# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ww
_audit_block_doi                 10.5517/ccdc.csd.cc1yy906
_database_code_depnum_ccdc_archive 'CCDC 1815608'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 N6 O43 Tb4'
_chemical_formula_weight         2016.48

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           orthorhombic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   16.7852(19)
_cell_length_b                   11.3430(13)
_cell_length_c                   15.3991(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2931.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1932
_exptl_absorpt_coefficient_mu    4.890
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22200
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         27.64
_reflns_number_total             3389
_reflns_number_gt                3119
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0412P)²+9.0774P] 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         3389
_refine_ls_number_parameters     249
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_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 0.466350(8) 0.854924(12) 0.126823(9) 0.01307(8) Uani 1 1 d . . .
C1 C 0.2905(2) 0.7650(3) 0.3259(2) 0.0196(7) Uani 1 1 d . . .
C2 C 0.2895(3) 0.6439(3) 0.3313(3) 0.0296(9) Uani 1 1 d . . .
H2A H 0.3277 0.6003 0.3016 0.036 Uiso 1 1 calc R . .
C3 C 0.2318(2) 0.5856(3) 0.3807(3) 0.0268(8) Uani 1 1 d . . .
H3A H 0.2318 0.5036 0.3830 0.032 Uiso 1 1 calc R . .
C4 C 0.1746(2) 0.6488(3) 0.4265(2) 0.0186(7) Uani 1 1 d . . .
C5 C 0.1762(2) 0.7705(3) 0.4242(2) 0.0209(7) Uani 1 1 d . . .
H5A H 0.1393 0.8143 0.4558 0.025 Uiso 1 1 calc R . .
C6 C 0.2337(2) 0.8266(3) 0.3742(2) 0.0202(7) Uani 1 1 d . . .
C7 C 0.10974(19) 0.5851(3) 0.4767(2) 0.0172(6) Uani 1 1 d . . .
C8 C 0.3496(2) 0.8207(3) 0.2635(2) 0.0186(7) Uani 1 1 d . . .
C9 C 0.5000 1.0948(4) 0.2500 0.0218(10) Uani 1 2 d S . .
C10 C 0.5000 1.2280(4) 0.2500 0.0207(10) Uani 1 2 d S . .
C11 C 0.5033(2) 1.2901(3) 0.1723(2) 0.0232(7) Uani 1 1 d . . .
H11A H 0.5048 1.2495 0.1199 0.028 Uiso 1 1 calc R . .
C12 C 0.5043(3) 1.4123(3) 0.1726(2) 0.0265(8) Uani 1 1 d . . .
C13 C 0.5000 1.4763(4) 0.2500 0.0239(11) Uani 1 2 d S . .
C14 C 0.5000 1.6089(4) 0.2500 0.0225(10) Uani 1 2 d S . .
N1 N 0.2345(2) 0.9546(3) 0.3723(2) 0.0323(8) Uani 1 1 d . . .
N2 N 0.5200(4) 1.4687(5) 0.0870(4) 0.0275(14) Uani 0.50 1 d P . .
O1 O 0.06627(17) 0.6478(2) 0.52540(19) 0.0259(6) Uani 1 1 d . . .
O2 O 0.10309(14) 0.4760(2) 0.46782(16) 0.0209(5) Uani 1 1 d . . .
O3 O 0.41892(15) 0.8467(2) 0.28752(18) 0.0225(6) Uani 1 1 d . . .
O4 O 0.33041(15) 0.8284(3) 0.18567(18) 0.0269(6) Uani 1 1 d . . .
O5 O 0.1848(3) 1.0076(3) 0.4135(4) 0.114(3) Uani 1 1 d . . .
O6 O 0.2854(2) 1.0049(3) 0.3304(2) 0.0481(9) Uani 1 1 d . . .
O7 O 0.48193(17) 1.0453(2) 0.17987(17) 0.0258(6) Uani 1 1 d . . .
O8 O 0.4712(4) 1.4571(6) 0.0311(5) 0.0029(14) Uiso 0.25 1 d P . .
O9 O 0.5828(4) 1.5232(6) 0.0746(4) 0.0474(17) Uani 0.50 1 d P . .
O10 O 0.47576(19) 1.6586(2) 0.18194(18) 0.0270(6) Uani 1 1 d . . .
O11 O 0.40460(19) 0.7220(3) 0.02867(19) 0.0342(7) Uani 1 1 d D . .
H1WB H 0.372(3) 0.746(5) -0.013(3) 0.060(18) Uiso 1 1 d D . .
H1WC H 0.391(4) 0.650(2) 0.043(5) 0.07(2) Uiso 1 1 d D . .
O12 O 0.3130(3) 0.7565(4) -0.1089(3) 0.0774(14) Uani 1 1 d . . .
H22A H 0.2794 0.8249 -0.1055 0.116 Uiso 1 1 d R . .
H22C H 0.2805 0.6873 -0.1150 0.116 Uiso 1 1 d 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 2.292(2) 8_565 ?
Tb1 O2 2.317(2) 4 ?
Tb1 O7 2.324(2) . ?
Tb1 O3 2.336(3) 2_655 ?
Tb1 O11 2.373(3) . ?
Tb1 O10 2.388(2) 1_545 ?
Tb1 O4 2.473(3) . ?
Tb1 O3 2.601(3) . ?
Tb1 C8 2.902(3) . ?
Tb1 Tb1 3.9582(5) 2_655 ?
C1 C2 1.376(5) . ?
C1 C6 1.397(5) . ?
C1 C8 1.519(4) . ?
C2 C3 1.398(5) . ?
C3 C4 1.391(5) . ?
C4 C5 1.381(5) . ?
C4 C7 1.518(4) . ?
C5 C6 1.389(5) . ?
C6 N1 1.452(5) . ?
C7 O2 1.251(4) . ?
C7 O1 1.265(4) . ?
C8 O4 1.244(4) . ?
C8 O3 1.256(4) . ?
C9 O7 1.254(3) . ?
C9 O7 1.254(3) 2_655 ?
C9 C10 1.510(7) . ?
C10 C11 1.389(4) 2_655 ?
C10 C11 1.389(4) . ?
C11 C12 1.387(5) . ?
C12 C13 1.397(4) . ?
C12 N2 1.489(7) . ?
C13 C12 1.397(4) 2_655 ?
C13 C14 1.504(7) . ?
C14 O10 1.258(4) 2_655 ?
C14 O10 1.258(4) . ?
N1 O5 1.208(5) . ?
N1 O6 1.214(4) . ?
N2 O8 1.194(10) . ?
N2 O9 1.237(9) . ?
O1 Tb1 2.292(2) 8_466 ?
O2 Tb1 2.317(2) 4_545 ?
O3 Tb1 2.336(3) 2_655 ?
O8 O8 1.673(14) 5_685 ?
O10 Tb1 2.388(2) 1_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
O1 Tb1 O2 86.99(9) 8_565 4 ?
O1 Tb1 O7 99.78(9) 8_565 . ?
O2 Tb1 O7 74.15(9) 4 . ?
O1 Tb1 O3 77.35(10) 8_565 2_655 ?
O2 Tb1 O3 142.51(9) 4 2_655 ?
O7 Tb1 O3 75.27(9) . 2_655 ?
O1 Tb1 O11 82.93(11) 8_565 . ?
O2 Tb1 O11 75.89(11) 4 . ?
O7 Tb1 O11 149.71(10) . . ?
O3 Tb1 O11 133.98(10) 2_655 . ?
O1 Tb1 O10 100.43(10) 8_565 1_545 ?
O2 Tb1 O10 144.04(10) 4 1_545 ?
O7 Tb1 O10 137.23(10) . 1_545 ?
O3 Tb1 O10 73.00(9) 2_655 1_545 ?
O11 Tb1 O10 70.30(10) . 1_545 ?
O1 Tb1 O4 157.37(11) 8_565 . ?
O2 Tb1 O4 80.71(9) 4 . ?
O7 Tb1 O4 95.06(10) . . ?
O3 Tb1 O4 123.28(9) 2_655 . ?
O11 Tb1 O4 75.70(11) . . ?
O10 Tb1 O4 79.47(10) 1_545 . ?
O1 Tb1 O3 150.67(10) 8_565 . ?
O2 Tb1 O3 117.75(8) 4 . ?
O7 Tb1 O3 74.53(8) . . ?
O3 Tb1 O3 73.37(9) 2_655 . ?
O11 Tb1 O3 116.71(9) . . ?
O10 Tb1 O3 69.44(9) 1_545 . ?
O4 Tb1 O3 50.56(9) . . ?
O1 Tb1 C8 170.60(10) 8_565 . ?
O2 Tb1 C8 101.29(9) 4 . ?
O7 Tb1 C8 86.87(10) . . ?
O3 Tb1 C8 98.16(10) 2_655 . ?
O11 Tb1 C8 94.70(10) . . ?
O10 Tb1 C8 70.25(10) 1_545 . ?
O4 Tb1 C8 25.18(9) . . ?
O3 Tb1 C8 25.65(9) . . ?
O1 Tb1 Tb1 116.38(8) 8_565 2_655 ?
O2 Tb1 Tb1 138.28(6) 4 2_655 ?
O7 Tb1 Tb1 68.34(6) . 2_655 ?
O3 Tb1 Tb1 39.07(6) 2_655 2_655 ?
O11 Tb1 Tb1 137.31(7) . 2_655 ?
O10 Tb1 Tb1 68.93(7) 1_545 2_655 ?
O4 Tb1 Tb1 84.96(6) . 2_655 ?
O3 Tb1 Tb1 34.47(6) . 2_655 ?
C8 Tb1 Tb1 59.84(7) . 2_655 ?
C2 C1 C6 117.3(3) . . ?
C2 C1 C8 117.5(3) . . ?
C6 C1 C8 125.1(3) . . ?
C1 C2 C3 120.9(3) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 C7 120.1(3) . . ?
