# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 Eu2 N4 O14'
_chemical_formula_weight         846.34

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           ORTHORHOMBIC
_symmetry_space_group_name_H-M   Pna(2)1

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'

_cell_length_a                   13.1154(16)
_cell_length_b                   6.6813(5)
_cell_length_c                   29.007(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2541.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7140
_cell_measurement_theta_min      2.0913
_cell_measurement_theta_max      27.5126

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.969
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7396
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28938
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5746
_reflns_number_gt                5294
_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)+(0.0287P)²+136.9048P] 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   0.45(6)
_refine_ls_number_reflns         5746
_refine_ls_number_parameters     361
_refine_ls_number_restraints     259
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.1679
_refine_ls_wR_factor_gt          0.1646
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.153
_refine_ls_shift/su_mean         0.011

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 0.65658(6) 0.32816(14) 0.06701(2) 0.0116(2) Uani 1 1 d . . .
Eu2 Eu 0.66590(6) 0.32869(16) 0.41890(2) 0.0150(2) Uani 1 1 d . . .
O2 O 0.9961(10) 0.214(2) 0.4407(6) 0.026(3) Uani 1 1 d U . .
C16 C 0.4052(10) 0.214(2) 0.0571(5) 0.005(3) Uani 1 1 d U . .
O8 O 0.6095(10) -0.329(2) 0.0572(5) 0.021(3) Uani 1 1 d U . .
O4 O 1.1212(10) 0.851(2) 0.4268(5) 0.020(3) Uani 1 1 d U . .
O7 O 0.3180(11) 0.301(2) 0.0494(6) 0.025(3) Uani 1 1 d U . .
C17 C 0.5790(12) -0.149(2) 0.0608(7) 0.014(4) Uani 1 1 d U . .
O10 O 0.6816(12) 0.364(3) -0.0145(6) 0.031(4) Uani 1 1 d . . .
H10E H 0.6938 0.2546 -0.0259 0.038 Uiso 1 1 calc R . .
H10B H 0.6743 0.4866 -0.0220 0.047 Uiso 1 1 d R . .
O13 O 0.6699(14) 0.133(3) 0.1398(7) 0.037(5) Uani 1 1 d . . .
O12 O 0.6800(13) 0.167(3) 0.3463(7) 0.030(4) Uani 1 1 d U . .
O5 O 0.6933(11) 0.355(2) 0.5006(5) 0.018(3) Uani 1 1 d U . .
H5B H 0.7095 0.2455 0.5110 0.022 Uiso 1 1 calc R . .
H5A H 0.6838 0.4755 0.5092 0.027 Uiso 1 1 d R . .
C11 C 1.0871(13) 0.679(3) 0.4239(7) 0.016(4) Uani 1 1 d U . .
C12 C 0.9150(13) 0.272(3) 0.4338(7) 0.018(4) Uani 1 1 d U . .
O3 O 1.1378(13) 0.517(3) 0.4394(6) 0.029(3) Uani 1 1 d U . .
O6 O 0.4880(9) 0.314(2) 0.0400(4) 0.012(3) Uani 1 1 d U . .
O11 O 0.5649(13) 0.400(2) 0.3499(5) 0.029(3) Uani 1 1 d U . .
O14 O 0.5549(12) 0.368(3) 0.1362(6) 0.031(4) Uani 1 1 d U . .
N4 N 0.4227(13) -0.288(3) 0.1005(6) 0.020(4) Uani 1 1 d U . .
H4B H 0.4502 -0.4011 0.1074 0.024 Uiso 1 1 calc R . .
N3 N 0.3180(15) -0.049(3) 0.0955(6) 0.024(4) Uani 1 1 d U . .
N1 N 0.8111(15) 0.540(3) 0.3932(6) 0.018(3) Uani 1 1 d U . .
C15 C 0.9106(11) 0.467(3) 0.4099(6) 0.009(3) Uani 1 1 d U . .
C19 C 0.4040(13) -0.001(3) 0.0754(7) 0.019(4) Uani 1 1 d U . .
N2 N 0.9342(12) 0.791(3) 0.3848(6) 0.015(3) Uani 1 1 d U . .
H2C H 0.9578 0.9084 0.3788 0.017 Uiso 1 1 calc R . .
C13 C 0.8345(16) 0.717(4) 0.3754(9) 0.028(5) Uani 1 1 d U . .
H13A H 0.7881 0.7886 0.3577 0.034 Uiso 1 1 calc R . .
C20 C 0.4738(13) -0.128(3) 0.0787(6) 0.014(4) Uani 1 1 d U . .
C18 C 0.3263(14) -0.241(4) 0.1091(8) 0.018(4) Uani 1 1 d U . .
H18A H 0.2759 -0.3219 0.1216 0.021 Uiso 1 1 calc R . .
C14 C 0.9842(14) 0.635(4) 0.4054(7) 0.021(4) Uani 1 1 d U . .
C6 C 0.5999(16) 0.259(3) 0.3302(7) 0.019(4) Uani 1 1 d U . .
O9 O 0.6279(11) -0.010(2) 0.0484(5) 0.018(3) Uani 1 1 d U . .
C7 C 0.5993(18) 0.217(3) 0.1581(9) 0.027(5) Uani 1 1 d U . .
C9 C 0.6789(12) 0.383(2) 0.2463(9) 0.035(4) Uani 1 1 d DU . .
H9A H 0.7304 0.3678 0.2696 0.053 Uiso 1 1 calc R . .
H9B H 0.6328 0.4877 0.2551 0.053 Uiso 1 1 calc R . .
H9C H 0.7105 0.4159 0.2175 0.053 Uiso 1 1 calc R . .
