# 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_2#Eu
_database_code_depnum_ccdc_archive 'CCDC 1023764'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        2#Eu
_chemical_name_common            Eu
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H20 Eu2 O30 S6'
_chemical_formula_sum            'C44.5 H42.5 Eu2 O30.75 S6'
_chemical_formula_weight         1524.90

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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   'P 21 21 21 '
_symmetry_space_group_name_Hall  ' P 2ac 2ab '

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

_cell_length_a                   9.749(5)
_cell_length_b                   21.935(5)
_cell_length_c                   31.167(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6665(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    20882
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2984
_exptl_absorpt_coefficient_mu    2.130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_process_details   sadabs(Sheldrick,1996)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20882
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11743
_reflns_number_gt                9887
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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.
ISOR  0.01 C20 C21 O20 O23 O25 O30 C99 C35B C18 C69 O16 C2 C87 C50 C71 O29 O16 C98 C3 C36 C97 C48 C36 C35 C36
FLAT     0.100 C21 C98 C99 C97
FLAT     0.100 C48 C50 C88 C87
DELU     0.010   0.010 C17 C18 C45 C90
SIMU     0.040   0.080   3.800 C17 C18 C45 C90
DELU     0.010   0.010 C27 C28 C30 C31
SIMU     0.040   0.080   3.800 C27 C28 C30 C31
DELU     0.010   0.010 C21 C98 C99 C97
SIMU     0.040   0.080   3.800 C21 C98 C99 C97
DELU     0.010   0.010 C1 C2 C3 C4 C5
SIMU     0.040   0.080   3.800 C1 C2 C3 C4 C5
DELU  0.010 0.010 C33 C36 C35B C36 C89
SIMU  0.040 0.080 3.800 C33 C36 C35B C36 C89
DELU     0.010   0.010 O27 O30 C41
SIMU     0.040   0.080   3.800 O27 O30 C41
DELU  0.010 0.010 C32 C35 C33 C89 C36
SIMU  0.040 0.080 3.800 C32 C35 C33 C89 C36
DELU     0.010   0.010 C1 C2 C3 C4 C5
SIMU     0.040   0.080   3.800 C1 C2 C3 C4 C5
DELU     0.010   0.010 S6 C35 C33 C89 C36
SIMU     0.040   0.080   3.800 C35 C33 C89 C36
DELU     0.010   0.010 O18 C70
SIMU     0.040   0.080   3.800 O18 C70
EXYZ C28A S3A
EXYZ C28B S3B
EADP C28A S3A
EADP C28B S3B
EXYZ C35A S6A
EXYZ C35B S6B
EADP C35A S6A
EADP C35B S6B
EXYZ C99A S2A
EXYZ C99B S2B
EADP C99A S2A
EADP C99B S2B
EXYZ C18A S4A
EXYZ C18B S4B
EADP C18A S4A
EADP C18B S4B
EADP S1A C3A
EADP S1B C3B
EXYZ S1A C3A
EXYZ S1B C3B
EXYZ C48A S5A
EXYZ C48B S5B
EADP C48A S5A
EADP C48B S5B
DFIX     1.626   0.020 C50 C48A
DFIX     1.745   0.020 C48A C87
DFIX     1.26   0.020 C87 C88
DFIX     1.607   0.020 C88 C48B
DFIX     1.607   0.020 C48B C50
DANG     2.42   0.040 C50 C87
DANG     2.360   0.040 C50 C88
DANG     2.8   0.040 C48A C48B
DANG     2.516   0.040 C48A C88
DANG     2.388   0.040 C48B C87
DELU     0.010   0.010 C50 C87 C88 C48A C48B S5B S5A
SIMU     0.040   0.080   3.800 C50 C87 C88 C48A C48B S5B S5A
During the refinement,c99a, c99b, s2a, s2b are highly disordered, and these atoms are refined by isotropic. 
 In addition, due to the operation of EXYZ, the H atoms on the five-membered rings can't be added.
;