C3 C4 C7 120.5(3) . . ?
C4 C5 C6 119.0(3) . . ?
C5 C6 C1 122.7(3) . . ?
C5 C6 N1 118.4(3) . . ?
C1 C6 N1 118.9(3) . . ?
O2 C7 O1 124.8(3) . . ?
O2 C7 C4 118.6(3) . . ?
O1 C7 C4 116.6(3) . . ?
O4 C8 O3 120.5(3) . . ?
O4 C8 C1 118.0(3) . . ?
O3 C8 C1 121.1(3) . . ?
O4 C8 Tb1 57.78(17) . . ?
O3 C8 Tb1 63.68(18) . . ?
C1 C8 Tb1 162.9(2) . . ?
O7 C9 O7 126.8(5) . 2_655 ?
O7 C9 C10 116.6(2) . . ?
O7 C9 C10 116.6(2) 2_655 . ?
C11 C10 C11 119.1(5) 2_655 . ?
C11 C10 C9 120.5(2) 2_655 . ?
C11 C10 C9 120.5(2) . . ?
C12 C11 C10 120.3(3) . . ?
C11 C12 C13 121.4(3) . . ?
C11 C12 N2 115.4(4) . . ?
C13 C12 N2 122.8(4) . . ?
C12 C13 C12 117.5(5) 2_655 . ?
C12 C13 C14 121.3(2) 2_655 . ?
C12 C13 C14 121.3(2) . . ?
O10 C14 O10 126.7(5) 2_655 . ?
O10 C14 C13 116.6(2) 2_655 . ?
O10 C14 C13 116.6(2) . . ?
O5 N1 O6 122.0(4) . . ?
O5 N1 C6 118.8(3) . . ?
O6 N1 C6 119.2(3) . . ?
O8 N2 O9 121.9(7) . . ?
O8 N2 C12 118.0(6) . . ?
O9 N2 C12 120.1(6) . . ?
C7 O1 Tb1 144.9(2) . 8_466 ?
C7 O2 Tb1 134.5(2) . 4_545 ?
C8 O3 Tb1 159.9(2) . 2_655 ?
C8 O3 Tb1 90.7(2) . . ?
Tb1 O3 Tb1 106.46(9) 2_655 . ?
C8 O4 Tb1 97.0(2) . . ?
C9 O7 Tb1 138.2(3) . . ?
N2 O8 O8 87.3(7) . 5_685 ?
C14 O10 Tb1 137.4(3) . 1_565 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.64
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.850
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.166
####################################################################### 
# 
# 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_ww_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc1yy917
_database_code_depnum_ccdc_archive 'CCDC 1815609'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H17 N4 O13 Tb'
_chemical_formula_weight         752.36

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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   11.9800(5)
_cell_length_b                   14.5780(6)
_cell_length_c                   15.2371(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.5310(10)
_cell_angle_gamma                90.00
_cell_volume                     2563.91(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    2.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_T_max  0.6143
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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-CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25667
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4506
_reflns_number_gt                3716
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0237P)²+1.2255P] 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         4506
_refine_ls_number_parameters     403
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0605
_refine_ls_wR_factor_gt          0.0577
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_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 0.847405(13) 0.435993(12) 0.014025(11) 0.01725(7) Uani 1 1 d . . .
C1 C 0.8620(3) 0.5270(3) -0.1522(2) 0.0216(8) Uani 1 1 d . . .
C2 C 0.8554(3) 0.5818(3) -0.2371(2) 0.0202(8) Uani 1 1 d . . .
C3 C 0.7997(3) 0.6655(3) -0.2460(2) 0.0254(9) Uani 1 1 d . . .
H3A H 0.7618 0.6829 -0.2027 0.030 Uiso 1 1 calc R . .
C4 C 0.7988(3) 0.7241(3) -0.3175(2) 0.0241(8) Uani 1 1 d . . .
H4A H 0.7617 0.7806 -0.3212 0.029 Uiso 1 1 calc R . .
C5 C 0.8532(3) 0.6991(3) -0.3839(2) 0.0200(8) Uani 1 1 d . . .
C6 C 0.9052(3) 0.6131(3) -0.3786(2) 0.0223(8) Uani 1 1 d . . .
H6A H 0.9389 0.5939 -0.4238 0.027 Uiso 1 1 calc R . .
C7 C 0.9063(3) 0.5567(2) -0.3059(2) 0.0210(8) Uani 1 1 d . . .
C8 C 0.8577(3) 0.7623(3) -0.4612(2) 0.0237(9) Uani 1 1 d . . .
C9 C 0.8540(3) 0.3422(3) 0.1735(3) 0.0247(9) Uani 1 1 d . . .
C10 C 0.8309(3) 0.2813(3) 0.2459(2) 0.0245(9) Uani 1 1 d . . .
C11 C 0.8302(3) 0.3164(3) 0.3301(2) 0.0234(8) Uani 1 1 d . . .
H11A H 0.8435 0.3784 0.3431 0.028 Uiso 1 1 calc R . .
C12 C 0.8092(3) 0.2566(3) 0.3946(2) 0.0208(8) Uani 1 1 d . . .
C13 C 0.7844(3) 0.1654(3) 0.3770(2) 0.0210(8) Uani 1 1 d . . .
C14 C 0.7824(3) 0.1323(3) 0.2908(2) 0.0279(9) Uani 1 1 d . . .
H14A H 0.7642 0.0712 0.2764 0.033 Uiso 1 1 calc R . .
C15 C 0.8075(3) 0.1901(3) 0.2269(2) 0.0285(9) Uani 1 1 d . . .
H15A H 0.8086 0.1669 0.1703 0.034 Uiso 1 1 calc R . .
C16 C 0.7511(3) 0.0967(3) 0.4392(2) 0.0225(8) Uani 1 1 d . . .
C17 C 0.9549(3) 0.7996(3) -0.7304(3) 0.0345(10) Uani 1 1 d . . .
H17A H 0.9451 0.7373 -0.7434 0.041 Uiso 1 1 calc R . .
C18 C 0.9701(3) 0.8596(3) -0.7949(3) 0.0322(10) Uani 1 1 d . . .
H18A H 0.9683 0.8385 -0.8529 0.039 Uiso 1 1 calc R . .
C19 C 0.9883(3) 0.9521(3) -0.7741(3) 0.0263(9) Uani 1 1 d . . .
C20 C 0.9953(3) 0.9805(3) -0.6859(3) 0.0322(10) Uani 1 1 d . . .
H20A H 1.0141 1.0409 -0.6684 0.039 Uiso 1 1 calc R . .
C21 C 0.9740(3) 0.9184(3) -0.6251(3) 0.0331(10) Uani 1 1 d . . .
H21A H 0.9735 0.9376 -0.5670 0.040 Uiso 1 1 calc R . .
C22 C 0.9937(3) 1.0203(3) -0.8455(2) 0.0261(9) Uani 1 1 d . . .
C23 C 1.0850(4) 1.0821(3) -0.8336(3) 0.0381(11) Uani 1 1 d . . .
H23A H 1.1466 1.0807 -0.7813 0.046 Uiso 1 1 calc R . .
C24 C 1.0817(4) 1.1455(3) -0.9017(3) 0.0421(11) Uani 1 1 d . . .
H24A H 1.1434 1.1861 -0.8938 0.050 Uiso 1 1 calc R . .
C25 C 0.9107(4) 1.0918(3) -0.9880(3) 0.0369(10) Uani 1 1 d . . .
H25A H 0.8503 1.0948 -1.0410 0.044 Uiso 1 1 calc R . .
C26 C 0.9058(3) 1.0253(3) -0.9252(3) 0.0327(10) Uani 1 1 d . . .
H26A H 0.8441 0.9843 -0.9362 0.039 Uiso 1 1 calc R . .
O1 O 0.7720(2) 0.4898(2) -0.14253(16) 0.0299(6) Uani 1 1 d . . .
O1W O 0.9404(2) 0.32704(17) -0.06006(17) 0.0247(6) Uani 1 1 d D . .
H1WB H 0.952(3) 0.2729(12) -0.039(3) 0.037 Uiso 1 1 d D . .
H1WA H 1.002(2) 0.349(3) -0.069(3) 0.037 Uiso 1 1 d D . .
O2 O 0.9555(2) 0.52544(17) -0.08950(16) 0.0227(6) Uani 1 1 d . . .
O3 O 0.9356(3) 0.4078(2) -0.2549(2) 0.0564(9) Uani 1 1 d . . .
O4 O 1.0310(3) 0.4541(2) -0.3476(2) 0.0490(8) Uani 1 1 d . . .
O5 O 0.9117(2) 0.7346(2) -0.51516(18) 0.0426(8) Uani 1 1 d . . .
O6 O 0.8095(2) 0.83992(19) -0.46417(18) 0.0316(7) Uani 1 1 d . . .
O7 O 0.8305(2) 0.42608(18) 0.17187(17) 0.0294(6) Uani 1 1 d . . .
O8 O 0.8918(2) 0.30536(19) 0.11207(17) 0.0340(7) Uani 1 1 d . . .
O9 O 0.8186(3) 0.3773(2) 0.49603(19) 0.0463(8) Uani 1 1 d . . .
O10 O 0.8126(2) 0.2402(2) 0.54600(18) 0.0387(7) Uani 1 1 d . . .
O11 O 0.6473(2) 0.09691(19) 0.44434(18) 0.0294(6) Uani 1 1 d . . .
O12 O 0.8198(2) 0.03448(18) 0.47378(18) 0.0275(6) Uani 1 1 d . . .
N1 N 0.9619(3) 0.4667(2) -0.3026(2) 0.0341(8) Uani 1 1 d . . .
N2 N 0.8139(3) 0.2942(3) 0.4854(2) 0.0276(8) Uani 1 1 d . . .
N3 N 0.9542(3) 0.8315(3) -0.6479(2) 0.0334(9) Uani 1 1 d . . .