C4 C 0.5533(11) 0.159(2) 0.2841(5) 0.022(3) Uani 1 1 d DU . .
H4A H 0.5323 0.0201 0.2887 0.026 Uiso 1 1 calc R . .
C1 C 0.5397(16) 0.229(3) 0.2028(6) 0.075(5) Uani 1 1 d DU . .
O1 O 0.8301(9) 0.187(2) 0.4322(5) 0.013(3) Uani 1 1 d U . .
C8 C 0.660(2) -0.022(3) 0.2293(9) 0.112(14) Uani 1 1 d DU . .
H8A H 0.7098 -0.0619 0.2518 0.168 Uiso 1 1 calc R . .
H8B H 0.6914 -0.0185 0.1994 0.168 Uiso 1 1 calc R . .
H8C H 0.6048 -0.1154 0.2292 0.168 Uiso 1 1 calc RD . .
C3 C 0.4618(15) 0.301(4) 0.2759(7) 0.058(4) Uani 1 1 d DU . .
H3A H 0.3981 0.2280 0.2780 0.069 Uiso 1 1 calc R . .
H3B H 0.4613 0.4075 0.2987 0.069 Uiso 1 1 calc R . .
C2 C 0.476(2) 0.387(4) 0.2275(6) 0.075(5) Uani 1 1 d DU . .
H2A H 0.5110 0.5147 0.2286 0.090 Uiso 1 1 calc R . .
H2B H 0.4104 0.4055 0.2124 0.090 Uiso 1 1 calc R . .
C10 C 0.475(2) 0.041(5) 0.1941(11) 0.101(13) Uani 1 1 d DU . .
H10A H 0.4260 0.0676 0.1704 0.151 Uiso 1 1 calc R . .
H10C H 0.4408 0.0033 0.2220 0.151 Uiso 1 1 calc R . .
H10D H 0.5190 -0.0669 0.1844 0.151 Uiso 1 1 calc RD . .
C5 C 0.6200(12) 0.187(2) 0.2413(7) 0.081(8) Uani 1 1 d DU . .


_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 O6 2.347(12) . ?
Eu1 O7 2.344(15) 3 ?
Eu1 O9 2.353(15) . ?
Eu1 O8 2.388(14) 1_565 ?
Eu1 O10 2.399(17) . ?
Eu1 O14 2.424(17) . ?
Eu1 O13 2.486(19) . ?
Eu1 N3 2.71(2) 3 ?
Eu1 C7 2.84(2) . ?
Eu1 C17 3.350(17) . ?
Eu2 O4 2.234(15) 3_465 ?
Eu2 O2 2.333(14) 3_455 ?
Eu2 O1 2.384(12) . ?
Eu2 O3 2.414(18) 3_455 ?
Eu2 O5 2.404(14) . ?
Eu2 O12 2.372(19) . ?
Eu2 O11 2.448(16) . ?
Eu2 N1 2.48(2) . ?
Eu2 C6 2.76(2) . ?
Eu2 H5A 2.8070 . ?
O2 C12 1.15(2) . ?
O2 Eu2 2.333(14) 3 ?
C16 O7 1.30(2) . ?
C16 O6 1.368(19) . ?
C16 C19 1.53(2) . ?
O8 C17 1.27(2) . ?
O8 Eu1 2.388(14) 1_545 ?
O4 C11 1.23(2) . ?
O4 Eu2 2.234(14) 3_565 ?
O7 Eu1 2.344(15) 3_455 ?
C17 O9 1.18(2) . ?
C17 C20 1.48(2) . ?
O10 H10E 0.8200 . ?
O10 H10B 0.8501 . ?
O13 C7 1.20(3) . ?
O12 C6 1.30(3) . ?
O5 H5B 0.8200 . ?
O5 H5A 0.8500 . ?
C11 O3 1.35(2) . ?
C11 C14 1.48(2) . ?
C12 O1 1.25(2) . ?
C12 C15 1.47(3) . ?
O3 Eu2 2.414(18) 3 ?
O11 C6 1.20(3) . ?
O14 C7 1.33(3) . ?
N4 C20 1.41(3) . ?
N4 C18 1.33(3) . ?
N4 H4B 0.8600 . ?
N3 C19 1.31(3) . ?
N3 C18 1.34(3) . ?
N3 Eu1 2.71(2) 3_455 ?
N1 C13 1.33(3) . ?
N1 C15 1.47(2) . ?
C15 C14 1.49(3) . ?
C19 C20 1.25(3) . ?
N2 C14 1.37(3) . ?
N2 C13 1.43(3) . ?
N2 H2C 0.8600 . ?
C13 H13A 0.9300 . ?
C18 H18A 0.9300 . ?
C6 C4 1.61(3) . ?
C7 C1 1.52(3) . ?
C9 C5 1.527(9) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C4 C5 1.529(10) . ?
C4 C3 1.546(9) . ?
C4 H4A 0.9800 . ?
C1 C10 1.537(19) . ?
C1 C2 1.529(5) . ?
C1 C5 1.563(16) . ?
C8 C5 1.529(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C3 C2 1.528(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10C 0.9600 . ?
C10 H10D 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
O6 Eu1 O7 139.8(5) . 3 ?
O6 Eu1 O9 74.6(5) . . ?
O7 Eu1 O9 74.9(5) 3 . ?
O6 Eu1 O8 75.8(5) . 1_565 ?
O7 Eu1 O8 124.2(5) 3 1_565 ?
O9 Eu1 O8 148.4(5) . 1_565 ?
O6 Eu1 O10 78.7(5) . . ?
