# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Zhang Hongjie'
_publ_contact_author_email       HONGJIE@CIAC.JL.CN

_publ_section_title              
;
Guest inducing p-sulfonatocalix[4]arene into three
dimensional capsule architecture and mixed A-B double layer framework
;
loop_
_publ_author_name
'Zhang Hongjie.'
'Yinyan Li.'
'Feng Zhang.'
'Guoli Zheng.'

# Attachment 'la.cif'

data_3
_database_code_depnum_ccdc_archive 'CCDC 682898'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H70 La1.50 N2 Na0.50 O39.50 S4'
_chemical_formula_weight         1463.00

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'
S S 0.1246 0.1234 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   c2/m

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

_cell_length_a                   20.365(5)
_cell_length_b                   19.046(5)
_cell_length_c                   30.480(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.768(5)
_cell_angle_gamma                90.00
_cell_volume                     11258(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5976
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            29596
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.04
_reflns_number_total             10693
_reflns_number_gt                7339
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

_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.

In order to make some distances chemical reasonable, we apply the restraints
between the O34 O38, O27 O29', O28' O30', and O49 O50. Some Q-peaks have large
electron density due to the weak crystal diffraction of these compounds.
It is chemical unreasonable to define atoms at these positions because these
Q-peaks have short distances with the neighboring atoms.
;