H3B H 0.9403 0.7940 -0.6086 0.040 Uiso 1 1 calc R . .
N4 N 0.9965(3) 1.1524(2) -0.9775(2) 0.0373(9) Uani 1 1 d . . .


_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 O6 2.304(2) 2_644 ?
Tb1 O1W 2.390(2) . ?
Tb1 O8 2.391(3) . ?
Tb1 O2 2.400(2) 3_765 ?
Tb1 O11 2.427(3) 2_655 ?
Tb1 O1 2.443(2) . ?
Tb1 O7 2.471(2) . ?
Tb1 O12 2.512(2) 2_655 ?
Tb1 O2 2.638(2) . ?
Tb1 C9 2.770(4) . ?
Tb1 C16 2.801(4) 2_655 ?
Tb1 C1 2.906(4) . ?
C1 O1 1.250(4) . ?
C1 O2 1.263(4) . ?
C1 C2 1.504(5) . ?
C2 C3 1.380(5) . ?
C2 C7 1.396(5) . ?
C3 C4 1.383(5) . ?
C4 C5 1.391(5) . ?
C5 C6 1.393(5) . ?
C5 C8 1.507(5) . ?
C6 C7 1.376(5) . ?
C7 N1 1.466(5) . ?
C8 O5 1.241(4) . ?
C8 O6 1.266(5) . ?
C9 O7 1.253(4) . ?
C9 O8 1.263(4) . ?
C9 C10 1.499(5) . ?
C10 C15 1.374(5) . ?
C10 C11 1.384(5) . ?
C11 C12 1.386(5) . ?
C12 C13 1.374(5) . ?
C12 N2 1.474(5) . ?
C13 C14 1.392(5) . ?
C13 C16 1.504(5) . ?
C14 C15 1.380(5) . ?
C16 O12 1.244(4) . ?
C16 O11 1.268(4) . ?
C16 Tb1 2.801(4) 2_645 ?
C17 N3 1.342(5) . ?
C17 C18 1.364(5) . ?
C18 C19 1.389(6) . ?
C19 C20 1.389(5) . ?
C19 C22 1.488(5) . ?
C20 C21 1.367(6) . ?
C21 N3 1.318(5) . ?
C22 C26 1.379(5) . ?
C22 C23 1.391(5) . ?
C23 C24 1.383(6) . ?
C24 N4 1.323(5) . ?
C25 N4 1.332(5) . ?
C25 C26 1.375(6) . ?
O2 Tb1 2.400(2) 3_765 ?
O3 N1 1.220(4) . ?
O4 N1 1.221(4) . ?
O6 Tb1 2.304(2) 2_654 ?
O9 N2 1.221(4) . ?
O10 N2 1.217(4) . ?
O11 Tb1 2.426(3) 2_645 ?
O12 Tb1 2.512(2) 2_645 ?

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
O6 Tb1 O1W 83.28(9) 2_644 . ?
O6 Tb1 O8 75.36(10) 2_644 . ?
O1W Tb1 O8 73.26(8) . . ?
O6 Tb1 O2 155.74(9) 2_644 3_765 ?
O1W Tb1 O2 81.88(8) . 3_765 ?
O8 Tb1 O2 82.03(9) . 3_765 ?
O6 Tb1 O11 129.48(9) 2_644 2_655 ?
O1W Tb1 O11 141.53(8) . 2_655 ?
O8 Tb1 O11 128.38(9) . 2_655 ?
O2 Tb1 O11 72.22(8) 3_765 2_655 ?
O6 Tb1 O1 79.50(9) 2_644 . ?
O1W Tb1 O1 81.34(9) . . ?
O8 Tb1 O1 145.92(10) . . ?
O2 Tb1 O1 116.85(8) 3_765 . ?
O11 Tb1 O1 85.51(9) 2_655 . ?
O6 Tb1 O7 90.75(9) 2_644 . ?
O1W Tb1 O7 126.21(9) . . ?
O8 Tb1 O7 53.68(8) . . ?
O2 Tb1 O7 82.74(8) 3_765 . ?
O11 Tb1 O7 78.78(9) 2_655 . ?
O1 Tb1 O7 149.77(9) . . ?
O6 Tb1 O12 77.01(9) 2_644 2_655 ?
O1W Tb1 O12 153.74(9) . 2_655 ?
O8 Tb1 O12 117.23(8) . 2_655 ?
O2 Tb1 O12 122.17(8) 3_765 2_655 ?
O11 Tb1 O12 52.67(8) 2_655 2_655 ?
O1 Tb1 O12 78.17(9) . 2_655 ?
O7 Tb1 O12 71.74(9) . 2_655 ?
O6 Tb1 O2 126.25(8) 2_644 . ?
O1W Tb1 O2 71.36(8) . . ?
O8 Tb1 O2 134.79(8) . . ?
O2 Tb1 O2 66.00(9) 3_765 . ?
O11 Tb1 O2 72.29(8) 2_655 . ?
O1 Tb1 O2 50.92(7) . . ?
O7 Tb1 O2 142.38(8) . . ?
O12 Tb1 O2 106.90(8) 2_655 . ?
O6 Tb1 C9 79.54(10) 2_644 . ?
O1W Tb1 C9 100.30(10) . . ?
O8 Tb1 C9 27.08(10) . . ?
O2 Tb1 C9 84.36(9) 3_765 . ?
O11 Tb1 C9 104.78(10) 2_655 . ?
O1 Tb1 C9 158.62(9) . . ?
O7 Tb1 C9 26.89(10) . . ?
O12 Tb1 C9 93.06(10) 2_655 . ?
O2 Tb1 C9 149.87(9) . . ?
O6 Tb1 C16 103.30(10) 2_644 2_655 ?
O1W Tb1 C16 163.32(9) . 2_655 ?
O8 Tb1 C16 123.07(9) . 2_655 ?
O2 Tb1 C16 96.29(10) 3_765 2_655 ?
O11 Tb1 C16 26.87(9) 2_655 2_655 ?
O1 Tb1 C16 84.79(10) . 2_655 ?
O7 Tb1 C16 69.58(9) . 2_655 ?
O12 Tb1 C16 26.36(9) 2_655 2_655 ?
O2 Tb1 C16 92.68(9) . 2_655 ?
C9 Tb1 C16 96.00(11) . 2_655 ?
O6 Tb1 C1 102.97(10) 2_644 . ?
O1W Tb1 C1 75.37(9) . . ?
O8 Tb1 C1 148.56(9) . . ?
O2 Tb1 C1 91.70(9) 3_765 . ?
O11 Tb1 C1 77.45(9) 2_655 . ?
O1 Tb1 C1 25.17(9) . . ?
O7 Tb1 C1 156.16(9) . . ?
O12 Tb1 C1 92.21(9) 2_655 . ?
O2 Tb1 C1 25.76(8) . . ?
C9 Tb1 C1 174.56(10) . . ?
C16 Tb1 C1 88.15(10) 2_655 . ?
O1 C1 O2 121.4(3) . . ?
O1 C1 C2 118.9(3) . . ?
O2 C1 C2 119.5(3) . . ?
O1 C1 Tb1 56.23(17) . . ?
O2 C1 Tb1 65.22(18) . . ?
C2 C1 Tb1 172.1(2) . . ?
C3 C2 C7 117.1(3) . . ?
C3 C2 C1 117.8(3) . . ?
C7 C2 C1 125.0(3) . . ?
C2 C3 C4 121.7(3) . . ?
C3 C4 C5 120.3(3) . . ?
C4 C5 C6 118.9(3) . . ?
C4 C5 C8 122.0(3) . . ?
C6 C5 C8 119.1(3) . . ?
C7 C6 C5 119.5(3) . . ?
C6 C7 C2 122.4(3) . . ?
C6 C7 N1 118.0(3) . . ?
C2 C7 N1 119.6(3) . . ?
O5 C8 O6 125.4(3) . . ?
O5 C8 C5 117.0(3) . . ?
O6 C8 C5 117.6(3) . . ?
O7 C9 O8 121.6(3) . . ?
O7 C9 C10 120.5(3) . . ?
O8 C9 C10 117.8(3) . . ?
O7 C9 Tb1 63.13(19) . . ?
O8 C9 Tb1 59.48(19) . . ?
C10 C9 Tb1 166.0(3) . . ?
C15 C10 C11 120.1(3) . . ?
C15 C10 C9 119.1(3) . . ?
C11 C10 C9 120.8(4) . . ?
C10 C11 C12 118.3(4) . . ?
C13 C12 C11 122.7(3) . . ?
C13 C12 N2 119.7(3) . . ?
C11 C12 N2 117.6(3) . . ?
C12 C13 C14 117.9(3) . . ?
C12 C13 C16 126.9(3) . . ?
C14 C13 C16 115.0(3) . . ?
C15 C14 C13 120.1(4) . . ?
C10 C15 C14 120.8(3) . . ?
O12 C16 O11 121.6(3) . . ?
O12 C16 C13 119.8(3) . . ?
O11 C16 C13 117.9(3) . . ?
O12 C16 Tb1 63.72(19) . 2_645 ?
O11 C16 Tb1 59.87(19) . 2_645 ?
C13 C16 Tb1 156.7(2) . 2_645 ?
N3 C17 C18 119.3(4) . . ?
C17 C18 C19 120.1(4) . . ?
C20 C19 C18 118.4(4) . . ?
C20 C19 C22 120.3(4) . . ?
C18 C19 C22 121.2(3) . . ?
C21 C20 C19 119.0(4) . . ?
N3 C21 C20 120.7(4) . . ?
C26 C22 C23 118.0(4) . . ?
C26 C22 C19 120.4(3) . . ?
C23 C22 C19 121.6(4) . . ?
C24 C23 C22 118.1(4) . . ?
N4 C24 C23 124.5(4) . . ?
N4 C25 C26 124.0(4) . . ?
C25 C26 C22 119.0(4) . . ?
