# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1009235'
_audit_update_record             
;
2014-11-20 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H45 Eu N8 O16'
_chemical_formula_weight         1189.91

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'

_cell_length_a                   16.688(7)
_cell_length_b                   16.688(7)
_cell_length_c                   17.360(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4835(5)
_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       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2412
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  2.442
_exptl_absorpt_correction_T_max  28.188
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_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  MoKα
_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            13597
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         27.09
_reflns_number_total             5330
_reflns_number_gt                4253
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0850P)²+3.5000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.400(18)
_refine_ls_number_reflns         5330
_refine_ls_number_parameters     367
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1442
_refine_ls_wR_factor_gt          0.1226
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_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
Eu1 Eu 0.5000 0.5000 0.68098(4) 0.02985(14) Uani 0.778(2) 2 d SP . .
Eu2 Eu 0.5000 0.5000 0.52035(12) 0.0377(8) Uani 0.222(2) 2 d SP . .
O1 O 0.5890(3) 0.5564(3) 0.7761(3) 0.0521(12) Uani 1 1 d . . .
O2 O 0.6448(3) 0.6601(3) 0.8339(3) 0.0496(12) Uani 1 1 d D . .
H2A H 0.625(5) 0.699(3) 0.856(4) 0.059 Uiso 1 1 d D . .
O3 O 0.6063(3) 0.8002(3) 0.8696(4) 0.0489(13) Uani 1 1 d . . .
O4 O 0.4942(3) 0.8724(3) 0.8737(3) 0.0549(13) Uani 1 1 d . . .
O5 O 0.5895(5) 0.0544(4) 0.6670(6) 0.104(3) Uani 1 1 d . . .
O6 O 0.6459(4) 0.1611(4) 0.6123(4) 0.0784(19) Uani 1 1 d . . .
H6A H 0.6339 0.2076 0.6022 0.118 Uiso 1 1 calc R . .
O7 O 0.6057(3) 0.3049(3) 0.5817(4) 0.0588(15) Uani 1 1 d . . .
O8 O 0.4974(3) 0.3818(4) 0.6064(3) 0.0651(16) Uani 1 1 d . . .
N1 N 0.4402(3) 0.6277(3) 0.7709(3) 0.0356(11) Uani 1 1 d . . .
N2 N 0.4059(3) 0.7504(3) 0.8078(3) 0.0347(11) Uani 1 1 d D . .
H2 H 0.376(4) 0.787(3) 0.828(4) 0.042 Uiso 1 1 d D . .
N3 N 0.4394(4) 0.1288(3) 0.6714(4) 0.0508(14) Uani 1 1 d . . .
N4 N 0.4061(3) 0.2535(3) 0.6441(4) 0.0391(11) Uani 1 1 d D . .
H4 H 0.376(3) 0.295(3) 0.642(4) 0.047 Uiso 1 1 d D . .
C1 C 0.5842(4) 0.6253(4) 0.8033(3) 0.0367(13) Uani 1 1 d . . .
C2 C 0.5059(4) 0.6664(4) 0.8010(3) 0.0361(13) Uani 1 1 d . . .
C3 C 0.4869(3) 0.7439(4) 0.8234(3) 0.0341(13) Uani 1 1 d . . .
C4 C 0.5322(4) 0.8114(4) 0.8583(4) 0.0363(14) Uani 1 1 d . . .
C5 C 0.3801(4) 0.6805(4) 0.7787(4) 0.0358(14) Uani 1 1 d . . .
C6 C 0.2951(4) 0.6638(4) 0.7580(4) 0.0391(14) Uani 1 1 d . . .
C7 C 0.2643(4) 0.5865(4) 0.7672(4) 0.0439(15) Uani 1 1 d . . .
H7A H 0.2982 0.5455 0.7832 0.053 Uiso 1 1 calc R . .
C8 C 0.1846(4) 0.5697(5) 0.7530(4) 0.0509(18) Uani 1 1 d . . .
C9 C 0.1339(4) 0.6301(5) 0.7284(4) 0.0548(19) Uani 1 1 d . . .
C10 C 0.1653(4) 0.7070(5) 0.7205(5) 0.059(2) Uani 1 1 d . . .
H10A H 0.1311 0.7479 0.7048 0.070 Uiso 1 1 calc R . .
C11 C 0.2439(4) 0.7255(5) 0.7345(4) 0.0477(16) Uani 1 1 d . . .
H11A H 0.2627 0.7776 0.7286 0.057 Uiso 1 1 calc R . .
C12 C 0.1554(6) 0.4848(6) 0.7645(6) 0.077(3) Uani 1 1 d . . .
H12A H 0.1311 0.4659 0.7178 0.116 Uiso 1 1 calc R . .
H12B H 0.1167 0.4837 0.8053 0.116 Uiso 1 1 calc R . .
H12C H 0.1999 0.4510 0.7775 0.116 Uiso 1 1 calc R . .
C13 C 0.0474(5) 0.6126(7) 0.7113(5) 0.080(3) Uani 1 1 d . . .