O7 Eu1 O10 72.5(6) 3 . ?
O9 Eu1 O10 83.8(6) . . ?
O8 Eu1 O10 79.7(6) 1_565 . ?
O6 Eu1 O14 76.2(5) . . ?
O7 Eu1 O14 135.9(6) 3 . ?
O9 Eu1 O14 101.9(6) . . ?
O8 Eu1 O14 81.5(6) 1_565 . ?
O10 Eu1 O14 151.6(6) . . ?
O6 Eu1 O13 109.1(5) . . ?
O7 Eu1 O13 85.9(6) 3 . ?
O9 Eu1 O13 72.7(6) . . ?
O8 Eu1 O13 128.4(6) 1_565 . ?
O10 Eu1 O13 151.7(6) . . ?
O14 Eu1 O13 52.6(6) . . ?
O6 Eu1 N3 149.3(6) . 3 ?
O7 Eu1 N3 64.0(6) 3 3 ?
O9 Eu1 N3 135.9(6) . 3 ?
O8 Eu1 N3 73.5(6) 1_565 3 ?
O10 Eu1 N3 98.0(6) . 3 ?
O14 Eu1 N3 96.8(6) . 3 ?
O13 Eu1 N3 88.4(6) . 3 ?
O6 Eu1 C7 92.9(5) . . ?
O7 Eu1 C7 110.1(7) 3 . ?
O9 Eu1 C7 85.4(6) . . ?
O8 Eu1 C7 107.0(6) 1_565 . ?
O10 Eu1 C7 167.8(6) . . ?
O14 Eu1 C7 27.7(7) . . ?
O13 Eu1 C7 24.9(6) . . ?
N3 Eu1 C7 93.8(6) 3 . ?
O6 Eu1 C17 70.0(4) . . ?
O7 Eu1 C17 84.9(5) 3 . ?
O9 Eu1 C17 13.0(5) . . ?
O8 Eu1 C17 145.8(4) 1_565 . ?
O10 Eu1 C17 94.8(6) . . ?
O14 Eu1 C17 88.9(6) . . ?
O13 Eu1 C17 64.5(6) . . ?
N3 Eu1 C17 140.5(6) 3 . ?
C7 Eu1 C17 73.8(6) . . ?
O4 Eu2 O2 80.8(5) 3_465 3_455 ?
O4 Eu2 O1 127.0(5) 3_465 . ?
O2 Eu2 O1 140.3(5) 3_455 . ?
O4 Eu2 O3 148.5(5) 3_465 3_455 ?
O2 Eu2 O3 70.7(5) 3_455 3_455 ?
O1 Eu2 O3 73.6(5) . 3_455 ?
O4 Eu2 O5 82.3(5) 3_465 . ?
O2 Eu2 O5 83.3(5) 3_455 . ?
O1 Eu2 O5 74.6(5) . . ?
O3 Eu2 O5 81.4(6) 3_455 . ?
O4 Eu2 O12 123.3(6) 3_465 . ?
O2 Eu2 O12 105.0(6) 3_455 . ?
O1 Eu2 O12 83.8(5) . . ?
O3 Eu2 O12 78.1(6) 3_455 . ?
O5 Eu2 O12 153.7(6) . . ?
O4 Eu2 O11 75.9(5) 3_465 . ?
O2 Eu2 O11 74.3(6) 3_455 . ?
O1 Eu2 O11 134.3(5) . . ?
O3 Eu2 O11 107.8(6) 3_455 . ?
O5 Eu2 O11 150.8(5) . . ?
O12 Eu2 O11 53.5(6) . . ?
O4 Eu2 N1 71.8(6) 3_465 . ?
O2 Eu2 N1 152.1(6) 3_455 . ?
O1 Eu2 N1 65.3(6) . . ?
O3 Eu2 N1 137.2(6) 3_455 . ?
O5 Eu2 N1 98.0(5) . . ?
O12 Eu2 N1 86.1(6) . . ?
O11 Eu2 N1 93.4(6) . . ?
O4 Eu2 C6 100.2(6) 3_465 . ?
O2 Eu2 C6 86.2(6) 3_455 . ?
O1 Eu2 C6 111.6(6) . . ?
O3 Eu2 C6 91.1(6) 3_455 . ?
O5 Eu2 C6 168.7(6) . . ?
O12 Eu2 C6 28.2(6) . . ?
O11 Eu2 C6 25.7(6) . . ?
N1 Eu2 C6 93.3(6) . . ?
O4 Eu2 H5A 65.8 3_465 . ?
O2 Eu2 H5A 82.5 3_455 . ?
O1 Eu2 H5A 84.9 . . ?
O3 Eu2 H5A 96.8 3_455 . ?
O5 Eu2 H5A 16.6 . . ?
O12 Eu2 H5A 168.6 . . ?
O11 Eu2 H5A 137.8 . . ?
N1 Eu2 H5A 91.0 . . ?
C6 Eu2 H5A 163.2 . . ?
C12 O2 Eu2 151.3(15) . 3 ?
O7 C16 O6 114.6(14) . . ?
O7 C16 C19 118.1(14) . . ?
O6 C16 C19 126.3(13) . . ?
C17 O8 Eu1 168.0(13) . 1_545 ?
C11 O4 Eu2 168.5(14) . 3_565 ?
C16 O7 Eu1 126.1(12) . 3_455 ?
O9 C17 O8 123.1(17) . . ?
O9 C17 C20 122.7(17) . . ?
O8 C17 C20 114.0(15) . . ?
O9 C17 Eu1 26.7(9) . . ?
O8 C17 Eu1 144.0(12) . . ?