_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)+(0.0751P)²+17.1642P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   0.00(2)
_refine_ls_number_reflns         11743
_refine_ls_number_parameters     729
_refine_ls_number_restraints     446
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1389
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      5.611
_refine_ls_shift/su_max          0.007
_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
C1 C -0.197(8) 0.577(4) 0.585(2) 0.11(2) Uani 1 1 d U . .
C2 C -0.096(8) 0.553(4) 0.572(2) 0.096(19) Uani 1 1 d U . .
C4 C -0.052(5) 0.566(2) 0.6455(13) 0.055(12) Uani 1 1 d U . .
C5 C 0.008(4) 0.567(2) 0.6896(12) 0.043(11) Uani 1 1 d U . .
C6 C 0.117(4) 0.5089(19) 0.7676(12) 0.033(10) Uani 1 1 d . . .
C7 C 0.196(4) 0.545(2) 0.7332(12) 0.036(10) Uani 1 1 d . . .
H7 H 0.2027 0.5877 0.7416 0.043 Uiso 1 1 calc R . .
C8 C 0.340(4) 0.5195(19) 0.7245(12) 0.035(10) Uani 1 1 d . . .
H8 H 0.3348 0.4758 0.7183 0.042 Uiso 1 1 calc R . .
C9 C 0.442(4) 0.5315(16) 0.7621(12) 0.031(9) Uani 1 1 d . . .
C10 C 0.284(3) 0.4290(15) 0.8476(11) 0.029(8) Uani 1 1 d . . .
C12 C -0.064(4) 0.5699(19) 0.8794(11) 0.037(10) Uani 1 1 d . . .
C13 C -0.205(4) 0.6001(19) 0.8760(12) 0.039(10) Uani 1 1 d . . .
H13 H -0.2518 0.5845 0.8504 0.047 Uiso 1 1 calc R . .
C14 C -0.294(3) 0.588(2) 0.9144(12) 0.039(10) Uani 1 1 d . . .
H14 H -0.3026 0.5435 0.9183 0.047 Uiso 1 1 calc R . .
C15 C -0.434(4) 0.615(2) 0.9089(13) 0.043(11) Uani 1 1 d . . .
C16 C -0.145(5) 0.687(2) 0.8347(16) 0.057(14) Uani 1 1 d . . .
C17 C -0.144(6) 0.753(3) 0.837(2) 0.10(2) Uani 1 1 d DU . .
C20 C -0.232(7) 0.592(3) 0.9895(16) 0.072(15) Uani 1 1 d U . .
C21 C -0.147(8) 0.623(3) 1.0222(19) 0.094(19) Uani 1 1 d DU . .
C26 C -0.570(5) 0.3407(18) 0.7790(13) 0.046(12) Uani 1 1 d . . .
C27 C -0.576(6) 0.278(2) 0.7634(18) 0.067(15) Uani 1 1 d U . .
C30 C -0.613(9) 0.168(3) 0.759(3) 0.12(2) Uani 1 1 d U . .
C31 C -0.574(8) 0.191(3) 0.721(2) 0.10(2) Uani 1 1 d U . .
C32 C -0.537(6) 0.362(3) 0.9510(15) 0.070(15) Uani 1 1 d U . .
C33 C -0.607(6) 0.317(3) 0.969(2) 0.088(17) Uani 1 1 d DU . .
C36 C -0.681(9) 0.255(4) 1.030(2) 0.114(3) Uani 1 1 d DU . .
C37 C -0.573(4) 0.4036(15) 0.8406(12) 0.028(9) Uani 1 1 d . . .
H37 H -0.5249 0.4311 0.8210 0.034 Uiso 1 1 calc R . .
C38 C -0.493(4) 0.4005(18) 0.8809(12) 0.035(10) Uani 1 1 d . . .
H38 H -0.4958 0.4405 0.8948 0.042 Uiso 1 1 calc R . .
C39 C -0.342(4) 0.3826(19) 0.8735(13) 0.038(10) Uani 1 1 d . . .
C41 C 0.397(6) 0.524(3) 0.6530(17) 0.080(16) Uani 1 1 d U . .
C45 C -0.122(8) 0.860(4) 0.817(3) 0.16(3) Uani 1 1 d DU . .
C50 C 0.421(7) 0.562(3) 0.6151(18) 0.112(14) Uani 1 1 d DU . .
C70 C 0.188(8) 0.720(4) 0.909(4) 0.17(4) Uani 1 1 d U . .
H70A H 0.2306 0.7559 0.9204 0.255 Uiso 1 1 calc R . .
H70B H 0.1406 0.6986 0.9310 0.255 Uiso 1 1 calc R . .
H70C H 0.1243 0.7316 0.8867 0.255 Uiso 1 1 calc R . .
C71 C 0.050(12) 0.365(5) 0.923(3) 0.17(3) Uani 1 1 d U . .
H71A H 0.0253 0.3298 0.9390 0.262 Uiso 1 1 calc R . .
H71B H 0.0378 0.4011 0.9400 0.262 Uiso 1 1 calc R . .
H71C H 0.1446 0.3622 0.9142 0.262 Uiso 1 1 calc R . .
C87 C 0.443(13) 0.603(3) 0.544(2) 0.164(18) Uani 1 1 d DU . .
C88 C 0.431(11) 0.649(3) 0.565(2) 0.15(2) Uani 1 1 d DU . .
C89 C -0.729(8) 0.222(3) 0.997(2) 0.103(19) Uani 1 1 d DU . .
C90 C -0.171(9) 0.857(4) 0.855(3) 0.14(3) Uani 1 1 d DU . .
C97 C 0.000(10) 0.691(4) 1.064(3) 0.146(6) Uani 1 1 d DU . .
C98 C -0.041(11) 0.646(4) 1.084(3) 0.140(6) Uani 1 1 d DU . .
O1 O -0.054(4) 0.5897(18) 0.7200(10) 0.070(11) Uani 1 1 d . . .
O2 O 0.129(3) 0.5400(14) 0.6923(8) 0.041(8) Uani 1 1 d . . .
O3 O 0.059(3) 0.4616(13) 0.7559(8) 0.041(7) Uani 1 1 d . . .
O4 O 0.107(3) 0.5283(13) 0.8055(7) 0.032(6) Uani 1 1 d . . .
O5 O 0.394(3) 0.5516(15) 0.7972(9) 0.048(8) Uani 1 1 d . . .
O6 O 0.563(3) 0.5195(16) 0.7548(10) 0.053(9) Uani 1 1 d . . .
O7 O -0.064(3) 0.5118(13) 0.8799(8) 0.040(7) Uani 1 1 d . . .
O8 O 0.040(3) 0.6021(14) 0.8796(10) 0.048(8) Uani 1 1 d . . .
O9 O 0.276(3) 0.4755(12) 0.8710(8) 0.038(7) Uani 1 1 d . . .
O10 O 0.184(3) 0.4026(13) 0.8298(10) 0.047(8) Uani 1 1 d . . .
O11 O -0.504(3) 0.5899(16) 0.8797(10) 0.055(9) Uani 1 1 d . . .
O12 O -0.470(3) 0.6604(17) 0.9308(11) 0.063(10) Uani 1 1 d . . .
O13 O -0.195(3) 0.6646(15) 0.8727(9) 0.046(8) Uani 1 1 d . . .
O14 O -0.219(3) 0.6133(14) 0.9507(8) 0.045(8) Uani 1 1 d . . .
O15 O -0.102(4) 0.657(2) 0.8064(11) 0.075(12) Uani 1 1 d . . .
O16 O -0.325(7) 0.555(3) 0.995(2) 0.142(5) Uani 1 1 d U . .
O17 O 0.185(4) 0.6581(14) 0.8055(11) 0.059(10) Uani 1 1 d . . .
H101 H 0.1362 0.6288 0.7966 0.071 Uiso 1 1 d R . .
H102 H 0.1351 0.6897 0.8066 0.071 Uiso 1 1 d R . .
O18 O 0.293(4) 0.6806(15) 0.8903(14) 0.080(12) Uani 1 1 d U . .
O19 O 0.260(4) 0.562(2) 0.9374(11) 0.087(13) Uani 1 1 d . . .
H103 H 0.2779 0.5243 0.9369 0.105 Uiso 1 1 d R . .
H104 H 0.1735 0.5663 0.9383 0.105 Uiso 1 1 d R . .
O20 O -0.128(6) 0.363(2) 0.7797(16) 0.124(17) Uani 1 1 d U . .
H105 H -0.1807 0.3457 0.7618 0.149 Uiso 1 1 d R . .
H106 H -0.0535 0.3717 0.7666 0.149 Uiso 1 1 d R . .
O21 O -0.278(3) 0.4189(14) 0.8489(10) 0.054(8) Uani 1 1 d . . .
O23 O -0.554(5) 0.3841(17) 0.7569(11) 0.082(12) Uani 1 1 d U . .
O24 O -0.574(3) 0.3449(11) 0.8217(8) 0.035(7) Uani 1 1 d . . .
O25 O -0.466(6) 0.399(2) 0.9673(13) 0.097(14) Uani 1 1 d U . .
O26 O -0.562(3) 0.3567(14) 0.9084(8) 0.044(8) Uani 1 1 d . . .
O27 O 0.393(3) 0.5520(17) 0.6882(9) 0.053(9) Uani 1 1 d U . .
O28 O -0.190(3) 0.5152(13) 0.7907(9) 0.040(7) Uani 1 1 d . . .
H107 H -0.1128 0.5249 0.7803 0.048 Uiso 1 1 d R . .
H108 H -0.2494 0.5401 0.7810 0.048 Uiso 1 1 d R . .
O29 O -0.036(4) 0.3693(18) 0.8847(13) 0.087(12) Uani 1 1 d U . .
O30 O 0.385(6) 0.469(3) 0.6485(17) 0.123(17) Uani 1 1 d U . .
O42 O -0.297(3) 0.3363(16) 0.8900(12) 0.069(11) Uani 1 1 d . . .
C28A C -0.544(6) 0.262(2) 0.7134(15) 0.109(15) Uani 0.33 1 d P . .
C28B C -0.627(3) 0.2214(9) 0.7975(10) 0.129(11) Uani 0.67 1 d P . .
S3A S -0.544(6) 0.262(2) 0.7134(15) 0.109(15) Uani 0.33 1 d P . .
S3B S -0.627(3) 0.2214(9) 0.7975(10) 0.129(11) Uani 0.67 1 d P . .
C35A C -0.687(4) 0.2572(15) 0.9512(12) 0.115(11) Uani 0.50 1 d P . .
S6A S -0.687(4) 0.2572(15) 0.9512(12) 0.115(11) Uani 0.50 1 d P . .
C35B C -0.606(4) 0.3116(19) 1.0263(10) 0.120(11) Uani 0.50 1 d PU . .
S6B S -0.606(4) 0.3116(19) 1.0263(10) 0.120(11) Uani 0.50 1 d P . .
C99A C -0.159(7) 0.601(3) 1.070(2) 0.14(2) Uiso 0.33 1 d P . .
C99B C -0.066(4) 0.6860(15) 1.0112(10) 0.139(10) Uiso 0.67 1 d P . .
S2A S -0.159(7) 0.601(3) 1.070(2) 0.14(2) Uiso 0.33 1 d P . .
S2B S -0.066(4) 0.6860(15) 1.0112(10) 0.139(10) Uiso 0.67 1 d P . .
C18A C -0.187(5) 0.7929(16) 0.8746(17) 0.119(16) Uani 0.40 1 d P . .
C18B C -0.091(3) 0.7952(15) 0.7953(10) 0.132(10) Uani 0.60 1 d P . .
S4A S -0.187(5) 0.7929(16) 0.8746(17) 0.119(16) Uani 0.40 1 d P . .
S4B S -0.091(3) 0.7952(15) 0.7953(10) 0.132(10) Uani 0.60 1 d P . .
C3A C 0.032(4) 0.5340(16) 0.6052(8) 0.118(10) Uani 0.60 1 d P . .
C3B C -0.205(3) 0.5903(19) 0.6363(10) 0.094(11) Uani 0.40 1 d PD . .
S1B S -0.205(3) 0.5903(19) 0.6363(10) 0.094(11) Uani 0.40 1 d P . .
S1A S 0.032(4) 0.5340(16) 0.6052(8) 0.118(10) Uani 0.60 1 d P . .
C48A C 0.430(6) 0.535(3) 0.5678(14) 0.151(13) Uani 0.40 1 d PDU . .
C48B C 0.425(4) 0.6318(16) 0.6151(10) 0.137(10) Uani 0.60 1 d PDU . .
S5B S 0.425(4) 0.6318(16) 0.6151(10) 0.137(10) Uani 0.60 1 d PU . .
S5A S 0.430(6) 0.535(3) 0.5678(14) 0.151(13) Uani 0.40 1 d PU . .
Eu1 Eu 0.26799(18) 0.57943(9) 0.85717(6) 0.0321(5) Uani 1 1 d . . .
Eu2 Eu -0.04989(19) 0.43898(9) 0.82579(6) 0.0341(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.20(10) . ?
C1 C3B 1.61(8) . ?
C2 C3A 1.68(8) . ?
C4 C5 1.49(6) . ?
C4 C3B 1.61(6) . ?
C4 C3A 1.66(5) . ?
C5 O1 1.22(5) . ?
C5 O2 1.33(5) . ?
C6 O3 1.23(5) . ?
C6 O4 1.26(4) . ?
C6 C7 1.54(5) . ?
C6 Eu2 2.88(4) . ?
C7 O2 1.43(4) . ?
C7 C8 1.53(5) . ?
C8 O27 1.44(5) . ?
C8 C9 1.56(5) . ?
C9 O6 1.23(5) . ?
C9 O5 1.27(5) . ?
C10 O9 1.26(4) . ?
C10 O10 1.26(4) . ?
C10 C37 1.52(5) 1_655 ?
C12 O8 1.24(5) . ?
C12 O7 1.27(5) . ?
C12 C13 1.53(6) . ?
C13 O13 1.42(5) . ?
C13 C14 1.50(5) . ?
C14 O14 1.45(5) . ?
C14 C15 1.50(5) . ?
C15 O12 1.26(5) . ?
C15 O11 1.26(5) . ?
C16 O15 1.18(6) . ?
C16 O13 1.37(5) . ?
C16 C17 1.47(8) . ?
C17 C18A 1.51(8) . ?
C17 C18B 1.68(6) . ?
C20 O16 1.23(8) . ?
C20 O14 1.30(6) . ?
C20 C21 1.48(8) . ?
C21 C99A 1.58(8) . ?
C21 C99B 1.62(8) . ?
C26 O23 1.19(5) . ?
C26 O24 1.34(5) . ?
C26 C27 1.45(6) . ?
C27 C28A 1.63(7) . ?
C27 C28B 1.71(6) . ?
C30 C31 1.34(11) . ?
C30 C28B 1.68(8) . ?
C31 C28A 1.61(9) . ?
C32 O25 1.19(7) . ?
C32 C33 1.32(8) . ?
C32 O26 1.35(6) . ?
C33 C35A 1.62(8) . ?
C33 C35B 1.79(7) . ?
C36 C89 1.34(7) . ?
C36 C35B 1.44(8) . ?
C37 O24 1.42(4) . ?
C37 C38 1.48(5) . ?
C37 C10 1.52(5) 1_455 ?
C38 O26 1.45(5) . ?
C38 C39 1.54(6) . ?
C39 O42 1.22(5) . ?
C39 O21 1.27(5) . ?
C41 O30 1.22(9) . ?
C41 O27 1.26(7) . ?
C41 C50 1.46(8) . ?
C45 C90 1.27(8) . ?
C45 C18B 1.59(9) . ?
C50 C48B 1.54(6) . ?
C50 C48A 1.59(6) . ?
C70 O18 1.46(8) . ?
C71 O29 1.46(11) . ?
C87 C88 1.23(8) . ?
C87 C48A 1.66(7) . ?
C88 C48B 1.60(6) . ?
C89 C35A 1.67(7) . ?
C90 C18A 1.54(9) . ?
C97 C98 1.24(8) . ?
C97 C99B 1.76(9) . ?
C98 C99A 1.58(11) . ?
O3 Eu2 2.48(3) . ?
O4 Eu1 2.51(2) . ?
O4 Eu2 2.57(3) . ?
O5 Eu1 2.32(3) . ?
O7 Eu2 2.33(3) . ?
O8 Eu1 2.38(3) . ?
O9 Eu1 2.32(3) . ?
O10 Eu2 2.42(3) . ?
O11 Eu1 2.35(3) 1_455 ?
O17 Eu1 2.49(3) . ?
O18 Eu1 2.46(3) . ?
O19 Eu1 2.53(3) . ?
O20 Eu2 2.33(5) . ?
O21 Eu2 2.38(3) . ?
O28 Eu2 2.42(3) . ?
O29 Eu2 2.39(4) . ?
Eu1 O11 2.35(3) 1_655 ?
Eu1 Eu2 4.478(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C3B 118(6) . . ?
C1 C2 C3A 120(6) . . ?
C5 C4 C3B 121(4) . . ?
C5 C4 C3A 121(4) . . ?
C3B C4 C3A 117(3) . . ?
O1 C5 O2 124(4) . . ?
O1 C5 C4 122(4) . . ?
O2 C5 C4 113(3) . . ?
O3 C6 O4 122(4) . . ?
O3 C6 C7 117(3) . . ?
O4 C6 C7 121(4) . . ?
O3 C6 Eu2 59(2) . . ?
O4 C6 Eu2 63(2) . . ?
C7 C6 Eu2 175(3) . . ?
O2 C7 C8 103(3) . . ?
O2 C7 C6 111(3) . . ?
C8 C7 C6 114(3) . . ?
O27 C8 C7 107(3) . . ?
O27 C8 C9 106(3) . . ?
C7 C8 C9 113(3) . . ?
O6 C9 O5 126(4) . . ?
O6 C9 C8 116(3) . . ?
O5 C9 C8 118(3) . . ?
O9 C10 O10 126(3) . . ?
O9 C10 C37 116(3) . 1_655 ?
O10 C10 C37 119(3) . 1_655 ?
O8 C12 O7 125(4) . . ?
O8 C12 C13 119(4) . . ?
O7 C12 C13 115(4) . . ?
O13 C13 C14 106(3) . . ?
O13 C13 C12 112(3) . . ?
C14 C13 C12 113(3) . . ?
O14 C14 C13 105(3) . . ?
O14 C14 C15 113(3) . . ?
C13 C14 C15 111(3) . . ?
O12 C15 O11 126(4) . . ?
O12 C15 C14 121(4) . . ?
O11 C15 C14 113(4) . . ?
O15 C16 O13 125(5) . . ?
O15 C16 C17 127(5) . . ?
O13 C16 C17 108(5) . . ?
C16 C17 C18A 128(5) . . ?
C16 C17 C18B 120(5) . . ?
C18A C17 C18B 112(4) . . ?
O16 C20 O14 115(5) . . ?
O16 C20 C21 129(6) . . ?
O14 C20 C21 115(5) . . ?
C20 C21 C99A 118(6) . . ?
C20 C21 C99B 121(5) . . ?
C99A C21 C99B 120(5) . . ?
O23 C26 O24 122(4) . . ?
O23 C26 C27 125(4) . . ?
O24 C26 C27 113(4) . . ?
C26 C27 C28A 121(5) . . ?
C26 C27 C28B 119(4) . . ?
C28A C27 C28B 120(4) . . ?
C31 C30 C28B 113(6) . . ?
C30 C31 C28A 123(6) . . ?
O25 C32 C33 129(5) . . ?
O25 C32 O26 125(5) . . ?
C33 C32 O26 105(5) . . ?
C32 C33 C35A 135(5) . . ?
C32 C33 C35B 118(5) . . ?
C35A C33 C35B 107(4) . . ?
C89 C36 C35B 126(6) . . ?
O24 C37 C38 108(3) . . ?
O24 C37 C10 113(3) . 1_455 ?
C38 C37 C10 112(3) . 1_455 ?
O26 C38 C37 107(3) . . ?
O26 C38 C39 111(3) . . ?
C37 C38 C39 113(3) . . ?
O42 C39 O21 127(4) . . ?
O42 C39 C38 119(4) . . ?
O21 C39 C38 114(3) . . ?
O30 C41 O27 125(6) . . ?
O30 C41 C50 119(6) . . ?
O27 C41 C50 116(6) . . ?
C90 C45 C18B 115(6) . . ?
C41 C50 C48B 125(5) . . ?
C41 C50 C48A 124(5) . . ?
C48B C50 C48A 111(4) . . ?
C88 C87 C48A 120(6) . . ?
C87 C88 C48B 109(6) . . ?
C36 C89 C35A 109(5) . . ?
C45 C90 C18A 117(7) . . ?
C98 C97 C99B 108(7) . . ?
C97 C98 C99A 127(8) . . ?
C5 O2 C7 115(3) . . ?
C6 O3 Eu2 96(2) . . ?
C6 O4 Eu1 135(2) . . ?
C6 O4 Eu2 91(2) . . ?
Eu1 O4 Eu2 123.7(9) . . ?
C9 O5 Eu1 169(3) . . ?
C12 O7 Eu2 133(2) . . ?
C12 O8 Eu1 130(3) . . ?
C10 O9 Eu1 134(2) . . ?
C10 O10 Eu2 127(2) . . ?
C15 O11 Eu1 140(3) . 1_455 ?
C16 O13 C13 116(3) . . ?
C20 O14 C14 123(4) . . ?
C70 O18 Eu1 129(4) . . ?
C39 O21 Eu2 139(3) . . ?
C26 O24 C37 118(3) . . ?
C32 O26 C38 116(4) . . ?
C41 O27 C8 117(4) . . ?
C71 O29 Eu2 134(5) . . ?
C31 C28A C27 92(4) . . ?
C30 C28B C27 92(4) . . ?
C33 C35A C89 101(4) . . ?
C36 C35B C33 97(4) . . ?
C21 C99A C98 90(5) . . ?
C21 C99B C97 92(4) . . ?
C17 C18A C90 100(5) . . ?
C45 C18B C17 96(4) . . ?
C4 C3A C2 90(3) . . ?
C4 C3B C1 94(4) . . ?
C50 C48A C87 95(4) . . ?
C50 C48B C88 104(4) . . ?
O5 Eu1 O9 82.7(11) . . ?
O5 Eu1 O11 76.4(10) . 1_655 ?
O9 Eu1 O11 90.5(11) . 1_655 ?
O5 Eu1 O8 141.8(10) . . ?
O9 Eu1 O8 100.5(10) . . ?
O11 Eu1 O8 140.9(10) 1_655 . ?
O5 Eu1 O18 121.5(13) . . ?
O9 Eu1 O18 143.6(12) . . ?
O11 Eu1 O18 72.0(12) 1_655 . ?
O8 Eu1 O18 77.4(12) . . ?
O5 Eu1 O17 80.4(11) . . ?
O9 Eu1 O17 144.1(10) . . ?
O11 Eu1 O17 115.6(12) 1_655 . ?
O8 Eu1 O17 75.2(11) . . ?
O18 Eu1 O17 71.3(12) . . ?
O5 Eu1 O4 72.3(9) . . ?
O9 Eu1 O4 72.6(9) . . ?
O11 Eu1 O4 145.9(10) 1_655 . ?
O8 Eu1 O4 72.5(9) . . ?
O18 Eu1 O4 137.3(11) . . ?
O17 Eu1 O4 72.2(10) . . ?
O5 Eu1 O19 140.7(12) . . ?
O9 Eu1 O19 70.8(12) . . ?
O11 Eu1 O19 75.3(12) 1_655 . ?
O8 Eu1 O19 73.3(12) . . ?
O18 Eu1 O19 73.8(15) . . ?
O17 Eu1 O19 137.0(13) . . ?
O4 Eu1 O19 123.3(12) . . ?
O5 Eu1 Eu2 90.5(8) . . ?
O9 Eu1 Eu2 52.2(7) . . ?
O11 Eu1 Eu2 142.1(9) 1_655 . ?
O8 Eu1 Eu2 64.1(7) . . ?
O18 Eu1 Eu2 141.4(9) . . ?
O17 Eu1 Eu2 96.4(8) . . ?
O4 Eu1 Eu2 28.5(6) . . ?
O19 Eu1 Eu2 95.3(10) . . ?
O20 Eu2 O7 156.9(15) . . ?
O20 Eu2 O21 75.5(15) . . ?
O7 Eu2 O21 81.5(11) . . ?
O20 Eu2 O29 92.0(17) . . ?
O7 Eu2 O29 83.5(13) . . ?
O21 Eu2 O29 72.6(12) . . ?
O20 Eu2 O10 95.9(16) . . ?
O7 Eu2 O10 104.2(11) . . ?
O21 Eu2 O10 143.5(10) . . ?
O29 Eu2 O10 72.3(13) . . ?
O20 Eu2 O28 91.8(16) . . ?
O7 Eu2 O28 79.6(10) . . ?
O21 Eu2 O28 74.7(10) . . ?
O29 Eu2 O28 145.0(12) . . ?
O10 Eu2 O28 141.7(10) . . ?
O20 Eu2 O3 74.9(14) . . ?
O7 Eu2 O3 121.7(10) . . ?
O21 Eu2 O3 134.9(10) . . ?
O29 Eu2 O3 141.2(13) . . ?
O10 Eu2 O3 72.9(10) . . ?
O28 Eu2 O3 73.0(9) . . ?
O20 Eu2 O4 126.1(13) . . ?
O7 Eu2 O4 71.9(9) . . ?
O21 Eu2 O4 140.7(10) . . ?
O29 Eu2 O4 130.1(12) . . ?
O10 Eu2 O4 72.7(9) . . ?
O28 Eu2 O4 72.5(9) . . ?
O3 Eu2 O4 51.2(9) . . ?
O20 Eu2 C6 100.1(15) . . ?
O7 Eu2 C6 97.1(11) . . ?
O21 Eu2 C6 144.8(10) . . ?
O29 Eu2 C6 142.4(13) . . ?
O10 Eu2 C6 71.2(10) . . ?
O28 Eu2 C6 70.5(10) . . ?
O3 Eu2 C6 25.2(10) . . ?
O4 Eu2 C6 25.9(9) . . ?
O20 Eu2 Eu1 148.5(12) . . ?
O7 Eu2 Eu1 53.9(7) . . ?
O21 Eu2 Eu1 135.1(8) . . ?
O29 Eu2 Eu1 103.5(11) . . ?
O10 Eu2 Eu1 64.2(7) . . ?
O28 Eu2 Eu1 90.9(7) . . ?
O3 Eu2 Eu1 75.9(7) . . ?
O4 Eu2 Eu1 27.8(5) . . ?
C6 Eu2 Eu1 51.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.133
# SQUEEZE RESULTS (APPEND TO CIF)
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
1 -0.065 0.330 0.681 297.4 17.5
2 0.107 -0.031 0.529 30.4 4.4
3 0.064 0.830 0.819 297.5 17.1
4 -0.107 0.469 0.971 30.3 5.1
5 0.435 0.170 0.319 297.6 18.5
6 0.564 0.670 0.180 297.7 18.0
7 0.393 0.031 0.029 30.4 4.6
8 0.607 0.531 0.471 30.4 4.6
_platon_squeeze_details          
; ?
;