H13A H 0.0233 0.6585 0.6873 0.120 Uiso 1 1 calc R . .
H13B H 0.0197 0.6006 0.7584 0.120 Uiso 1 1 calc R . .
H13C H 0.0439 0.5674 0.6771 0.120 Uiso 1 1 calc R . .
C14 C 0.5837(5) 0.1243(5) 0.6430(5) 0.063(2) Uani 1 1 d . . .
C15 C 0.5068(4) 0.1688(4) 0.6457(4) 0.0475(16) Uani 1 1 d . . .
C16 C 0.4866(4) 0.2463(4) 0.6275(4) 0.0415(14) Uani 1 1 d . . .
C17 C 0.5338(4) 0.3159(5) 0.6028(4) 0.0451(17) Uani 1 1 d . . .
C18 C 0.3786(4) 0.1808(4) 0.6696(4) 0.0439(15) Uani 1 1 d . . .
C19 C 0.2950(4) 0.1640(4) 0.6883(5) 0.0428(15) Uani 1 1 d . . .
C20 C 0.2667(4) 0.0850(4) 0.6809(5) 0.0523(16) Uani 1 1 d . . .
H20A H 0.3021 0.0446 0.6666 0.063 Uiso 1 1 calc R . .
C21 C 0.1875(5) 0.0665(5) 0.6945(4) 0.058(2) Uani 1 1 d . . .
C22 C 0.1351(5) 0.1279(6) 0.7185(5) 0.065(2) Uani 1 1 d . . .
C23 C 0.1646(4) 0.2057(5) 0.7276(5) 0.061(2) Uani 1 1 d . . .
H23A H 0.1300 0.2458 0.7444 0.074 Uiso 1 1 calc R . .
C24 C 0.2430(4) 0.2246(5) 0.7126(5) 0.0520(17) Uani 1 1 d . . .
H24A H 0.2613 0.2769 0.7184 0.062 Uiso 1 1 calc R . .
C25 C 0.1590(7) -0.0190(6) 0.6814(6) 0.085(3) Uani 1 1 d . . .
H25A H 0.2035 -0.0518 0.6659 0.128 Uiso 1 1 calc R . .
H25B H 0.1190 -0.0195 0.6417 0.128 Uiso 1 1 calc R . .
H25C H 0.1366 -0.0398 0.7282 0.128 Uiso 1 1 calc R . .
C26 C 0.0453(5) 0.1147(8) 0.7368(6) 0.094(4) Uani 1 1 d . . .
H26A H 0.0198 0.0893 0.6936 0.141 Uiso 1 1 calc R . .
H26B H 0.0202 0.1654 0.7466 0.141 Uiso 1 1 calc R . .
H26C H 0.0403 0.0811 0.7814 0.141 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
Eu1 O4 2.352(5) 4_464 ?
Eu1 O4 2.352(5) 7_644 ?
Eu1 O8 2.360(6) . ?
Eu1 O8 2.360(6) 6_554 ?
Eu1 O1 2.412(5) . ?
Eu1 O1 2.412(5) 6_554 ?
Eu1 Eu2 2.789(3) . ?
Eu1 N1 2.824(5) . ?
Eu1 N1 2.824(5) 6_554 ?
Eu2 O8 2.474(6) . ?
Eu2 O8 2.474(7) 6_554 ?
Eu2 O5 2.505(9) 4_564 ?
Eu2 O5 2.505(9) 7_544 ?
Eu2 O4 2.786(6) 4_464 ?
Eu2 O4 2.786(6) 7_644 ?
Eu2 N3 2.932(6) 7_544 ?
Eu2 N3 2.932(6) 4_564 ?
O1 C1 1.247(8) . ?
O2 C1 1.280(8) . ?
O2 H2A 0.825(10) . ?
O3 C4 1.265(8) . ?
O4 C4 1.229(8) . ?
O4 Eu1 2.352(5) 3_655 ?
O4 Eu2 2.786(6) 3_655 ?
O5 C14 1.244(11) . ?
O5 Eu2 2.505(9) 3_645 ?
O6 C14 1.319(12) . ?
O6 H6A 0.8200 . ?
O7 C17 1.269(9) . ?
O8 C17 1.257(9) . ?
N1 C5 1.342(8) . ?
N1 C2 1.375(8) . ?
N2 C5 1.342(8) . ?
N2 C3 1.383(7) . ?
N2 H2 0.863(10) . ?
N3 C18 1.336(9) . ?
N3 C15 1.381(10) . ?
N3 Eu2 2.932(6) 3_645 ?
N4 C18 1.370(9) . ?
N4 C16 1.379(8) . ?
N4 H4 0.860(10) . ?
C1 C2 1.476(8) . ?
C2 C3 1.387(9) . ?
C3 C4 1.487(9) . ?
C5 C6 1.489(9) . ?
C6 C7 1.397(9) . ?
C6 C11 1.400(10) . ?
C7 C8 1.382(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.384(11) . ?
C8 C12 1.511(11) . ?
C9 C10 1.392(12) . ?
C9 C13 1.503(10) . ?
