# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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 1481266'
_audit_update_record             
;
2016-05-23 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H9 Eu N O9'
_chemical_formula_weight         571.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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'
'-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                   19.6675(3)
_cell_length_b                   11.9457(2)
_cell_length_c                   21.9773(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.166(2)
_cell_angle_gamma                90.00
_cell_volume                     5123.06(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100
_cell_measurement_reflns_used    5488
_cell_measurement_theta_min      4.0210
_cell_measurement_theta_max      73.2110

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_absorpt_coefficient_mu    17.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.53368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5022
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.05
_diffrn_reflns_theta_max         73.40
_reflns_number_total             5022
_reflns_number_gt                4500
_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. 
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.032 0.250 443 158 ' '
2 0.000 -0.057 0.750 443 159 ' '
3 0.500 -0.034 0.250 443 158 ' '
4 0.500 0.008 0.750 443 159 ' '
_platon_squeeze_details          
;
;

_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)+(0.0410P)²+42.6834P] 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         5022
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.1023
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.002

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 0.331553(12) 0.32989(2) -0.025682(11) 0.00724(9) Uani 1 1 d . . .
O8 O 0.30013(17) 0.1561(3) 0.01561(14) 0.0125(6) Uani 1 1 d . . .
O2 O 0.17794(16) 0.1358(3) -0.08155(14) 0.0119(6) Uani 1 1 d . . .
O7 O 0.24169(17) 0.0007(3) 0.02346(16) 0.0178(7) Uani 1 1 d . . .
O1 O 0.26671(16) 0.2331(3) -0.10824(14) 0.0136(7) Uani 1 1 d . . .
O5 O 0.55136(17) -0.2787(3) -0.02269(16) 0.0175(7) Uani 1 1 d . . .
O9 O 0.39671(19) 0.5087(3) 0.01344(16) 0.0211(7) Uani 1 1 d . . .
C4 C 0.1643(3) 0.1732(4) -0.2889(2) 0.0156(9) Uani 1 1 d . . .
H4 H 0.1514 0.2286 -0.3192 0.019 Uiso 1 1 calc R . .
O4 O 0.1515(2) -0.0712(3) -0.38567(15) 0.0211(8) Uani 1 1 d . . .
O6 O 0.58393(19) -0.2151(4) 0.06972(16) 0.0243(8) Uani 1 1 d . . .
C10 C 0.1883(3) -0.1816(4) -0.1545(2) 0.0197(10) Uani 1 1 d . . .
H10 H 0.1491 -0.1944 -0.1835 0.024 Uiso 1 1 calc R . .
O3 O 0.09562(19) 0.0907(3) -0.40171(15) 0.0179(7) Uani 1 1 d . . .
C1 C 0.2184(2) 0.1665(4) -0.1186(2) 0.0111(9) Uani 1 1 d . . .
C16 C 0.4761(2) -0.1527(4) 0.0210(2) 0.0133(9) Uani 1 1 d . . .
C15 C 0.4201(3) -0.1750(4) -0.0230(2) 0.0143(9) Uani 1 1 d . . .
H15 H 0.4223 -0.2349 -0.0511 0.017 Uiso 1 1 calc R . .
N1 N 0.2768(2) -0.0549(3) -0.11077(18) 0.0128(8) Uani 1 1 d . . .
C13 C 0.2998(2) -0.1363(4) -0.0716(2) 0.0130(9) Uani 1 1 d . . .
C6 C 0.1344(2) 0.0244(4) -0.3692(2) 0.0131(9) Uani 1 1 d . . .
C20 C 0.3591(2) -0.0186(4) 0.0139(2) 0.0128(9) Uani 1 1 d . . .
C2 C 0.2035(2) 0.1239(4) -0.1837(2) 0.0127(9) Uani 1 1 d . . .
C19 C 0.4163(3) 0.0044(4) 0.0570(2) 0.0161(9) Uani 1 1 d . . .
H19 H 0.4158 0.0675 0.0833 0.019 Uiso 1 1 calc R . .
