B H 0.3600 0.5721 0.1003 0.085 Uiso 1 1 calc R . .
H14C H 0.2480 0.5315 0.1271 0.085 Uiso 1 1 calc R . .
C11 C 0.3436(7) 0.3961(7) 0.3389(4) 0.072(3) Uani 1 1 d U . .
H11A H 0.2583 0.3520 0.3290 0.108 Uiso 1 1 calc R . .
H11B H 0.3677 0.4658 0.3619 0.108 Uiso 1 1 calc R . .
H11C H 0.3838 0.3625 0.3670 0.108 Uiso 1 1 calc R . .
C46 C -0.1194(9) 0.1689(7) 0.1682(5) 0.098(4) Uani 1 1 d U . .
H46A H -0.1700 0.1837 0.1321 0.147 Uiso 1 1 calc R . .
H46B H -0.1646 0.0978 0.1778 0.147 Uiso 1 1 calc R . .
H46C H -0.0523 0.1735 0.1554 0.147 Uiso 1 1 calc R . .
Cl1 Cl 0.3621(4) 0.8911(3) 0.2021(2) 0.1754(17) Uani 1 1 d . . .
C66 C 0.5122(7) 0.7507(6) 0.5339(4) 0.055(3) Uani 1 1 d U . .
H66 H 0.5649 0.7483 0.5122 0.066 Uiso 1 1 calc R . .
C63 C 0.4776(7) 0.8145(7) 0.6262(5) 0.063(3) Uani 1 1 d U . .
H63 H 0.5089 0.8580 0.6677 0.076 Uiso 1 1 calc R . .
C62 C 0.2686(7) 0.7564(7) 0.6350(4) 0.076(4) Uani 1 1 d U . .
H62A H 0.3127 0.8123 0.6733 0.114 Uiso 1 1 calc R . .
H62B H 0.2300 0.6879 0.6495 0.114 Uiso 1 1 calc R . .
H62C H 0.2089 0.7699 0.6052 0.114 Uiso 1 1 calc R . .
C61 C 0.3523(8) 0.7551(7) 0.5991(5) 0.057(3) Uani 1 1 d U . .
C64 C 0.5567(8) 0.8120(7) 0.5949(5) 0.060(3) Uani 1 1 d U . .
C65 C 0.6895(7) 0.8745(7) 0.6278(5) 0.090(4) Uani 1 1 d U . .
H65A H 0.7230 0.8261 0.6323 0.134 Uiso 1 1 calc R . .
H65B H 0.7052 0.9102 0.6715 0.134 Uiso 1 1 calc R . .
H65C H 0.7256 0.9271 0.6008 0.134 Uiso 1 1 calc R . .
O8 O 0.4374(10) 0.9425(7) 0.1665(6) 0.276(5) Uani 1 1 d . . .
O9 O 0.3525(10) 0.7900(7) 0.2060(5) 0.214(5) Uani 1 1 d . . .
O10 O 0.3600(10) 0.9383(7) 0.2517(5) 0.215(5) Uani 1 1 d . . .
O7 O 0.2691(19) 0.8868(13) 0.1510(7) 0.388(12) Uani 1 1 d . . .
C44 C -0.0225(7) 0.2359(7) 0.2937(4) 0.055(3) Uani 1 1 d U . .
H44 H -0.0139 0.1742 0.2979 0.066 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O3 2.250(4) . ?
Tb1 O3 2.250(4) 2_665 ?
Tb1 O1 2.292(5) 2_665 ?
Tb1 O1 2.292(5) . ?
Tb1 O2 2.281(5) . ?
Tb1 O2 2.281(5) 2_665 ?
Tb1 Zn1 3.0145(10) 2_665 ?
Zn1 N2 2.111(7) . ?
Zn1 N1 2.124(6) . ?
Zn1 N3 2.129(5) . ?
Zn1 O2 2.136(5) . ?
Zn1 O3 2.145(5) . ?
Zn1 O1 2.170(5) . ?
N2 C3 1.467(8) . ?