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_3#Gd
_database_code_depnum_ccdc_archive 'CCDC 1023765'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        3#Gd
_chemical_name_common            Gd
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H21 Gd2 O30 S6, C H4 O '
_chemical_formula_sum            'C46 H25 Gd2 O31 S6 '
_chemical_formula_weight         1580.52

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  ' P 2ac 2ab '

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

_cell_length_a                   9.728(5)
_cell_length_b                   22.100(5)
_cell_length_c                   31.176(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6703(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    19675
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3092
_exptl_absorpt_coefficient_mu    2.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_process_details   sadabs(Sheldrick,1996)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19675
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11808
_reflns_number_gt                10689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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.
ISOR  0.01 C8 C30 C46 O16 O20 O29 C48 C42 O16 O30 C47 C31 C22 O25 C40
FLAT     0.100 C7 C8 C45 C46
FLAT     0.100 C27 C29 C30 C31
FLAT     0.100 C40 C42 C60 C61
DELU     0.010   0.010 C27 C29 C30 C31
SIMU     0.040   0.080   3.800 C27 C29 C30 C31
SIMU     0.040   0.080   3.800 C40 C42 C60 C61
SIMU     0.040   0.080   3.800 C11 C12 C14 C44 
DELU     0.010   0.010 O25 C63
SIMU     0.040   0.080   3.800 O25 C63
DELU     0.010   0.010 O5 C48
SIMU     0.040   0.080   3.800 O5 C48
DELU     0.010   0.010 C6 O16
SIMU     0.040   0.080   3.800 C6 O16
DELU     0.010   0.010 O30 C47
SIMU     0.040   0.080   3.800 O30 C47
EXYZ C19A S1A
EXYZ C19B S1B
EADP C19A S1A
EADP C19B S1B
EXYZ C22A S2A
EXYZ C22B S2B
EADP C22A S2A
EADP C22B S2B
EXYZ C31B S4B
EXYZ C31A S4A
EADP C31A S4A
EADP C31B S4B
EXYZ C12A S5A
EXYZ C12B S5B
EADP C12A S5A
EADP C12B S5B
EXYZ C42A S6A
EXYZ C42B S6B
EADP C42A S6A
EADP C42B S6B
DANG     2.928   0.040 C42B C42A
DANG     2.413   0.040 C42B C61
DANG     2.466   0.040 C42A C60
DFIX     1.610   0.020 C40 C42B
DELU     0.010   0.010 C40 C60 C61 C42A C42B S6B S6A
SIMU     0.040   0.080   3.800 C40 C60 C61 C42A C42B S6B S6A
 In addition, due to the operation of EXYZ, the H atoms on the five-membered rings can't be added.
;