C10 C11 1.369(10) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.483(11) . ?
C15 C16 1.374(10) . ?
C16 C17 1.467(10) . ?
C18 C19 1.461(9) . ?
C19 C24 1.398(10) . ?
C19 C20 1.405(9) . ?
C20 C21 1.377(10) . ?
C20 H20A 0.9300 . ?
C21 C22 1.410(13) . ?
C21 C25 1.523(11) . ?
C22 C23 1.398(12) . ?
C22 C26 1.546(11) . ?
C23 C24 1.372(10) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 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
O4 Eu1 O4 130.0(3) 4_464 7_644 ?
O4 Eu1 O8 77.6(2) 4_464 . ?
O4 Eu1 O8 75.51(19) 7_644 . ?
O4 Eu1 O8 75.51(19) 4_464 6_554 ?
O4 Eu1 O8 77.6(2) 7_644 6_554 ?
O8 Eu1 O8 113.4(3) . 6_554 ?
O4 Eu1 O1 146.18(17) 4_464 . ?
O4 Eu1 O1 75.4(2) 7_644 . ?
O8 Eu1 O1 135.47(18) . . ?
O8 Eu1 O1 92.21(19) 6_554 . ?
O4 Eu1 O1 75.4(2) 4_464 6_554 ?
O4 Eu1 O1 146.18(17) 7_644 6_554 ?
O8 Eu1 O1 92.21(19) . 6_554 ?
O8 Eu1 O1 135.47(18) 6_554 6_554 ?
O1 Eu1 O1 93.6(3) . 6_554 ?
O4 Eu1 Eu2 64.98(15) 4_464 . ?
O4 Eu1 Eu2 64.98(15) 7_644 . ?
O8 Eu1 Eu2 56.72(15) . . ?
O8 Eu1 Eu2 56.72(15) 6_554 . ?
O1 Eu1 Eu2 133.21(14) . . ?
O1 Eu1 Eu2 133.21(14) 6_554 . ?
O4 Eu1 N1 83.26(18) 4_464 . ?
O4 Eu1 N1 125.82(16) 7_644 . ?
O8 Eu1 N1 158.06(17) . . ?
O8 Eu1 N1 71.3(2) 6_554 . ?
O1 Eu1 N1 62.92(15) . . ?
O1 Eu1 N1 72.42(15) 6_554 . ?
Eu2 Eu1 N1 123.58(11) . . ?
O4 Eu1 N1 125.82(16) 4_464 6_554 ?
O4 Eu1 N1 83.26(18) 7_644 6_554 ?
O8 Eu1 N1 71.3(2) . 6_554 ?
O8 Eu1 N1 158.06(17) 6_554 6_554 ?
O1 Eu1 N1 72.42(15) . 6_554 ?
O1 Eu1 N1 62.92(15) 6_554 6_554 ?
Eu2 Eu1 N1 123.58(11) . 6_554 ?
N1 Eu1 N1 112.8(2) . 6_554 ?
O8 Eu2 O8 105.8(3) . 6_554 ?
O8 Eu2 O5 87.9(2) . 4_564 ?
O8 Eu2 O5 154.4(2) 6_554 4_564 ?
O8 Eu2 O5 154.4(2) . 7_544 ?
O8 Eu2 O5 87.9(2) 6_554 7_544 ?
O5 Eu2 O5 88.5(4) 4_564 7_544 ?
O8 Eu2 O4 68.04(18) . 4_464 ?
O8 Eu2 O4 66.22(18) 6_554 4_464 ?
O5 Eu2 O4 139.36(18) 4_564 4_464 ?
O5 Eu2 O4 99.4(2) 7_544 4_464 ?
O8 Eu2 O4 66.22(18) . 7_644 ?
O8 Eu2 O4 68.04(18) 6_554 7_644 ?
O5 Eu2 O4 99.4(2) 4_564 7_644 ?
O5 Eu2 O4 139.36(18) 7_544 7_644 ?
O4 Eu2 O4 99.8(2) 4_464 7_644 ?
O8 Eu2 Eu1 52.88(14) . . ?
O8 Eu2 Eu1 52.88(14) 6_554 . ?
O5 Eu2 Eu1 135.8(2) 4_564 . ?
O5 Eu2 Eu1 135.8(2) 7_544 . ?
O4 Eu2 Eu1 49.92(11) 4_464 . ?
O4 Eu2 Eu1 49.92(11) 7_644 . ?
O8 Eu2 N3 93.80(19) . 7_544 ?
O8 Eu2 N3 129.89(18) 6_554 7_544 ?
O5 Eu2 N3 68.9(2) 4_564 7_544 ?
O5 Eu2 N3 61.3(2) 7_544 7_544 ?
O4 Eu2 N3 80.16(17) 4_464 7_544 ?
O4 Eu2 N3 157.79(16) 7_644 7_544 ?
Eu1 Eu2 N3 125.89(13) . 7_544 ?
O8 Eu2 N3 129.89(18) . 4_564 ?
O8 Eu2 N3 93.80(19) 6_554 4_564 ?