N2 C2 1.486(9) . ?
N2 C25 1.493(9) . ?
O2 C33 1.337(9) . ?
C8 C9 1.364(11) . ?
C8 C15 1.390(10) . ?
C8 C7 1.492(10) . ?
N1 C1 1.440(9) . ?
N1 C7 1.461(8) . ?
N1 C6 1.489(9) . ?
N3 C16 1.476(9) . ?
N3 C5 1.480(9) . ?
N3 C4 1.482(9) . ?
C15 O1 1.339(9) . ?
C15 C13 1.377(11) . ?
C23 C22 1.502(10) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C17 C18 1.396(9) . ?
C17 C24 1.397(10) . ?
C17 C16 1.498(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C22 C21 1.387(9) . ?
C22 C24 1.403(11) . ?
C19 C21 1.367(10) . ?
C19 C18 1.383(11) . ?
C19 C20 1.499(9) . ?
C24 O3 1.347(7) . ?
C18 H18 0.9300 . ?
C6 C5 1.493(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C21 H21 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C1 C2 1.552(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.527(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
Tb2 O4 2.277(6) . ?
Tb2 O4 2.277(6) 2_566 ?
Tb2 O6 2.274(5) . ?
Tb2 O6 2.274(5) 2_566 ?
Tb2 O5 2.298(6) . ?
Tb2 O5 2.298(6) 2_566 ?
Tb2 Zn2 3.0156(11) 2_566 ?
Zn2 N6 2.083(7) . ?
Zn2 N5 2.110(7) . ?
Zn2 N4 2.116(6) . ?
Zn2 O5 2.147(6) . ?
Zn2 O6 2.149(5) . ?
Zn2 O4 2.146(5) . ?
C51 O5 1.327(9) . ?
C51 C50 1.372(10) . ?
C51 C52 1.412(11) . ?
C41 O4 1.368(9) . ?
C41 C42 1.369(11) . ?
C41 C40 1.397(10) . ?
C45 C47 1.378(12) . ?
C45 C44 1.386(11) . ?
C45 C46 1.520(12) . ?
C50 C57 1.364(12) . ?
C50 C49 1.499(11) . ?
C42 C44 1.355(10) . ?
C42 C43 1.507(10) . ?
C52 C54 1.360(12) . ?
C52 C53 1.473(11) . ?
C57 C55 1.359(12) . ?
C57 H57 0.9300 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C47 C40 1.374(11) . ?
C47 H47 0.9300 . ?
C54 C55 1.374(12) . ?
C54 H54 0.9300 . ?
C55 C56 1.559(13) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C49 N5 1.456(11) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
O6 C60 1.349(8) . ?
N6 C37 1.454(10) . ?
N6 C36 1.499(9) . ?
N6 C58 1.501(10) . ?
N4 C48 1.447(10) . ?
N4 C39 1.480(8) . ?
N4 C38 1.497(10) . ?
C33 C26 1.409(10) . ?
C33 C31 1.417(9) . ?
N5 C35 1.443(9) . ?
N5 C34 1.493(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C25 C26 1.501(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C31 C30 1.350(10) . ?
C31 C32 1.474(10) . ?
C39 C40 1.478(11) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C26 C27 1.361(10) . ?
C28 C30 1.374(11) . ?
C28 C27 1.374(9) . ?
C28 C29 1.499(11) . ?
C27 H27 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C30 H30 0.9300 . ?
C58 C59 1.489(11) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C35 C36 1.496(12) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C60 C59 1.377(12) . ?
C60 C61 1.420(12) . ?
C34 C48 1.520(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C38 C37 1.530(11) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C59 C66 1.414(10) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C13 C12 1.355(11) . ?
C13 C14 1.508(10) . ?
C12 C10 1.400(11) . ?
C12 H12 0.9300 . ?
C9 C10 1.352(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.531(12) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
Cl1 O10 1.235(9) . ?
Cl1 O8 1.339(10) . ?
Cl1 O9 1.380(10) . ?
Cl1 O7 1.373(18) . ?