_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)+(0.0841P)²+44.1598P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   0.030(3)
_refine_ls_number_reflns         11808
_refine_ls_number_parameters     767
_refine_ls_number_restraints     301
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_ref         0.1724
_refine_ls_wR_factor_gt          0.1672
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2857(11) 1.0726(6) 0.8480(4) 0.031(3) Uani 1 1 d . . .
C2 C -0.0639(12) 0.9319(6) 0.8785(3) 0.033(3) Uani 1 1 d . . .
C3 C -0.2053(12) 0.9029(7) 0.8754(4) 0.038(3) Uani 1 1 d . . .
H3 H -0.2523 0.9195 0.8502 0.045 Uiso 1 1 calc R . .
C4 C 0.7083(11) 0.9151(6) 0.9139(3) 0.034(3) Uani 1 1 d . . .
H4 H 0.6993 0.9588 0.9182 0.041 Uiso 1 1 calc R . .
C5 C 0.5673(12) 0.8867(7) 0.9089(4) 0.043(3) Uani 1 1 d . . .
C6 C 0.764(3) 0.9080(10) 0.9880(5) 0.082(6) Uani 1 1 d U . .
C7 C 0.835(2) 0.8791(8) 1.0218(5) 0.090(7) Uani 1 1 d D . .
C10 C -0.1469(14) 0.8177(7) 0.8342(4) 0.047(4) Uani 1 1 d . . .
C11 C -0.1445(18) 0.7504(9) 0.8347(7) 0.082(6) Uani 1 1 d DU . .
C14 C -0.186(3) 0.6491(13) 0.8534(10) 0.124(8) Uani 1 1 d DU . .
C15 C 0.425(2) 1.3097(13) 0.7224(9) 0.103(9) Uani 1 1 d . . .
C16 C 0.382(3) 1.3318(12) 0.7599(13) 0.121(11) Uani 1 1 d . . .
C18 C 0.4205(17) 1.2260(8) 0.7668(5) 0.058(4) Uani 1 1 d . . .
C20 C 0.4337(19) 1.1628(7) 0.7798(4) 0.052(4) Uani 1 1 d . . .
C21 C 0.273(3) 1.2751(13) 0.9960(12) 0.120(11) Uani 1 1 d . . .
C25 C 0.4655(17) 1.1403(10) 0.9508(5) 0.063(5) Uani 1 1 d . . .
C26 C 0.0068(13) 0.9375(7) 0.6898(4) 0.043(3) Uani 1 1 d . . .
C27 C -0.0473(15) 0.9402(9) 0.6456(4) 0.065(4) Uani 1 1 d DU . .
C29 C -0.189(2) 0.9273(13) 0.5858(6) 0.102(7) Uani 1 1 d DU . .
C30 C -0.086(3) 0.9529(13) 0.5715(6) 0.108(7) Uani 1 1 d DU . .
C32 C 0.5117(13) 1.1015(6) 0.8809(4) 0.036(3) Uani 1 1 d . . .
H32 H 0.5092 1.0615 0.8945 0.043 Uiso 1 1 calc R . .
C33 C 0.3434(11) 0.9823(6) 0.7267(4) 0.028(3) Uani 1 1 d . . .
H33 H 0.3385 1.0258 0.7204 0.034 Uiso 1 1 calc R . .
C34 C 0.4457(13) 0.9703(5) 0.7635(4) 0.031(3) Uani 1 1 d . . .
C35 C 0.6613(13) 1.1184(6) 0.8736(4) 0.036(3) Uani 1 1 d . . .
C36 C 0.1178(11) 0.9928(6) 0.7675(4) 0.027(3) Uani 1 1 d . . .
C37 C 0.1980(11) 0.9567(7) 0.7346(3) 0.035(3) Uani 1 1 d . . .
H37 H 0.2030 0.9140 0.7430 0.042 Uiso 1 1 calc R . .
C38 C 0.4314(11) 1.0982(5) 0.8400(3) 0.027(2) Uani 1 1 d . . .
H38 H 0.4797 1.0715 0.8200 0.032 Uiso 1 1 calc R . .
C39 C 0.4009(19) 0.9770(11) 0.6527(5) 0.072(6) Uani 1 1 d . . .
C40 C 0.421(3) 0.9383(8) 0.6169(7) 0.105(4) Uani 1 1 d DU . .
C41 C 0.3933(16) 1.1887(10) 0.9728(6) 0.068(5) Uani 1 1 d . . .
C43 C 0.314(3) 1.2469(16) 1.0305(8) 0.115(11) Uani 1 1 d . . .
C44 C -0.133(3) 0.6455(12) 0.8111(10) 0.130(9) Uani 1 1 d DU . .
C45 C 0.986(2) 0.8138(14) 1.0625(7) 0.22(3) Uani 1 1 d D . .
C46 C 0.939(3) 0.8542(13) 1.0847(9) 0.185(19) Uani 1 1 d DU . .
C47 C 0.078(3) 1.1514(15) 0.9110(9) 0.135(9) Uani 1 1 d U . .
H47A H 0.0464 1.1831 0.9296 0.202 Uiso 1 1 calc R . .
H47B H 0.1533 1.1660 0.8939 0.202 Uiso 1 1 calc R . .
H47C H 0.1078 1.1176 0.9279 0.202 Uiso 1 1 calc R . .
C48 C 0.185(3) 0.9836(14) 0.9614(9) 0.138(9) Uani 1 1 d U . .
H48A H 0.2075 0.9772 0.9910 0.207 Uiso 1 1 calc R . .
H48B H 0.0875 0.9783 0.9575 0.207 Uiso 1 1 calc R . .
H48C H 0.2101 1.0240 0.9532 0.207 Uiso 1 1 calc R . .
C49 C 0.190(3) 0.7830(14) 0.9068(14) 0.19(2) Uani 1 1 d . . .
H49A H 0.2326 0.7468 0.9175 0.282 Uiso 1 1 calc R . .
H49B H 0.1262 0.7727 0.8844 0.282 Uiso 1 1 calc R . .
H49C H 0.1416 0.8027 0.9298 0.282 Uiso 1 1 calc R . .
O31 O -0.279(2) 1.1101(14) 0.7164(10) 0.200(12) Uani 1 1 d . . .
H771 H -0.3580 1.1139 0.7291 0.240 Uiso 1 1 d R . .
C60 C 0.437(4) 0.8506(12) 0.5696(10) 0.147(6) Uani 1 1 d DU . .
C61 C 0.439(4) 0.8966(16) 0.5475(7) 0.152(6) Uani 1 1 d DU . .
O1 O 0.2784(9) 1.0255(4) 0.8706(3) 0.0358(19) Uani 1 1 d . . .
O2 O 0.1852(8) 1.0988(4) 0.8307(4) 0.047(2) Uani 1 1 d . . .
O3 O 0.1099(8) 0.9734(4) 0.8051(2) 0.0324(19) Uani 1 1 d . . .
O4 O 0.2937(12) 0.8230(5) 0.8901(5) 0.075(4) Uani 1 1 d . . .
O5 O 0.2578(12) 0.9408(7) 0.9353(3) 0.075(3) Uani 1 1 d U . .
O6 O 0.0423(9) 0.9000(4) 0.8793(3) 0.041(2) Uani 1 1 d . . .
O7 O 0.0630(8) 1.0410(4) 0.7562(3) 0.039(2) Uani 1 1 d . . .
O8 O -0.0620(9) 0.9901(4) 0.8797(3) 0.039(2) Uani 1 1 d . . .
O9 O -0.1238(17) 1.1375(7) 0.7791(5) 0.121(7) Uani 1 1 d . . .
H101 H -0.1091 1.1751 0.7845 0.146 Uiso 1 1 d R . .
H102 H -0.0730 1.1280 0.7581 0.146 Uiso 1 1 d R . .
O10 O 0.7246(9) 1.0825(4) 0.8499(3) 0.047(2) Uani 1 1 d . . .
O11 O -0.1884(8) 0.9888(4) 0.7904(3) 0.034(2) Uani 1 1 d . . .
H103 H -0.1378 0.9829 0.7686 0.041 Uiso 1 1 d R . .
H104 H -0.2705 0.9933 0.7816 0.041 Uiso 1 1 d R . .
O12 O 0.4962(9) 0.9121(5) 0.8795(3) 0.053(3) Uani 1 1 d . . .
O13 O 0.5307(11) 0.8424(6) 0.9301(4) 0.063(3) Uani 1 1 d . . .
O14 O 0.7814(9) 0.8883(5) 0.9498(3) 0.045(2) Uani 1 1 d . . .
O15 O -0.1962(9) 0.8390(5) 0.8705(3) 0.043(2) Uani 1 1 d . . .
O16 O 0.670(2) 0.9476(10) 0.9942(6) 0.129(6) Uani 1 1 d U . .
O17 O -0.1018(11) 0.8475(6) 0.8062(3) 0.064(3) Uani 1 1 d . . .
O18 O 0.3942(9) 0.9505(5) 0.7977(3) 0.048(3) Uani 1 1 d . . .
O19 O 0.7073(10) 1.1660(6) 0.8896(4) 0.068(4) Uani 1 1 d . . .
O20 O 0.4465(17) 1.1174(6) 0.7573(4) 0.081(4) Uani 1 1 d U . .
O21 O 0.4278(9) 1.1569(4) 0.8227(3) 0.0365(19) Uani 1 1 d . . .
O22 O 0.4411(9) 1.1433(5) 0.9085(3) 0.043(2) Uani 1 1 d . . .
O23 O 0.5384(18) 1.1011(8) 0.9673(4) 0.098(5) Uani 1 1 d . . .
O24 O -0.0553(12) 0.9166(7) 0.7205(3) 0.078(4) Uani 1 1 d . . .
O25 O 0.1866(11) 0.8456(5) 0.8057(3) 0.055(3) Uani 1 1 d U . .
H109 H 0.2150 0.8221 0.8254 0.066 Uiso 1 1 d R . .
H110 H 0.1049 0.8560 0.8120 0.066 Uiso 1 1 d R . .
O26 O 0.5634(9) 0.9838(5) 0.7563(3) 0.048(2) Uani 1 1 d . . .
O27 O 0.1316(9) 0.9630(4) 0.6929(3) 0.039(2) Uani 1 1 d . . .
O28 O 0.3971(9) 0.9496(5) 0.6899(3) 0.048(3) Uani 1 1 d . . .
O29 O 0.3876(19) 1.0324(9) 0.6498(5) 0.107(5) Uani 1 1 d U . .
O30 O -0.0316(14) 1.1329(7) 0.8834(5) 0.088(4) Uani 1 1 d U . .
C51 C -0.241(3) 1.065(2) 0.6881(12) 0.180(16) Uani 1 1 d . . .
H51A H -0.1519 1.0494 0.6959 0.269 Uiso 1 1 calc R . .
H51B H -0.2376 1.0806 0.6595 0.269 Uiso 1 1 calc R . .
H51C H -0.3070 1.0324 0.6894 0.269 Uiso 1 1 calc R . .
C19A C 0.455(2) 1.2431(8) 0.7182(6) 0.124(6) Uani 0.33 1 d P . .
C19B C 0.3667(10) 1.2804(3) 0.7994(3) 0.108(3) Uani 0.67 1 d P . .
S1B S 0.3667(10) 1.2804(3) 0.7994(3) 0.108(3) Uani 0.67 1 d P . .
S1A S 0.455(2) 1.2431(8) 0.7182(6) 0.124(6) Uani 0.33 1 d P . .
C22A C 0.3185(13) 1.2420(6) 0.9526(5) 0.134(5) Uani 0.50 1 d P . .
C22B C 0.3948(12) 1.1904(7) 1.0263(3) 0.117(4) Uani 0.50 1 d P . .
S2B S 0.3948(12) 1.1904(7) 1.0263(3) 0.117(4) Uani 0.50 1 d P . .
S2A S 0.3185(13) 1.2420(6) 0.9526(5) 0.134(5) Uani 0.50 1 d P . .
C8 C 0.837(2) 0.9008(9) 1.0689(4) 0.082(5) Uani 1 1 d DU . .
S3 S 0.9327(11) 0.8149(6) 1.0095(3) 0.180(5) Uani 1 1 d D . .
C31B C 0.0369(11) 0.9680(5) 0.6069(2) 0.093(3) Uani 0.50 1 d P . .
C31A C -0.1980(10) 0.9127(6) 0.6344(3) 0.111(4) Uani 0.50 1 d P . .
S4A S -0.1980(10) 0.9127(6) 0.6344(3) 0.111(4) Uani 0.50 1 d P . .
S4B S 0.0369(11) 0.9680(5) 0.6069(2) 0.093(3) Uani 0.50 1 d P . .
C12A C -0.1975(15) 0.7108(5) 0.8703(4) 0.080(4) Uani 0.33 1 d P . .
C12B C -0.0917(9) 0.7126(5) 0.7919(3) 0.126(4) Uani 0.67 1 d P . .
S5B S -0.0917(9) 0.7126(5) 0.7919(3) 0.126(4) Uani 0.67 1 d P . .
S5A S -0.1975(15) 0.7108(5) 0.8703(4) 0.080(4) Uani 0.33 1 d P . .
C42A C 0.4313(15) 0.9606(7) 0.5682(4) 0.141(4) Uani 0.50 1 d PDU . .
C42B C 0.4248(12) 0.8684(6) 0.6184(4) 0.116(3) Uani 0.50 1 d PDU . .
S6B S 0.4248(12) 0.8684(6) 0.6184(4) 0.116(3) Uani 0.50 1 d PU . .
S6A S 0.4313(15) 0.9606(7) 0.5682(4) 0.141(4) Uani 0.50 1 d PU . .
Gd1 Gd 0.26886(5) 0.92287(3) 0.857322(18) 0.02918(16) Uani 1 1 d . . .
Gd2 Gd -0.04623(5) 1.06257(3) 0.826293(18) 0.02925(16) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.258(15) . ?
C1 O2 1.258(14) . ?
C1 C38 1.547(15) . ?
C2 O6 1.251(15) . ?
C2 O8 1.286(16) . ?
C2 C3 1.521(16) . ?
C3 O15 1.423(17) . ?
C3 C4 1.490(16) 1_455 ?
C4 O14 1.452(14) . ?
C4 C3 1.490(16) 1_655 ?
C4 C5 1.517(17) . ?
C5 O13 1.234(17) . ?
C5 O12 1.276(15) . ?
C6 O14 1.279(19) . ?
C6 O16 1.28(3) . ?
C6 C7 1.42(2) . ?
C7 C8 1.544(16) . ?
C7 S3 1.748(16) . ?
C10 O17 1.181(17) . ?
C10 O15 1.314(15) . ?
C10 C11 1.49(3) . ?
C11 C12A 1.51(2) . ?
C11 C12B 1.655(17) . ?
C14 C44 1.420(17) . ?
C14 C12A 1.46(3) . ?
C15 C16 1.34(4) . ?
C15 C19A 1.51(3) . ?
C16 C19B 1.68(3) . ?
C18 C20 1.46(2) . ?
C18 C19A 1.60(2) . ?
C18 C19B 1.66(2) . ?
C20 O20 1.232(19) . ?
C20 O21 1.345(16) . ?
C21 C43 1.30(4) . ?
C21 C22A 1.60(3) . ?
C25 O23 1.23(2) . ?
C25 O22 1.342(18) . ?
C25 C41 1.45(2) . ?
C26 O24 1.223(17) . ?
C26 O27 1.342(16) . ?
C26 C27 1.477(17) . ?
C27 C31B 1.582(19) . ?
C27 C31A 1.625(17) . ?
C29 C30 1.240(18) . ?
C29 C31A 1.55(2) . ?
C30 C31B 1.66(2) . ?
C32 O22 1.437(15) . ?
C32 C38 1.497(16) . ?
C32 C35 1.519(18) . ?
C33 O28 1.454(14) . ?
C33 C34 1.543(17) . ?
C33 C37 1.543(16) . ?
C34 O26 1.205(15) . ?
C34 O18 1.258(15) . ?
C35 O19 1.246(16) . ?
C35 O10 1.248(15) . ?
C36 O7 1.243(15) . ?
C36 O3 1.251(14) . ?
C36 C37 1.516(16) . ?
C36 Gd2 2.878(12) . ?
C37 O27 1.457(13) . ?
C38 O21 1.405(14) . ?
C39 O29 1.23(3) . ?
C39 O28 1.31(2) . ?
C39 C40 1.42(2) . ?
C40 C42B 1.545(17) . ?
C40 C42A 1.60(2) . ?
C41 C22A 1.52(3) . ?
C41 C22B 1.67(2) . ?
C43 C22B 1.48(4) . ?
C44 C12B 1.65(3) . ?
C45 C46 1.22(2) . ?
C45 S3 1.734(17) . ?
C46 C8 1.514(19) . ?
C47 O30 1.43(3) . ?
C48 O5 1.44(3) . ?
C49 O4 1.44(3) . ?
O31 C51 1.39(4) . ?
C60 C61 1.228(19) . ?
C60 C42B 1.57(3) . ?
C61 C42A 1.56(3) . ?
O1 Gd1 2.308(8) . ?
O2 Gd2 2.393(8) . ?
O3 Gd1 2.508(8) . ?
O3 Gd2 2.574(8) . ?
O4 Gd1 2.444(10) . ?
O5 Gd1 2.464(10) . ?
O6 Gd1 2.363(9) . ?
O7 Gd2 2.477(8) . ?
O8 Gd2 2.315(9) . ?
O9 Gd2 2.341(12) . ?
O10 Gd2 2.389(8) 1_655 ?
O11 Gd2 2.413(8) . ?
O12 Gd1 2.330(8) . ?
O18 Gd1 2.305(9) . ?
O25 Gd1 2.478(10) . ?
O30 Gd2 2.368(11) . ?
Gd2 O10 2.389(9) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 125.3(11) . . ?
O1 C1 C38 116.4(10) . . ?
O2 C1 C38 118.3(11) . . ?
O6 C2 O8 123.5(11) . . ?
O6 C2 C3 120.6(12) . . ?
O8 C2 C3 115.9(11) . . ?
O15 C3 C4 107.6(10) . 1_455 ?
O15 C3 C2 111.7(11) . . ?
C4 C3 C2 112.4(11) 1_455 . ?
O14 C4 C3 105.7(9) . 1_655 ?
O14 C4 C5 110.7(10) . . ?
C3 C4 C5 110.6(11) 1_655 . ?
O13 C5 O12 125.2(12) . . ?
O13 C5 C4 122.3(12) . . ?
O12 C5 C4 112.5(11) . . ?
O14 C6 O16 117.9(17) . . ?
O14 C6 C7 118.5(19) . . ?
O16 C6 C7 123.0(17) . . ?
C6 C7 C8 124.9(15) . . ?
C6 C7 S3 117.8(13) . . ?
C8 C7 S3 117.2(11) . . ?
O17 C10 O15 124.9(15) . . ?
O17 C10 C11 124.1(14) . . ?
O15 C10 C11 110.8(13) . . ?
C10 C11 C12A 125.7(12) . . ?
C10 C11 C12B 120.1(16) . . ?
C12A C11 C12B 114.0(13) . . ?
C44 C14 C12A 115(2) . . ?
C16 C15 C19A 120(2) . . ?
C15 C16 C19B 115(2) . . ?
C20 C18 C19A 118.1(15) . . ?
C20 C18 C19B 123.4(13) . . ?
C19A C18 C19B 118.4(13) . . ?
O20 C20 O21 119.4(14) . . ?
O20 C20 C18 129.1(14) . . ?
O21 C20 C18 111.5(13) . . ?
C43 C21 C22A 113(2) . . ?
O23 C25 O22 123.2(15) . . ?
O23 C25 C41 126.8(16) . . ?
O22 C25 C41 110.0(18) . . ?
O24 C26 O27 123.3(11) . . ?
O24 C26 C27 124.8(13) . . ?
O27 C26 C27 111.9(12) . . ?
C26 C27 C31B 122.9(12) . . ?
C26 C27 C31A 120.5(13) . . ?
C31B C27 C31A 116.6(9) . . ?
C30 C29 C31A 119.4(16) . . ?
C29 C30 C31B 115.9(16) . . ?
O22 C32 C38 107.0(9) . . ?
O22 C32 C35 112.9(10) . . ?
C38 C32 C35 112.7(10) . . ?
O28 C33 C34 105.7(9) . . ?
O28 C33 C37 105.8(9) . . ?
C34 C33 C37 114.2(10) . . ?
O26 C34 O18 128.6(12) . . ?
O26 C34 C33 115.6(11) . . ?
O18 C34 C33 115.7(11) . . ?
O19 C35 O10 126.6(12) . . ?
O19 C35 C32 119.4(11) . . ?
O10 C35 C32 113.9(11) . . ?
O7 C36 O3 122.3(11) . . ?
O7 C36 C37 118.7(10) . . ?
O3 C36 C37 119.0(11) . . ?
O7 C36 Gd2 58.9(6) . . ?
O3 C36 Gd2 63.4(6) . . ?
C37 C36 Gd2 176.8(8) . . ?
O27 C37 C36 108.9(10) . . ?
O27 C37 C33 103.2(9) . . ?
C36 C37 C33 112.7(10) . . ?
O21 C38 C32 107.1(10) . . ?
O21 C38 C1 112.2(9) . . ?
C32 C38 C1 111.1(9) . . ?
O29 C39 O28 121.5(16) . . ?
O29 C39 C40 123.6(19) . . ?
O28 C39 C40 115(2) . . ?
C39 C40 C42B 125.5(19) . . ?
C39 C40 C42A 124.8(17) . . ?
C42B C40 C42A 109.5(14) . . ?
C25 C41 C22A 127.2(16) . . ?
C25 C41 C22B 119.0(18) . . ?
C22A C41 C22B 113.7(13) . . ?
C21 C43 C22B 119(2) . . ?
C14 C44 C12B 112.0(19) . . ?
C46 C45 S3 115(2) . . ?
C45 C46 C8 124(2) . . ?
C61 C60 C42B 110(2) . . ?
C60 C61 C42A 121(2) . . ?
C1 O1 Gd1 135.6(7) . . ?
C1 O2 Gd2 127.0(8) . . ?
C36 O3 Gd1 136.3(7) . . ?
C36 O3 Gd2 90.8(7) . . ?
Gd1 O3 Gd2 122.5(3) . . ?
C49 O4 Gd1 129.6(13) . . ?
C48 O5 Gd1 133.3(15) . . ?
C2 O6 Gd1 130.1(8) . . ?
C36 O7 Gd2 95.6(7) . . ?
C2 O8 Gd2 132.2(7) . . ?
C35 O10 Gd2 139.5(8) . 1_655 ?
C5 O12 Gd1 140.5(8) . . ?
C6 O14 C4 121.0(13) . . ?
C10 O15 C3 118.1(11) . . ?
C34 O18 Gd1 170.8(9) . . ?
C20 O21 C38 118.1(10) . . ?
C25 O22 C32 118.2(12) . . ?
C26 O27 C37 115.2(9) . . ?
C39 O28 C33 118.6(13) . . ?
C47 O30 Gd2 133.2(15) . . ?
C15 C19A C18 96.3(18) . . ?
C18 C19B C16 90.7(15) . . ?
C41 C22A C21 97.7(18) . . ?
C43 C22B C41 95.9(15) . . ?
C46 C8 C7 95.9(15) . . ?
C45 S3 C7 87.9(12) . . ?
C27 C31B C30 93.3(11) . . ?
C29 C31A C27 94.9(11) . . ?
C14 C12A C11 104.4(15) . . ?
C44 C12B C11 95.0(12) . . ?
C61 C42A C40 96.7(13) . . ?
C40 C42B C60 102.9(14) . . ?
O18 Gd1 O1 82.1(3) . . ?
O18 Gd1 O12 76.4(3) . . ?
O1 Gd1 O12 90.5(4) . . ?
O18 Gd1 O6 141.6(3) . . ?
O1 Gd1 O6 101.3(3) . . ?
O12 Gd1 O6 141.0(3) . . ?
O18 Gd1 O4 121.6(4) . . ?
O1 Gd1 O4 144.0(4) . . ?
O12 Gd1 O4 71.9(4) . . ?
O6 Gd1 O4 77.2(4) . . ?
O18 Gd1 O5 140.8(4) . . ?
O1 Gd1 O5 70.6(4) . . ?
O12 Gd1 O5 76.4(4) . . ?
O6 Gd1 O5 73.0(3) . . ?
O4 Gd1 O5 74.8(5) . . ?
O18 Gd1 O25 80.2(4) . . ?
O1 Gd1 O25 143.8(3) . . ?
O12 Gd1 O25 115.4(4) . . ?
O6 Gd1 O25 74.9(3) . . ?
O4 Gd1 O25 71.4(4) . . ?
O5 Gd1 O25 137.4(4) . . ?
O18 Gd1 O3 71.6(3) . . ?
O1 Gd1 O3 72.8(3) . . ?
O12 Gd1 O3 145.5(3) . . ?
O6 Gd1 O3 73.0(3) . . ?
O4 Gd1 O3 137.2(4) . . ?
O5 Gd1 O3 122.8(4) . . ?
O25 Gd1 O3 71.7(3) . . ?
O8 Gd2 O9 157.0(4) . . ?
O8 Gd2 O30 85.3(5) . . ?
O9 Gd2 O30 91.6(6) . . ?
O8 Gd2 O10 81.0(3) . 1_455 ?
O9 Gd2 O10 76.3(4) . 1_455 ?
O30 Gd2 O10 72.7(4) . 1_455 ?
O8 Gd2 O2 104.6(3) . . ?
O9 Gd2 O2 95.9(5) . . ?
O30 Gd2 O2 71.4(4) . . ?
O10 Gd2 O2 143.0(3) 1_455 . ?
O8 Gd2 O11 80.1(3) . . ?
O9 Gd2 O11 90.1(6) . . ?
O30 Gd2 O11 145.8(4) . . ?
O10 Gd2 O11 74.5(3) 1_455 . ?
O2 Gd2 O11 142.3(3) . . ?
O8 Gd2 O7 122.0(3) . . ?
O9 Gd2 O7 73.7(4) . . ?
O30 Gd2 O7 139.8(4) . . ?
O10 Gd2 O7 135.1(3) 1_455 . ?
O2 Gd2 O7 73.2(3) . . ?
O11 Gd2 O7 72.9(3) . . ?
O8 Gd2 O3 72.2(3) . . ?
O9 Gd2 O3 124.8(4) . . ?
O30 Gd2 O3 131.3(4) . . ?
O10 Gd2 O3 140.4(3) 1_455 . ?
O2 Gd2 O3 73.5(3) . . ?
O11 Gd2 O3 72.7(3) . . ?
O7 Gd2 O3 51.2(3) . . ?
O8 Gd2 C36 97.1(3) . . ?
O9 Gd2 C36 99.1(4) . . ?
O30 Gd2 C36 142.9(4) . . ?
O10 Gd2 C36 144.3(3) 1_455 . ?
O2 Gd2 C36 72.2(3) . . ?
O11 Gd2 C36 70.1(3) . . ?
O7 Gd2 C36 25.4(3) . . ?
O3 Gd2 C36 25.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.151
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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#La
_database_code_depnum_ccdc_archive 'CCDC 1023766'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        1#La
_chemical_name_common            La
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H26 La2 O31 S6, C H4 O, H2 O '
_chemical_formula_sum            'C49 H56 La2 O33 S6'
_chemical_formula_weight         1618.93

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  ' P 2ac 2ab '