O5 Eu2 N3 61.3(2) 4_564 4_564 ?
O5 Eu2 N3 68.9(2) 7_544 4_564 ?
O4 Eu2 N3 157.79(16) 4_464 4_564 ?
O4 Eu2 N3 80.16(17) 7_644 4_564 ?
Eu1 Eu2 N3 125.89(13) . 4_564 ?
N3 Eu2 N3 108.2(3) 7_544 4_564 ?
C1 O1 Eu1 125.5(4) . . ?
C1 O2 H2A 104(6) . . ?
C4 O4 Eu1 145.1(5) . 3_655 ?
C4 O4 Eu2 118.4(5) . 3_655 ?
Eu1 O4 Eu2 65.10(14) 3_655 3_655 ?
C14 O5 Eu2 122.2(6) . 3_645 ?
C14 O6 H6A 109.5 . . ?
C17 O8 Eu1 138.5(5) . . ?
C17 O8 Eu2 131.2(5) . . ?
Eu1 O8 Eu2 70.40(18) . . ?
C5 N1 C2 104.4(5) . . ?
C5 N1 Eu1 144.6(4) . . ?
C2 N1 Eu1 106.4(4) . . ?
C5 N2 C3 108.6(5) . . ?
C5 N2 H2 126(5) . . ?
C3 N2 H2 122(5) . . ?
C18 N3 C15 107.3(6) . . ?
C18 N3 Eu2 138.8(5) . 3_645 ?
C15 N3 Eu2 105.2(4) . 3_645 ?
C18 N4 C16 108.4(5) . . ?
C18 N4 H4 122(5) . . ?
C16 N4 H4 130(5) . . ?
O1 C1 O2 121.6(6) . . ?
O1 C1 C2 118.3(6) . . ?
O2 C1 C2 120.0(5) . . ?
N1 C2 C3 111.2(5) . . ?
N1 C2 C1 119.9(5) . . ?
C3 C2 C1 128.8(6) . . ?
N2 C3 C2 104.0(5) . . ?
N2 C3 C4 121.2(5) . . ?
C2 C3 C4 134.8(6) . . ?
O4 C4 O3 126.4(6) . . ?
O4 C4 C3 116.9(6) . . ?
O3 C4 C3 116.6(5) . . ?
N2 C5 N1 111.7(6) . . ?
N2 C5 C6 124.0(6) . . ?
N1 C5 C6 124.4(6) . . ?
C7 C6 C11 119.2(6) . . ?
C7 C6 C5 119.7(6) . . ?
C11 C6 C5 120.9(6) . . ?
C8 C7 C6 121.4(7) . . ?
C8 C7 H7A 119.3 . . ?
C6 C7 H7A 119.3 . . ?
C9 C8 C7 119.7(7) . . ?
C9 C8 C12 121.8(7) . . ?
C7 C8 C12 118.5(8) . . ?
C8 C9 C10 118.1(7) . . ?
C8 C9 C13 120.4(8) . . ?
C10 C9 C13 121.4(8) . . ?
C11 C10 C9 123.4(8) . . ?
C11 C10 H10A 118.3 . . ?
C9 C10 H10A 118.3 . . ?
C10 C11 C6 118.1(7) . . ?
C10 C11 H11A 121.0 . . ?
C6 C11 H11A 121.0 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 O6 120.7(8) . . ?
O5 C14 C15 121.8(9) . . ?
O6 C14 C15 117.5(8) . . ?
C16 C15 N3 109.2(6) . . ?
C16 C15 C14 132.6(7) . . ?
N3 C15 C14 118.2(7) . . ?
C15 C16 N4 105.9(6) . . ?
C15 C16 C17 132.9(6) . . ?
N4 C16 C17 121.0(6) . . ?
O8 C17 O7 126.7(7) . . ?
O8 C17 C16 114.8(6) . . ?
O7 C17 C16 118.5(7) . . ?
N3 C18 N4 109.2(6) . . ?
N3 C18 C19 126.6(6) . . ?
N4 C18 C19 124.2(6) . . ?
C24 C19 C20 119.9(6) . . ?
C24 C19 C18 121.4(6) . . ?
C20 C19 C18 118.7(6) . . ?
C21 C20 C19 121.1(7) . . ?
C21 C20 H20A 119.4 . . ?
C19 C20 H20A 119.4 . . ?
C20 C21 C22 118.9(7) . . ?
C20 C21 C25 119.0(8) . . ?
C22 C21 C25 122.1(8) . . ?
C23 C22 C21 119.3(7) . . ?
C23 C22 C26 116.7(9) . . ?
C21 C22 C26 124.0(9) . . ?
C24 C23 C22 121.9(8) . . ?
C24 C23 H23A 119.1 . . ?
C22 C23 H23A 119.1 . . ?
C23 C24 C19 118.9(7) . . ?
C23 C24 H24A 120.6 . . ?