_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)+(0.1297P)²+72.2970P] 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_number_reflns         10693
_refine_ls_number_parameters     746
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0786
_refine_ls_wR_factor_ref         0.2224
_refine_ls_wR_factor_gt          0.1943
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      8.132
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.7977(3) 0.0000 0.39413(15) 0.0417(17) Uani 1 2 d S . .
La2 La -0.0108(2) 0.2254(2) 0.77079(13) 0.0521(16) Uani 1 1 d . . .
Na Na 0.586(2) 0.5000 0.9061(14) 0.065(12) Uani 1 2 d S . .
S1 S 0.9932(11) 0.0000 0.6616(7) 0.038(5) Uani 1 2 d S . .
S2 S 0.7667(8) 0.3124(7) 0.6228(4) 0.034(3) Uani 1 1 d . . .
S3 S 0.6046(15) 0.0000 0.6654(8) 0.053(6) Uani 1 2 d S . .
S4 S 0.377(2) 0.5000 0.8434(10) 0.076(10) Uani 1 2 d S . .
S5 S 0.1459(10) 0.1833(8) 0.8780(5) 0.047(4) Uani 1 1 d . . .
S6 S -0.0514(15) 0.5000 0.8350(8) 0.057(7) Uani 1 2 d S . .
C1 C 0.602(4) 0.0000 0.608(3) 0.04(2) Uani 1 2 d S . .
C2 C 0.600(3) 0.064(3) 0.585(2) 0.032(12) Uani 1 1 d . . .
H2 H 0.6039 0.1056 0.6008 0.039 Uiso 1 1 calc R . .
C3 C 0.593(3) 0.065(3) 0.5376(19) 0.030(12) Uani 1 1 d . . .
C4 C 0.586(4) 0.0000 0.514(3) 0.029(16) Uani 1 2 d S . .
C5 C 0.593(3) 0.135(3) 0.5148(19) 0.031(12) Uani 1 1 d . . .
H5A H 0.5797 0.1293 0.4817 0.037 Uiso 1 1 calc R . .
H5B H 0.5607 0.1665 0.5221 0.037 Uiso 1 1 calc R . .
C6 C 0.665(3) 0.167(3) 0.5311(17) 0.026(11) Uani 1 1 d . . .
C7 C 0.681(3) 0.221(3) 0.5636(18) 0.027(11) Uani 1 1 d . . .
H7 H 0.6469 0.2405 0.5742 0.032 Uiso 1 1 calc R . .
C8 C 0.748(3) 0.247(3) 0.5803(17) 0.029(12) Uani 1 1 d . . .
C9 C 0.800(3) 0.219(2) 0.5651(16) 0.022(10) Uani 1 1 d . . .
H9 H 0.8448 0.2367 0.5767 0.027 Uiso 1 1 calc R . .
C10 C 0.785(3) 0.165(2) 0.5319(16) 0.022(10) Uani 1 1 d . . .
C11 C 0.718(3) 0.140(2) 0.5161(16) 0.021(10) Uani 1 1 d . . .
C12 C 0.843(3) 0.135(2) 0.5159(16) 0.023(10) Uani 1 1 d . . .
H12A H 0.8812 0.1675 0.5232 0.027 Uiso 1 1 calc R . .
H12B H 0.8268 0.1287 0.4827 0.027 Uiso 1 1 calc R . .
C13 C 0.845(4) 0.0000 0.517(2) 0.021(14) Uani 1 2 d S . .
C14 C 0.868(2) 0.064(2) 0.5385(15) 0.017(9) Uani 1 1 d . . .
C15 C 0.916(3) 0.064(3) 0.5828(16) 0.025(10) Uani 1 1 d . . .
H15 H 0.9323 0.1055 0.5980 0.030 Uiso 1 1 calc R . .
C16 C 0.939(4) 0.0000 0.603(2) 0.027(16) Uani 1 2 d S . .
C17 C -0.002(5) 0.5000 0.892(3) 0.05(2) Uani 1 2 d S . .
C18 C 0.018(3) 0.437(3) 0.916(2) 0.034(13) Uani 1 1 d . . .
H18 H 0.0050 0.3951 0.9005 0.041 Uiso 1 1 calc R . .