C20 C17 Eu1 100.2(11) . . ?
Eu1 O10 H10E 109.5 . . ?
Eu1 O10 H10B 109.4 . . ?
H10E O10 H10B 141.1 . . ?
C7 O13 Eu1 94.5(16) . . ?
C6 O12 Eu2 92.5(13) . . ?
Eu2 O5 H5B 109.5 . . ?
Eu2 O5 H5A 109.7 . . ?
H5B O5 H5A 140.8 . . ?
O4 C11 O3 123.0(17) . . ?
O4 C11 C14 122.7(18) . . ?
O3 C11 C14 114.2(17) . . ?
O1 C12 O2 132(2) . . ?
O1 C12 C15 110.5(15) . . ?
O2 C12 C15 114.6(17) . . ?
C11 O3 Eu2 139.7(13) . 3 ?
C16 O6 Eu1 130.4(10) . . ?
C6 O11 Eu2 91.7(14) . . ?
C7 O14 Eu1 94.1(14) . . ?
C20 N4 C18 110.9(19) . . ?
C20 N4 H4B 124.6 . . ?
C18 N4 H4B 124.6 . . ?
C19 N3 C18 107.0(18) . . ?
C19 N3 Eu1 113.9(14) . 3_455 ?
C18 N3 Eu1 132.2(15) . 3_455 ?
C13 N1 C15 102.5(17) . . ?
C13 N1 Eu2 143.1(15) . . ?
C15 N1 Eu2 113.2(12) . . ?
N1 C15 C14 107.3(16) . . ?
N1 C15 C12 118.7(15) . . ?
C14 C15 C12 132.9(15) . . ?
N3 C19 C20 115.5(18) . . ?
N3 C19 C16 113.1(16) . . ?
C20 C19 C16 130.9(16) . . ?
C14 N2 C13 104.9(19) . . ?
C14 N2 H2C 127.6 . . ?
C13 N2 H2C 127.6 . . ?
N1 C13 N2 117(2) . . ?
N1 C13 H13A 121.7 . . ?
N2 C13 H13A 121.6 . . ?
C19 C20 N4 101.5(16) . . ?
C19 C20 C17 135.8(19) . . ?
N4 C20 C17 122.1(18) . . ?
N3 C18 N4 104.5(19) . . ?
N3 C18 H18A 127.7 . . ?
N4 C18 H18A 127.8 . . ?
N2 C14 C15 107.6(16) . . ?
N2 C14 C11 116.3(19) . . ?
C15 C14 C11 135.2(18) . . ?
O12 C6 O11 121(2) . . ?
O12 C6 C4 114.3(16) . . ?
O11 C6 C4 125.1(19) . . ?
O12 C6 Eu2 59.3(12) . . ?
O11 C6 Eu2 62.6(12) . . ?
C4 C6 Eu2 164.4(12) . . ?
C17 O9 Eu1 140.3(13) . . ?
O14 C7 O13 119(2) . . ?
O14 C7 C1 98(2) . . ?
O13 C7 C1 143(2) . . ?
O14 C7 Eu1 58.2(12) . . ?
O13 C7 Eu1 60.6(14) . . ?
C1 C7 Eu1 156.3(17) . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C4 C3 104.3(8) . . ?
C5 C4 C6 114.0(14) . . ?
C3 C4 C6 99.8(15) . . ?
C5 C4 H4A 112.6 . . ?
C3 C4 H4A 112.6 . . ?
C6 C4 H4A 112.7 . . ?
C7 C1 C10 95.7(19) . . ?
C7 C1 C2 136.2(18) . . ?
C10 C1 C2 110(2) . . ?
C7 C1 C5 104.8(16) . . ?
C10 C1 C5 109.8(12) . . ?
C2 C1 C5 99.2(9) . . ?
C12 O1 Eu2 128.9(13) . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C3 C4 106.2(8) . . ?
C2 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
C2 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C2 C1 103.7(10) . . ?
C3 C2 H2A 111.0 . . ?
C1 C2 H2A 111.0 . . ?
C3 C2 H2B 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
C1 C10 H10D 109.5 . . ?
H10A C10 H10D 109.5 . . ?
H10C C10 H10D 109.5 . . ?
C9 C5 C8 128.9(17) . . ?
C9 C5 C4 108.3(11) . . ?
C8 C5 C4 105.9(12) . . ?
C9 C5 C1 104.7(11) . . ?
C8 C5 C1 103.5(12) . . ?
C4 C5 C1 102.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.236
_refine_diff_density_min         -4.252
_refine_diff_density_rms         0.346
_database_code_depnum_ccdc_archive 'CCDC 1006630'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H17 N4 O14 Tb2'
_chemical_formula_weight         855.22

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   Pna21

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'

_cell_length_a                   13.149(2)
_cell_length_b                   6.6803(12)
_cell_length_c                   29.165(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2561.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6189
_cell_measurement_theta_min      2.6011
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1628
_exptl_absorpt_coefficient_mu    5.555
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6269
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18155
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         27.52
_reflns_number_total             5452
_reflns_number_gt                4612
_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)+(0.0394P)²+23.9292P] 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   0.47(4)
_refine_ls_number_reflns         5452
_refine_ls_number_parameters     415
_refine_ls_number_restraints     253
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.111
_refine_ls_shift/su_mean         0.011

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 0.66698(4) 0.32984(10) 0.267712(14) 0.01745(16) Uani 1 1 d . . .
Tb2 Tb 0.65766(4) 0.33026(10) -0.083191(13) 0.01638(15) Uani 1 1 d . . .
O22 O 0.8313(6) 0.1907(16) 0.2816(3) 0.020(2) Uani 1 1 d U . .