C17 C 0.5403(3) -0.2204(4) 0.0227(2) 0.0151(9) Uani 1 1 d . . .
C8 C 0.2011(2) 0.0105(4) -0.1988(2) 0.0121(9) Uani 1 1 d . . .
C9 C 0.2225(3) -0.0786(4) -0.1526(2) 0.0150(9) Uani 1 1 d . . .
C7 C 0.1801(2) -0.0203(4) -0.2598(2) 0.0140(9) Uani 1 1 d . . .
H7 H 0.1794 -0.0972 -0.2709 0.017 Uiso 1 1 calc R . .
C18 C 0.4736(3) -0.0646(4) 0.0616(2) 0.0163(10) Uani 1 1 d . . .
H18 H 0.5111 -0.0512 0.0924 0.020 Uiso 1 1 calc R . .
C3 C 0.1872(3) 0.2049(4) -0.2293(2) 0.0144(9) Uani 1 1 d . . .
H3 H 0.1920 0.2821 -0.2193 0.017 Uiso 1 1 calc R . .
C21 C 0.2967(2) 0.0495(4) 0.0170(2) 0.0121(9) Uani 1 1 d . . .
C14 C 0.3605(2) -0.1091(4) -0.0258(2) 0.0132(9) Uani 1 1 d . . .
C11 C 0.2128(2) -0.2644(4) -0.1135(2) 0.0172(10) Uani 1 1 d . . .
H11 H 0.1907 -0.3351 -0.1138 0.021 Uiso 1 1 calc R . .
C5 C 0.1602(2) 0.0603(4) -0.3045(2) 0.0137(9) Uani 1 1 d . . .
C12 C 0.2700(3) -0.2424(4) -0.0719(2) 0.0171(10) Uani 1 1 d . . .
H12 H 0.2888 -0.2986 -0.0441 0.021 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 2.338(3) 4_554 ?
Eu1 O8 2.378(3) . ?
Eu1 O1 2.383(3) . ?
Eu1 O2 2.422(3) 7 ?
Eu1 O6 2.445(4) 5_655 ?
Eu1 O7 2.488(3) 7 ?
Eu1 O5 2.489(3) 5_655 ?
Eu1 O9 2.583(4) . ?
Eu1 O8 2.632(3) 7 ?
Eu1 C17 2.833(5) 5_655 ?
Eu1 C21 2.931(5) 7 ?
Eu1 Eu1 4.0139(5) 7 ?
O8 C21 1.275(6) . ?
O8 Eu1 2.632(3) 7 ?
O2 C1 1.262(6) . ?
O2 Eu1 2.422(3) 7 ?
O7 C21 1.252(6) . ?
O7 Eu1 2.488(3) 7 ?
O1 C1 1.238(6) . ?
O5 C17 1.258(6) . ?
O5 Eu1 2.489(3) 5_655 ?
C4 C3 1.383(7) . ?
C4 C5 1.393(7) . ?
O4 C6 1.256(6) . ?
O4 Eu1 2.338(3) 4_544 ?
O6 C17 1.260(6) . ?
O6 Eu1 2.445(4) 5_655 ?
C10 C11 1.385(7) . ?
C10 C9 1.399(7) . ?
O3 C6 1.259(6) . ?
C1 C2 1.511(6) . ?
C16 C18 1.385(7) . ?
C16 C15 1.398(7) . ?
C16 C17 1.495(7) . ?
C15 C14 1.407(7) . ?
N1 C13 1.339(6) . ?
N1 C9 1.349(6) . ?
C13 C12 1.396(7) . ?
C13 C14 1.499(7) . ?
C6 C5 1.509(6) . ?
C20 C14 1.391(7) . ?
C20 C19 1.405(7) . ?
C20 C21 1.481(6) . ?
C2 C8 1.395(7) . ?
C2 C3 1.402(7) . ?
C19 C18 1.390(7) . ?
C17 Eu1 2.833(5) 5_655 ?
C8 C7 1.402(6) . ?