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

_cell_length_a                   9.887(5)
_cell_length_b                   22.183(5)
_cell_length_c                   31.491(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6907(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    29322
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3200
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_process_details   sadabs(Sheldrick,1996)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29322
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12170
_reflns_number_gt                11664
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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.
ISOR 0.01 C39 C38 C44 O1W O26 O9 C34 C37 C3 C30 C46 C12 c17 C22 O34 C56 C16
DELU     0.010   0.010 O34 C56
SIMU     0.040   0.080   3.800 O34 C56
DELU     0.010   0.010 C48 C49 C50 C51
SIMU     0.040   0.080   3.800 C48 C49 C50 C51
DELU     0.010   0.010 C35 C36 O25 O26
SIMU     0.040   0.080   3.800 C35 C36 O25 O26
DELU     0.010   0.010 C36 C37 C38 C39
SIMU     0.040   0.080   3.800 C36 C37 C38 C39
DELU     0.010   0.010 C15 O9
SIMU     0.040   0.080   3.800 C15 O9
DELU     0.010   0.010 C30 C31 C32 C33
SIMU     0.040   0.080   3.800 C30 C31 C32 C33
DELU     0.010   0.010 C17 O11
SIMU     0.040   0.080   3.800 C17 O11
DELU     0.010   0.010 C19 C20 C21 C22
SIMU     0.040   0.080   3.800 C19 C20 C21 C22
DELU     0.010   0.010 C11 C12
SIMU     0.040   0.080   3.800 C11 C12
DELU     0.010   0.010 O34 C56 
SIMU     0.040   0.080   3.800 O34 C56 
DELU     0.010   0.010 C16 O10
SIMU     0.040   0.080   3.800 C16 O10
EXYZ C22A S3A
EXYZ C22B S3B
EADP C22A S3A
EADP C22B S3B
EXYZ C30A S4A
EXYZ C30B S4B
EADP C30A S4A
EADP C30B S4B
EXYZ C37A S5A
EXYZ C37B S5B
EADP C37A S5A
EADP C37B S5B
EXYZ C49A S6A
EXYZ C49B S6B
EADP C49A S6A
EADP C49B S6B
EXYZ S1A C3A
EXYZ S1B C3B
EADP S1A C3A
EADP S1B C3B
EXYZ C99A S2A
EXYZ C99B S2B
EADP C99A S2A
EADP C99B S2B
DFIX     1.666   0.020 C48 C49A
DFIX     1.613   0.020 C49A C50
DFIX     1.362   0.020 C50 C51
DFIX     1.645   0.020 C51 C49B
DFIX     1.687   0.020 C49B C48
DANG     2.347   0.040 C48 C50
DANG     2.408   0.040 C48 C51
DANG     2.509   0.040 C49A C51
DANG     2.895   0.040 C49A C49B
DANG     2.544   0.040 C50 C49B
 In addition, due to the operation of EXYZ, the H atoms on the five-membered rings can't be added.
;

_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)+(0.0519P)²+62.5136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   0.03(3)
_refine_ls_number_reflns         12170
_refine_ls_number_parameters     818
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1662
_refine_ls_wR_factor_gt          0.1643
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.211
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3064(17) -0.0769(8) 0.9124(5) 0.073(5) Uani 1 1 d . . .
C2 C 0.4211(18) -0.0540(9) 0.9248(5) 0.074(5) Uani 1 1 d . . .
C4 C 0.4493(12) -0.0646(5) 0.8515(4) 0.037(3) Uani 1 1 d . . .
C5 C 0.5023(10) -0.0666(5) 0.8077(3) 0.029(2) Uani 1 1 d . . .
C6 C 0.6190(9) -0.0114(5) 0.7312(3) 0.024(2) Uani 1 1 d . . .
C7 C 0.6952(9) -0.0474(4) 0.7655(3) 0.020(2) Uani 1 1 d . . .
H7 H 0.6991 -0.0899 0.7571 0.024 Uiso 1 1 calc R . .
C8 C 0.8391(10) -0.0246(4) 0.7743(3) 0.0187(19) Uani 1 1 d . . .
H8 H 0.8364 0.0178 0.7831 0.022 Uiso 1 1 calc R . .
C9 C 0.9435(11) -0.0333(5) 0.7389(3) 0.026(2) Uani 1 1 d . . .
C10 C 0.8925(14) -0.0405(7) 0.8482(5) 0.051(3) Uani 1 1 d . . .
C11 C 0.9115(10) -0.0883(6) 0.8791(3) 0.038(3) Uani 1 1 d . . .
C15 C 0.725(3) -0.2138(11) 0.7237(10) 0.151(12) Uani 1 1 d U . .
H15A H 0.8022 -0.2321 0.7105 0.181 Uiso 1 1 calc R . .
H15B H 0.6530 -0.2427 0.7256 0.181 Uiso 1 1 calc R . .
H15C H 0.7486 -0.2001 0.7516 0.181 Uiso 1 1 calc R . .
C16 C 0.717(2) -0.2452(9) 0.6032(7) 0.097(5) Uani 1 1 d U . .
H16A H 0.6465 -0.2486 0.6241 0.117 Uiso 1 1 calc R . .
H16B H 0.7673 -0.2821 0.6022 0.117 Uiso 1 1 calc R . .
H16C H 0.6773 -0.2374 0.5759 0.117 Uiso 1 1 calc R . .
C17 C 0.696(3) -0.0357(11) 0.5359(8) 0.112(7) Uani 1 1 d U . .
H17A H 0.6514 -0.0065 0.5534 0.168 Uiso 1 1 calc R . .
H17B H 0.6305 -0.0561 0.5186 0.168 Uiso 1 1 calc R . .
H17C H 0.7607 -0.0158 0.5180 0.168 Uiso 1 1 calc R . .
C19 C 0.527(2) -0.1853(8) 0.4428(6) 0.087(5) Uani 1 1 d DU . .
C20 C 0.5052(19) -0.1335(9) 0.4206(5) 0.080(5) Uani 1 1 d DU . .
C21 C 0.3744(14) -0.1220(6) 0.4825(4) 0.048(3) Uani 1 1 d DU . .
C23 C 0.2839(13) -0.0961(5) 0.5155(4) 0.039(3) Uani 1 1 d . . .
C24 C 0.4388(11) -0.0870(6) 0.6225(3) 0.033(2) Uani 1 1 d . . .
C25 C 0.3008(10) -0.1169(5) 0.6255(3) 0.031(2) Uani 1 1 d . . .
H25 H 0.2546 -0.1017 0.6509 0.037 Uiso 1 1 calc R . .
C26 C 0.2154(10) -0.1034(4) 0.5875(3) 0.025(2) Uani 1 1 d . . .
H26 H 0.2081 -0.0596 0.5845 0.030 Uiso 1 1 calc R . .
C27 C 0.0738(10) -0.1294(5) 0.5913(4) 0.035(3) Uani 1 1 d . . .
C29 C 0.5747(16) 0.1240(7) 0.5682(5) 0.065(4) Uani 1 1 d . . .
H29A H 0.5263 0.1492 0.5486 0.077 Uiso 1 1 calc R . .
H29B H 0.6427 0.1016 0.5532 0.077 Uiso 1 1 calc R . .
H29C H 0.6169 0.1487 0.5894 0.077 Uiso 1 1 calc R . .
C31 C -0.2106(14) 0.2660(6) 0.4764(5) 0.055(3) Uani 1 1 d U . .
C32 C -0.1186(12) 0.1965(6) 0.5289(4) 0.038(3) Uani 1 1 d U . .
C33 C -0.2515(14) 0.2826(6) 0.5152(5) 0.056(3) Uani 1 1 d U . .
C34 C -0.0437(11) 0.1481(4) 0.5490(3) 0.026(2) Uani 1 1 d U . .
C35 C -0.0845(16) 0.1517(6) 0.7178(4) 0.049(3) Uani 1 1 d U . .
C36 C -0.0918(14) 0.2110(6) 0.7368(5) 0.055(3) Uani 1 1 d U . .
C38 C -0.080(2) 0.2955(10) 0.7825(7) 0.087(5) Uani 1 1 d U . .
C39 C -0.1135(19) 0.3220(8) 0.7464(7) 0.080(5) Uani 1 1 d U . .
C40 C 0.1520(11) 0.1184(5) 0.6229(3) 0.028(2) Uani 1 1 d . . .
C41 C -0.0726(9) 0.0933(4) 0.6563(3) 0.0205(19) Uani 1 1 d . . .
H41 H -0.0240 0.0653 0.6749 0.025 Uiso 1 1 calc R . .
C42 C 0.0053(9) 0.0990(4) 0.6149(3) 0.0195(19) Uani 1 1 d . . .
H42 H 0.0035 0.0606 0.5996 0.023 Uiso 1 1 calc R . .
C44 C 0.507(2) 0.2251(9) 0.6664(7) 0.102(6) Uani 1 1 d U . .
H44A H 0.4797 0.2378 0.6942 0.153 Uiso 1 1 calc R . .
H44B H 0.4890 0.2566 0.6463 0.153 Uiso 1 1 calc R . .
H44C H 0.6025 0.2165 0.6665 0.153 Uiso 1 1 calc R . .
C46 C -0.2153(10) 0.0683(4) 0.6485(3) 0.0188(19) Uani 1 1 d U . .
C47 C 0.3638(11) -0.2055(7) 0.6636(5) 0.052(4) Uani 1 1 d . . .
C48 C 0.3659(15) -0.2695(6) 0.6639(5) 0.088(6) Uani 1 1 d DU . .
C50 C 0.339(2) -0.3724(7) 0.6424(7) 0.128(8) Uani 1 1 d DU . .
C51 C 0.390(3) -0.3779(7) 0.6815(7) 0.140(9) Uani 1 1 d DU . .
C54 C 0.212(3) 0.0692(10) 0.8334(7) 0.131(10) Uani 1 1 d . . .
H54A H 0.2911 0.0857 0.8468 0.196 Uiso 1 1 calc R . .
H54B H 0.1692 0.0412 0.8523 0.196 Uiso 1 1 calc R . .
H54C H 0.1503 0.1011 0.8266 0.196 Uiso 1 1 calc R . .
C56 C 0.218(2) 0.1334(10) 0.7338(7) 0.101(5) Uani 1 1 d U . .
H56A H 0.1816 0.1246 0.7614 0.121 Uiso 1 1 calc R . .
H56B H 0.1585 0.1184 0.7123 0.121 Uiso 1 1 calc R . .
H56C H 0.2286 0.1762 0.7307 0.121 Uiso 1 1 calc R . .
O1 O 0.4451(8) -0.0878(4) 0.7769(2) 0.0378(17) Uani 1 1 d . . .
O2 O 0.6267(7) -0.0424(3) 0.8058(2) 0.0279(16) Uani 1 1 d . . .
O1W O 0.3047(11) 0.0658(5) 0.5254(3) 0.066(3) Uani 1 1 d U . .
H103 H 0.2257 0.0801 0.5290 0.079 Uiso 1 1 d R . .
H104 H 0.2960 0.0295 0.5171 0.079 Uiso 1 1 d R . .
O3 O 0.5641(7) 0.0371(3) 0.7409(2) 0.0287(16) Uani 1 1 d . . .
O4 O 0.6110(7) -0.0330(3) 0.6935(2) 0.0262(16) Uani 1 1 d . . .
O5 O 0.9009(7) -0.0537(4) 0.7044(2) 0.0338(17) Uani 1 1 d . . .
O6 O 1.0596(8) -0.0218(4) 0.7472(2) 0.0420(19) Uani 1 1 d . . .
O7 O 0.8878(7) -0.0618(4) 0.8091(2) 0.0390(19) Uani 1 1 d . . .
O8 O 0.8800(11) 0.0113(5) 0.8569(3) 0.064(3) Uani 1 1 d . . .
O9 O 0.6808(9) -0.1630(4) 0.6984(3) 0.044(2) Uani 1 1 d U . .
O10 O 0.8076(10) -0.1954(4) 0.6147(4) 0.063(3) Uani 1 1 d U . .
O11 O 0.7645(11) -0.0787(5) 0.5623(3) 0.069(3) Uani 1 1 d U . .
O12 O 0.5404(8) -0.1207(4) 0.6211(3) 0.0400(19) Uani 1 1 d . . .
O13 O 0.4387(8) -0.0299(4) 0.6192(2) 0.0353(18) Uani 1 1 d . . .
O14 O 0.2139(12) -0.0514(5) 0.5098(3) 0.067(3) Uani 1 1 d . . .
O15 O 0.2864(8) -0.1270(3) 0.5509(2) 0.0331(17) Uani 1 1 d . . .
O16 O 0.0060(8) -0.1040(5) 0.6207(3) 0.049(2) Uani 1 1 d . . .
O17 O 0.0350(9) -0.1697(4) 0.5675(3) 0.057(3) Uani 1 1 d . . .
O18 O 0.3075(8) -0.1817(4) 0.6281(3) 0.040(2) Uani 1 1 d . . .
O19 O 0.3056(7) -0.0253(4) 0.7066(2) 0.0350(19) Uani 1 1 d . . .
H101 H 0.3585 -0.0370 0.7263 0.042 Uiso 1 1 d R . .
H102 H 0.2357 -0.0103 0.7183 0.042 Uiso 1 1 d R . .
O20 O 0.4855(9) 0.0844(5) 0.5874(3) 0.058(3) Uani 1 1 d . . .
O23 O 0.0342(9) 0.1149(4) 0.5309(2) 0.0390(19) Uani 1 1 d . . .
O24 O -0.0678(7) 0.1455(3) 0.5905(2) 0.0233(15) Uani 1 1 d . . .
O25 O -0.0776(7) 0.1507(3) 0.6765(2) 0.0257(15) Uani 1 1 d U . .
O26 O -0.0992(13) 0.1038(4) 0.7392(3) 0.068(3) Uani 1 1 d U . .
O27 O 0.2186(7) 0.0774(3) 0.6416(3) 0.0335(17) Uani 1 1 d . . .
O28 O 0.1929(7) 0.1685(3) 0.6123(2) 0.0329(18) Uani 1 1 d . . .
O30 O 0.4311(10) 0.1697(4) 0.6541(4) 0.061(3) Uani 1 1 d . . .
O31 O -0.2178(8) 0.0187(3) 0.6279(2) 0.0303(16) Uani 1 1 d . . .
O32 O -0.3137(6) 0.0951(3) 0.6632(3) 0.0324(17) Uani 1 1 d . . .
O33 O 0.4030(9) -0.1742(5) 0.6936(3) 0.056(3) Uani 1 1 d . . .
O34 O 0.3354(11) 0.1077(4) 0.7300(3) 0.060(2) Uani 1 1 d U . .
O35 O 0.2494(15) 0.0397(5) 0.7966(4) 0.089(4) Uani 1 1 d . . .
H302 H 0.1979 0.0236 0.7782 0.106 Uiso 1 1 d R . .
La1 La 0.44844(6) 0.05610(3) 0.667248(19) 0.02643(15) Uani 1 1 d U . .
La2 La 0.77127(6) -0.08813(3) 0.643075(19) 0.02738(15) Uani 1 1 d . . .
C22A C 0.4030(13) -0.0826(6) 0.4384(3) 0.068(3) Uani 0.30 1 d P . .
C22B C 0.4526(7) -0.1891(3) 0.4895(2) 0.110(2) Uani 0.70 1 d P . .
S3A S 0.4030(13) -0.0826(6) 0.4384(3) 0.068(3) Uani 0.30 1 d P . .
S3B S 0.4526(7) -0.1891(3) 0.4895(2) 0.110(2) Uani 0.70 1 d P . .
C30A C -0.2074(9) 0.2455(4) 0.5544(4) 0.065(3) Uani 0.33 1 d P . .
C30B C -0.1104(5) 0.2032(3) 0.47411(15) 0.0685(15) Uani 0.67 1 d P . .
S4B S -0.1104(5) 0.2032(3) 0.47411(15) 0.0685(15) Uani 0.67 1 d P . .
S4A S -0.2074(9) 0.2455(4) 0.5544(4) 0.065(3) Uani 0.33 1 d P . .
C37A C -0.0674(13) 0.2251(5) 0.7860(4) 0.071(3) Uani 0.30 1 d P . .
C37B C -0.1269(7) 0.2724(2) 0.7054(2) 0.0897(19) Uani 0.70 1 d P . .
S5B S -0.1269(7) 0.2724(2) 0.7054(2) 0.0897(19) Uani 0.70 1 d P . .
S5A S -0.0674(13) 0.2251(5) 0.7860(4) 0.071(3) Uani 0.30 1 d P . .
C49A C 0.3193(19) -0.3067(5) 0.6252(6) 0.118(9) Uani 0.25 1 d PD . .
C49B C 0.4219(6) -0.3128(3) 0.70473(18) 0.0954(19) Uani 0.75 1 d PD . .
S6B S 0.4219(6) -0.3128(3) 0.70473(18) 0.0954(19) Uani 0.75 1 d P . .
S6A S 0.3193(19) -0.3067(5) 0.6252(6) 0.118(9) Uani 0.25 1 d P . .
C3A C 0.5307(10) -0.0436(4) 0.8913(2) 0.057(2) Uani 0.33 1 d P . .
C3B C 0.2889(5) -0.0894(3) 0.86024(16) 0.0706(13) Uani 0.67 1 d P . .
S1B S 0.2889(5) -0.0894(3) 0.86024(16) 0.0706(13) Uani 0.67 1 d P . .
S1A S 0.5307(10) -0.0436(4) 0.8913(2) 0.057(2) Uani 0.33 1 d P . .
C97 C 0.941(2) -0.1476(8) 0.9426(5) 0.069(5) Uani 1 1 d . . .
C98 C 0.931(2) -0.1876(8) 0.9077(6) 0.084(6) Uani 1 1 d . . .
C99A C 0.9040(10) -0.1558(5) 0.8684(4) 0.101(4) Uani 0.40 1 d P . .
C99B C 0.9290(7) -0.0765(3) 0.93163(16) 0.0703(16) Uani 0.60 1 d P . .
S2B S 0.9290(7) -0.0765(3) 0.93163(16) 0.0703(16) Uani 0.60 1 d P . .
S2A S 0.9040(10) -0.1558(5) 0.8684(4) 0.101(4) Uani 0.40 1 d P . .