C66 C64 1.353(11) . ?
C66 H66 0.9300 . ?
C63 C64 1.375(13) . ?
C63 C61 1.402(11) . ?
C63 H63 0.9300 . ?
C62 C61 1.486(12) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C64 C65 1.497(10) . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C44 H44 0.9300 . ?

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
O3 Tb1 O3 180.0(3) . 2_665 ?
O3 Tb1 O1 103.60(17) . 2_665 ?
O3 Tb1 O1 76.40(17) 2_665 2_665 ?
O3 Tb1 O1 76.40(17) . . ?
O3 Tb1 O1 103.60(17) 2_665 . ?
O1 Tb1 O1 180.0(2) 2_665 . ?
O3 Tb1 O2 76.34(16) . . ?
O3 Tb1 O2 103.66(16) 2_665 . ?
O1 Tb1 O2 104.59(19) 2_665 . ?
O1 Tb1 O2 75.41(19) . . ?
O3 Tb1 O2 103.66(16) . 2_665 ?
O3 Tb1 O2 76.34(16) 2_665 2_665 ?
O1 Tb1 O2 75.41(19) 2_665 2_665 ?
O1 Tb1 O2 104.59(19) . 2_665 ?
O2 Tb1 O2 180.000(1) . 2_665 ?
O3 Tb1 Zn1 134.75(13) . 2_665 ?
O3 Tb1 Zn1 45.25(13) 2_665 2_665 ?
O1 Tb1 Zn1 45.82(13) 2_665 2_665 ?
O1 Tb1 Zn1 134.18(13) . 2_665 ?
O2 Tb1 Zn1 135.03(12) . 2_665 ?
O2 Tb1 Zn1 44.97(12) 2_665 2_665 ?
N2 Zn1 N1 84.6(2) . . ?
N2 Zn1 N3 83.5(2) . . ?
N1 Zn1 N3 83.3(2) . . ?
N2 Zn1 O2 90.8(2) . . ?
N1 Zn1 O2 105.0(2) . . ?
N3 Zn1 O2 169.5(2) . . ?
N2 Zn1 O3 104.9(2) . . ?
N1 Zn1 O3 168.5(2) . . ?
N3 Zn1 O3 91.2(2) . . ?
O2 Zn1 O3 81.72(18) . . ?
N2 Zn1 O1 169.08(18) . . ?
N1 Zn1 O1 90.5(2) . . ?
N3 Zn1 O1 105.6(2) . . ?
O2 Zn1 O1 81.00(19) . . ?
O3 Zn1 O1 81.23(19) . . ?
C3 N2 C2 110.0(6) . . ?
C3 N2 C25 111.4(6) . . ?
C2 N2 C25 112.2(6) . . ?
C3 N2 Zn1 104.7(5) . . ?
C2 N2 Zn1 108.8(5) . . ?
C25 N2 Zn1 109.4(5) . . ?
C33 O2 Zn1 121.1(4) . . ?
C33 O2 Tb1 151.8(5) . . ?
Zn1 O2 Tb1 86.03(18) . . ?
C9 C8 C15 117.0(8) . . ?
C9 C8 C7 121.6(8) . . ?
C15 C8 C7 121.1(8) . . ?
C1 N1 C7 111.6(5) . . ?
C1 N1 C6 112.2(6) . . ?
C7 N1 C6 112.5(6) . . ?
C1 N1 Zn1 102.7(5) . . ?
C7 N1 Zn1 108.7(4) . . ?
C6 N1 Zn1 108.6(4) . . ?
C16 N3 C5 111.5(6) . . ?
C16 N3 C4 111.3(6) . . ?
C5 N3 C4 110.8(6) . . ?
C16 N3 Zn1 109.6(4) . . ?
C5 N3 Zn1 103.9(4) . . ?
C4 N3 Zn1 109.5(5) . . ?
O1 C15 C13 119.8(8) . . ?
O1 C15 C8 119.0(8) . . ?
C13 C15 C8 121.2(8) . . ?
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 . . ?
C18 C17 C24 119.6(8) . . ?