C19 C 0.056(3) 0.436(3) 0.963(2) 0.034(13) Uani 1 1 d . . .
C20 C 0.073(4) 0.5000 0.986(3) 0.031(17) Uani 1 2 d S . .
C21 C 0.078(3) 0.364(3) 0.9850(19) 0.033(12) Uani 1 1 d . . .
H21A H 0.0953 0.3700 1.0182 0.039 Uiso 1 1 calc R . .
H21B H 0.0387 0.3333 0.9778 0.039 Uiso 1 1 calc R . .
C22 C 0.134(3) 0.333(3) 0.9678(19) 0.032(12) Uani 1 1 d . A .
C23 C 0.119(3) 0.279(3) 0.9356(19) 0.034(13) Uani 1 1 d . . .
H23 H 0.0747 0.2613 0.9251 0.041 Uiso 1 1 calc R A .
C24 C 0.169(3) 0.252(3) 0.919(2) 0.037(13) Uani 1 1 d . A .
C25 C 0.235(3) 0.279(3) 0.9324(18) 0.032(12) Uani 1 1 d . . .
H25 H 0.2682 0.2605 0.9203 0.038 Uiso 1 1 calc R A .
C26 C 0.253(3) 0.335(3) 0.9647(18) 0.031(12) Uani 1 1 d . A .
C27 C 0.200(3) 0.360(3) 0.9822(17) 0.028(11) Uani 1 1 d . . .
C28 C 0.323(3) 0.365(3) 0.9792(19) 0.031(12) Uani 1 1 d . . .
H28A H 0.3544 0.3316 0.9721 0.038 Uiso 1 1 calc R A .
H28B H 0.3377 0.3713 1.0123 0.038 Uiso 1 1 calc R . .
C29 C 0.323(4) 0.5000 0.977(3) 0.034(18) Uani 1 2 d S . .
C30 C 0.330(3) 0.436(3) 0.9567(18) 0.031(12) Uani 1 1 d . A .
C31 C 0.342(3) 0.436(3) 0.9139(18) 0.030(12) Uani 1 1 d . . .
H31 H 0.3456 0.3939 0.8993 0.036 Uiso 1 1 calc R A .
C32 C 0.349(5) 0.5000 0.893(3) 0.04(2) Uani 1 2 d S . .
C33 C 0.171(5) 0.465(5) 0.870(3) 0.08(3) Uani 1 1 d . . .
H33 H 0.1629 0.4412 0.8940 0.092 Uiso 1 1 calc R . .
C34 C 0.186(7) 0.465(5) 0.798(3) 0.09(4) Uani 1 1 d . . .
H34 H 0.1888 0.4417 0.7716 0.110 Uiso 1 1 calc R . .
C35 C 0.806(5) 0.034(4) 0.708(2) 0.057(19) Uani 1 1 d . . .
H35 H 0.8150 0.0582 0.7358 0.068 Uiso 1 1 calc R . .
C36 C 0.779(3) 0.036(4) 0.629(2) 0.049(16) Uani 1 1 d . . .
H36 H 0.7697 0.0607 0.6016 0.059 Uiso 1 1 calc R . .
N1 N 0.793(3) 0.071(3) 0.6691(19) 0.052(15) Uani 1 1 d . . .
N2 N 0.182(5) 0.429(3) 0.834(2) 0.08(2) Uani 1 1 d . . .
O1 O 1.034(2) 0.063(2) 0.6684(14) 0.042(10) Uani 1 1 d . . .
O2 O 0.949(3) 0.0000 0.691(2) 0.049(16) Uani 1 2 d S . .
O3 O 0.841(3) 0.317(4) 0.641(2) 0.08(2) Uani 1 1 d . . .
O4 O 0.732(3) 0.296(2) 0.6565(16) 0.056(13) Uani 1 1 d . . .
O5 O 0.741(2) 0.3775(19) 0.5996(14) 0.038(10) Uani 1 1 d . . .
O6 O 0.643(4) 0.062(3) 0.6863(18) 0.081(19) Uani 1 1 d . . .
O7 O 0.533(5) 0.0000 0.664(3) 0.08(3) Uani 1 2 d S . .
O8 O 0.798(3) 0.0000 0.4742(14) 0.021(10) Uani 1 2 d S . .
O9 O 0.700(2) 0.0871(19) 0.4847(12) 0.031(8) Uani 1 1 d . . .
O10 O 0.576(3) 0.0000 0.4676(17) 0.031(12) Uani 1 2 d S . .
O11 O 0.455(5) 0.5000 0.861(4) 0.11(4) Uani 1 2 d S . .
O12 O 0.352(5) 0.436(3) 0.818(2) 0.09(2) Uani 1 1 d . . .
O13 O 0.206(3) 0.156(4) 0.871(3) 0.11(3) Uani 1 1 d . A .