_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
C1 C2 1.30(2) . ?
C1 C3B 1.674(17) . ?
C2 C3A 1.532(17) . ?
C4 C5 1.476(15) . ?
C4 C3A 1.560(15) . ?
C4 C3B 1.701(12) . ?
C5 O1 1.216(13) . ?
C5 O2 1.343(12) . ?
C6 O3 1.243(12) . ?
C6 O4 1.283(12) . ?
C6 C7 1.540(13) . ?
C6 La1 3.023(10) . ?
C7 O2 1.444(11) . ?
C7 C8 1.535(13) . ?
C8 O7 1.453(11) . ?
C8 C9 1.533(14) . ?
C9 O6 1.204(13) . ?
C9 O5 1.251(13) . ?
C10 O8 1.189(16) . ?
C10 O7 1.319(16) . ?
C10 C11 1.451(18) . ?
C11 C99A 1.537(19) . ?
C11 C99B 1.683(12) . ?
C15 O9 1.44(2) . ?
C16 O10 1.47(2) . ?
C17 O11 1.43(2) . ?
C19 C20 1.361(16) . ?
C19 C22B 1.645(18) . ?
C20 C22A 1.62(2) . ?
C21 C23 1.488(17) . ?
C21 C22A 1.665(16) . ?
C21 C22B 1.691(16) . ?
C23 O14 1.222(15) . ?
C23 O15 1.310(13) . ?
C24 O12 1.253(15) . ?
C24 O13 1.270(14) . ?
C24 C25 1.519(15) . ?
C25 O18 1.441(14) . ?
C25 C26 1.495(14) . ?
C26 O15 1.447(12) . ?
C26 C27 1.518(14) . ?
C27 O17 1.227(14) . ?
C27 O16 1.276(14) . ?
C29 O20 1.384(15) . ?
C31 C33 1.34(2) . ?
C31 C30B 1.711(16) . ?
C32 C34 1.451(15) . ?
C32 C30A 1.611(17) . ?
C32 C30B 1.735(12) . ?
C33 C30A 1.548(15) . ?
C34 O23 1.208(13) . ?
C34 O24 1.329(12) . ?
C35 O26 1.267(16) . ?
C35 O25 1.305(14) . ?
C35 C36 1.446(18) . ?
C36 C37A 1.596(19) . ?
C36 C37B 1.719(17) . ?
C38 C39 1.32(3) . ?
C38 C37A 1.57(2) . ?
C39 C37B 1.701(19) . ?
C40 O28 1.228(13) . ?
C40 O27 1.269(12) . ?
C40 C42 1.534(14) . ?
C41 O25 1.424(11) . ?
C41 C42 1.518(13) . ?
C41 C46 1.535(13) . ?
C42 O24 1.476(10) . ?
C44 O30 1.49(2) . ?
C46 O32 1.231(11) . ?
C46 O31 1.278(11) . ?
C47 O33 1.233(18) . ?
C47 O18 1.357(14) . ?
C47 C48 1.42(2) . ?
C48 C49A 1.542(16) . ?
C48 C49B 1.696(12) . ?
C50 C51 1.337(17) . ?
C50 C49A 1.567(15) . ?
C51 C49B 1.651(16) . ?
C54 O35 1.38(2) . ?
C56 O34 1.29(2) . ?
O3 La1 2.619(7) . ?
O4 La2 2.554(7) . ?
O4 La1 2.678(7) . ?
O5 La2 2.439(7) . ?
O9 La2 2.569(9) . ?
O10 La2 2.568(9) . ?
O11 La2 2.554(9) . ?
O12 La2 2.492(8) . ?
O13 La1 2.437(8) . ?
O16 La2 2.450(8) 1_455 ?
O19 La1 2.606(7) . ?
O20 La1 2.617(9) . ?
O27 La1 2.458(7) . ?
O30 La1 2.560(9) . ?
O31 La2 2.420(7) 1_455 ?
O32 La1 2.508(6) 1_455 ?
O34 La1 2.543(10) . ?
La1 O32 2.508(6) 1_655 ?
La2 O31 2.420(7) 1_655 ?
La2 O16 2.450(8) 1_655 ?
C97 C98 1.42(2) . ?
C97 C99B 1.619(17) . ?
C98 C99A 1.448(19) . ?

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
C2 C1 C3B 116.8(12) . . ?
C1 C2 C3A 117.8(14) . . ?
C5 C4 C3A 125.2(9) . . ?
C5 C4 C3B 118.2(9) . . ?
C3A C4 C3B 116.6(7) . . ?
O1 C5 O2 123.0(10) . . ?
O1 C5 C4 126.2(10) . . ?
O2 C5 C4 110.7(9) . . ?
O3 C6 O4 121.6(9) . . ?
O3 C6 C7 119.3(9) . . ?
O4 C6 C7 119.1(9) . . ?
O3 C6 La1 59.4(5) . . ?
O4 C6 La1 62.2(5) . . ?
C7 C6 La1 175.4(6) . . ?
O2 C7 C8 104.4(7) . . ?
O2 C7 C6 110.4(7) . . ?
C8 C7 C6 114.2(7) . . ?
O7 C8 C9 104.8(7) . . ?
O7 C8 C7 104.9(7) . . ?
C9 C8 C7 116.8(8) . . ?
O6 C9 O5 125.8(10) . . ?
O6 C9 C8 117.3(9) . . ?
O5 C9 C8 116.9(9) . . ?
O8 C10 O7 123.9(13) . . ?
O8 C10 C11 124.4(14) . . ?
O7 C10 C11 111.7(12) . . ?
C10 C11 C99A 123.9(11) . . ?
C10 C11 C99B 123.9(11) . . ?
C99A C11 C99B 111.9(8) . . ?
C20 C19 C22B 115.7(14) . . ?
C19 C20 C22A 120.6(14) . . ?
C23 C21 C22A 118.8(11) . . ?
C23 C21 C22B 121.6(9) . . ?
C22A C21 C22B 119.6(9) . . ?
O14 C23 O15 124.2(11) . . ?
O14 C23 C21 123.4(11) . . ?
O15 C23 C21 112.4(10) . . ?
O12 C24 O13 126.3(11) . . ?
O12 C24 C25 117.5(11) . . ?
O13 C24 C25 116.0(11) . . ?
O18 C25 C26 105.6(8) . . ?
O18 C25 C24 113.4(9) . . ?
C26 C25 C24 111.7(8) . . ?
O15 C26 C25 106.9(8) . . ?
O15 C26 C27 111.8(8) . . ?
C25 C26 C27 112.5(9) . . ?
O17 C27 O16 126.9(10) . . ?
O17 C27 C26 121.2(10) . . ?
O16 C27 C26 111.9(9) . . ?
C33 C31 C30B 116.0(9) . . ?
C34 C32 C30A 124.1(10) . . ?
C34 C32 C30B 118.3(10) . . ?
C30A C32 C30B 117.7(7) . . ?
C31 C33 C30A 119.8(12) . . ?
O23 C34 O24 123.6(9) . . ?
O23 C34 C32 124.8(10) . . ?
O24 C34 C32 111.7(10) . . ?
O26 C35 O25 121.3(12) . . ?
O26 C35 C36 122.6(12) . . ?
O25 C35 C36 115.6(12) . . ?
C35 C36 C37A 124.9(13) . . ?
C35 C36 C37B 119.5(12) . . ?
C37A C36 C37B 115.7(9) . . ?
C39 C38 C37A 121.4(16) . . ?
C38 C39 C37B 112.7(15) . . ?
O28 C40 O27 127.1(10) . . ?
O28 C40 C42 121.4(9) . . ?
O27 C40 C42 111.4(8) . . ?
O25 C41 C42 109.0(7) . . ?
O25 C41 C46 111.3(7) . . ?
C42 C41 C46 111.1(7) . . ?
O24 C42 C41 104.9(7) . . ?
O24 C42 C40 110.6(7) . . ?
C41 C42 C40 111.3(8) . . ?
O32 C46 O31 126.2(9) . . ?
O32 C46 C41 119.5(8) . . ?
O31 C46 C41 114.2(8) . . ?
O33 C47 O18 122.8(14) . . ?
O33 C47 C48 123.5(12) . . ?
O18 C47 C48 113.6(14) . . ?
C47 C48 C49A 121.6(11) . . ?
C47 C48 C49B 125.1(12) . . ?
C49A C48 C49B 113.2(10) . . ?
C51 C50 C49A 116.6(15) . . ?
C50 C51 C49B 113.7(13) . . ?
C5 O2 C7 115.9(8) . . ?
C6 O3 La1 96.5(6) . . ?
C6 O4 La2 135.7(6) . . ?
C6 O4 La1 92.7(6) . . ?
La2 O4 La1 122.3(2) . . ?
C9 O5 La2 167.9(7) . . ?
C10 O7 C8 120.9(10) . . ?
C15 O9 La2 140.5(12) . . ?
C16 O10 La2 134.2(10) . . ?
C17 O11 La2 130.1(12) . . ?
C24 O12 La2 123.5(7) . . ?
C24 O13 La1 136.9(7) . . ?
C23 O15 C26 118.7(8) . . ?
C27 O16 La2 140.3(7) . 1_455 ?
C47 O18 C25 116.9(10) . . ?
C29 O20 La1 131.5(9) . . ?
C34 O24 C42 117.0(8) . . ?
C35 O25 C41 117.7(8) . . ?
C40 O27 La1 140.4(6) . . ?
C44 O30 La1 137.3(11) . . ?
C46 O31 La2 138.0(6) . 1_455 ?
C46 O32 La1 126.5(6) . 1_455 ?
C56 O34 La1 131.5(12) . . ?
O13 La1 O27 84.9(3) . . ?
O13 La1 O32 106.0(3) . 1_655 ?
O27 La1 O32 141.6(2) . 1_655 ?
O13 La1 O34 144.8(3) . . ?
O27 La1 O34 76.2(3) . . ?
O32 La1 O34 107.3(3) 1_655 . ?
O13 La1 O30 131.9(3) . . ?
O27 La1 O30 72.3(3) . . ?
O32 La1 O30 73.5(3) 1_655 . ?
O34 La1 O30 69.7(3) . . ?
O13 La1 O19 74.4(3) . . ?
O27 La1 O19 77.8(2) . . ?
O32 La1 O19 140.4(2) 1_655 . ?
O34 La1 O19 72.7(3) . . ?
O30 La1 O19 136.3(3) . . ?
O13 La1 O20 66.3(3) . . ?
O27 La1 O20 76.6(3) . . ?
O32 La1 O20 74.8(3) 1_655 . ?
O34 La1 O20 134.5(3) . . ?
O30 La1 O20 67.5(3) . . ?
O19 La1 O20 134.4(3) . . ?
O13 La1 O3 116.1(2) . . ?
O27 La1 O3 136.5(2) . . ?
O32 La1 O3 72.0(2) 1_655 . ?
O34 La1 O3 64.9(3) . . ?
O30 La1 O3 109.3(3) . . ?
O19 La1 O3 72.8(2) . . ?
O20 La1 O3 145.9(2) . . ?
O13 La1 O4 68.7(2) . . ?
O27 La1 O4 143.0(2) . . ?
O32 La1 O4 73.0(2) 1_655 . ?
O34 La1 O4 110.9(3) . . ?
O30 La1 O4 144.8(3) . . ?
O19 La1 O4 70.6(2) . . ?
O20 La1 O4 112.9(3) . . ?
O3 La1 O4 49.2(2) . . ?
O13 La1 C6 92.7(3) . . ?
O27 La1 C6 146.1(2) . . ?
O32 La1 C6 71.4(2) 1_655 . ?
O34 La1 C6 87.2(3) . . ?
O30 La1 C6 129.3(3) . . ?
O19 La1 C6 69.0(2) . . ?
O20 La1 C6 132.9(3) . . ?
O3 La1 C6 24.1(2) . . ?
O4 La1 C6 25.1(3) . . ?
O31 La2 O5 80.0(3) 1_655 . ?
O31 La2 O16 92.4(3) 1_655 1_655 ?
O5 La2 O16 77.0(3) . 1_655 ?
O31 La2 O12 105.7(3) 1_655 . ?
O5 La2 O12 142.3(2) . . ?
O16 La2 O12 138.3(3) 1_655 . ?
O31 La2 O11 74.0(3) 1_655 . ?
O5 La2 O11 140.9(3) . . ?
O16 La2 O11 75.6(3) 1_655 . ?
O12 La2 O11 74.0(3) . . ?
O31 La2 O4 71.5(2) 1_655 . ?
O5 La2 O4 71.6(2) . . ?
O16 La2 O4 146.6(3) 1_655 . ?
O12 La2 O4 75.1(2) . . ?
O11 La2 O4 124.3(3) . . ?
O31 La2 O10 146.3(3) 1_655 . ?
O5 La2 O10 119.5(3) . . ?
O16 La2 O10 68.5(3) 1_655 . ?
O12 La2 O10 76.3(3) . . ?
O11 La2 O10 74.5(4) . . ?
O4 La2 O10 138.3(3) . . ?
O31 La2 O9 141.6(3) 1_655 . ?
O5 La2 O9 81.3(3) . . ?
O16 La2 O9 115.6(3) 1_655 . ?
O12 La2 O9 71.4(3) . . ?
O11 La2 O9 136.0(3) . . ?
O4 La2 O9 70.9(3) . . ?
O10 La2 O9 71.7(3) . . ?
C20 C22A C21 91.6(10) . . ?
C19 C22B C21 92.3(9) . . ?
C33 C30A C32 96.6(10) . . ?
C31 C30B C32 90.0(7) . . ?
C38 C37A C36 96.7(12) . . ?
C39 C37B C36 93.4(9) . . ?
C48 C49A C50 100.9(11) . . ?
C51 C49B C48 95.5(9) . . ?
C2 C3A C4 98.3(10) . . ?
C1 C3B C4 90.5(8) . . ?
C98 C97 C99B 116.0(11) . . ?
C97 C98 C99A 111.8(15) . . ?
C98 C99A C11 106.1(12) . . ?
C97 C99B C11 93.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.394
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.155
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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#Tb
_database_code_depnum_ccdc_archive 'CCDC 1023767'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        4#Tb
_chemical_name_common            Tb
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H18 O30 S6 Tb2, C H3 O '
_chemical_formula_sum            'C45 H44 Tb2 O31 S6'
_chemical_formula_weight         1567.84