C8 C9 1.495(7) . ?
C7 C5 1.397(7) . ?
C21 Eu1 2.931(5) 7 ?
C11 C12 1.383(7) . ?

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 O8 146.11(12) 4_554 . ?
O4 Eu1 O1 74.27(12) 4_554 . ?
O8 Eu1 O1 74.16(11) . . ?
O4 Eu1 O2 139.60(12) 4_554 7 ?
O8 Eu1 O2 73.82(11) . 7 ?
O1 Eu1 O2 136.40(11) . 7 ?
O4 Eu1 O6 77.24(14) 4_554 5_655 ?
O8 Eu1 O6 83.30(13) . 5_655 ?
O1 Eu1 O6 75.66(12) . 5_655 ?
O2 Eu1 O6 128.22(11) 7 5_655 ?
O4 Eu1 O7 75.42(13) 4_554 7 ?
O8 Eu1 O7 121.59(11) . 7 ?
O1 Eu1 O7 98.83(11) . 7 ?
O2 Eu1 O7 74.22(11) 7 7 ?
O6 Eu1 O7 152.57(12) 5_655 7 ?
O4 Eu1 O5 105.05(13) 4_554 5_655 ?
O8 Eu1 O5 83.87(12) . 5_655 ?
O1 Eu1 O5 125.79(11) . 5_655 ?
O2 Eu1 O5 78.78(11) 7 5_655 ?
O6 Eu1 O5 52.64(11) 5_655 5_655 ?
O7 Eu1 O5 134.30(11) 7 5_655 ?
O4 Eu1 O9 75.11(11) 4_554 . ?
O8 Eu1 O9 137.46(11) . . ?
O1 Eu1 O9 148.33(11) . . ?
O2 Eu1 O9 68.36(11) 7 . ?
O6 Eu1 O9 105.18(13) 5_655 . ?
O7 Eu1 O9 65.49(12) 7 . ?
O5 Eu1 O9 70.53(12) 5_655 . ?
O4 Eu1 O8 106.37(12) 4_554 7 ?
O8 Eu1 O8 73.63(12) . 7 ?
O1 Eu1 O8 69.89(10) . 7 ?
O2 Eu1 O8 73.22(10) 7 7 ?
O6 Eu1 O8 142.51(12) 5_655 7 ?
O7 Eu1 O8 50.83(10) 7 7 ?
O5 Eu1 O8 147.92(11) 5_655 7 ?
O9 Eu1 O8 111.84(11) . 7 ?
O4 Eu1 C17 91.93(14) 4_554 5_655 ?
O8 Eu1 C17 82.01(12) . 5_655 ?
O1 Eu1 C17 100.58(13) . 5_655 ?
O2 Eu1 C17 103.42(12) 7 5_655 ?
O6 Eu1 C17 26.32(13) 5_655 5_655 ?
O7 Eu1 C17 152.95(13) 7 5_655 ?
O5 Eu1 C17 26.34(13) 5_655 5_655 ?
O9 Eu1 C17 88.34(13) . 5_655 ?
O8 Eu1 C17 155.42(12) 7 5_655 ?
O4 Eu1 C21 91.08(13) 4_554 7 ?
O8 Eu1 C21 97.90(12) . 7 ?
O1 Eu1 C21 84.53(12) . 7 ?
O2 Eu1 C21 71.48(11) 7 7 ?
O6 Eu1 C21 159.06(12) 5_655 7 ?
O7 Eu1 C21 25.05(13) 7 7 ?
O5 Eu1 C21 148.28(12) 5_655 7 ?
O9 Eu1 C21 88.13(13) . 7 ?
O8 Eu1 C21 25.79(12) 7 7 ?
C17 Eu1 C21 174.62(13) 5_655 7 ?
O4 Eu1 Eu1 132.58(9) 4_554 7 ?
O8 Eu1 Eu1 38.99(8) . 7 ?
O1 Eu1 Eu1 67.22(8) . 7 ?
O2 Eu1 Eu1 69.24(8) 7 7 ?