O21 O 1.1093(6) 0.8364(14) -0.0916(4) 0.027(2) Uani 1 1 d U . .
O20 O 0.8191(7) 0.1972(17) -0.1014(4) 0.023(2) Uani 1 1 d U . .
O19 O 1.1220(7) 0.8364(14) 0.2766(4) 0.028(3) Uani 1 1 d U . .
C16 C 1.0792(9) 0.661(2) -0.0890(5) 0.020(3) Uani 1 1 d U . .
O18 O 0.6830(8) 0.372(2) -0.1637(4) 0.037(3) Uani 1 1 d . . .
H18A H 0.6439 0.2988 -0.1777 0.044 Uiso 1 1 calc R . .
H18B H 0.7274 0.4542 -0.1735 0.044 Uiso 1 1 d R . .
O17 O 1.1292(7) 0.5109(15) -0.1021(3) 0.0237(19) Uani 1 1 d U . .
O16 O 0.6912(8) 0.3547(17) 0.3490(3) 0.025(2) Uani 1 1 d . . .
H16A H 0.6426 0.3039 0.3622 0.030 Uiso 1 1 calc R . .
H16B H 0.7443 0.4104 0.3596 0.030 Uiso 1 1 d R . .
O15 O 0.9958(7) 0.1947(15) 0.2906(4) 0.028(2) Uani 1 1 d U . .
C15 C 1.0887(9) 0.663(2) 0.2742(5) 0.018(3) Uani 1 1 d U . .
O14 O 0.6798(10) 0.147(2) 0.1953(5) 0.048(4) Uani 1 1 d . . .
O13 O 0.9888(6) 0.2023(18) -0.1084(3) 0.026(2) Uani 1 1 d U . .
O12 O 0.6720(10) 0.163(3) -0.0108(5) 0.051(5) Uani 1 1 d . . .
O11 O 1.1387(8) 0.5142(15) 0.2871(4) 0.035(2) Uani 1 1 d U . .
N4 N 0.9325(9) 0.790(2) 0.2363(4) 0.025(3) Uani 1 1 d U . .
H4B H 0.9563 0.9086 0.2318 0.029 Uiso 1 1 calc R . .
N2 N 0.8109(9) 0.547(2) -0.0567(5) 0.026(3) Uani 1 1 d . . .
C13 C 0.9131(8) 0.4867(18) 0.2601(4) 0.015(3) Uani 1 1 d . . .
N3 N 0.9263(9) 0.783(2) -0.0473(4) 0.025(3) Uani 1 1 d U . .
H3C H 0.9545 0.8907 -0.0376 0.030 Uiso 1 1 calc R . .
C11 C 0.9157(9) 0.267(2) 0.2801(5) 0.021(3) Uani 1 1 d U . .
C31 C 0.9029(9) 0.477(2) -0.0737(4) 0.021(3) Uani 1 1 d U . .
O31 O 0.5601(9) 0.392(2) -0.0129(4) 0.044(3) Uani 1 1 d . . .
O30 O 0.5671(10) 0.382(2) 0.2003(4) 0.047(3) Uani 1 1 d . . .
C30 C 0.9863(9) 0.629(2) 0.2550(4) 0.016(3) Uani 1 1 d U . .
C29 C 0.8275(10) 0.732(4) -0.0408(7) 0.030(4) Uani 1 1 d U . .
H29A H 0.7786 0.8132 -0.0273 0.037 Uiso 1 1 calc R . .
C7 C 0.6024(11) 0.263(2) 0.1779(5) 0.029(4) Uani 1 1 d . . .
C27 C 0.9736(9) 0.636(2) -0.0714(4) 0.022(3) Uani 1 1 d U . .
C26 C 0.8379(9) 0.730(3) 0.2264(6) 0.023(3) Uani 1 1 d U . .
H26A H 0.7897 0.8082 0.2114 0.028 Uiso 1 1 calc R . .
C20 C 0.9080(7) 0.2877(19) -0.0946(4) 0.011(2) Uani 1 1 d U . .
N1 N 0.8218(9) 0.543(2) 0.2406(4) 0.018(3) Uani 1 1 d U . .
C6 C 0.6000(13) 0.227(2) 0.0057(6) 0.033(4) Uani 1 1 d . . .