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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   'P 21 21 21 '
_symmetry_space_group_name_Hall  ' P 2ac 2ab '

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

_cell_length_a                   9.717(5)
_cell_length_b                   21.798(5)
_cell_length_c                   30.791(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6522(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18595
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3060
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_process_details   sadabs(Sheldrick,1996)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18595
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11522
_reflns_number_gt                10519
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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.
FLAT     0.100 C46 C48 C60 C59
ISOR  0.01 C10 C12 C60 C35 O25 C21 C46 C48 C59 O5 C19 O22 C29 C33 C41 C42 C3 C11 C26 O30 C38 c37 O6 c18 C53 S5A C60A
DELU     0.010   0.010 C2 C3 C4 C5
SIMU     0.040   0.080   3.800 C2 C3 C4 C5
DELU     0.010   0.010 C9 C10 C11 C12 O2 O3
SIMU     0.040   0.080   3.800 C9 C10 C11 C12 O2 O3
DELU  0.010 0.010 C22 C24 C25 C26 C26
SIMU  0.040 0.080 3.800 C22 C24 C25 C26 C26
DELU     0.010   0.010 C29 C34 O24 O25
SIMU     0.040   0.080   3.800 C29 C34 O24 O25
DELU     0.010   0.010 C22 C24 C25 C26
SIMU     0.040   0.080   3.800 C22 C24 C25 C26
DELU     0.010   0.010 C32 C33 C41 C42
SIMU     0.040   0.080   3.800 C32 C33 C41 C42
DELU     0.010   0.010 C19 O7
SIMU     0.040   0.080   3.800 C19 O7
DELU     0.010   0.010 C59 C60
SIMU     0.040   0.080   3.800 C59 C60
FLAT  0.100 C35 C37 C44 S6B C53
EXYZ C7A S1A
EXYZ C7B S1B
EADP C7A S1A
EADP C7B S1B
EXYZ C3A S2A
EXYZ C3B S2B
EADP C3A S2A
EADP C3B S2B
EXYZ C26A S4A
EXYZ C26B S4B
EADP C26A S4A
EADP C26B S4B
EXYZ C60A S5A
EXYZ C60B S5B
EADP C60A S5A
EADP C60B S5B
EXYZ C37A S6A
EXYZ C37B S6B
EADP C37A S6A
EADP C37B S6B
EXYZ C33A S7A
EXYZ C33B S7B
EADP C33A S7A
EADP C33B S7B
FLAT     0.100 C35 C44 C53 C37A C37B S6B S6A
DFIX     1.624   0.020 C46 C60A
DFIX     1.572   0.020 C60A C59
DFIX     1.320   0.020 C59 C48
DFIX     1.599   0.020 C48 C60B
DFIX     1.650   0.020 C60B C46
DANG     2.396   0.040 C46 C59
DANG     2.423   0.040 C46 C48
DANG     2.735   0.040 C60A C60B
DANG     2.476   0.040 C60A C48
DANG     2.473   0.040 C60B C59
During the refinement,c37a, c37b, s6a, s6b are highly disordered, and these atoms are refined by isotropic. 
 In addition, due to the operation of EXYZ, the H atoms on the five-membered rings can't be added.
;