C18 C17 C16 119.1(7) . . ?
C24 C17 C16 121.2(6) . . ?
N1 C7 C8 111.7(6) . . ?
N1 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N1 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C21 C22 C24 118.0(7) . . ?
C21 C22 C23 120.5(8) . . ?
C24 C22 C23 121.5(6) . . ?
C21 C19 C18 117.4(7) . . ?
C21 C19 C20 122.8(8) . . ?
C18 C19 C20 119.8(7) . . ?
O3 C24 C22 120.3(7) . . ?
O3 C24 C17 120.2(7) . . ?
C22 C24 C17 119.5(6) . . ?
C19 C18 C17 121.5(7) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C5 C6 N1 112.9(6) . . ?
C5 C6 H6A 109.0 . . ?
N1 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
N1 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C19 C21 C22 123.9(8) . . ?
C19 C21 H21 118.0 . . ?
C22 C21 H21 118.0 . . ?
N3 C16 C17 111.6(7) . . ?
N3 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
N3 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
N3 C5 C6 111.5(7) . . ?
N3 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N3 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C1 C2 113.3(6) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N2 C2 C1 110.8(7) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 112.5(6) . . ?
N2 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
O4 Tb2 O4 180.00(8) . 2_566 ?
O4 Tb2 O6 75.51(18) . . ?
O4 Tb2 O6 104.49(18) 2_566 . ?
O4 Tb2 O6 104.49(18) . 2_566 ?
O4 Tb2 O6 75.51(18) 2_566 2_566 ?
O6 Tb2 O6 180.000(1) . 2_566 ?
O4 Tb2 O5 76.4(2) . . ?
O4 Tb2 O5 103.6(2) 2_566 . ?
O6 Tb2 O5 75.76(19) . . ?
O6 Tb2 O5 104.24(19) 2_566 . ?
O4 Tb2 O5 103.6(2) . 2_566 ?
O4 Tb2 O5 76.4(2) 2_566 2_566 ?
O6 Tb2 O5 104.24(19) . 2_566 ?
O6 Tb2 O5 75.76(19) 2_566 2_566 ?
O5 Tb2 O5 180.000(1) . 2_566 ?
O4 Tb2 Zn2 134.79(13) . 2_566 ?
O4 Tb2 Zn2 45.21(13) 2_566 2_566 ?
O6 Tb2 Zn2 134.69(13) . 2_566 ?
O6 Tb2 Zn2 45.31(13) 2_566 2_566 ?
O5 Tb2 Zn2 134.80(15) . 2_566 ?
O5 Tb2 Zn2 45.20(15) 2_566 2_566 ?
N6 Zn2 N5 83.6(3) . . ?
N6 Zn2 N4 85.7(3) . . ?
N5 Zn2 N4 85.0(3) . . ?
N6 Zn2 O5 170.1(2) . . ?
N5 Zn2 O5 91.5(3) . . ?
N4 Zn2 O5 102.5(2) . . ?
N6 Zn2 O6 91.3(2) . . ?
N5 Zn2 O6 104.5(2) . . ?
N4 Zn2 O6 169.7(3) . . ?
O5 Zn2 O6 81.6(2) . . ?
N6 Zn2 O4 103.3(2) . . ?
N5 Zn2 O4 171.3(2) . . ?
N4 Zn2 O4 90.2(2) . . ?
O5 Zn2 O4 82.5(2) . . ?
O6 Zn2 O4 80.91(19) . . ?
O5 C51 C50 122.1(8) . . ?
O5 C51 C52 119.0(8) . . ?
C50 C51 C52 118.8(9) . . ?
O4 C41 C42 121.1(7) . . ?
O4 C41 C40 117.5(8) . . ?
C42 C41 C40 121.3(8) . . ?
C47 C45 C44 116.8(8) . . ?
C47 C45 C46 121.3(8) . . ?
C44 C45 C46 122.0(9) . . ?
C51 C50 C57 120.2(8) . . ?
C51 C50 C49 120.8(8) . . ?