O6 Eu1 Eu1 116.82(10) 5_655 7 ?
O7 Eu1 Eu1 84.05(8) 7 7 ?
O5 Eu1 Eu1 119.49(9) 5_655 7 ?
O9 Eu1 Eu1 132.88(8) . 7 ?
O8 Eu1 Eu1 34.64(7) 7 7 ?
C17 Eu1 Eu1 120.93(10) 5_655 7 ?
C21 Eu1 Eu1 59.41(9) 7 7 ?
C21 O8 Eu1 153.9(3) . . ?
C21 O8 Eu1 90.3(3) . 7 ?
Eu1 O8 Eu1 106.37(12) . 7 ?
C1 O2 Eu1 135.2(3) . 7 ?
C21 O7 Eu1 97.7(3) . 7 ?
C1 O1 Eu1 141.0(3) . . ?
C17 O5 Eu1 92.3(3) . 5_655 ?
C3 C4 C5 120.1(4) . . ?
C6 O4 Eu1 140.4(3) . 4_544 ?
C17 O6 Eu1 94.3(3) . 5_655 ?
C11 C10 C9 118.7(5) . . ?
O1 C1 O2 126.8(4) . . ?
O1 C1 C2 116.4(4) . . ?
O2 C1 C2 116.7(4) . . ?
C18 C16 C15 120.1(4) . . ?
C18 C16 C17 119.5(4) . . ?
C15 C16 C17 120.3(4) . . ?
C16 C15 C14 120.2(4) . . ?
C13 N1 C9 117.4(4) . . ?
N1 C13 C12 123.3(4) . . ?
N1 C13 C14 116.8(4) . . ?
C12 C13 C14 119.9(4) . . ?
O4 C6 O3 124.9(4) . . ?
O4 C6 C5 117.3(4) . . ?
O3 C6 C5 117.7(4) . . ?
C14 C20 C19 119.8(4) . . ?
C14 C20 C21 122.5(4) . . ?
C19 C20 C21 117.4(4) . . ?
C8 C2 C3 120.2(4) . . ?
C8 C2 C1 123.3(4) . . ?
C3 C2 C1 116.4(4) . . ?
C18 C19 C20 120.5(4) . . ?
O5 C17 O6 120.7(4) . . ?
O5 C17 C16 120.6(4) . . ?
O6 C17 C16 118.7(4) . . ?
O5 C17 Eu1 61.4(2) . 5_655 ?
O6 C17 Eu1 59.4(3) . 5_655 ?
C16 C17 Eu1 174.8(3) . 5_655 ?
C2 C8 C7 118.7(4) . . ?
C2 C8 C9 122.1(4) . . ?
C7 C8 C9 119.2(4) . . ?
N1 C9 C10 122.8(4) . . ?
N1 C9 C8 116.4(4) . . ?
C10 C9 C8 120.7(4) . . ?
C5 C7 C8 121.1(5) . . ?
C16 C18 C19 119.9(4) . . ?
C4 C3 C2 120.4(4) . . ?
O7 C21 O8 121.1(4) . . ?
O7 C21 C20 118.8(4) . . ?
O8 C21 C20 120.0(4) . . ?
O7 C21 Eu1 57.3(2) . 7 ?
O8 C21 Eu1 63.9(2) . 7 ?
C20 C21 Eu1 176.0(3) . 7 ?
C20 C14 C15 119.4(4) . . ?
C20 C14 C13 120.8(4) . . ?
C15 C14 C13 119.8(4) . . ?
C12 C11 C10 118.9(5) . . ?
C4 C5 C7 119.4(4) . . ?
C4 C5 C6 120.7(4) . . ?
C7 C5 C6 119.9(4) . . ?