C1 C 0.5530(11) 0.176(2) 0.0513(5) 0.050(4) Uani 0.50 1 d PDU A 1
C2 C 0.468(2) 0.321(5) 0.0683(8) 0.064(6) Uani 0.50 1 d PDU A 1
H2A H 0.4817 0.4561 0.0577 0.076 Uiso 0.50 1 calc PR A 1
H2B H 0.4025 0.2790 0.0569 0.076 Uiso 0.50 1 calc PR A 1
C3 C 0.471(2) 0.312(5) 0.1208(8) 0.064(6) Uani 0.50 1 d PDU A 1
H3A H 0.4071 0.2613 0.1327 0.077 Uiso 0.50 1 calc PR A 1
H3B H 0.4831 0.4436 0.1335 0.077 Uiso 0.50 1 calc PR A 1
C4 C 0.5599(11) 0.167(2) 0.1336(4) 0.045(4) Uani 0.50 1 d PDU A 1
H4A H 0.5368 0.0292 0.1383 0.053 Uiso 0.50 1 calc PR A 1
C5 C 0.6292(11) 0.188(2) 0.0921(7) 0.044(5) Uani 0.50 1 d PDU A 1
C8 C 0.682(2) 0.389(4) 0.0913(10) 0.037(18) Uani 0.50 1 d PDU A 1
H8A H 0.7300 0.3962 0.1162 0.055 Uiso 0.50 1 calc PR A 1
H8B H 0.6330 0.4940 0.0944 0.055 Uiso 0.50 1 calc PR A 1
H8C H 0.7179 0.4045 0.0627 0.055 Uiso 0.50 1 calc PR A 1
C9 C 0.6923(13) 0.000(3) 0.0903(11) 0.042(5) Uani 0.50 1 d PDU A 1
H9A H 0.7411 0.0013 0.1147 0.064 Uiso 0.50 1 calc PR A 1
H9B H 0.7271 -0.0070 0.0614 0.064 Uiso 0.50 1 calc PR A 1
H9C H 0.6487 -0.1146 0.0935 0.064 Uiso 0.50 1 calc PR A 1
C10 C 0.487(2) 0.005(5) 0.0454(9) 0.043(6) Uani 0.50 1 d PU A 1
H10A H 0.4455 0.0242 0.0186 0.064 Uiso 0.50 1 calc PR A 1
H10B H 0.4440 -0.0084 0.0719 0.064 Uiso 0.50 1 calc PR A 1
H10C H 0.5272 -0.1136 0.0418 0.064 Uiso 0.50 1 calc PR A 1
C1A C 0.5530(11) 0.176(2) 0.0513(5) 0.050(4) Uani 0.50 1 d PD A 2
H1AA H 0.4794 0.1600 0.0476 0.060 Uiso 0.50 1 calc PR A 2
C2A C 0.601(4) -0.028(4) 0.0646(8) 0.12(2) Uani 0.50 1 d PDU A 2
H2AA H 0.5574 -0.1371 0.0548 0.140 Uiso 0.50 1 calc PR A 2
H2AB H 0.6668 -0.0433 0.0501 0.140 Uiso 0.50 1 calc PR A 2
C3A C 0.612(2) -0.030(3) 0.1168(7) 0.039(7) Uani 0.50 1 d PDU A 2
H3AA H 0.6835 -0.0315 0.1255 0.047 Uiso 0.50 1 calc PR A 2
H3AB H 0.5791 -0.1462 0.1299 0.047 Uiso 0.50 1 calc PR A 2
C4A C 0.5599(11) 0.167(2) 0.1336(4) 0.045(4) Uani 0.50 1 d PD A 2
C5A C 0.5748(10) 0.3035(18) 0.0925(7) 0.025(4) Uani 0.50 1 d PDU A 2
C8A C 0.4905(16) 0.459(3) 0.0950(11) 0.048(6) Uani 0.50 1 d PDU A 2
H8AA H 0.5009 0.5426 0.1213 0.072 Uiso 0.50 1 calc PR A 2
H8AB H 0.4260 0.3922 0.0976 0.072 Uiso 0.50 1 calc PR A 2
H8AC H 0.4914 0.5389 0.0677 0.072 Uiso 0.50 1 calc PR A 2
C9A C 0.683(2) 0.383(6) 0.0912(11) 0.05(2) Uani 0.50 1 d PD A 2
H9AA H 0.6954 0.4632 0.1180 0.076 Uiso 0.50 1 calc PR A 2
H9AB H 0.6922 0.4638 0.0643 0.076 Uiso 0.50 1 calc PR A 2
H9AC H 0.7300 0.2732 0.0906 0.076 Uiso 0.50 1 calc PR A 2
C10A C 0.457(3) 0.080(6) 0.1403(12) 0.062(10) Uani 0.50 1 d PU A 2
H10D H 0.4124 0.1806 0.1525 0.093 Uiso 0.50 1 calc PR A 2
H10E H 0.4613 -0.0300 0.1613 0.093 Uiso 0.50 1 calc PR A 2
H10F H 0.4313 0.0337 0.1114 0.093 Uiso 0.50 1 calc PR 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 O19 2.321(10) 3_465 ?
Tb1 O15 2.353(9) 3_455 ?
Tb1 O30 2.390(12) . ?
Tb1 O11 2.396(11) 3_455 ?
Tb1 O22 2.386(8) . ?
Tb1 O16 2.397(9) . ?
Tb1 O14 2.447(15) . ?
Tb1 N1 2.609(12) . ?
Tb1 C7 2.788(15) . ?
Tb2 O21 2.329(9) 3_465 ?
Tb2 O13 2.350(8) 3_455 ?
Tb2 O20 2.362(10) . ?
Tb2 O17 2.375(10) 3_455 ?
Tb2 O18 2.388(11) . ?
Tb2 O12 2.397(13) . ?
Tb2 O31 2.453(10) . ?
Tb2 N2 2.598(14) . ?
Tb2 C6 2.788(17) . ?
O22 C11 1.223(14) . ?
O21 C16 1.241(17) . ?
O21 Tb2 2.329(9) 3_565 ?
O20 C20 1.330(14) . ?
O19 C15 1.243(17) . ?
O19 Tb1 2.321(9) 3_565 ?
C16 O17 1.257(17) . ?
C16 C27 1.489(17) . ?
O18 H18A 0.8200 . ?
O18 H18B 0.8499 . ?
O17 Tb2 2.375(10) 3 ?
O16 H16A 0.8200 . ?
O16 H16B 0.8500 . ?
O15 C11 1.200(15) . ?
O15 Tb1 2.353(9) 3 ?
C15 O11 1.247(17) . ?
C15 C30 1.476(16) . ?
O14 C7 1.376(18) . ?
O13 C20 1.271(14) . ?
O13 Tb2 2.350(8) 3 ?
O12 C6 1.15(2) . ?
O11 Tb1 2.396(11) 3 ?
N4 C26 1.339(17) . ?