C19 C24 H24A 120.6 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.09
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.157
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.103
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1009236'
_audit_update_record             
;
2014-11-20 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H45 N8 O16 Tb'
_chemical_formula_weight         1196.88

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           tetragonal
_symmetry_space_group_name_H-M   I4(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'

_cell_length_a                   16.6140(4)
_cell_length_b                   16.6140(4)
_cell_length_c                   17.3352(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4784.9(3)
_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       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2424
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  2.452
_exptl_absorpt_correction_T_max  27.435
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_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  MoKα
_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            15389
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         27.44
_reflns_number_total             5425
_reflns_number_gt                4615
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0400P)²+2.2000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.374(10)
_refine_ls_number_reflns         5425
_refine_ls_number_parameters     370
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.002
_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 0.5000 0.5000 0.68106(2) 0.02690(8) Uani 0.7343(11) 2 d SP . .
Tb2 Tb 0.5000 0.5000 0.52034(5) 0.0334(3) Uani 0.2657(11) 2 d SP . .
O1 O 0.58767(17) 0.55625(17) 0.77583(19) 0.0487(7) Uani 1 1 d . . .
O2 O 0.64476(19) 0.65968(18) 0.8338(2) 0.0496(7) Uani 1 1 d D . .
H2A H 0.631(3) 0.7043(15) 0.851(3) 0.059 Uiso 1 1 d D . .
O3 O 0.60580(17) 0.80050(19) 0.8699(2) 0.0467(8) Uani 1 1 d . . .
O4 O 0.49413(18) 0.87321(18) 0.8729(2) 0.0625(10) Uani 1 1 d . . .
H4A H 0.5082 0.8898 0.9173 0.094 Uiso 0.50 1 d PR . .
O5 O 0.5865(3) 0.0519(2) 0.6691(4) 0.1033(16) Uani 1 1 d . . .
O6 O 0.6449(3) 0.1599(3) 0.6143(3) 0.0814(12) Uani 1 1 d . . .
O7 O 0.60507(19) 0.3059(2) 0.5822(2) 0.0547(9) Uani 1 1 d D . .
H7 H 0.626(3) 0.2611(15) 0.586(3) 0.066 Uiso 1 1 d D . .
O8 O 0.4965(2) 0.3827(2) 0.6058(2) 0.0707(11) Uani 1 1 d . . .
N1 N 0.43975(18) 0.62838(18) 0.77161(19) 0.0355(7) Uani 1 1 d . . .
N2 N 0.40532(18) 0.75164(18) 0.8076(2) 0.0327(7) Uani 1 1 d D . .
H2 H 0.379(2) 0.7916(17) 0.826(2) 0.039 Uiso 1 1 d D . .
N3 N 0.4382(2) 0.1285(2) 0.6709(2) 0.0471(8) Uani 1 1 d . . .
N4 N 0.40497(19) 0.25332(19) 0.6439(2) 0.0355(7) Uani 1 1 d D . .
H4 H 0.377(2) 0.2969(15) 0.643(2) 0.043 Uiso 1 1 d D . .
C1 C 0.5834(2) 0.6248(2) 0.8031(2) 0.0376(8) Uani 1 1 d . . .
C2 C 0.5053(2) 0.6665(2) 0.8013(2) 0.0330(8) Uani 1 1 d . . .
C3 C 0.4857(2) 0.7444(2) 0.8234(2) 0.0304(8) Uani 1 1 d . . .
C4 C 0.5321(3) 0.8114(2) 0.8573(2) 0.0387(9) Uani 1 1 d . . .
C5 C 0.3779(2) 0.6807(2) 0.7779(3) 0.0346(9) Uani 1 1 d . . .
C6 C 0.2947(2) 0.6646(2) 0.7581(2) 0.0366(9) Uani 1 1 d . . .
C7 C 0.2642(2) 0.5874(3) 0.7665(3) 0.0420(9) Uani 1 1 d . . .
H7A H 0.2984 0.5461 0.7818 0.050 Uiso 1 1 calc R . .
C8 C 0.1841(3) 0.5707(3) 0.7525(2) 0.0490(11) Uani 1 1 d . . .
C9 C 0.1333(3) 0.6317(3) 0.7270(3) 0.0542(12) Uani 1 1 d . . .
C10 C 0.1635(3) 0.7085(3) 0.7195(3) 0.0559(14) Uani 1 1 d . . .
H10A H 0.1293 0.7496 0.7037 0.067 Uiso 1 1 calc R . .
C11 C 0.2435(2) 0.7262(3) 0.7347(3) 0.0471(10) Uani 1 1 d . . .
H11A H 0.2627 0.7785 0.7294 0.057 Uiso 1 1 calc R . .
C12 C 0.1551(4) 0.4842(4) 0.7636(4) 0.0747(17) Uani 1 1 d . . .
H12A H 0.1281 0.4663 0.7178 0.112 Uiso 1 1 calc R . .
H12B H 0.1185 0.4819 0.8065 0.112 Uiso 1 1 calc R . .
H12C H 0.2004 0.4499 0.7737 0.112 Uiso 1 1 calc R . .
C13 C 0.0451(3) 0.6157(4) 0.7097(3) 0.0796(19) Uani 1 1 d . . .