C1 O1 Tb1 98.6(2) . . ?
C1 O2 Tb1 156.6(2) . 3_765 ?
C1 O2 Tb1 89.02(19) . . ?
Tb1 O2 Tb1 114.00(9) 3_765 . ?
C8 O6 Tb1 151.6(3) . 2_654 ?
C9 O7 Tb1 90.0(2) . . ?
C9 O8 Tb1 93.4(2) . . ?
C16 O11 Tb1 93.3(2) . 2_645 ?
C16 O12 Tb1 89.9(2) . 2_645 ?
O3 N1 O4 123.4(4) . . ?
O3 N1 C7 117.6(3) . . ?
O4 N1 C7 119.0(3) . . ?
O10 N2 O9 123.3(3) . . ?
O10 N2 C12 117.8(3) . . ?
O9 N2 C12 118.9(3) . . ?
C21 N3 C17 122.3(4) . . ?
C24 N4 C25 116.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_ww_CCDC2
_audit_block_doi                 10.5517/ccdc.csd.cc1yy928
_database_code_depnum_ccdc_archive 'CCDC 1815610'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H17 N4 O13 Tb'
_chemical_formula_weight         752.36

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           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   11.7024(8)
_cell_length_b                   14.5744(9)
_cell_length_c                   15.8996(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.519(2)
_cell_angle_gamma                90.00
_cell_volume                     2612.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5921
_exptl_absorpt_correction_T_max  0.6194
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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-CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34170
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4596
_reflns_number_gt                4199
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0383P)²+0.6227P] 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         4596
_refine_ls_number_parameters     403
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_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 -0.166107(9) 0.445001(7) 0.505654(6) 0.01625(6) Uani 1 1 d . . .
O1 O -0.13955(15) 0.59473(12) 0.57231(12) 0.0281(4) Uani 1 1 d . . .
O1W O -0.07798(16) 0.34242(12) 0.42319(12) 0.0264(4) Uani 1 1 d D . .
H1WB H -0.0104(14) 0.359(2) 0.4190(19) 0.040 Uiso 1 1 d D . .
H1WA H -0.080(3) 0.2847(7) 0.4178(19) 0.040 Uiso 1 1 d D . .
O2 O -0.32578(17) 0.55099(11) 0.53271(13) 0.0272(4) Uani 1 1 d . . .
O3 O -0.2784(2) 0.75766(14) 0.49115(12) 0.0481(5) Uani 1 1 d . . .
O4 O -0.3192(3) 0.88528(15) 0.54231(17) 0.0750(8) Uani 1 1 d . . .
O5 O -0.35268(18) 0.79819(12) 0.91550(12) 0.0334(4) Uani 1 1 d . . .
O6 O -0.31370(18) 0.91964(13) 0.84696(12) 0.0318(4) Uani 1 1 d . . .
O7 O -0.22927(16) 0.52782(15) 0.36712(12) 0.0343(4) Uani 1 1 d . . .
O8 O -0.03802(15) 0.54130(11) 0.42049(11) 0.0226(4) Uani 1 1 d . . .
O9 O -0.0873(2) 0.43144(14) 0.25212(15) 0.0516(6) Uani 1 1 d . . .
O10 O 0.0160(2) 0.46966(17) 0.16448(17) 0.0602(7) Uani 1 1 d . . .
O11 O -0.06124(19) 0.75949(14) 0.01684(13) 0.0446(5) Uani 1 1 d . . .
O12 O -0.16503(15) 0.86770(12) 0.06169(11) 0.0298(4) Uani 1 1 d . . .
C1 C -0.2457(2) 0.60172(16) 0.57603(15) 0.0213(5) Uani 1 1 d . . .
C2 C -0.2712(2) 0.66546(17) 0.64385(15) 0.0220(5) Uani 1 1 d . . .
C3 C -0.2738(2) 0.62727(18) 0.72296(16) 0.0297(6) Uani 1 1 d . . .
H3A H -0.2629 0.5644 0.7314 0.036 Uiso 1 1 calc R . .
C4 C -0.2923(2) 0.68116(17) 0.78968(16) 0.0300(6) Uani 1 1 d . . .
H4A H -0.2938 0.6541 0.8423 0.036 Uiso 1 1 calc R . .
C5 C -0.3085(2) 0.77454(16) 0.77900(15) 0.0225(5) Uani 1 1 d . . .
C6 C -0.3054(2) 0.81449(17) 0.70068(16) 0.0242(5) Uani 1 1 d . . .
H6A H -0.3144 0.8776 0.6929 0.029 Uiso 1 1 calc R . .
C7 C -0.2888(2) 0.75969(17) 0.63437(15) 0.0230(5) Uani 1 1 d . . .
C8 C -0.3267(2) 0.83430(17) 0.85162(15) 0.0236(5) Uani 1 1 d . . .
C9 C -0.1320(2) 0.55664(15) 0.36166(17) 0.0217(6) Uani 1 1 d . . .
C10 C -0.1268(2) 0.61525(17) 0.28445(15) 0.0223(5) Uani 1 1 d . . .
C11 C -0.1641(2) 0.70563(18) 0.28221(16) 0.0267(6) Uani 1 1 d . . .
H11A H -0.1910 0.7286 0.3280 0.032 Uiso 1 1 calc R . .
C12 C -0.1619(2) 0.76243(17) 0.21258(15) 0.0253(5) Uani 1 1 d . . .
H12A H -0.1891 0.8225 0.2116 0.030 Uiso 1 1 calc R . .
C13 C -0.1196(2) 0.73057(17) 0.14446(15) 0.0219(5) Uani 1 1 d . . .
C14 C -0.0809(2) 0.64024(17) 0.14598(16) 0.0250(5) Uani 1 1 d . . .
H14A H -0.0524 0.6176 0.1008 0.030 Uiso 1 1 calc R . .
C15 C -0.0853(2) 0.58471(17) 0.21487(16) 0.0234(5) Uani 1 1 d . . .
C16 C -0.1150(2) 0.79029(17) 0.06802(16) 0.0250(5) Uani 1 1 d . . .
C17 C -0.1160(3) 0.1185(2) 0.47461(19) 0.0435(8) Uani 1 1 d . . .
H17A H -0.1149 0.1618 0.5178 0.052 Uiso 1 1 calc R . .
C18 C -0.1570(3) 0.0324(2) 0.4850(2) 0.0429(8) Uani 1 1 d . . .
H18A H -0.1831 0.0180 0.5338 0.051 Uiso 1 1 calc R . .
C19 C -0.1586(3) -0.0319(2) 0.4222(2) 0.0433(7) Uani 1 1 d . . .
H19A H -0.1868 -0.0908 0.4269 0.052 Uiso 1 1 calc R . .
C20 C -0.1174(3) -0.0072(2) 0.35143(19) 0.0373(7) Uani 1 1 d . . .
H20A H -0.1171 -0.0500 0.3081 0.045 Uiso 1 1 calc R . .
C21 C -0.0770(2) 0.08045(19) 0.34522(16) 0.0265(6) Uani 1 1 d . . .
C22 C -0.0360(2) 0.11022(17) 0.26871(16) 0.0238(5) Uani 1 1 d . . .
C23 C -0.0313(2) 0.20214(19) 0.24796(17) 0.0308(6) Uani 1 1 d . . .
H23A H -0.0487 0.2468 0.2845 0.037 Uiso 1 1 calc R . .
C24 C -0.0012(2) 0.2274(2) 0.17404(17) 0.0331(6) Uani 1 1 d . . .
H24A H 0.0014 0.2892 0.1601 0.040 Uiso 1 1 calc R . .
C25 C 0.0240(2) 0.0749(2) 0.13973(19) 0.0322(6) Uani 1 1 d . . .
H25A H 0.0436 0.0321 0.1024 0.039 Uiso 1 1 calc R . .
C26 C -0.0054(2) 0.04614(18) 0.21302(19) 0.0299(6) Uani 1 1 d . . .
H26A H -0.0051 -0.0161 0.2259 0.036 Uiso 1 1 calc R . .
N1 N -0.2942(2) 0.80359(16) 0.55031(15) 0.0358(6) Uani 1 1 d . . .
N2 N -0.0491(2) 0.48843(16) 0.21040(15) 0.0353(6) Uani 1 1 d . . .
N3 N 0.02447(19) 0.16373(16) 0.12181(14) 0.0315(5) Uani 1 1 d . . .
H3B H 0.0419 0.1808 0.0750 0.038 Uiso 1 1 calc R . .
N4 N -0.0775(2) 0.14403(15) 0.40648(14) 0.0344(5) Uani 1 1 d . . .


_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 O12 2.2778(16) 2_445 ?
Tb1 O8 2.3715(17) 3_566 ?
Tb1 O1W 2.3961(17) . ?
Tb1 O1 2.4095(17) . ?
Tb1 O6 2.4455(18) 2_446 ?
Tb1 O7 2.4461(18) . ?
Tb1 O5 2.4598(18) 2_446 ?
Tb1 O2 2.5481(18) . ?
Tb1 O8 2.6714(18) . ?
Tb1 C8 2.804(2) 2_446 ?
Tb1 C1 2.809(2) . ?
Tb1 C9 2.922(2) . ?
O1 C1 1.263(3) . ?
O2 C1 1.247(3) . ?
O3 N1 1.208(3) . ?
O4 N1 1.225(3) . ?
O5 C8 1.252(3) . ?
O5 Tb1 2.4598(18) 2_456 ?
O6 C8 1.258(3) . ?
O6 Tb1 2.4455(18) 2_456 ?
O7 C9 1.238(3) . ?
O8 C9 1.258(3) . ?
O8 Tb1 2.3715(17) 3_566 ?
O9 N2 1.220(3) . ?
O10 N2 1.219(3) . ?
O11 C16 1.239(3) . ?
O12 C16 1.262(3) . ?
O12 Tb1 2.2778(16) 2_455 ?