C11 C12 C13 118.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        73.40
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.127
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1481268'
_audit_update_record             
;
2016-05-23 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H11 N O9 Tb'
_chemical_formula_weight         580.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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'
'-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                   19.6084(4)
_cell_length_b                   11.9016(3)
_cell_length_c                   21.9364(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.186(2)
_cell_angle_gamma                90.00
_cell_volume                     5079.1(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100
_cell_measurement_reflns_used    4289
_cell_measurement_theta_min      4.0510
_cell_measurement_theta_max      73.0320

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2248
_exptl_absorpt_coefficient_mu    14.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4915
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.06
_diffrn_reflns_theta_max         73.16
_reflns_number_total             4915
_reflns_number_gt                4309
_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. 
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.002 0.250 404 132 ' '
2 0.000 -0.048 0.750 404 132 ' '
3 0.500 -0.053 0.250 404 132 ' '
4 0.500 -0.030 0.750 404 132 ' '
_platon_squeeze_details          
;
;


_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)+(0.0446P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4915
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0733
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_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 0.830757(8) 0.330838(14) 0.474263(7) 0.00868(7) Uani 1 1 d . . .
O8 O 0.80021(11) 0.15739(17) 0.51471(9) 0.0121(4) Uani 1 1 d . . .
O2 O 0.67796(11) 0.13537(18) 0.41949(9) 0.0115(4) Uani 1 1 d . . .
O7 O 0.74268(11) 0.00212(19) 0.52434(10) 0.0184(5) Uani 1 1 d . . .
O1 O 0.76697(11) 0.23539(19) 0.39205(9) 0.0143(4) Uani 1 1 d . . .
C4 C 0.66408(17) 0.1744(3) 0.21109(14) 0.0152(6) Uani 1 1 d . . .
H4 H 0.6505 0.2299 0.1808 0.018 Uiso 1 1 calc R . .
O9 O 0.89518(6) 0.50763(9) 0.51326(5) 0.0200(5) Uani 1 1 d . . .
H9A H 0.9292 0.4908 0.5413 0.030 Uiso 1 1 d R . .
H9B H 0.9118 0.5420 0.4832 0.030 Uiso 1 1 d R . .
O5 O 1.05228(6) -0.28004(9) 0.47769(6) 0.0195(5) Uani 1 1 d R . .
O6 O 1.08600(7) -0.21778(9) 0.57034(6) 0.0224(5) Uani 1 1 d R . .
C1 C 0.71848(7) 0.16747(9) 0.38192(7) 0.0129(6) Uani 1 1 d R . .
O3 O 0.59540(7) 0.09071(9) 0.09798(6) 0.0186(5) Uani 1 1 d R . .
C10 C 0.68855(6) -0.18282(9) 0.34566(5) 0.0194(7) Uani 1 1 d R . .
H10 H 0.6493 -0.1962 0.3166 0.023 Uiso 1 1 calc R . .
C15 C 0.92061(17) -0.1760(3) 0.47762(14) 0.0145(6) Uani 1 1 d . . .
H15 H 0.9225 -0.2364 0.4496 0.017 Uiso 1 1 calc R . .
O4 O 0.65282(14) -0.0704(2) 0.11425(10) 0.0228(5) Uani 1 1 d . . .
C13 C 0.80073(16) -0.1364(3) 0.42918(13) 0.0131(6) Uani 1 1 d . . .
C8 C 0.70080(15) 0.0109(3) 0.30168(13) 0.0129(6) Uani 1 1 d . . .
C2 C 0.70320(16) 0.1253(3) 0.31697(13) 0.0131(6) Uani 1 1 d . . .
C16 C 0.97711(16) -0.1535(3) 0.52218(14) 0.0133(6) Uani 1 1 d . . .
N1 N 0.77696(14) -0.0549(2) 0.38954(12) 0.0146(5) Uani 1 1 d . . .
C20 C 0.86133(16) -0.0176(3) 0.51470(14) 0.0130(6) Uani 1 1 d . . .
C9 C 0.72289(17) -0.0779(3) 0.34791(13) 0.0144(6) Uani 1 1 d . . .
C17 C 1.04178(17) -0.2221(3) 0.52357(14) 0.0152(6) Uani 1 1 d . . .