O14 O 0.098(3) 0.212(3) 0.8363(16) 0.053(12) Uani 1 1 d . A .
O15 O 0.110(5) 0.131(3) 0.897(2) 0.11(3) Uani 1 1 d . . .
O16 O -0.087(5) 0.562(3) 0.824(3) 0.12(4) Uani 1 1 d . . .
O17 O 0.000(7) 0.5000 0.811(4) 0.25(14) Uani 1 2 d S . .
O18 O 0.106(3) 0.5000 1.0315(19) 0.041(14) Uani 1 2 d S . .
O19 O 0.214(2) 0.411(2) 1.0147(14) 0.038(9) Uani 1 1 d . A .
O20 O 0.311(3) 0.5000 1.018(2) 0.037(13) Uiso 1 2 d S . .
O21 O 0.184(5) 0.361(4) 0.835(3) 0.10(2) Uani 1 1 d . . .
O22 O 0.794(4) 0.140(3) 0.669(2) 0.09(2) Uani 1 1 d . . .
O23 O -0.065(3) 0.191(3) 0.6851(17) 0.068(16) Uani 1 1 d . A .
O24 O -0.141(3) 0.207(4) 0.751(2) 0.09(2) Uani 1 1 d . A .
O25 O -0.040(5) 0.163(5) 0.836(2) 0.11(3) Uani 1 1 d . A .
O26 O -0.073(4) 0.333(4) 0.726(2) 0.10(2) Uani 1 1 d . A .
O27 O 0.070(10) 0.147(11) 0.744(7) 0.05(8) Uiso 0.2(2) 1 d PD A 1
O27' O 0.080(11) 0.207(12) 0.729(8) 0.20(9) Uiso 0.8(2) 1 d P A 2
O28 O -0.046(5) 0.303(4) 0.828(3) 0.07(3) Uiso 0.77(17) 1 d P A 1
O28' O 0.003(11) 0.322(11) 0.825(7) 0.05(8) Uiso 0.23(17) 1 d PD A 2
O29 O -0.033(8) 0.089(7) 0.767(4) 0.08(5) Uiso 0.5(2) 1 d P B 1
O29' O 0.011(9) 0.104(8) 0.761(6) 0.10(7) Uiso 0.5(2) 1 d PD A 2
O30 O 0.072(9) 0.311(9) 0.760(6) 0.13(7) Uiso 0.6(3) 1 d P A 1
O30' O 0.057(9) 0.340(11) 0.786(7) 0.08(9) Uiso 0.4(3) 1 d PD A 2
O31 O 0.834(3) -0.077(2) 0.3367(16) 0.048(11) Uani 1 1 d . . .
O32 O 0.671(4) 0.0000 0.396(3) 0.07(2) Uani 1 2 d S . .
O33 O 0.699(4) 0.0000 0.316(3) 0.07(2) Uani 1 2 d S . .
O34 O 0.909(3) -0.065(3) 0.4375(18) 0.059(13) Uani 1 1 d D . .
O35 O 0.675(6) 0.5000 0.891(2) 0.09(3) Uani 1 2 d S . .
O36 O 0.563(8) 0.5000 0.819(4) 0.14(6) Uani 1 2 d S . .
O37 O 0.305(5) 0.116(6) 0.749(3) 0.09(4) Uiso 0.8(2) 1 d P C 1
O37' O 0.281(15) 0.064(15) 0.760(10) 0.07(11) Uiso 0.2(2) 1 d P C 2
O38 O 0.0000 0.0000 0.5000 0.12(6) Uiso 1 4 d SD . .
O39' O 0.203(13) 0.19(2) 0.769(11) 0.14(10) Uiso 0.5(4) 1 d P D 1
O39 O 0.201(6) 0.155(8) 0.784(4) 0.06(5) Uiso 0.5(4) 1 d P D 2
O40 O 0.791(5) 0.220(6) 0.817(3) 0.13(3) Uani 1 1 d . . .
O41 O 0.566(3) 0.905(3) 0.3951(17) 0.065(15) Uani 1 1 d . . .
O42 O 0.633(4) 0.204(4) 0.675(3) 0.10(2) Uani 1 1 d . . .
O44 O 0.993(5) 0.262(5) 0.621(3) 0.11(2) Uani 1 1 d . . .
O45 O 0.974(3) 0.804(3) 0.453(3) 0.09(2) Uani 1 1 d . . .
O46 O 0.947(8) 0.523(7) 0.720(5) 0.03(4) Uiso 0.25 1 d P . .
O47 O 0.167(4) 0.403(5) 0.101(3) 0.11(2) Uiso 1 1 d . . .
O48 O 0.907(8) 0.262(8) 0.900(5) 0.10(4) Uiso 0.50 1 d P . .
O49 O 0.0000 0.0000 0.0000 0.12(6) Uiso 1 4 d SD . .
O50 O 0.0000 0.149(8) 0.0000 0.16(11) Uiso 0.50 2 d SPD . .