C1 C2 1.512(3) . ?
C2 C3 1.383(4) . ?
C2 C7 1.391(3) . ?
C3 C4 1.383(4) . ?
C4 C5 1.378(4) . ?
C5 C6 1.384(3) . ?
C5 C8 1.506(3) . ?
C6 C7 1.377(3) . ?
C7 N1 1.468(3) . ?
C8 Tb1 2.804(2) 2_456 ?
C9 C10 1.510(3) . ?
C10 C11 1.385(4) . ?
C10 C15 1.395(3) . ?
C11 C12 1.388(3) . ?
C12 C13 1.385(3) . ?
C13 C14 1.390(3) . ?
C13 C16 1.508(3) . ?
C14 C15 1.374(3) . ?
C15 N2 1.473(3) . ?
C17 N4 1.333(4) . ?
C17 C18 1.369(4) . ?
C18 C19 1.365(5) . ?
C19 C20 1.385(4) . ?
C20 C21 1.375(4) . ?
C21 N4 1.345(3) . ?
C21 C22 1.487(4) . ?
C22 C23 1.384(4) . ?
C22 C26 1.398(4) . ?
C23 C24 1.365(4) . ?
C24 N3 1.332(4) . ?
C25 N3 1.327(4) . ?
C25 C26 1.366(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Tb1 O8 155.05(6) 2_445 3_566 ?
O12 Tb1 O1W 83.13(6) 2_445 . ?
O8 Tb1 O1W 78.43(6) 3_566 . ?
O12 Tb1 O1 130.41(6) 2_445 . ?
O8 Tb1 O1 73.24(6) 3_566 . ?
O1W Tb1 O1 141.45(6) . . ?
O12 Tb1 O6 94.68(7) 2_445 2_446 ?
O8 Tb1 O6 83.17(6) 3_566 2_446 ?
O1W Tb1 O6 126.59(6) . 2_446 ?
O1 Tb1 O6 75.50(6) . 2_446 ?
O12 Tb1 O7 78.79(6) 2_445 . ?
O8 Tb1 O7 115.21(6) 3_566 . ?
O1W Tb1 O7 83.44(7) . . ?
O1 Tb1 O7 85.50(7) . . ?
O6 Tb1 O7 148.66(7) 2_446 . ?
O12 Tb1 O5 75.96(7) 2_445 2_446 ?
O8 Tb1 O5 83.11(6) 3_566 2_446 ?
O1W Tb1 O5 75.12(6) . 2_446 ?
O1 Tb1 O5 125.47(7) . 2_446 ?
O6 Tb1 O5 53.02(6) 2_446 2_446 ?
O7 Tb1 O5 148.47(7) . 2_446 ?
O12 Tb1 O2 78.23(6) 2_445 . ?
O8 Tb1 O2 123.53(6) 3_566 . ?
O1W Tb1 O2 155.93(6) . . ?
O1 Tb1 O2 52.47(6) . . ?
O6 Tb1 O2 70.53(6) 2_446 . ?
O7 Tb1 O2 78.13(7) . . ?
O5 Tb1 O2 114.26(6) 2_446 . ?
O12 Tb1 O8 123.74(6) 2_445 . ?
O8 Tb1 O8 65.12(6) 3_566 . ?
O1W Tb1 O8 70.64(6) . . ?
O1 Tb1 O8 73.94(6) . . ?
O6 Tb1 O8 140.92(6) 2_446 . ?
O7 Tb1 O8 50.18(6) . . ?
O5 Tb1 O8 136.85(6) 2_446 . ?
O2 Tb1 O8 107.66(6) . . ?
O12 Tb1 C8 83.44(7) 2_445 2_446 ?
O8 Tb1 C8 83.81(6) 3_566 2_446 ?
O1W Tb1 C8 101.21(7) . 2_446 ?
O1 Tb1 C8 101.15(7) . 2_446 ?
O6 Tb1 C8 26.61(7) 2_446 2_446 ?
O7 Tb1 C8 160.98(6) . 2_446 ?
O5 Tb1 C8 26.49(7) 2_446 2_446 ?
O2 Tb1 C8 91.72(7) . 2_446 ?
O8 Tb1 C8 148.76(6) . 2_446 ?
O12 Tb1 C1 104.54(7) 2_445 . ?
O8 Tb1 C1 97.56(7) 3_566 . ?
O1W Tb1 C1 164.19(7) . . ?
O1 Tb1 C1 26.62(6) . . ?
O6 Tb1 C1 67.29(6) 2_446 . ?
O7 Tb1 C1 84.55(7) . . ?
O5 Tb1 C1 119.88(6) 2_446 . ?
O2 Tb1 C1 26.34(6) . . ?
O8 Tb1 C1 93.75(6) . . ?
C8 Tb1 C1 93.47(7) 2_446 . ?
O12 Tb1 C9 100.97(7) 2_445 . ?
O8 Tb1 C9 90.60(7) 3_566 . ?
O1W Tb1 C9 75.50(6) . . ?
O1 Tb1 C9 79.15(6) . . ?
O6 Tb1 C9 154.62(7) 2_446 . ?
O7 Tb1 C9 24.69(6) . . ?
O5 Tb1 C9 150.62(6) 2_446 . ?
O2 Tb1 C9 93.14(7) . . ?
O8 Tb1 C9 25.50(6) . . ?
C8 Tb1 C9 174.02(7) 2_446 . ?
C1 Tb1 C9 89.35(7) . . ?
C1 O1 Tb1 94.64(14) . . ?
C1 O2 Tb1 88.61(15) . . ?
C8 O5 Tb1 92.29(15) . 2_456 ?
C8 O6 Tb1 92.80(15) . 2_456 ?
C9 O7 Tb1 99.71(15) . . ?
C9 O8 Tb1 156.52(16) . 3_566 ?
C9 O8 Tb1 88.44(14) . . ?
Tb1 O8 Tb1 114.88(6) 3_566 . ?
C16 O12 Tb1 143.58(16) . 2_455 ?
O2 C1 O1 122.0(2) . . ?
O2 C1 C2 119.7(2) . . ?
O1 C1 C2 117.8(2) . . ?
O2 C1 Tb1 65.05(13) . . ?
O1 C1 Tb1 58.74(12) . . ?
C2 C1 Tb1 158.91(16) . . ?
C3 C2 C7 117.2(2) . . ?
C3 C2 C1 117.2(2) . . ?
C7 C2 C1 125.5(2) . . ?
C4 C3 C2 121.0(2) . . ?
C5 C4 C3 120.7(2) . . ?
C4 C5 C6 119.4(2) . . ?
C4 C5 C8 121.3(2) . . ?
C6 C5 C8 119.3(2) . . ?
C7 C6 C5 119.2(2) . . ?
C6 C7 C2 122.5(2) . . ?
C6 C7 N1 117.6(2) . . ?
C2 C7 N1 119.9(2) . . ?
O5 C8 O6 121.5(2) . . ?
O5 C8 C5 119.6(2) . . ?
O6 C8 C5 118.9(2) . . ?
O5 C8 Tb1 61.23(13) . 2_456 ?
O6 C8 Tb1 60.59(13) . 2_456 ?
C5 C8 Tb1 173.80(16) . 2_456 ?
O7 C9 O8 121.6(2) . . ?
O7 C9 C10 119.1(2) . . ?
O8 C9 C10 119.2(2) . . ?
O7 C9 Tb1 55.61(12) . . ?
O8 C9 Tb1 66.06(13) . . ?
C10 C9 Tb1 174.66(17) . . ?
C11 C10 C15 117.2(2) . . ?
C11 C10 C9 118.5(2) . . ?
C15 C10 C9 124.2(2) . . ?
C10 C11 C12 121.0(2) . . ?
C13 C12 C11 120.7(2) . . ?
C12 C13 C14 119.1(2) . . ?
C12 C13 C16 122.3(2) . . ?
C14 C13 C16 118.6(2) . . ?
C15 C14 C13 119.4(2) . . ?
C14 C15 C10 122.6(2) . . ?
C14 C15 N2 116.8(2) . . ?
C10 C15 N2 120.5(2) . . ?
O11 C16 O12 125.3(2) . . ?
O11 C16 C13 117.0(2) . . ?
O12 C16 C13 117.7(2) . . ?
N4 C17 C18 124.1(3) . . ?
C19 C18 C17 118.5(3) . . ?
C18 C19 C20 118.5(3) . . ?
C21 C20 C19 120.0(3) . . ?
N4 C21 C20 121.3(2) . . ?
N4 C21 C22 117.1(2) . . ?
C20 C21 C22 121.5(2) . . ?
C23 C22 C26 117.5(2) . . ?
C23 C22 C21 121.3(2) . . ?
C26 C22 C21 121.1(2) . . ?
C24 C23 C22 120.1(3) . . ?
N3 C24 C23 120.2(3) . . ?
N3 C25 C26 119.9(3) . . ?
C25 C26 C22 120.1(3) . . ?
O3 N1 O4 122.7(2) . . ?
O3 N1 C7 119.3(2) . . ?
O4 N1 C7 118.0(2) . . ?
O10 N2 O9 123.5(3) . . ?
O10 N2 C15 118.5(2) . . ?
O9 N2 C15 118.1(2) . . ?
C25 N3 C24 122.1(2) . . ?
C17 N4 C21 117.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.092
####################################################################### 
# 
# 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.cc1yy939
_database_code_depnum_ccdc_archive 'CCDC 1815611'
_audit_update_record             
;
2018-01-09 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H15 N3 O13 Tb'
_chemical_formula_weight         712.31

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           monoclinic
_symmetry_space_group_name_H-M   P21/a

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

_cell_length_a                   15.308(3)
_cell_length_b                   15.900(3)
_cell_length_c                   11.580(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.12(3)
_cell_angle_gamma                90.00
_cell_volume                     2485.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.075
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.4692
_exptl_absorpt_correction_T_max  0.8106
_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  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32271
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4376
_reflns_number_gt                3227
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1108P)²+10.9315P] 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         4376
_refine_ls_number_parameters     399
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1622
_refine_ls_wR_factor_gt          0.1459
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_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 0.63349(2) 0.500406(19) 0.16709(3) 0.01633(18) Uani 1 1 d . . .