C19 C 0.91787(17) 0.0045(3) 0.55822(14) 0.0168(6) Uani 1 1 d . . .
H19 H 0.9171 0.0671 0.5850 0.020 Uiso 1 1 calc R . .
C18 C 0.97525(18) -0.0647(3) 0.56244(15) 0.0192(7) Uani 1 1 d . . .
H18 H 1.0131 -0.0510 0.5930 0.023 Uiso 1 1 calc R . .
C6 C 0.63489(16) 0.0242(3) 0.13103(13) 0.0138(6) Uani 1 1 d . . .
C7 C 0.68047(16) -0.0192(3) 0.24021(14) 0.0140(6) Uani 1 1 d . . .
H7 H 0.6803 -0.0963 0.2290 0.017 Uiso 1 1 calc R . .
C21 C 0.79766(17) 0.0515(3) 0.51725(13) 0.0142(6) Uani 1 1 d . . .
C14 C 0.86182(16) -0.1092(3) 0.47482(14) 0.0145(6) Uani 1 1 d . . .
C3 C 0.68729(17) 0.2061(3) 0.27073(14) 0.0164(6) Uani 1 1 d . . .
H3 H 0.6925 0.2836 0.2806 0.020 Uiso 1 1 calc R . .
C5 C 0.66058(16) 0.0605(3) 0.19545(14) 0.0144(6) Uani 1 1 d . . .
C12 C 0.77108(17) -0.2436(3) 0.42885(14) 0.0165(6) Uani 1 1 d . . .
H12 H 0.7898 -0.3000 0.4567 0.020 Uiso 1 1 calc R . .
C11 C 0.71372(18) -0.2651(3) 0.38688(15) 0.0200(7) Uani 1 1 d . . .
H11 H 0.6917 -0.3363 0.3865 0.024 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 2.326(2) 4_655 ?
Tb1 O8 2.354(2) . ?
Tb1 O1 2.354(2) . ?
Tb1 O2 2.392(2) 7_656 ?
Tb1 O6 2.4149(10) 5_756 ?
Tb1 O7 2.457(2) 7_656 ?
Tb1 O5 2.4763(11) 5_756 ?
Tb1 O9 2.5465(11) . ?
Tb1 O8 2.613(2) 7_656 ?
Tb1 C17 2.810(3) 5_756 ?
Tb1 C21 2.908(3) 7_656 ?
Tb1 Tb1 3.9878(3) 7_656 ?
O8 C21 1.263(4) . ?
O8 Tb1 2.613(2) 7_656 ?
O2 C1 1.273(3) . ?
O2 Tb1 2.392(2) 7_656 ?
O7 C21 1.254(4) . ?
O7 Tb1 2.457(2) 7_656 ?
O1 C1 1.247(2) . ?
C4 C3 1.383(4) . ?
C4 C5 1.398(4) . ?
O5 C17 1.258(3) . ?
O5 Tb1 2.4763(11) 5_756 ?
O6 C17 1.259(3) . ?
O6 Tb1 2.4149(14) 5_756 ?
C1 C2 1.505(3) . ?
O3 C6 1.270(3) . ?
C10 C11 1.382(4) . ?
C10 C9 1.416(3) . ?
C15 C14 1.395(4) . ?
C15 C16 1.408(5) . ?
O4 C6 1.248(4) . ?
O4 Tb1 2.326(2) 4_645 ?
C13 N1 1.346(4) . ?
C13 C12 1.402(5) . ?
C13 C14 1.497(5) . ?
C8 C7 1.404(4) . ?
C8 C2 1.402(4) . ?
C8 C9 1.491(4) . ?
C2 C3 1.404(5) . ?
C16 C18 1.380(5) . ?
C16 C17 1.506(4) . ?
N1 C9 1.338(4) . ?
C20 C14 1.398(4) . ?
C20 C19 1.395(5) . ?
C20 C21 1.502(4) . ?
C17 Tb1 2.810(3) 5_756 ?
C19 C18 1.388(5) . ?
C6 C5 1.503(4) . ?
C7 C5 1.386(4) . ?