N4 C30 1.403(18) . ?
N4 H4B 0.8600 . ?
N2 C29 1.34(3) . ?
N2 C31 1.387(16) . ?
C13 C30 1.359(18) . ?
C13 N1 1.382(15) . ?
C13 C11 1.577(18) . ?
N3 C29 1.356(17) . ?
N3 C27 1.356(19) . ?
N3 H3C 0.8600 . ?
C31 C20 1.407(18) . ?
C31 C27 1.41(2) . ?
O31 C6 1.34(2) . ?
O30 C7 1.13(2) . ?
C29 H29A 0.9300 . ?
C7 C4 1.55(2) . ?
C26 N1 1.33(2) . ?
C26 H26A 0.9300 . ?
C6 C1 1.50(2) . ?
C1 C10 1.44(3) . ?
C1 C2 1.557(10) . ?
C1 C5 1.56(2) . ?
C2 C3 1.533(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.559(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.521(10) . ?
C4 H4A 0.9800 . ?
C5 C9 1.508(10) . ?
C5 C8 1.513(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C2A C3A 1.530(10) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C5A C8A 1.518(9) . ?
C5A C9A 1.521(10) . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9600 . ?
C10A H10D 0.9600 . ?
C10A H10E 0.9600 . ?
C10A H10F 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
O19 Tb1 O15 78.0(3) 3_465 3_455 ?
O19 Tb1 O30 79.2(4) 3_465 . ?
O15 Tb1 O30 73.6(4) 3_455 . ?
O19 Tb1 O11 148.8(4) 3_465 3_455 ?
O15 Tb1 O11 73.6(4) 3_455 3_455 ?
O30 Tb1 O11 104.4(4) . 3_455 ?
O19 Tb1 O22 125.9(3) 3_465 . ?
O15 Tb1 O22 142.3(4) 3_455 . ?
O30 Tb1 O22 133.9(4) . . ?
O11 Tb1 O22 74.2(3) 3_455 . ?
O19 Tb1 O16 81.8(4) 3_465 . ?
O15 Tb1 O16 81.5(4) 3_455 . ?
O30 Tb1 O16 151.2(4) . . ?
O11 Tb1 O16 81.6(4) 3_455 . ?
O22 Tb1 O16 74.9(3) . . ?
O19 Tb1 O14 126.4(4) 3_465 . ?
O15 Tb1 O14 106.0(4) 3_455 . ?
O30 Tb1 O14 53.1(4) . . ?
O11 Tb1 O14 74.6(5) 3_455 . ?
O22 Tb1 O14 83.6(4) . . ?
O16 Tb1 O14 151.5(4) . . ?
O19 Tb1 N1 73.0(4) 3_465 . ?
O15 Tb1 N1 150.5(4) 3_455 . ?
O30 Tb1 N1 95.7(4) . . ?
O11 Tb1 N1 135.9(4) 3_455 . ?
O22 Tb1 N1 63.8(4) . . ?
O16 Tb1 N1 99.1(4) . . ?
O14 Tb1 N1 87.6(5) . . ?
O19 Tb1 C7 100.4(4) 3_465 . ?
O15 Tb1 C7 87.9(4) 3_455 . ?
O30 Tb1 C7 23.6(4) . . ?
O11 Tb1 C7 91.2(4) 3_455 . ?
O22 Tb1 C7 111.8(4) . . ?
O16 Tb1 C7 168.5(4) . . ?
O14 Tb1 C7 29.6(4) . . ?
N1 Tb1 C7 92.3(4) . . ?
O21 Tb2 O13 78.3(4) 3_465 3_455 ?
O21 Tb2 O20 125.5(4) 3_465 . ?
O13 Tb2 O20 138.1(4) 3_455 . ?
O21 Tb2 O17 148.2(4) 3_465 3_455 ?
O13 Tb2 O17 71.9(4) 3_455 3_455 ?
O20 Tb2 O17 74.2(4) . 3_455 ?
O21 Tb2 O18 79.7(5) 3_465 . ?
O13 Tb2 O18 80.5(4) 3_455 . ?
O20 Tb2 O18 72.4(4) . . ?
O17 Tb2 O18 84.6(4) 3_455 . ?
O21 Tb2 O12 124.1(5) 3_465 . ?
O13 Tb2 O12 107.9(4) 3_455 . ?
O20 Tb2 O12 87.2(4) . . ?
O17 Tb2 O12 76.6(5) 3_455 . ?
O18 Tb2 O12 155.5(5) . . ?
O21 Tb2 O31 77.6(4) 3_465 . ?
O13 Tb2 O31 77.5(4) 3_455 . ?
O20 Tb2 O31 136.1(4) . . ?
O17 Tb2 O31 105.8(4) 3_455 . ?
O18 Tb2 O31 151.0(4) . . ?
O12 Tb2 O31 51.9(5) . . ?
O21 Tb2 N2 73.2(4) 3_465 . ?
O13 Tb2 N2 151.4(4) 3_455 . ?
O20 Tb2 N2 65.1(4) . . ?
O17 Tb2 N2 136.6(4) 3_455 . ?
O18 Tb2 N2 96.8(4) . . ?
O12 Tb2 N2 86.4(5) . . ?
O31 Tb2 N2 93.7(5) . . ?
O21 Tb2 C6 105.1(5) 3_465 . ?
O13 Tb2 C6 90.6(4) 3_455 . ?
O20 Tb2 C6 111.1(5) . . ?
O17 Tb2 C6 86.3(4) 3_455 . ?
O18 Tb2 C6 168.9(4) . . ?
O12 Tb2 C6 24.1(5) . . ?