O3 O 0.6254(5) 0.4272(4) 0.3534(5) 0.0365(14) Uani 1 1 d . . .
C4 C 0.3805(6) 0.4932(4) 0.0961(8) 0.0187(17) Uani 1 1 d . . .
C5 C 0.6305(6) 0.4982(4) 0.5382(8) 0.0254(19) Uani 1 1 d . . .
O6 O 0.4635(4) 0.5006(3) 0.0996(5) 0.0236(12) Uani 1 1 d . . .
C7 C 0.3775(6) 0.4921(4) 0.2256(8) 0.0202(17) Uani 1 1 d . . .
C8 C 0.6294(7) 0.4260(5) 0.6027(8) 0.0314(19) Uani 1 1 d . . .
H8 H 0.6308 0.3738 0.5674 0.038 Uiso 1 1 calc R . .
C9 C 0.6322(6) 0.4951(5) 0.4091(8) 0.0254(19) Uani 1 1 d . . .
O10 O 0.5810(4) 0.3656(3) 0.0815(5) 0.0256(12) Uani 1 1 d . . .
O11 O 0.5719(4) 0.6360(3) 0.0893(5) 0.0246(11) Uani 1 1 d . . .
C12 C 0.3739(7) 0.5693(5) 0.2786(8) 0.035(2) Uani 1 1 d . . .
H12 H 0.3737 0.6185 0.2350 0.042 Uiso 1 1 calc R . .
C14 C 0.6267(7) 0.5748(5) 0.5896(7) 0.032(2) Uani 1 1 d . . .
H14 H 0.6265 0.6239 0.5458 0.038 Uiso 1 1 calc R . .
O15 O 0.6400(4) 0.5638(4) 0.3596(5) 0.0335(13) Uani 1 1 d . . .
O16 O 0.7768(4) 0.4085(4) 0.2679(6) 0.0439(15) Uani 1 1 d . . .
H16A H 0.7758 0.3805 0.3309 0.066 Uiso 1 1 d R . .
H16B H 0.8300 0.4382 0.2988 0.066 Uiso 1 1 d R . .
C17 C 0.3769(6) 0.4208(5) 0.2934(8) 0.0293(18) Uani 1 1 d . . .
C18 C 0.5144(5) 0.3382(4) -0.0262(7) 0.0193(15) Uani 1 1 d . . .
C20 C 0.6050(5) 0.1489(5) -0.2152(7) 0.0266(17) Uani 1 1 d . . .
C21 C 0.4855(6) 0.0622(5) 0.0745(7) 0.0327(18) Uani 1 1 d . . .
C22 C 0.6658(5) 0.1436(5) 0.4731(7) 0.0256(17) Uani 1 1 d . . .
H22 H 0.7056 0.1237 0.5575 0.031 Uiso 1 1 calc R . .
C23 C 0.6435(5) 0.2508(4) -0.0436(7) 0.0274(17) Uani 1 1 d . . .
H23 H 0.6909 0.2789 0.0296 0.033 Uiso 1 1 calc R . .
C24 C 0.5447(5) 0.2680(4) -0.0883(7) 0.0224(16) Uani 1 1 d . . .
C25 C 0.6735(5) 0.1919(5) -0.1067(7) 0.0280(18) Uani 1 1 d . . .
H25 H 0.7406 0.1813 -0.0753 0.034 Uiso 1 1 calc R . .
O27 O 0.9218(5) 0.5223(4) 0.3302(8) 0.055(2) Uani 1 1 d . . .
C28 C 0.8637(6) 0.5791(5) 0.2750(7) 0.0258(17) Uani 1 1 d . . .
C29 C 0.5880(7) 0.1054(5) 0.3832(9) 0.037(2) Uani 1 1 d . . .
H29 H 0.5625 0.0544 0.3933 0.045 Uiso 1 1 calc R . .
N30 N 0.3812(7) 0.3389(4) 0.2406(7) 0.049(2) Uani 1 1 d . . .
C31 C 0.5779(6) 0.0494(6) 0.0838(9) 0.048(2) Uani 1 1 d . . .
H31 H 0.6311 0.0825 0.1401 0.058 Uiso 1 1 calc R . .
C32 C 0.4082(7) 0.0131(6) -0.0091(11) 0.049(3) Uani 1 1 d . . .
H32 H 0.3457 0.0213 -0.0164 0.059 Uiso 1 1 calc R . .
C33 C 0.4656(7) 0.1305(6) 0.1497(8) 0.047(2) Uani 1 1 d . . .
H33A H 0.4440 0.1807 0.0958 0.056 Uiso 1 1 calc R . .
H33B H 0.4119 0.1127 0.1661 0.056 Uiso 1 1 calc R . .
N34 N 0.5513(5) 0.1518(4) 0.2746(6) 0.0334(16) Uani 1 1 d . . .
C37 C 0.5064(6) 0.1702(7) -0.2584(9) 0.052(3) Uani 1 1 d U . .
C39 C 0.4755(6) 0.2267(7) -0.1973(9) 0.051(3) Uani 1 1 d . A .
C40 C 0.6070(8) 0.2224(6) 0.3015(10) 0.054(3) Uani 1 1 d . . .
H40 H 0.5969 0.2671 0.2448 0.065 Uiso 1 1 calc R . .
C3 C 0.6795(7) 0.2156(6) 0.4250(9) 0.051(2) Uani 1 1 d . . .
H3 H 0.7301 0.2542 0.4691 0.061 Uiso 1 1 calc R . .
O1 O 0.3932(4) 0.3330(3) 0.1474(5) 0.0374(14) Uani 1 1 d . . .
O2 O 0.3706(10) 0.2764(5) 0.2960(9) 0.126(4) Uani 1 1 d U . .
O4 O 0.7775(4) 0.5856(3) 0.2627(5) 0.0285(12) Uani 1 1 d . . .
O8 O 0.3021(4) 0.4943(3) -0.0076(6) 0.0315(14) Uani 1 1 d . . .
N1 N 0.4335(8) 0.1456(7) -0.3931(13) 0.048(3) Uani 0.655(8) 1 d PU A 1
O5 O 0.3588(9) 0.1183(10) -0.3970(14) 0.104(5) Uani 0.655(8) 1 d PU A 1
N5 N 0.3708(13) 0.2071(11) -0.208(2) 0.031(5) Uani 0.345(8) 1 d P A 2
O7 O 0.3476(12) 0.2010(10) -0.1213(18) 0.042(5) Uani 0.345(8) 1 d PU A 2
O9 O 0.4494(10) 0.1530(9) -0.4855(11) 0.089(4) Uani 0.655(8) 1 d PU A 1
O12 O 0.3128(16) 0.2114(15) -0.321(2) 0.072(7) Uani 0.345(8) 1 d PU A 2


_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 O6 2.338(5) . ?
Tb1 O10 2.339(5) . ?
Tb1 O11 2.355(5) . ?
Tb1 O4 2.371(5) . ?
Tb1 O15 2.406(5) . ?
Tb1 O16 2.428(6) . ?
Tb1 O8 2.471(6) 3_665 ?
Tb1 O3 2.505(5) . ?
Tb1 O6 2.724(6) 3_665 ?
Tb1 C9 2.813(8) . ?
Tb1 C4 2.955(8) 3_665 ?
O3 C9 1.237(9) . ?
C4 O8 1.234(10) . ?
C4 O6 1.258(10) . ?
C4 C7 1.522(11) . ?
C4 Tb1 2.955(8) 3_665 ?
C5 C14 1.368(11) . ?
C5 C8 1.374(11) . ?
C5 C9 1.509(11) . ?
O6 Tb1 2.724(6) 3_665 ?
C7 C17 1.381(11) . ?
C7 C12 1.384(10) . ?
C8 C12 1.401(12) 3_666 ?
C9 O15 1.266(9) . ?
O10 C18 1.259(8) . ?
O11 C18 1.240(8) 3_665 ?
C12 C8 1.401(12) 3_666 ?
C14 C17 1.383(11) 3_666 ?
C17 C14 1.383(11) 3_666 ?
C17 N30 1.453(10) . ?
C18 O11 1.240(8) 3_665 ?
C18 C24 1.513(10) . ?
C20 C25 1.379(10) . ?
C20 C37 1.390(11) . ?
C20 C28 1.500(10) 2_645 ?
C21 C32 1.366(12) . ?
C21 C31 1.383(11) . ?
C21 C33 1.510(12) . ?
C22 C29 1.305(11) . ?
C22 C3 1.332(12) . ?
C23 C24 1.376(10) . ?
C23 C25 1.393(10) . ?
C24 C39 1.373(10) . ?
O27 C28 1.216(9) . ?
C28 O4 1.263(9) . ?
C28 C20 1.500(10) 2_655 ?
C29 N34 1.333(10) . ?
N30 O1 1.182(8) . ?
N30 O2 1.235(9) . ?
C31 C32 1.397(14) 3_655 ?
C32 C31 1.397(14) 3_655 ?
C33 N34 1.462(10) . ?
N34 C40 1.355(11) . ?
C37 C39 1.361(12) . ?
C37 N1 1.480(14) . ?
C39 N5 1.58(2) . ?
C40 C3 1.338(13) . ?
O8 Tb1 2.471(6) 3_665 ?
N1 O5 1.204(17) . ?
N1 O9 1.210(17) . ?
N5 O12 1.18(3) . ?
N5 O7 1.22(3) . ?

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
O6 Tb1 O10 75.73(16) . . ?
O6 Tb1 O11 71.88(16) . . ?
O10 Tb1 O11 132.91(19) . . ?