C21 Tb1 2.908(3) 7_656 ?
C12 C11 1.385(5) . ?

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 O8 145.69(8) 4_655 . ?
O4 Tb1 O1 73.74(8) 4_655 . ?
O8 Tb1 O1 74.32(7) . . ?
O4 Tb1 O2 139.69(8) 4_655 7_656 ?
O8 Tb1 O2 74.19(7) . 7_656 ?
O1 Tb1 O2 137.02(7) . 7_656 ?
O4 Tb1 O6 76.83(7) 4_655 5_756 ?
O8 Tb1 O6 83.15(6) . 5_756 ?
O1 Tb1 O6 75.05(6) . 5_756 ?
O2 Tb1 O6 128.51(6) 7_656 5_756 ?
O4 Tb1 O7 75.18(9) 4_655 7_656 ?
O8 Tb1 O7 121.85(7) . 7_656 ?
O1 Tb1 O7 98.28(8) . 7_656 ?
O2 Tb1 O7 74.83(7) 7_656 7_656 ?
O6 Tb1 O7 151.98(6) 5_756 7_656 ?
O4 Tb1 O5 105.13(7) 4_655 5_756 ?
O8 Tb1 O5 83.75(6) . 5_756 ?
O1 Tb1 O5 125.68(6) . 5_756 ?
O2 Tb1 O5 78.56(6) 7_656 5_756 ?
O6 Tb1 O5 53.1 5_756 5_756 ?
O7 Tb1 O5 134.85(6) 7_656 5_756 ?
O4 Tb1 O9 75.43(6) 4_655 . ?
O8 Tb1 O9 137.47(6) . . ?
O1 Tb1 O9 148.18(6) . . ?
O2 Tb1 O9 68.08(6) 7_656 . ?
O6 Tb1 O9 105.34(3) 5_756 . ?
O7 Tb1 O9 66.05(6) 7_656 . ?
O5 Tb1 O9 70.41(4) 5_756 . ?
O4 Tb1 O8 106.89(8) 4_655 7_656 ?
O8 Tb1 O8 73.31(8) . 7_656 ?
O1 Tb1 O8 70.29(7) . 7_656 ?
O2 Tb1 O8 73.14(7) 7_656 7_656 ?
O6 Tb1 O8 142.12(5) 5_756 7_656 ?
O7 Tb1 O8 51.04(7) 7_656 7_656 ?
O5 Tb1 O8 147.38(6) 5_756 7_656 ?
O9 Tb1 O8 112.12(5) . 7_656 ?
O4 Tb1 C17 91.78(9) 4_655 5_756 ?
O8 Tb1 C17 81.80(8) . 5_756 ?
O1 Tb1 C17 100.19(8) . 5_756 ?
O2 Tb1 C17 103.46(8) 7_656 5_756 ?
O6 Tb1 C17 26.53(7) 5_756 5_756 ?
O7 Tb1 C17 153.37(9) 7_656 5_756 ?
O5 Tb1 C17 26.59(7) 5_756 5_756 ?
O9 Tb1 C17 88.40(7) . 5_756 ?
O8 Tb1 C17 154.89(8) 7_656 5_756 ?
O4 Tb1 C21 91.23(9) 4_655 7_656 ?
O8 Tb1 C21 97.77(8) . 7_656 ?
O1 Tb1 C21 84.27(8) . 7_656 ?
O2 Tb1 C21 71.86(8) 7_656 7_656 ?
O6 Tb1 C21 158.28(7) 5_756 7_656 ?
O7 Tb1 C21 25.30(9) 7_656 7_656 ?
O5 Tb1 C21 148.62(7) 5_756 7_656 ?
O9 Tb1 C21 88.72(7) . 7_656 ?
O8 Tb1 C21 25.75(8) 7_656 7_656 ?
C17 Tb1 C21 175.18(9) 5_756 7_656 ?
O4 Tb1 Tb1 132.68(6) 4_655 7_656 ?
O8 Tb1 Tb1 38.88(5) . 7_656 ?