O31 Tb2 C6 28.6(5) . . ?
N2 Tb2 C6 94.2(4) . . ?
C11 O22 Tb1 130.7(9) . . ?
C16 O21 Tb2 170.1(10) . 3_565 ?
C20 O20 Tb2 125.8(8) . . ?
C15 O19 Tb1 168.8(9) . 3_565 ?
O21 C16 O17 124.6(12) . . ?
O21 C16 C27 115.0(12) . . ?
O17 C16 C27 120.3(12) . . ?
Tb2 O18 H18A 109.5 . . ?
Tb2 O18 H18B 120.1 . . ?
H18A O18 H18B 130.4 . . ?
C16 O17 Tb2 140.9(9) . 3 ?
Tb1 O16 H16A 109.5 . . ?
Tb1 O16 H16B 119.9 . . ?
H16A O16 H16B 130.6 . . ?
C11 O15 Tb1 142.7(10) . 3 ?
O19 C15 O11 122.7(12) . . ?
O19 C15 C30 119.1(12) . . ?
O11 C15 C30 118.2(12) . . ?
C7 O14 Tb1 89.1(10) . . ?
C20 O13 Tb2 137.1(8) . 3 ?
C6 O12 Tb2 97.5(11) . . ?
C15 O11 Tb1 140.7(9) . 3 ?
C26 N4 C30 108.7(14) . . ?
C26 N4 H4B 125.7 . . ?
C30 N4 H4B 125.7 . . ?
C29 N2 C31 106.9(12) . . ?
C29 N2 Tb2 138.1(10) . . ?
C31 N2 Tb2 112.6(10) . . ?
C30 C13 N1 112.3(12) . . ?
C30 C13 C11 132.3(10) . . ?
N1 C13 C11 115.2(10) . . ?
C29 N3 C27 109.4(15) . . ?
C29 N3 H3C 125.3 . . ?
C27 N3 H3C 125.3 . . ?
O15 C11 O22 128.2(13) . . ?
O15 C11 C13 119.3(11) . . ?
O22 C11 C13 112.5(10) . . ?
N2 C31 C20 119.9(12) . . ?
N2 C31 C27 107.7(13) . . ?
C20 C31 C27 131.7(11) . . ?
C6 O31 Tb2 89.7(10) . . ?
C7 O30 Tb1 98.4(10) . . ?
C13 C30 N4 102.9(11) . . ?
C13 C30 C15 135.5(12) . . ?
N4 C30 C15 119.3(13) . . ?
N2 C29 N3 109.9(15) . . ?
N2 C29 H29A 125.1 . . ?
N3 C29 H29A 125.1 . . ?
O30 C7 O14 119.3(15) . . ?
O30 C7 C4 128.7(14) . . ?
O14 C7 C4 109.9(14) . . ?
O30 C7 Tb1 58.0(9) . . ?
O14 C7 Tb1 61.3(8) . . ?
C4 C7 Tb1 164.0(10) . . ?
N3 C27 C31 105.3(11) . . ?
N3 C27 C16 121.9(13) . . ?
C31 C27 C16 132.8(13) . . ?
N1 C26 N4 111.3(14) . . ?
N1 C26 H26A 124.3 . . ?
N4 C26 H26A 124.3 . . ?
O13 C20 O20 118.9(12) . . ?
O13 C20 C31 125.5(11) . . ?
O20 C20 C31 115.6(10) . . ?
C26 N1 C13 104.3(11) . . ?
C26 N1 Tb1 137.0(10) . . ?
C13 N1 Tb1 113.7(8) . . ?
O12 C6 O31 117.6(15) . . ?
O12 C6 C1 128.7(16) . . ?
O31 C6 C1 112.6(16) . . ?
O12 C6 Tb2 58.5(10) . . ?
O31 C6 Tb2 61.6(8) . . ?
C1 C6 Tb2 171.6(12) . . ?
C10 C1 C6 108.8(14) . . ?
C10 C1 C2 96(2) . . ?
C6 C1 C2 115.7(15) . . ?
C10 C1 C5 121.4(16) . . ?
C6 C1 C5 113.5(12) . . ?
C2 C1 C5 100.5(10) . . ?
C3 C2 C1 106.1(9) . . ?
C3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
C3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C2 C3 C4 106.3(9) . . ?
C2 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
C2 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C5 C4 C7 114.2(14) . . ?
C5 C4 C3 101.6(10) . . ?
C7 C4 C3 102.3(15) . . ?
C5 C4 H4A 112.6 . . ?
C7 C4 H4A 112.6 . . ?
C3 C4 H4A 112.6 . . ?
C9 C5 C8 119(2) . . ?
C9 C5 C4 106.3(12) . . ?
C8 C5 C4 111.8(13) . . ?
C9 C5 C1 106.3(14) . . ?
C8 C5 C1 109.4(14) . . ?
C4 C5 C1 102.5(9) . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3A C2A H2AA 110.3 . . ?
C3A C2A H2AB 110.3 . . ?
H2AA C2A H2AB 108.5 . . ?
C2A C3A H3AA 110.7 . . ?
C2A C3A H3AB 110.7 . . ?
H3AA C3A H3AB 108.8 . . ?
C8A C5A C9A 116(2) . . ?
C5A C8A H8AA 109.5 . . ?
C5A C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C5A C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C5A C9A H9AA 109.5 . . ?
C5A C9A H9AB 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
C5A C9A H9AC 109.4 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
H10D C10A H10E 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.879
_refine_diff_density_min         -1.975
_refine_diff_density_rms         0.205
_database_code_depnum_ccdc_archive 'CCDC 1006631'