H13A H 0.0220 0.6620 0.6850 0.119 Uiso 1 1 calc R . .
H13B H 0.0169 0.6051 0.7570 0.119 Uiso 1 1 calc R . .
H13C H 0.0406 0.5700 0.6762 0.119 Uiso 1 1 calc R . .
C14 C 0.5819(3) 0.1230(4) 0.6433(3) 0.0653(14) Uani 1 1 d . . .
C15 C 0.5057(3) 0.1690(2) 0.6457(3) 0.0421(9) Uani 1 1 d . . .
C16 C 0.4855(2) 0.2465(2) 0.6279(2) 0.0375(9) Uani 1 1 d . . .
C17 C 0.5333(3) 0.3164(3) 0.6018(3) 0.0448(11) Uani 1 1 d . . .
C18 C 0.3779(2) 0.1816(2) 0.6689(2) 0.0377(9) Uani 1 1 d . . .
C19 C 0.2940(2) 0.1644(2) 0.6880(3) 0.0425(10) Uani 1 1 d . . .
C20 C 0.2651(3) 0.0861(2) 0.6807(3) 0.0503(10) Uani 1 1 d . . .
H20A H 0.3003 0.0454 0.6658 0.060 Uiso 1 1 calc R . .
C21 C 0.1859(3) 0.0672(3) 0.6950(3) 0.0541(12) Uani 1 1 d . . .
C22 C 0.1334(3) 0.1278(4) 0.7177(3) 0.0603(14) Uani 1 1 d . . .
C23 C 0.1632(3) 0.2072(3) 0.7272(3) 0.0606(14) Uani 1 1 d . . .
H23A H 0.1288 0.2478 0.7437 0.073 Uiso 1 1 calc R . .
C24 C 0.2421(2) 0.2247(3) 0.7123(3) 0.0489(10) Uani 1 1 d . . .
H24A H 0.2610 0.2770 0.7185 0.059 Uiso 1 1 calc R . .
C25 C 0.1569(4) -0.0181(3) 0.6812(4) 0.0871(18) Uani 1 1 d . . .
H25A H 0.2015 -0.0511 0.6657 0.131 Uiso 1 1 calc R . .
H25B H 0.1168 -0.0181 0.6414 0.131 Uiso 1 1 calc R . .
H25C H 0.1341 -0.0391 0.7280 0.131 Uiso 1 1 calc R . .
C26 C 0.0444(3) 0.1145(5) 0.7355(4) 0.089(2) Uani 1 1 d . . .
H26A H 0.0181 0.0930 0.6907 0.133 Uiso 1 1 calc R . .
H26B H 0.0200 0.1648 0.7493 0.133 Uiso 1 1 calc R . .
H26C H 0.0393 0.0772 0.7775 0.133 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 O4 2.338(3) 4_464 ?
Tb1 O4 2.338(3) 7_644 ?
Tb1 O8 2.346(4) . ?
Tb1 O8 2.346(4) 6_554 ?
Tb1 O1 2.386(3) . ?
Tb1 O1 2.386(3) 6_554 ?
Tb1 Tb2 2.7861(10) . ?
Tb1 N1 2.831(3) . ?
Tb1 N1 2.831(3) 6_554 ?
Tb2 O5 2.427(5) 4_564 ?
Tb2 O5 2.427(5) 7_544 ?
Tb2 O8 2.449(4) . ?
Tb2 O8 2.449(4) 6_554 ?
Tb2 O4 2.758(4) 7_644 ?
Tb2 O4 2.758(4) 4_464 ?
Tb2 N3 2.930(4) 7_544 ?
Tb2 N3 2.930(4) 4_564 ?
O1 C1 1.236(5) . ?
O2 C1 1.287(5) . ?
O2 H2A 0.833(10) . ?
O3 C4 1.256(5) . ?
O4 C4 1.236(5) . ?
O4 Tb1 2.338(3) 3_655 ?
O4 Tb2 2.758(4) 3_655 ?
O4 H4A 0.8502 . ?
O5 C14 1.265(7) . ?
O5 Tb2 2.427(5) 3_645 ?
O6 C14 1.313(7) . ?
O7 C17 1.252(5) . ?
O7 H7 0.821(10) . ?
O8 C17 1.262(6) . ?
N1 C5 1.350(5) . ?
N1 C2 1.362(5) . ?
N2 C5 1.365(5) . ?
N2 C3 1.369(5) . ?
N2 H2 0.861(10) . ?
N3 C18 1.336(5) . ?
N3 C15 1.379(6) . ?
N3 Tb2 2.930(4) 3_645 ?
N4 C18 1.345(5) . ?
N4 C16 1.370(5) . ?
N4 H4 0.858(10) . ?
C1 C2 1.471(5) . ?
C2 C3 1.389(5) . ?
C3 C4 1.476(5) . ?
C5 C6 1.449(5) . ?
C6 C7 1.386(6) . ?
C6 C11 1.391(6) . ?
C7 C8 1.382(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.391(7) . ?
C8 C12 1.528(7) . ?