O1 Tb1 Tb1 67.63(5) . 7_656 ?
O2 Tb1 Tb1 69.46(5) 7_656 7_656 ?
O6 Tb1 Tb1 116.54(3) 5_756 7_656 ?
O7 Tb1 Tb1 84.23(5) 7_656 7_656 ?
O5 Tb1 Tb1 119.19(3) 5_756 7_656 ?
O9 Tb1 Tb1 132.98(2) . 7_656 ?
O8 Tb1 Tb1 34.43(4) 7_656 7_656 ?
C17 Tb1 Tb1 120.61(6) 5_756 7_656 ?
C21 Tb1 Tb1 59.30(6) 7_656 7_656 ?
C21 O8 Tb1 154.9(2) . . ?
C21 O8 Tb1 90.26(19) . 7_656 ?
Tb1 O8 Tb1 106.69(8) . 7_656 ?
C1 O2 Tb1 134.98(14) . 7_656 ?
C21 O7 Tb1 97.87(19) . 7_656 ?
C1 O1 Tb1 140.33(15) . . ?
C3 C4 C5 119.8(3) . . ?
C17 O5 Tb1 91.65(16) . 5_756 ?
C17 O6 Tb1 94.51(16) . 5_756 ?
O1 C1 O2 127.09(17) . . ?
O1 C1 C2 116.24(19) . . ?
O2 C1 C2 116.51(17) . . ?
C11 C10 C9 118.2(2) . . ?
C14 C15 C16 119.7(3) . . ?
C6 O4 Tb1 140.8(2) . 4_645 ?
N1 C13 C12 122.9(3) . . ?
N1 C13 C14 117.4(3) . . ?
C12 C13 C14 119.8(3) . . ?
C7 C8 C2 118.3(3) . . ?
C7 C8 C9 119.7(3) . . ?
C2 C8 C9 121.9(3) . . ?
C8 C2 C3 119.6(3) . . ?
C8 C2 C1 123.2(2) . . ?
C3 C2 C1 117.1(3) . . ?
C18 C16 C15 120.5(3) . . ?
C18 C16 C17 119.5(3) . . ?
C15 C16 C17 119.9(3) . . ?
C9 N1 C13 118.3(3) . . ?
C14 C20 C19 120.6(3) . . ?
C14 C20 C21 121.4(3) . . ?
C19 C20 C21 117.7(3) . . ?
N1 C9 C10 122.5(3) . . ?
N1 C9 C8 117.2(3) . . ?
C10 C9 C8 120.3(3) . . ?
O5 C17 O6 120.6(3) . . ?
O5 C17 C16 120.2(3) . . ?
O6 C17 C16 119.1(3) . . ?
O5 C17 Tb1 61.76(14) . 5_756 ?
O6 C17 Tb1 58.96(14) . 5_756 ?
C16 C17 Tb1 174.6(2) . 5_756 ?
C18 C19 C20 120.1(3) . . ?
C16 C18 C19 119.8(3) . . ?
O4 C6 O3 124.6(3) . . ?
O4 C6 C5 117.6(3) . . ?
O3 C6 C5 117.8(3) . . ?
C5 C7 C8 121.8(3) . . ?
O7 C21 O8 120.8(3) . . ?
O7 C21 C20 118.7(3) . . ?
O8 C21 C20 120.5(3) . . ?
O7 C21 Tb1 56.84(16) . 7_656 ?
O8 C21 Tb1 63.99(17) . 7_656 ?
C20 C21 Tb1 175.4(2) . 7_656 ?
C15 C14 C20 119.1(3) . . ?
C15 C14 C13 119.6(3) . . ?
C20 C14 C13 121.3(3) . . ?
C4 C3 C2 120.9(3) . . ?
C7 C5 C4 119.3(3) . . ?
C7 C5 C6 120.0(3) . . ?
C4 C5 C6 120.7(3) . . ?
C11 C12 C13 118.3(3) . . ?
C10 C11 C12 119.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        73.16
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.098