C57 C50 C49 118.9(8) . . ?
C44 C42 C41 119.4(8) . . ?
C44 C42 C43 119.2(8) . . ?
C41 C42 C43 121.4(8) . . ?
C54 C52 C51 118.7(8) . . ?
C54 C52 C53 122.0(8) . . ?
C51 C52 C53 119.2(8) . . ?
C55 C57 C50 122.0(9) . . ?
C55 C57 H57 119.0 . . ?
C50 C57 H57 119.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C47 C45 123.4(8) . . ?
C40 C47 H47 118.3 . . ?
C45 C47 H47 118.3 . . ?
C52 C54 C55 122.3(9) . . ?
C52 C54 H54 118.8 . . ?
C55 C54 H54 118.8 . . ?
C57 C55 C54 117.9(10) . . ?
C57 C55 C56 123.4(9) . . ?
C54 C55 C56 118.7(9) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N5 C49 C50 115.5(7) . . ?
N5 C49 H49A 108.4 . . ?
C50 C49 H49A 108.4 . . ?
N5 C49 H49B 108.4 . . ?
C50 C49 H49B 108.4 . . ?
H49A C49 H49B 107.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C15 O1 Zn1 117.7(5) . . ?
C15 O1 Tb1 157.4(5) . . ?
Zn1 O1 Tb1 84.95(19) . . ?
C24 O3 Zn1 117.5(5) . . ?
C24 O3 Tb1 155.9(5) . . ?
Zn1 O3 Tb1 86.59(15) . . ?
C51 O5 Zn2 119.8(5) . . ?
C51 O5 Tb2 153.4(6) . . ?
Zn2 O5 Tb2 85.4(2) . . ?
C41 O4 Zn2 121.6(5) . . ?
C41 O4 Tb2 151.2(5) . . ?
Zn2 O4 Tb2 85.9(2) . . ?
C60 O6 Zn2 117.6(5) . . ?
C60 O6 Tb2 156.0(5) . . ?
Zn2 O6 Tb2 85.92(16) . . ?
C37 N6 C36 112.3(7) . . ?
C37 N6 C58 110.3(7) . . ?
C36 N6 C58 112.8(6) . . ?
C37 N6 Zn2 103.7(5) . . ?
C36 N6 Zn2 108.1(5) . . ?
C58 N6 Zn2 109.2(5) . . ?
C48 N4 C39 112.6(6) . . ?
C48 N4 C38 112.4(7) . . ?
C39 N4 C38 112.5(7) . . ?
C48 N4 Zn2 102.9(5) . . ?
C39 N4 Zn2 109.3(5) . . ?
C38 N4 Zn2 106.6(4) . . ?
O2 C33 C26 121.0(6) . . ?
O2 C33 C31 121.1(7) . . ?
C26 C33 C31 117.9(7) . . ?
C35 N5 C49 110.3(7) . . ?
C35 N5 C34 114.3(7) . . ?
C49 N5 C34 109.9(7) . . ?
C35 N5 Zn2 105.0(5) . . ?
C49 N5 Zn2 109.3(5) . . ?
C34 N5 Zn2 107.8(5) . . ?
N3 C4 C3 111.4(6) . . ?
N3 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C25 C26 112.9(6) . . ?
N2 C25 H25A 109.0 . . ?
C26 C25 H25A 109.0 . . ?
N2 C25 H25B 109.0 . . ?
C26 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C30 C31 C33 117.9(8) . . ?
C30 C31 C32 124.5(7) . . ?
C33 C31 C32 117.6(7) . . ?
N4 C39 C40 114.2(7) . . ?
N4 C39 H39A 108.7 . . ?
C40 C39 H39A 108.7 . . ?
N4 C39 H39B 108.7 . . ?
C40 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
C27 C26 C33 120.6(7) . . ?
C27 C26 C25 120.1(7) . . ?
C33 C26 C25 119.2(7) . . ?
C30 C28 C27 116.5(8) . . ?
C30 C28 C29 122.9(7) . . ?