C9 C10 1.378(7) . ?
C9 C13 1.520(6) . ?
C10 C11 1.387(6) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.479(7) . ?
C15 C16 1.367(5) . ?
C16 C17 1.478(6) . ?
C18 C19 1.461(5) . ?
C19 C24 1.388(6) . ?
C19 C20 1.393(5) . ?
C20 C21 1.375(6) . ?
C20 H20A 0.9300 . ?
C21 C22 1.389(8) . ?
C21 C25 1.515(6) . ?
C22 C23 1.418(7) . ?
C22 C26 1.526(7) . ?
C23 C24 1.367(6) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 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
O4 Tb1 O4 128.9(2) 4_464 7_644 ?
O4 Tb1 O8 76.83(13) 4_464 . ?
O4 Tb1 O8 75.40(13) 7_644 . ?
O4 Tb1 O8 75.40(13) 4_464 6_554 ?
O4 Tb1 O8 76.83(13) 7_644 6_554 ?
O8 Tb1 O8 112.44(19) . 6_554 ?
O4 Tb1 O1 146.18(11) 4_464 . ?
O4 Tb1 O1 76.31(12) 7_644 . ?
O8 Tb1 O1 136.34(11) . . ?
O8 Tb1 O1 92.42(12) 6_554 . ?
O4 Tb1 O1 76.31(12) 4_464 6_554 ?
O4 Tb1 O1 146.18(11) 7_644 6_554 ?
O8 Tb1 O1 92.42(12) . 6_554 ?
O8 Tb1 O1 136.34(11) 6_554 6_554 ?
O1 Tb1 O1 92.98(16) . 6_554 ?
O4 Tb1 Tb2 64.44(10) 4_464 . ?
O4 Tb1 Tb2 64.44(10) 7_644 . ?
O8 Tb1 Tb2 56.22(9) . . ?
O8 Tb1 Tb2 56.22(9) 6_554 . ?
O1 Tb1 Tb2 133.51(8) . . ?
O1 Tb1 Tb2 133.51(8) 6_554 . ?
O4 Tb1 N1 83.64(11) 4_464 . ?
O4 Tb1 N1 126.11(10) 7_644 . ?
O8 Tb1 N1 157.72(10) . . ?
O8 Tb1 N1 72.01(12) 6_554 . ?
O1 Tb1 N1 62.55(9) . . ?
O1 Tb1 N1 72.39(9) 6_554 . ?
Tb2 Tb1 N1 123.67(6) . . ?
O4 Tb1 N1 126.11(10) 4_464 6_554 ?
O4 Tb1 N1 83.64(11) 7_644 6_554 ?
O8 Tb1 N1 72.01(12) . 6_554 ?
O8 Tb1 N1 157.72(10) 6_554 6_554 ?
O1 Tb1 N1 72.39(9) . 6_554 ?
O1 Tb1 N1 62.55(9) 6_554 6_554 ?
Tb2 Tb1 N1 123.67(6) . 6_554 ?
N1 Tb1 N1 112.65(13) . 6_554 ?
O5 Tb2 O5 87.4(3) 4_564 7_544 ?
O5 Tb2 O8 88.54(16) 4_564 . ?
O5 Tb2 O8 154.20(12) 7_544 . ?
O5 Tb2 O8 154.20(12) 4_564 6_554 ?
O5 Tb2 O8 88.54(16) 7_544 6_554 ?
O8 Tb2 O8 105.54(19) . 6_554 ?
O5 Tb2 O4 99.98(14) 4_564 7_644 ?
O5 Tb2 O4 139.33(11) 7_544 7_644 ?
O8 Tb2 O4 66.43(11) . 7_644 ?
O8 Tb2 O4 67.66(12) 6_554 7_644 ?
O5 Tb2 O4 139.33(11) 4_564 4_464 ?
O5 Tb2 O4 99.98(14) 7_544 4_464 ?
O8 Tb2 O4 67.66(12) . 4_464 ?
O8 Tb2 O4 66.43(11) 6_554 4_464 ?
O4 Tb2 O4 99.74(13) 7_644 4_464 ?
O5 Tb2 Tb1 136.30(14) 4_564 . ?
O5 Tb2 Tb1 136.30(14) 7_544 . ?
O8 Tb2 Tb1 52.77(9) . . ?
O8 Tb2 Tb1 52.77(9) 6_554 . ?
O4 Tb2 Tb1 49.87(7) 7_644 . ?
O4 Tb2 Tb1 49.87(7) 4_464 . ?
O5 Tb2 N3 68.04(12) 4_564 7_544 ?
O5 Tb2 N3 61.51(12) 7_544 7_544 ?
O8 Tb2 N3 93.42(11) . 7_544 ?
O8 Tb2 N3 130.72(11) 6_554 7_544 ?
O4 Tb2 N3 157.42(9) 7_644 7_544 ?
O4 Tb2 N3 80.51(10) 4_464 7_544 ?
Tb1 Tb2 N3 126.05(8) . 7_544 ?
O5 Tb2 N3 61.51(12) 4_564 4_564 ?