O6 Tb1 O4 143.03(17) . . ?
O10 Tb1 O4 141.23(18) . . ?
O11 Tb1 O4 76.83(18) . . ?
O6 Tb1 O15 82.10(19) . . ?
O10 Tb1 O15 129.26(18) . . ?
O11 Tb1 O15 78.75(19) . . ?
O4 Tb1 O15 72.82(18) . . ?
O6 Tb1 O16 140.58(18) . . ?
O10 Tb1 O16 72.80(19) . . ?
O11 Tb1 O16 147.44(18) . . ?
O4 Tb1 O16 71.9(2) . . ?
O15 Tb1 O16 100.0(2) . . ?
O6 Tb1 O8 121.6(2) . 3_665 ?
O10 Tb1 O8 83.85(17) . 3_665 ?
O11 Tb1 O8 84.93(17) . 3_665 ?
O4 Tb1 O8 73.67(18) . 3_665 ?
O15 Tb1 O8 145.23(18) . 3_665 ?
O16 Tb1 O8 78.0(2) . 3_665 ?
O6 Tb1 O3 77.8(2) . . ?
O10 Tb1 O3 78.04(18) . . ?
O11 Tb1 O3 125.55(17) . . ?
O4 Tb1 O3 106.02(19) . . ?
O15 Tb1 O3 52.7(2) . . ?
O16 Tb1 O3 72.9(2) . . ?
O8 Tb1 O3 149.15(18) 3_665 . ?
O6 Tb1 O6 72.2(2) . 3_665 ?
O10 Tb1 O6 67.61(15) . 3_665 ?
O11 Tb1 O6 70.48(15) . 3_665 ?
O4 Tb1 O6 115.01(16) . 3_665 ?
O15 Tb1 O6 144.63(18) . 3_665 ?
O16 Tb1 O6 115.30(18) . 3_665 ?
O8 Tb1 O6 49.38(18) 3_665 3_665 ?
O3 Tb1 O6 138.74(17) . 3_665 ?
O6 Tb1 C9 78.7(2) . . ?
O10 Tb1 C9 103.4(2) . . ?
O11 Tb1 C9 102.7(2) . . ?
O4 Tb1 C9 89.6(2) . . ?
O15 Tb1 C9 26.63(19) . . ?
O16 Tb1 C9 86.1(2) . . ?
O8 Tb1 C9 159.8(2) 3_665 . ?
O3 Tb1 C9 26.07(19) . . ?
O6 Tb1 C9 150.8(2) 3_665 . ?
O6 Tb1 C4 97.3(2) . 3_665 ?
O10 Tb1 C4 75.57(17) . 3_665 ?
O11 Tb1 C4 75.68(18) . 3_665 ?
O4 Tb1 C4 93.52(19) . 3_665 ?
O15 Tb1 C4 153.21(18) . 3_665 ?
O16 Tb1 C4 97.3(2) . 3_665 ?
O8 Tb1 C4 24.3(2) 3_665 3_665 ?
O3 Tb1 C4 153.54(18) . 3_665 ?
O6 Tb1 C4 25.2(2) 3_665 3_665 ?
C9 Tb1 C4 176.0(2) . 3_665 ?
C9 O3 Tb1 91.0(5) . . ?
O8 C4 O6 122.3(7) . . ?
O8 C4 C7 119.4(7) . . ?
O6 C4 C7 118.0(7) . . ?
O8 C4 Tb1 55.4(4) . 3_665 ?
O6 C4 Tb1 67.1(4) . 3_665 ?
C7 C4 Tb1 174.6(6) . 3_665 ?
C14 C5 C8 119.5(8) . . ?
C14 C5 C9 119.0(7) . . ?
C8 C5 C9 121.4(7) . . ?
C4 O6 Tb1 163.6(5) . . ?
C4 O6 Tb1 87.7(5) . 3_665 ?
Tb1 O6 Tb1 107.8(2) . 3_665 ?
C17 C7 C12 117.6(8) . . ?
C17 C7 C4 125.5(6) . . ?
C12 C7 C4 116.9(6) . . ?
C5 C8 C12 120.3(7) . 3_666 ?
O3 C9 O15 121.4(8) . . ?
O3 C9 C5 120.6(7) . . ?
O15 C9 C5 118.0(7) . . ?
O3 C9 Tb1 62.9(4) . . ?
O15 C9 Tb1 58.5(4) . . ?
C5 C9 Tb1 176.4(5) . . ?
C18 O10 Tb1 133.9(4) . . ?
C18 O11 Tb1 130.6(5) 3_665 . ?
C7 C12 C8 120.6(7) . 3_666 ?
C5 C14 C17 120.0(7) . 3_666 ?
C9 O15 Tb1 94.9(5) . . ?
C7 C17 C14 121.9(7) . 3_666 ?
C7 C17 N30 118.9(7) . . ?
C14 C17 N30 119.2(7) 3_666 . ?
O11 C18 O10 127.5(7) 3_665 . ?
O11 C18 C24 116.4(6) 3_665 . ?
O10 C18 C24 116.1(6) . . ?
C25 C20 C37 115.9(7) . . ?
C25 C20 C28 121.1(6) . 2_645 ?
C37 C20 C28 122.9(7) . 2_645 ?
C32 C21 C31 118.9(8) . . ?
C32 C21 C33 118.5(8) . . ?
C31 C21 C33 122.5(8) . . ?
C29 C22 C3 109.3(7) . . ?
C24 C23 C25 120.8(7) . . ?
C39 C24 C23 119.0(7) . . ?
C39 C24 C18 120.9(6) . . ?
C23 C24 C18 119.8(6) . . ?
C20 C25 C23 121.0(7) . . ?
O27 C28 O4 125.9(7) . . ?
O27 C28 C20 118.6(7) . 2_655 ?
O4 C28 C20 115.5(6) . 2_655 ?
C22 C29 N34 108.4(8) . . ?
O1 N30 O2 121.7(7) . . ?
O1 N30 C17 120.9(7) . . ?
O2 N30 C17 117.4(7) . . ?
C21 C31 C32 120.3(8) . 3_655 ?
C21 C32 C31 120.8(8) . 3_655 ?
N34 C33 C21 114.0(7) . . ?
C29 N34 C40 107.6(7) . . ?
C29 N34 C33 126.1(8) . . ?
C40 N34 C33 126.4(7) . . ?
C39 C37 C20 124.0(8) . . ?
C39 C37 N1 116.6(8) . . ?
C20 C37 N1 117.8(8) . . ?
C37 C39 C24 119.2(7) . . ?
C37 C39 N5 114.6(10) . . ?
C24 C39 N5 118.9(10) . . ?
C3 C40 N34 107.1(8) . . ?
C22 C3 C40 107.6(8) . . ?
C28 O4 Tb1 134.3(5) . . ?
C4 O8 Tb1 100.4(5) . 3_665 ?
O5 N1 O9 125.9(14) . . ?
O5 N1 C37 111.4(13) . . ?
O9 N1 C37 122.7(12) . . ?
O12 N5 O7 124(2) . . ?
O12 N5 C39 106.5(19) . . ?
O7 N5 C39 129.0(17) . . ?

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
O6 Tb1 O3 C9 -89.0(5) . . . . ?
O10 Tb1 O3 C9 -166.8(5) . . . . ?
O11 Tb1 O3 C9 -32.0(6) . . . . ?
O4 Tb1 O3 C9 53.0(5) . . . . ?
O15 Tb1 O3 C9 0.2(5) . . . . ?
O16 Tb1 O3 C9 117.8(5) . . . . ?
O8 Tb1 O3 C9 137.9(5) 3_665 . . . ?
O6 Tb1 O3 C9 -133.1(5) 3_665 . . . ?
C4 Tb1 O3 C9 -170.9(5) 3_665 . . . ?
O8 C4 O6 Tb1 -165.4(11) . . . . ?
C7 C4 O6 Tb1 21.0(18) . . . . ?
Tb1 C4 O6 Tb1 -161.0(15) 3_665 . . . ?
O8 C4 O6 Tb1 -4.5(6) . . . 3_665 ?
C7 C4 O6 Tb1 -178.0(5) . . . 3_665 ?
O10 Tb1 O6 C4 89.3(15) . . . . ?
O11 Tb1 O6 C4 -125.3(15) . . . . ?
O4 Tb1 O6 C4 -91.8(15) . . . . ?
O15 Tb1 O6 C4 -44.7(15) . . . . ?
O16 Tb1 O6 C4 51.5(16) . . . . ?
O8 Tb1 O6 C4 162.7(15) 3_665 . . . ?
O3 Tb1 O6 C4 8.8(15) . . . . ?
O6 Tb1 O6 C4 160.0(16) 3_665 . . . ?
C9 Tb1 O6 C4 -17.9(15) . . . . ?
C4 Tb1 O6 C4 162.4(14) 3_665 . . . ?
O10 Tb1 O6 Tb1 -70.66(17) . . . 3_665 ?
O11 Tb1 O6 Tb1 74.67(18) . . . 3_665 ?
O4 Tb1 O6 Tb1 108.2(3) . . . 3_665 ?
O15 Tb1 O6 Tb1 155.4(2) . . . 3_665 ?
O16 Tb1 O6 Tb1 -108.5(3) . . . 3_665 ?
O8 Tb1 O6 Tb1 2.7(2) 3_665 . . 3_665 ?
O3 Tb1 O6 Tb1 -151.21(19) . . . 3_665 ?
O6 Tb1 O6 Tb1 0.0 3_665 . . 3_665 ?
C9 Tb1 O6 Tb1 -177.8(2) . . . 3_665 ?
C4 Tb1 O6 Tb1 2.38(18) 3_665 . . 3_665 ?
O8 C4 C7 C17 91.3(10) . . . . ?
O6 C4 C7 C17 -95.0(9) . . . . ?
Tb1 C4 C7 C17 105(5) 3_665 . . . ?
O8 C4 C7 C12 -88.0(9) . . . . ?