C27 C28 C29 120.6(8) . . ?
C26 C27 C28 122.0(8) . . ?
C26 C27 H27 119.0 . . ?
C28 C27 H27 119.0 . . ?
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 . . ?
C31 C30 C28 125.2(7) . . ?
C31 C30 H30 117.4 . . ?
C28 C30 H30 117.4 . . ?
C59 C58 N6 111.2(7) . . ?
C59 C58 H58A 109.4 . . ?
N6 C58 H58A 109.4 . . ?
C59 C58 H58B 109.4 . . ?
N6 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
N5 C35 C36 110.4(7) . . ?
N5 C35 H35A 109.6 . . ?
C36 C35 H35A 109.6 . . ?
N5 C35 H35B 109.6 . . ?
C36 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C35 C36 N6 113.0(7) . . ?
C35 C36 H36A 109.0 . . ?
N6 C36 H36A 109.0 . . ?
C35 C36 H36B 109.0 . . ?
N6 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
O6 C60 C59 120.3(8) . . ?
O6 C60 C61 119.1(9) . . ?
C59 C60 C61 120.6(8) . . ?
N5 C34 C48 112.3(7) . . ?
N5 C34 H34A 109.1 . . ?
C48 C34 H34A 109.1 . . ?
N5 C34 H34B 109.1 . . ?
C48 C34 H34B 109.1 . . ?
H34A C34 H34B 107.9 . . ?
N4 C38 C37 112.8(7) . . ?
N4 C38 H38A 109.0 . . ?
C37 C38 H38A 109.0 . . ?
N4 C38 H38B 109.0 . . ?
C37 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
N4 C48 C34 114.1(7) . . ?
N4 C48 H48A 108.7 . . ?
C34 C48 H48A 108.7 . . ?
N4 C48 H48B 108.7 . . ?
C34 C48 H48B 108.7 . . ?
H48A C48 H48B 107.6 . . ?
N6 C37 C38 112.4(7) . . ?
N6 C37 H37A 109.1 . . ?
C38 C37 H37A 109.1 . . ?
N6 C37 H37B 109.1 . . ?
C38 C37 H37B 109.1 . . ?
H37A C37 H37B 107.9 . . ?
C60 C59 C66 119.8(8) . . ?
C60 C59 C58 120.7(7) . . ?
C66 C59 C58 119.5(9) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C12 C13 C15 118.3(8) . . ?
C12 C13 C14 120.0(8) . . ?
C15 C13 C14 121.7(8) . . ?
C13 C12 C10 123.1(9) . . ?
C13 C12 H12 118.5 . . ?
C10 C12 H12 118.5 . . ?
C47 C40 C41 116.9(8) . . ?
C47 C40 C39 121.0(8) . . ?
C41 C40 C39 122.2(8) . . ?
C10 C9 C8 124.9(8) . . ?
C10 C9 H9 117.5 . . ?
C8 C9 H9 117.5 . . ?
C9 C10 C12 115.4(8) . . ?
C9 C10 C11 123.0(8) . . ?
C12 C10 C11 121.5(9) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O10 Cl1 O8 122.0(7) . . ?
O10 Cl1 O9 117.7(7) . . ?
O8 Cl1 O9 108.7(7) . . ?
O10 Cl1 O7 103.8(11) . . ?
O8 Cl1 O7 89.3(10) . . ?
O9 Cl1 O7 110.9(8) . . ?
C64 C66 C59 121.0(9) . . ?
C64 C66 H66 119.5 . . ?
C59 C66 H66 119.5 . . ?
C64 C63 C61 123.7(9) . . ?
C64 C63 H63 118.1 . . ?
C61 C63 H63 118.1 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C63 C61 C60 116.2(10) . . ?
C63 C61 C62 122.7(9) . . ?
C60 C61 C62 121.1(8) . . ?
C66 C64 C63 118.7(8) . . ?
C66 C64 C65 120.4(10) . . ?
C63 C64 C65 120.9(9) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C42 C44 C45 122.2(9) . . ?
C42 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        21.02
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.121