_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)+(0.0928P)²+101.7205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_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   0.98(2)
_refine_ls_number_reflns         11522
_refine_ls_number_parameters     748
_refine_ls_number_restraints     393
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0735
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1876
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0258(19) 0.1382(8) 0.5483(5) 0.041(4) Uani 1 1 d . . .
C2 C 0.0961(16) 0.1851(8) 0.5251(5) 0.042(4) Uani 1 1 d U . .
C4 C 0.220(2) 0.2753(10) 0.5038(8) 0.064(5) Uani 1 1 d U . .
C5 C 0.190(2) 0.2500(10) 0.4692(7) 0.060(5) Uani 1 1 d U . .
C6 C 0.0769(17) 0.2192(7) 0.7354(6) 0.040(4) Uani 1 1 d . . .
C8 C 0.082(2) 0.3062(12) 0.7794(10) 0.077(7) Uani 1 1 d . . .
C9 C -0.1695(14) 0.1123(7) 0.6255(4) 0.028(3) Uani 1 1 d U . .
C10 C -0.0195(12) 0.0936(6) 0.6166(4) 0.020(2) Uani 1 1 d U . .
H10 H -0.0168 0.0535 0.6022 0.024 Uiso 1 1 calc R . .
C11 C 0.0624(12) 0.0913(6) 0.6591(4) 0.017(2) Uani 1 1 d U . .
H11 H 0.0140 0.0642 0.6794 0.021 Uiso 1 1 calc R . .
C12 C 0.2104(13) 0.0656(5) 0.6521(4) 0.019(2) Uani 1 1 d U . .
C13 C 0.118(2) 0.3296(9) 0.7394(12) 0.082(9) Uani 1 1 d . . .
C14 C 0.0605(16) 0.1555(7) 0.7213(5) 0.035(3) Uani 1 1 d . . .
C15 C 0.0481(14) -0.0359(6) 0.7354(4) 0.021(3) Uani 1 1 d . . .
C16 C 0.1520(12) -0.0255(6) 0.7738(4) 0.021(3) Uani 1 1 d . . .
H16 H 0.1603 0.0185 0.7799 0.025 Uiso 1 1 calc R . .
C17 C 0.2930(13) -0.0525(7) 0.7656(4) 0.025(3) Uani 1 1 d . . .
H17 H 0.2843 -0.0956 0.7569 0.030 Uiso 1 1 calc R . .
C18 C 0.3758(14) -0.0178(6) 0.7322(4) 0.023(3) Uani 1 1 d U . .
C19 C 0.418(3) 0.1552(14) 0.5898(9) 0.093(8) Uani 1 1 d U . .
H19A H 0.4502 0.1913 0.5751 0.139 Uiso 1 1 calc R . .
H19B H 0.3364 0.1648 0.6060 0.139 Uiso 1 1 calc R . .
H19C H 0.3979 0.1239 0.5689 0.139 Uiso 1 1 calc R . .
C20 C 0.0939(19) -0.0245(13) 0.8477(6) 0.064(6) Uani 1 1 d . . .
C21 C 0.4865(14) -0.0737(7) 0.8099(5) 0.034(3) Uani 1 1 d U . .
C22 C 0.5428(16) -0.0709(7) 0.8529(5) 0.037(3) Uani 1 1 d U . .
C24 C 0.695(2) -0.0782(11) 0.9154(8) 0.072(6) Uani 1 1 d U . .
C25 C 0.581(2) -0.0533(11) 0.9286(6) 0.063(5) Uani 1 1 d U . .
C27 C 0.5542(13) -0.0716(6) 0.6181(4) 0.024(3) Uani 1 1 d . . .
C28 C 0.6965(14) -0.1028(6) 0.6218(4) 0.024(3) Uani 1 1 d . . .
H28 H 0.7430 -0.0867 0.6476 0.029 Uiso 1 1 calc R . .
C29 C 0.7847(14) -0.0904(6) 0.5833(4) 0.026(3) Uani 1 1 d U . .
H29 H 0.7962 -0.0459 0.5806 0.031 Uiso 1 1 calc R . .
C30 C 0.9246(15) -0.1187(7) 0.5887(5) 0.037(4) Uani 1 1 d . . .
C31 C 0.6374(16) -0.1892(8) 0.6639(5) 0.038(4) Uani 1 1 d . . .
C32 C 0.6398(19) -0.2556(11) 0.6650(7) 0.066(6) Uani 1 1 d U . .
C34 C 0.754(3) -0.0890(11) 0.5077(5) 0.071(5) Uani 1 1 d U . .
C35 C 0.689(3) -0.1254(11) 0.4698(8) 0.092(7) Uani 1 1 d DU . .
C38 C 0.305(3) -0.2147(15) 0.5800(10) 0.112(8) Uani 1 1 d DU . .
H38A H 0.2695 -0.2531 0.5697 0.168 Uiso 1 1 calc R . .
H38B H 0.3855 -0.2220 0.5974 0.168 Uiso 1 1 calc R . .
H38C H 0.3295 -0.1894 0.5556 0.168 Uiso 1 1 calc R . .
C41 C 0.681(3) -0.3598(13) 0.6481(10) 0.092(7) Uani 1 1 d U . .
C42 C 0.633(3) -0.3561(14) 0.6916(10) 0.088(7) Uani 1 1 d U . .
C44 C 0.521(3) -0.1666(14) 0.4221(10) 0.119(9) Uani 1 1 d DU . .
C46 C 0.066(2) -0.0568(8) 0.8851(5) 0.079(7) Uani 1 1 d DU . .
C48 C 0.060(3) -0.1364(10) 0.9427(6) 0.094(8) Uani 1 1 d DU . .
C53 C 0.599(3) -0.1340(15) 0.4017(10) 0.142(10) Uani 1 1 d DU . .
C59 C 0.043(4) -0.0825(11) 0.9601(7) 0.134(12) Uani 1 1 d DU . .
C88 C 0.730(2) 0.0537(15) 0.8108(7) 0.093(9) Uani 1 1 d . . .
H88A H 0.7833 0.0500 0.8369 0.140 Uiso 1 1 calc R . .
H88B H 0.7348 0.0160 0.7948 0.140 Uiso 1 1 calc R . .
H88C H 0.6358 0.0621 0.8182 0.140 Uiso 1 1 calc R . .
O1 O -0.0506(15) 0.1014(7) 0.5310(3) 0.055(3) Uani 1 1 d . . .
O2 O 0.0531(10) 0.1383(4) 0.5909(3) 0.026(2) Uani 1 1 d U . .
O3 O 0.0676(8) 0.1501(4) 0.6773(3) 0.0228(18) Uani 1 1 d U . .
O4 O 0.0458(19) 0.1121(5) 0.7445(3) 0.062(4) Uani 1 1 d . . .
O5 O -0.2317(9) 0.0739(4) 0.6492(3) 0.031(2) Uani 1 1 d U . .
O6 O -0.2128(12) 0.1602(5) 0.6106(3) 0.039(2) Uani 1 1 d U . .
O7 O 0.5248(13) 0.1332(6) 0.6196(5) 0.061(4) Uani 1 1 d U . .
O8 O 0.2147(10) 0.0172(4) 0.6277(3) 0.0230(19) Uani 1 1 d . . .
O9 O 0.6800(11) -0.0187(5) 0.7082(3) 0.036(3) Uani 1 1 d . . .
H222 H 0.6365 -0.0438 0.7242 0.043 Uiso 1 1 d R . .
H223 H 0.7627 -0.0174 0.7171 0.043 Uiso 1 1 d R . .
O10 O -0.0716(9) -0.0234(5) 0.7433(3) 0.032(2) Uani 1 1 d . . .
O11 O 0.1007(9) -0.0555(5) 0.7002(3) 0.030(2) Uani 1 1 d . . .
O12 O 0.9961(10) -0.0943(6) 0.6185(4) 0.046(3) Uani 1 1 d . . .
O13 O 0.4360(10) 0.0312(4) 0.7434(3) 0.025(2) Uani 1 1 d . . .
O14 O 0.5479(14) -0.0945(7) 0.7785(4) 0.057(3) Uani 1 1 d . . .
O15 O 0.3619(9) -0.0484(5) 0.8076(3) 0.029(2) Uani 1 1 d . . .
O16 O 0.0962(10) -0.0567(5) 0.8113(3) 0.032(2) Uani 1 1 d . . .
O18 O 0.5983(12) -0.1575(8) 0.6922(4) 0.058(4) Uani 1 1 d . . .
O19 O 0.6886(10) -0.1686(5) 0.6257(3) 0.033(2) Uani 1 1 d . . .
O20 O 0.4524(11) -0.1073(5) 0.6170(3) 0.037(2) Uani 1 1 d . . .
O21 O 0.5510(10) -0.0145(4) 0.6166(3) 0.0239(19) Uani 1 1 d . . .
O22 O 0.1980(15) -0.1828(6) 0.6068(5) 0.070(4) Uani 1 1 d DU . .
O23 O 0.3104(11) -0.1622(5) 0.6919(4) 0.038(3) Uani 1 1 d . . .
H224 H 0.3795 -0.1384 0.6903 0.045 Uiso 1 1 d R . .
H225 H 0.3086 -0.1839 0.6690 0.045 Uiso 1 1 d R . .
O24 O 0.7130(11) -0.1125(5) 0.5448(3) 0.033(2) Uani 1 1 d U . .
O25 O 0.865(2) -0.0568(10) 0.5052(6) 0.103(5) Uani 1 1 d U . .
O26 O 0.9590(12) -0.1632(6) 0.5668(4) 0.051(3) Uani 1 1 d . . .
O27 O 0.6123(14) 0.1314(6) 0.7197(4) 0.052(3) Uani 1 1 d . . .
H226 H 0.6330 0.1120 0.7427 0.062 Uiso 1 1 d R . .
H227 H 0.5833 0.1667 0.7271 0.062 Uiso 1 1 d R . .
O28 O 0.3860(8) -0.0353(4) 0.6927(3) 0.0214(19) Uani 1 1 d . . .
O29 O 0.3070(9) 0.0901(5) 0.6702(3) 0.031(2) Uani 1 1 d . . .
O30 O 0.100(3) 0.0302(12) 0.8493(8) 0.121(8) Uani 1 1 d U . .
O31 O 0.2286(13) -0.0679(7) 0.5612(4) 0.061(4) Uani 1 1 d . . .
O88 O 0.7826(17) 0.1022(8) 0.7851(5) 0.077(4) Uani 1 1 d . . .
C7A C 0.045(2) 0.2358(9) 0.7827(9) 0.094(8) Uani 0.25 1 d P . .
C7B C 0.1286(8) 0.2749(2) 0.6994(2) 0.078(2) Uani 0.75 1 d P . .
S1B S 0.1286(8) 0.2749(2) 0.6994(2) 0.078(2) Uani 0.75 1 d P . .
S1A S 0.045(2) 0.2358(9) 0.7827(9) 0.094(8) Uani 0.25 1 d P . .
C3A C 0.1714(11) 0.2420(5) 0.5490(4) 0.085(3) Uani 0.50 1 d P . .
C3B C 0.0957(9) 0.1887(5) 0.4699(3) 0.064(2) Uani 0.50 1 d P . .
S2B S 0.0957(9) 0.1887(5) 0.4699(3) 0.064(2) Uani 0.50 1 d P . .
S2A S 0.1714(11) 0.2420(5) 0.5490(4) 0.085(3) Uani 0.50 1 d P . .
C26A C 0.6960(10) -0.0972(4) 0.8652(3) 0.071(3) Uani 0.50 1 d P . .
C26B C 0.4652(9) -0.0384(4) 0.8944(2) 0.0522(18) Uani 0.50 1 d P . .
S4B S 0.4652(9) -0.0384(4) 0.8944(2) 0.0522(18) Uani 0.50 1 d P . .
S4A S 0.6960(10) -0.0972(4) 0.8652(3) 0.071(3) Uani 0.50 1 d P . .
C60A C 0.062(2) -0.0261(8) 0.9321(6) 0.109(6) Uani 0.33 1 d PDU . .
C60B C 0.0733(8) -0.1305(5) 0.8902(3) 0.097(3) Uani 0.67 1 d PD . .
S5B S 0.0733(8) -0.1305(5) 0.8902(3) 0.097(3) Uani 0.67 1 d P . .
S5A S 0.062(2) -0.0261(8) 0.9321(6) 0.109(6) Uani 0.33 1 d PU . .
C37A C 0.7464(15) -0.0971(6) 0.4200(5) 0.108(4) Uiso 0.50 1 d PD . .
C37B C 0.5546(19) -0.1784(8) 0.4803(5) 0.131(5) Uiso 0.50 1 d PD . .
S6B S 0.5546(19) -0.1784(8) 0.4803(5) 0.131(5) Uiso 0.50 1 d PD . .
S6A S 0.7464(15) -0.0971(6) 0.4200(5) 0.108(4) Uiso 0.50 1 d PD . .
C33A C 0.688(2) -0.2962(7) 0.6301(8) 0.105(7) Uani 0.33 1 d P . .
C33B C 0.5911(8) -0.2923(5) 0.7099(3) 0.109(4) Uani 0.67 1 d P . .
S7B S 0.5911(8) -0.2923(5) 0.7099(3) 0.109(4) Uani 0.67 1 d P . .
S7A S 0.688(2) -0.2962(7) 0.6301(8) 0.105(7) Uani 0.33 1 d P . .
Tb1 Tb 0.54034(6) 0.05440(3) 0.67312(2) 0.02125(16) Uani 1 1 d . . .
Tb2 Tb 0.22413(6) -0.08499(3) 0.64027(2) 0.02179(16) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.22(2) . ?
C1 O2 1.340(18) . ?
C1 C2 1.42(2) . ?
C2 C3A 1.62(2) . ?
C2 C3B 1.703(17) . ?
C4 C5 1.23(3) . ?
C4 C3A 1.64(2) . ?
C5 C3B 1.62(2) . ?
C6 C14 1.46(2) . ?
C6 C7A 1.53(3) . ?
C6 C7B 1.720(18) . ?
C8 C13 1.38(4) . ?
C8 C7A 1.58(3) . ?
C9 O6 1.216(17) . ?
C9 O5 1.262(16) . ?
C9 C10 1.539(18) . ?
C10 O2 1.441(14) . ?
C10 C11 1.533(16) . ?
C11 O3 1.399(15) . ?
C11 C12 1.558(17) . ?
C12 O29 1.215(15) . ?
C12 O8 1.296(15) . ?
C13 C7B 1.72(2) . ?
C14 O4 1.195(19) . ?
C14 O3 1.363(18) . ?
C15 O10 1.219(17) . ?
C15 O11 1.272(16) . ?
C15 C16 1.571(17) . ?
C16 O16 1.447(15) . ?
C16 C17 1.513(17) . ?
C17 O15 1.459(15) . ?
C17 C18 1.509(18) . ?
C18 O13 1.267(16) . ?
C18 O28 1.279(16) . ?
C18 Tb1 2.889(13) . ?
C19 O7 1.46(3) . ?
C20 O30 1.19(3) . ?
C20 O16 1.32(2) . ?
C20 C46 1.38(2) . ?
C21 O14 1.223(19) . ?
C21 O15 1.332(17) . ?
C21 C22 1.43(2) . ?
C22 C26A 1.641(18) . ?
C22 C26B 1.644(18) . ?
C24 C25 1.30(3) . ?
C24 C26A 1.60(3) . ?
C25 C26B 1.58(2) . ?
C27 O21 1.245(16) . ?
C27 O20 1.260(17) . ?
C27 C28 1.545(18) . ?
C28 O19 1.441(17) . ?
C28 C29 1.489(17) . ?
C29 O24 1.457(15) . ?
C29 C30 1.50(2) . ?
C30 O26 1.228(18) . ?
C30 O12 1.269(19) . ?
C31 O18 1.18(2) . ?
C31 O19 1.355(17) . ?
C31 C32 1.45(3) . ?
C32 C33A 1.47(3) . ?
C32 C33B 1.667(19) . ?
C34 O25 1.29(3) . ?
C34 O24 1.31(2) . ?
C34 C35 1.54(3) . ?
C35 C37A 1.74(3) . ?
C35 C37B 1.78(3) . ?
C38 O22 1.501(18) . ?
C41 C42 1.42(4) . ?
C41 C33A 1.50(3) . ?
C42 C33B 1.55(3) . ?
C44 C53 1.215(19) . ?
C44 C37B 1.84(3) . ?
C46 C60A 1.596(17) . ?
C46 C60B 1.615(16) . ?
C48 C59 1.301(14) . ?
C48 C60B 1.628(16) . ?
C53 C37A 1.73(4) . ?
C59 C60A 1.513(17) . ?
C88 O88 1.42(3) . ?
O5 Tb1 2.373(9) 1_455 ?
O7 Tb1 2.385(12) . ?
O8 Tb2 2.263(9) . ?
O9 Tb1 2.355(10) . ?
O11 Tb2 2.293(9) . ?
O12 Tb2 2.323(10) 1_655 ?
O13 Tb1 2.443(8) . ?
O20 Tb2 2.381(11) . ?
O21 Tb1 2.301(9) . ?
O22 Tb2 2.382(13) . ?
O23 Tb2 2.462(10) . ?
O27 Tb1 2.317(12) . ?
O28 Tb2 2.501(8) . ?
O28 Tb1 2.536(9) . ?
O29 Tb1 2.399(9) . ?
O31 Tb2 2.463(11) . ?
Tb1 O5 2.373(9) 1_655 ?
Tb2 O12 2.323(10) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 123.4(14) . . ?
O1 C1 C2 123.3(15) . . ?
O2 C1 C2 113.3(16) . . ?
C1 C2 C3A 122.7(14) . . ?
C1 C2 C3B 122.2(15) . . ?
C3A C2 C3B 114.8(11) . . ?
C5 C4 C3A 117.8(18) . . ?
C4 C5 C3B 119.5(16) . . ?
C14 C6 C7A 119.0(16) . . ?
C14 C6 C7B 120.7(13) . . ?
C7A C6 C7B 120.3(13) . . ?
C13 C8 C7A 118(2) . . ?
O6 C9 O5 128.4(14) . . ?
O6 C9 C10 119.2(12) . . ?
O5 C9 C10 112.4(11) . . ?
O2 C10 C11 103.7(10) . . ?
O2 C10 C9 112.5(10) . . ?
C11 C10 C9 110.4(10) . . ?
O3 C11 C10 109.2(10) . . ?
O3 C11 C12 110.5(9) . . ?
C10 C11 C12 111.9(9) . . ?
O29 C12 O8 126.8(12) . . ?
O29 C12 C11 119.4(10) . . ?
O8 C12 C11 113.7(11) . . ?
C8 C13 C7B 113.6(17) . . ?
O4 C14 O3 122.1(14) . . ?
O4 C14 C6 126.0(15) . . ?
O3 C14 C6 111.9(13) . . ?
O10 C15 O11 128.9(13) . . ?
O10 C15 C16 115.5(11) . . ?
O11 C15 C16 115.6(11) . . ?
O16 C16 C17 106.8(10) . . ?
O16 C16 C15 107.0(10) . . ?
C17 C16 C15 113.6(11) . . ?
O15 C17 C18 109.2(10) . . ?
O15 C17 C16 104.1(10) . . ?
C18 C17 C16 113.7(11) . . ?
O13 C18 O28 118.3(12) . . ?
O13 C18 C17 118.9(11) . . ?
O28 C18 C17 122.8(12) . . ?
O13 C18 Tb1 57.0(6) . . ?
O28 C18 Tb1 61.3(7) . . ?
C17 C18 Tb1 175.9(9) . . ?
O30 C20 O16 124(2) . . ?
O30 C20 C46 119(2) . . ?
O16 C20 C46 116(2) . . ?
O14 C21 O15 123.8(13) . . ?
O14 C21 C22 124.0(13) . . ?
O15 C21 C22 112.2(13) . . ?
C21 C22 C26A 123.1(13) . . ?
C21 C22 C26B 124.2(12) . . ?
C26A C22 C26B 112.7(9) . . ?
C25 C24 C26A 114.6(15) . . ?
C24 C25 C26B 119.1(16) . . ?
O21 C27 O20 126.7(13) . . ?
O21 C27 C28 117.7(12) . . ?
O20 C27 C28 115.6(12) . . ?
O19 C28 C29 106.2(10) . . ?
O19 C28 C27 113.4(11) . . ?
C29 C28 C27 112.0(11) . . ?
O24 C29 C28 108.2(11) . . ?
O24 C29 C30 112.8(11) . . ?
C28 C29 C30 110.9(12) . . ?
O26 C30 O12 125.5(14) . . ?
O26 C30 C29 120.6(14) . . ?
O12 C30 C29 113.8(12) . . ?
O18 C31 O19 124.5(16) . . ?
O18 C31 C32 125.3(16) . . ?
O19 C31 C32 110.2(16) . . ?
C31 C32 C33A 126.2(16) . . ?
C31 C32 C33B 119.7(17) . . ?
C33A C32 C33B 114.0(16) . . ?
O25 C34 O24 121.1(18) . . ?
O25 C34 C35 125(2) . . ?
O24 C34 C35 110(2) . . ?
C34 C35 C37A 110.8(19) . . ?
C34 C35 C37B 119.7(19) . . ?
C37A C35 C37B 128.7(15) . . ?
C42 C41 C33A 108(2) . . ?
C41 C42 C33B 119(2) . . ?
C53 C44 C37B 118(2) . . ?
C20 C46 C60A 123.3(18) . . ?
C20 C46 C60B 125.7(17) . . ?
C60A C46 C60B 109.3(11) . . ?
C59 C48 C60B 110.4(14) . . ?
C44 C53 C37A 128(3) . . ?
C48 C59 C60A 118.9(16) . . ?
C1 O2 C10 116.1(12) . . ?
C14 O3 C11 118.4(10) . . ?
C9 O5 Tb1 138.1(9) . 1_455 ?
C19 O7 Tb1 135.5(14) . . ?
C12 O8 Tb2 134.7(7) . . ?
C15 O11 Tb2 171.9(9) . . ?
C30 O12 Tb2 140.1(9) . 1_655 ?
C18 O13 Tb1 97.2(7) . . ?
C21 O15 C17 116.0(10) . . ?
C20 O16 C16 115.6(14) . . ?
C31 O19 C28 115.0(11) . . ?
C27 O20 Tb2 126.7(9) . . ?
C27 O21 Tb1 128.8(8) . . ?
C38 O22 Tb2 125.4(16) . . ?
C34 O24 C29 115.7(14) . . ?
C18 O28 Tb2 133.9(8) . . ?
C18 O28 Tb1 92.5(8) . . ?
Tb2 O28 Tb1 123.6(3) . . ?
C12 O29 Tb1 127.2(8) . . ?
C6 C7A C8 97(2) . . ?
C13 C7B C6 90.5(13) . . ?
C2 C3A C4 94.8(12) . . ?
C5 C3B C2 92.8(11) . . ?
C24 C26A C22 97.3(11) . . ?
C25 C26B C22 95.9(11) . . ?
C59 C60A C46 100.3(12) . . ?
C46 C60B C48 99.9(10) . . ?
C53 C37A C35 81.9(14) . . ?
C35 C37B C44 82.0(14) . . ?
C32 C33A C41 105.8(19) . . ?
C42 C33B C32 93.2(15) . . ?
O21 Tb1 O27 158.1(4) . . ?
O21 Tb1 O9 83.0(4) . . ?
O27 Tb1 O9 91.8(4) . . ?
O21 Tb1 O5 80.8(3) . 1_655 ?
O27 Tb1 O5 77.3(4) . 1_655 ?
O9 Tb1 O5 74.1(3) . 1_655 ?
O21 Tb1 O7 87.2(4) . . ?
O27 Tb1 O7 85.7(5) . . ?
O9 Tb1 O7 147.2(4) . . ?
O5 Tb1 O7 73.5(4) 1_655 . ?
O21 Tb1 O29 103.1(3) . . ?
O27 Tb1 O29 94.2(4) . . ?
O9 Tb1 O29 141.3(3) . . ?
O5 Tb1 O29 144.4(3) 1_655 . ?
O7 Tb1 O29 71.4(4) . . ?
O21 Tb1 O13 123.6(3) . . ?
O27 Tb1 O13 74.1(4) . . ?
O9 Tb1 O13 72.1(3) . . ?
O5 Tb1 O13 134.4(3) 1_655 . ?
O7 Tb1 O13 137.3(4) . . ?
O29 Tb1 O13 73.0(3) . . ?
O21 Tb1 O28 72.7(3) . . ?
O27 Tb1 O28 126.1(4) . . ?
O9 Tb1 O28 73.2(3) . . ?
O5 Tb1 O28 139.8(3) 1_655 . ?
O7 Tb1 O28 133.0(4) . . ?
O29 Tb1 O28 72.5(3) . . ?
O13 Tb1 O28 52.0(3) . . ?
O21 Tb1 C18 98.3(3) . . ?
O27 Tb1 C18 99.9(4) . . ?
O9 Tb1 C18 70.2(4) . . ?
O5 Tb1 C18 144.1(3) 1_655 . ?
O7 Tb1 C18 142.4(4) . . ?
O29 Tb1 C18 71.1(4) . . ?
O13 Tb1 C18 25.8(3) . . ?
O28 Tb1 C18 26.2(3) . . ?
O8 Tb2 O11 80.8(3) . . ?
O8 Tb2 O12 89.9(4) . 1_455 ?
O11 Tb2 O12 75.9(4) . 1_455 ?
O8 Tb2 O20 100.8(4) . . ?
O11 Tb2 O20 141.9(3) . . ?
O12 Tb2 O20 141.6(3) 1_455 . ?
O8 Tb2 O22 143.4(4) . . ?
O11 Tb2 O22 122.9(5) . . ?
O12 Tb2 O22 72.3(5) 1_455 . ?
O20 Tb2 O22 77.7(4) . . ?
O8 Tb2 O23 142.8(4) . . ?
O11 Tb2 O23 81.4(4) . . ?
O12 Tb2 O23 116.8(4) 1_455 . ?
O20 Tb2 O23 74.8(4) . . ?
O22 Tb2 O23 72.8(5) . . ?
O8 Tb2 O31 71.5(4) . . ?
O11 Tb2 O31 139.7(4) . . ?
O12 Tb2 O31 75.3(4) 1_455 . ?
O20 Tb2 O31 73.6(4) . . ?
O22 Tb2 O31 73.1(5) . . ?
O23 Tb2 O31 137.4(4) . . ?
O8 Tb2 O28 73.1(3) . . ?
O11 Tb2 O28 71.8(3) . . ?
O12 Tb2 O28 145.4(3) 1_455 . ?
O20 Tb2 O28 72.3(3) . . ?
O22 Tb2 O28 137.3(4) . . ?
O23 Tb2 O28 70.4(4) . . ?
O31 Tb2 O28 124.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.722
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.209
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_preparation       Luminescent