O5 Tb2 N3 68.04(12) 7_544 4_564 ?
O8 Tb2 N3 130.73(11) . 4_564 ?
O8 Tb2 N3 93.42(11) 6_554 4_564 ?
O4 Tb2 N3 80.51(10) 7_644 4_564 ?
O4 Tb2 N3 157.42(9) 4_464 4_564 ?
Tb1 Tb2 N3 126.05(8) . 4_564 ?
N3 Tb2 N3 107.90(15) 7_544 4_564 ?
C1 O1 Tb1 126.1(2) . . ?
C1 O2 H2A 109(4) . . ?
C4 O4 Tb1 145.3(3) . 3_655 ?
C4 O4 Tb2 118.4(3) . 3_655 ?
Tb1 O4 Tb2 65.69(8) 3_655 3_655 ?
C4 O4 H4A 109.1 . . ?
Tb1 O4 H4A 46.1 3_655 . ?
Tb2 O4 H4A 109.1 3_655 . ?
C14 O5 Tb2 123.5(4) . 3_645 ?
C17 O7 H7 120(4) . . ?
C17 O8 Tb1 138.1(3) . . ?
C17 O8 Tb2 130.5(3) . . ?
Tb1 O8 Tb2 71.01(10) . . ?
C5 N1 C2 106.2(3) . . ?
C5 N1 Tb1 143.0(3) . . ?
C2 N1 Tb1 106.1(2) . . ?
C5 N2 C3 109.0(3) . . ?
C5 N2 H2 129(3) . . ?
C3 N2 H2 120(3) . . ?
C18 N3 C15 106.2(3) . . ?
C18 N3 Tb2 139.4(3) . 3_645 ?
C15 N3 Tb2 104.9(2) . 3_645 ?
C18 N4 C16 108.6(3) . . ?
C18 N4 H4 125(3) . . ?
C16 N4 H4 126(3) . . ?
O1 C1 O2 121.9(4) . . ?
O1 C1 C2 118.4(3) . . ?
O2 C1 C2 119.7(3) . . ?
N1 C2 C3 110.5(3) . . ?
N1 C2 C1 119.7(3) . . ?
C3 C2 C1 129.8(3) . . ?
N2 C3 C2 104.8(3) . . ?
N2 C3 C4 121.5(3) . . ?
C2 C3 C4 133.6(3) . . ?
O4 C4 O3 125.4(4) . . ?
O4 C4 C3 116.6(4) . . ?
O3 C4 C3 118.0(4) . . ?
N1 C5 N2 109.4(3) . . ?
N1 C5 C6 126.1(4) . . ?
N2 C5 C6 124.6(4) . . ?
C7 C6 C11 119.3(4) . . ?
C7 C6 C5 119.6(4) . . ?
C11 C6 C5 121.0(4) . . ?
C8 C7 C6 121.3(4) . . ?
C8 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C7 C8 C9 119.6(4) . . ?
C7 C8 C12 118.1(5) . . ?
C9 C8 C12 122.3(4) . . ?
C10 C9 C8 119.0(4) . . ?
C10 C9 C13 119.6(5) . . ?
C8 C9 C13 121.4(5) . . ?
C9 C10 C11 121.8(5) . . ?
C9 C10 H10A 119.1 . . ?
C11 C10 H10A 119.1 . . ?
C10 C11 C6 119.0(4) . . ?
C10 C11 H11A 120.5 . . ?
C6 C11 H11A 120.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 O6 121.6(5) . . ?
O5 C14 C15 121.6(5) . . ?
O6 C14 C15 116.8(5) . . ?
C16 C15 N3 109.3(4) . . ?
C16 C15 C14 133.7(4) . . ?
N3 C15 C14 116.9(4) . . ?
C15 C16 N4 105.8(3) . . ?
C15 C16 C17 132.6(4) . . ?
N4 C16 C17 121.5(3) . . ?
O7 C17 O8 126.8(4) . . ?
O7 C17 C16 119.1(4) . . ?
O8 C17 C16 114.1(4) . . ?
N3 C18 N4 110.1(3) . . ?
N3 C18 C19 125.5(3) . . ?
N4 C18 C19 124.4(3) . . ?
C24 C19 C20 119.2(4) . . ?
C24 C19 C18 121.4(4) . . ?
C20 C19 C18 119.4(4) . . ?
C21 C20 C19 121.8(4) . . ?
C21 C20 H20A 119.1 . . ?
C19 C20 H20A 119.1 . . ?
C20 C21 C22 119.1(4) . . ?
C20 C21 C25 119.2(5) . . ?
C22 C21 C25 121.6(5) . . ?
C21 C22 C23 119.2(4) . . ?
C21 C22 C26 124.0(5) . . ?
C23 C22 C26 116.8(5) . . ?
C24 C23 C22 120.7(5) . . ?
C24 C23 H23A 119.6 . . ?
C22 C23 H23A 119.6 . . ?
C23 C24 C19 120.0(4) . . ?
C23 C24 H24A 120.0 . . ?
C19 C24 H24A 120.0 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.058