O6 C4 C7 C12 85.7(9) . . . . ?
Tb1 C4 C7 C12 -74(5) 3_665 . . . ?
C14 C5 C8 C12 -1.2(15) . . . 3_666 ?
C9 C5 C8 C12 -178.9(9) . . . 3_666 ?
Tb1 O3 C9 O15 -0.4(9) . . . . ?
Tb1 O3 C9 C5 179.1(7) . . . . ?
C14 C5 C9 O3 -172.5(8) . . . . ?
C8 C5 C9 O3 5.2(14) . . . . ?
C14 C5 C9 O15 7.0(13) . . . . ?
C8 C5 C9 O15 -175.3(8) . . . . ?
C14 C5 C9 Tb1 -6(10) . . . . ?
C8 C5 C9 Tb1 172(9) . . . . ?
O6 Tb1 C9 O3 85.5(5) . . . . ?
O10 Tb1 C9 O3 13.3(5) . . . . ?
O11 Tb1 C9 O3 153.7(5) . . . . ?
O4 Tb1 C9 O3 -129.8(5) . . . . ?
O15 Tb1 C9 O3 -179.6(9) . . . . ?
O16 Tb1 C9 O3 -58.0(5) . . . . ?
O8 Tb1 C9 O3 -96.0(7) 3_665 . . . ?
O6 Tb1 C9 O3 81.2(6) 3_665 . . . ?
C4 Tb1 C9 O3 89(3) 3_665 . . . ?
O6 Tb1 C9 O15 -95.0(5) . . . . ?
O10 Tb1 C9 O15 -167.1(5) . . . . ?
O11 Tb1 C9 O15 -26.7(5) . . . . ?
O4 Tb1 C9 O15 49.7(5) . . . . ?
O16 Tb1 C9 O15 121.6(5) . . . . ?
O8 Tb1 C9 O15 83.6(7) 3_665 . . . ?
O3 Tb1 C9 O15 179.6(9) . . . . ?
O6 Tb1 C9 O15 -99.2(5) 3_665 . . . ?
C4 Tb1 C9 O15 -92(3) 3_665 . . . ?
O6 Tb1 C9 C5 -82(10) . . . . ?
O10 Tb1 C9 C5 -154(10) . . . . ?
O11 Tb1 C9 C5 -13(10) . . . . ?
O4 Tb1 C9 C5 63(10) . . . . ?
O15 Tb1 C9 C5 13(10) . . . . ?
O16 Tb1 C9 C5 135(10) . . . . ?
O8 Tb1 C9 C5 97(10) 3_665 . . . ?
O3 Tb1 C9 C5 -167(10) . . . . ?
O6 Tb1 C9 C5 -86(10) 3_665 . . . ?
C4 Tb1 C9 C5 -79(10) 3_665 . . . ?
O6 Tb1 O10 C18 53.7(6) . . . . ?
O11 Tb1 O10 C18 6.1(8) . . . . ?
O4 Tb1 O10 C18 -125.2(6) . . . . ?
O15 Tb1 O10 C18 120.7(6) . . . . ?
O16 Tb1 O10 C18 -150.3(7) . . . . ?
O8 Tb1 O10 C18 -71.1(6) 3_665 . . . ?
O3 Tb1 O10 C18 134.0(7) . . . . ?
O6 Tb1 O10 C18 -22.6(6) 3_665 . . . ?
C9 Tb1 O10 C18 128.1(6) . . . . ?
C4 Tb1 O10 C18 -47.9(6) 3_665 . . . ?
O6 Tb1 O11 C18 -12.5(6) . . . 3_665 ?
O10 Tb1 O11 C18 36.3(7) . . . 3_665 ?
O4 Tb1 O11 C18 -172.6(6) . . . 3_665 ?
O15 Tb1 O11 C18 -97.8(6) . . . 3_665 ?
O16 Tb1 O11 C18 171.2(6) . . . 3_665 ?
O8 Tb1 O11 C18 113.0(6) 3_665 . . 3_665 ?
O3 Tb1 O11 C18 -72.1(6) . . . 3_665 ?
O6 Tb1 O11 C18 64.5(6) 3_665 . . 3_665 ?
C9 Tb1 O11 C18 -86.0(6) . . . 3_665 ?
C4 Tb1 O11 C18 90.3(6) 3_665 . . 3_665 ?
C17 C7 C12 C8 0.5(15) . . . 3_666 ?
C4 C7 C12 C8 179.8(8) . . . 3_666 ?
C8 C5 C14 C17 0.9(15) . . . 3_666 ?
C9 C5 C14 C17 178.7(8) . . . 3_666 ?
O3 C9 O15 Tb1 0.4(9) . . . . ?
C5 C9 O15 Tb1 -179.1(7) . . . . ?
O6 Tb1 O15 C9 80.5(5) . . . . ?
O10 Tb1 O15 C9 16.2(6) . . . . ?
O11 Tb1 O15 C9 153.5(5) . . . . ?
O4 Tb1 O15 C9 -127.0(5) . . . . ?
O16 Tb1 O15 C9 -59.7(5) . . . . ?
O8 Tb1 O15 C9 -142.9(5) 3_665 . . . ?
O3 Tb1 O15 C9 -0.2(5) . . . . ?
O6 Tb1 O15 C9 123.8(5) 3_665 . . . ?
C4 Tb1 O15 C9 171.0(5) 3_665 . . . ?
C12 C7 C17 C14 -0.2(15) . . . 3_666 ?
C4 C7 C17 C14 -179.5(8) . . . 3_666 ?
C12 C7 C17 N30 -179.7(7) . . . . ?
C4 C7 C17 N30 1.1(13) . . . . ?
Tb1 O10 C18 O11 -43.1(11) . . . 3_665 ?
Tb1 O10 C18 C24 134.2(6) . . . . ?
C25 C23 C24 C39 -0.6(12) . . . . ?
C25 C23 C24 C18 -174.1(7) . . . . ?
O11 C18 C24 C39 -10.2(11) 3_665 . . . ?
O10 C18 C24 C39 172.1(8) . . . . ?
O11 C18 C24 C23 163.1(7) 3_665 . . . ?
O10 C18 C24 C23 -14.5(10) . . . . ?
C37 C20 C25 C23 2.0(12) . . . . ?
C28 C20 C25 C23 -173.6(7) 2_645 . . . ?
C24 C23 C25 C20 -0.3(12) . . . . ?
C3 C22 C29 N34 1.1(10) . . . . ?
C7 C17 N30 O1 6.3(13) . . . . ?
C14 C17 N30 O1 -173.2(9) 3_666 . . . ?
C7 C17 N30 O2 -172.9(10) . . . . ?
C14 C17 N30 O2 7.7(14) 3_666 . . . ?
C32 C21 C31 C32 -0.3(16) . . . 3_655 ?
C33 C21 C31 C32 -178.0(9) . . . 3_655 ?
C31 C21 C32 C31 0.3(17) . . . 3_655 ?
C33 C21 C32 C31 178.1(9) . . . 3_655 ?
C32 C21 C33 N34 152.5(9) . . . . ?
C31 C21 C33 N34 -29.7(12) . . . . ?
C22 C29 N34 C40 -2.3(10) . . . . ?
C22 C29 N34 C33 178.3(7) . . . . ?
C21 C33 N34 C29 -74.0(11) . . . . ?
C21 C33 N34 C40 106.7(11) . . . . ?
C25 C20 C37 C39 -2.9(15) . . . . ?
C28 C20 C37 C39 172.6(10) 2_645 . . . ?
C25 C20 C37 N1 162.5(10) . . . . ?
C28 C20 C37 N1 -22.1(15) 2_645 . . . ?
C20 C37 C39 C24 2.1(17) . . . . ?
N1 C37 C39 C24 -163.4(11) . . . . ?
C20 C37 C39 N5 -147.7(12) . . . . ?
N1 C37 C39 N5 46.7(16) . . . . ?
C23 C24 C39 C37 -0.2(15) . . . . ?
C18 C24 C39 C37 173.2(9) . . . . ?
C23 C24 C39 N5 148.3(11) . . . . ?
C18 C24 C39 N5 -38.3(15) . . . . ?
C29 N34 C40 C3 2.6(11) . . . . ?
C33 N34 C40 C3 -178.0(8) . . . . ?
C29 C22 C3 C40 0.5(11) . . . . ?
N34 C40 C3 C22 -1.9(12) . . . . ?
O27 C28 O4 Tb1 -59.0(12) . . . . ?
C20 C28 O4 Tb1 121.2(6) 2_655 . . . ?
O6 Tb1 O4 C28 -166.8(6) . . . . ?
O10 Tb1 O4 C28 11.5(8) . . . . ?
O11 Tb1 O4 C28 -134.1(7) . . . . ?
O15 Tb1 O4 C28 143.7(7) . . . . ?
O16 Tb1 O4 C28 36.7(7) . . . . ?
O8 Tb1 O4 C28 -45.6(6) 3_665 . . . ?
O3 Tb1 O4 C28 102.2(7) . . . . ?
O6 Tb1 O4 C28 -73.3(7) 3_665 . . . ?
C9 Tb1 O4 C28 122.8(7) . . . . ?
C4 Tb1 O4 C28 -59.7(7) 3_665 . . . ?
O6 C4 O8 Tb1 5.0(7) . . . 3_665 ?
C7 C4 O8 Tb1 178.5(5) . . . 3_665 ?
C39 C37 N1 O5 -56.2(16) . . . . ?
C20 C37 N1 O5 137.4(13) . . . . ?
C39 C37 N1 O9 123.8(14) . . . . ?
C20 C37 N1 O9 -42.6(18) . . . . ?
C37 C39 N5 O12 -64(2) . . . . ?
C24 C39 N5 O12 146.5(16) . . . . ?
C37 C39 N5 O7 126.8(18) . . . . ?
C24 C39 N5 O7 -23(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.111