_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
La1 O8 2.44(4) . ?
La1 O5 2.49(4) 4_646 ?
La1 O5 2.49(4) 7_656 ?
La1 O31 2.56(4) . ?
La1 O31 2.56(4) 6 ?
La1 O34 2.57(6) 6 ?
La1 O34 2.57(6) . ?
La1 O33 2.60(8) . ?
La1 O32 2.60(9) . ?
La2 O29' 2.39(16) . ?
La2 O30 2.44(17) . ?
La2 O28' 2.4(2) . ?
La2 O14 2.51(5) . ?
La2 O27 2.5(2) . ?
La2 O25 2.54(7) . ?
La2 O28 2.54(8) . ?
La2 O30' 2.5(2) . ?
La2 O24 2.56(7) . ?
La2 O27' 2.6(2) . ?
La2 O26 2.58(7) . ?
La2 O23 2.59(5) . ?
Na O35 2.00(13) . ?
Na O36 2.54(14) . ?
Na O15 2.58(6) 3 ?
Na O15 2.58(6) 8 ?
Na O11 2.60(11) . ?
Na O20 2.60(7) 5_667 ?
S1 O1 1.44(4) . ?
S1 O1 1.44(4) 6 ?
S1 O2 1.46(7) . ?
S1 C16 1.78(7) . ?
S2 O3 1.44(6) . ?
S2 O5 1.44(4) . ?
S2 O4 1.45(5) . ?
S2 C8 1.76(5) . ?
S3 O6 1.44(6) . ?
S3 O6 1.44(6) 6 ?
S3 O7 1.45(10) . ?
S3 C1 1.74(8) . ?
S4 O12 1.44(7) . ?
S4 O12 1.44(7) 6_565 ?
S4 O11 1.52(10) . ?
S4 C32 1.76(9) . ?
S5 O13 1.39(7) . ?
S5 O15 1.45(7) . ?
S5 O14 1.45(5) . ?
S5 C24 1.76(6) . ?
S6 O16 1.38(7) 6_565 ?
S6 O16 1.38(7) . ?
S6 O17 1.46(13) . ?
S6 C17 1.73(9) . ?
C1 C2 1.40(7) 6 ?
C1 C2 1.40(7) . ?
C2 C3 1.40(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.41(7) . ?
C3 C5 1.52(8) . ?
C4 O10 1.37(9) . ?
C4 C3 1.41(7) 6 ?
C5 C6 1.51(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.39(7) . ?
C6 C11 1.41(7) . ?
C7 C8 1.38(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.39(8) . ?
C9 C10 1.41(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.38(7) . ?
C10 C12 1.52(7) . ?
C11 O9 1.36(6) . ?
C12 C14 1.53(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 O8 1.36(8) . ?
C13 C14 1.40(6) . ?
C13 C14 1.40(6) 6 ?
C14 C15 1.40(7) . ?
C15 C16 1.38(6) . ?
C15 H15 0.9300 . ?
C16 C15 1.38(6) 6 ?
C17 C18 1.39(7) 6_565 ?
C17 C18 1.39(7) . ?
C18 C19 1.39(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.41(7) . ?
C19 C21 1.52(8) . ?
C20 O18 1.35(9) . ?
C20 C19 1.41(7) 6_565 ?
C21 C22 1.51(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.39(8) . ?
C22 C27 1.39(8) . ?
C23 C24 1.37(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.39(9) . ?
C25 C26 1.42(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.42(8) . ?
C26 C28 1.47(8) . ?
C27 O19 1.35(7) . ?
C28 C30 1.53(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 O20 1.35(10) . ?
C29 C30 1.41(7) . ?
C29 C30 1.41(7) 6_565 ?
C30 C31 1.40(7) . ?
C31 C32 1.40(7) . ?
C31 H31 0.9300 . ?
C32 C31 1.40(7) 6_565 ?
C33 C33 1.3(2) 6_565 ?
C33 N2 1.37(12) . ?
C33 H33 0.9300 . ?
C34 C34 1.31(18) 6_565 ?
C34 N2 1.33(11) . ?
C34 H34 0.9300 . ?
C35 C35 1.31(14) 6 ?
C35 N1 1.33(9) . ?
C35 H35 0.9300 . ?
C36 N1 1.34(9) . ?
C36 C36 1.38(15) 6 ?
C36 H36 0.9300 . ?
N1 O22 1.31(8) . ?
N2 O21 1.29(9) . ?
O5 La1 2.49(4) 7_656 ?
O15 Na 2.58(6) 3_445 ?
O20 Na 2.60(7) 5_667 ?
O46 O46 0.9(3) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 La1 O5 80.1(10) . 4_646 ?
O8 La1 O5 80.1(10) . 7_656 ?
O5 La1 O5 140(2) 4_646 7_656 ?
O8 La1 O31 140.5(12) . . ?
O5 La1 O31 71.2(14) 4_646 . ?
O5 La1 O31 138.9(14) 7_656 . ?
O8 La1 O31 140.5(12) . 6 ?
O5 La1 O31 138.9(14) 4_646 6 ?
O5 La1 O31 71.2(14) 7_656 6 ?
O31 La1 O31 70(2) . 6 ?
O8 La1 O34 75.8(15) . 6 ?
O5 La1 O34 131.3(16) 4_646 6 ?
O5 La1 O34 76.2(16) 7_656 6 ?
O31 La1 O34 103.4(16) . 6 ?
O31 La1 O34 71.4(16) 6 6 ?
O8 La1 O34 75.8(15) . . ?
O5 La1 O34 76.2(15) 4_646 . ?
O5 La1 O34 131.3(16) 7_656 . ?
O31 La1 O34 71.4(16) . . ?
O31 La1 O34 103.4(16) 6 . ?
O34 La1 O34 57(2) 6 . ?
O8 La1 O33 133(2) . . ?
O5 La1 O33 84.0(11) 4_646 . ?
O5 La1 O33 84.0(11) 7_656 . ?
O31 La1 O33 71.4(17) . . ?
O31 La1 O33 71.4(17) 6 . ?
O34 La1 O33 141.8(16) 6 . ?
O34 La1 O33 141.8(16) . . ?
O8 La1 O32 71(2) . . ?
O5 La1 O32 70.1(11) 4_646 . ?
O5 La1 O32 70.1(11) 7_656 . ?
O31 La1 O32 120.8(18) . . ?
O31 La1 O32 120.8(18) 6 . ?
O34 La1 O32 135.8(18) 6 . ?
O34 La1 O32 135.8(18) . . ?
O33 La1 O32 62(3) . . ?
O29' La2 O30 118(6) . . ?
O29' La2 O28' 146(6) . . ?
O30 La2 O28' 69(6) . . ?
O29' La2 O14 82(4) . . ?
O30 La2 O14 72(4) . . ?
O28' La2 O14 69(5) . . ?
O29' La2 O27 39(4) . . ?
O30 La2 O27 79(6) . . ?
O28' La2 O27 136(6) . . ?
O14 La2 O27 72(5) . . ?
O29' La2 O25 75(4) . . ?
O30 La2 O25 139(5) . . ?
O28' La2 O25 80(5) . . ?
O14 La2 O25 72(2) . . ?
O27 La2 O25 108(5) . . ?
O29' La2 O28 139(4) . . ?
O30 La2 O28 93(5) . . ?
O28' La2 O28 25(4) . . ?
O14 La2 O28 83(2) . . ?
O27 La2 O28 155(5) . . ?
O25 La2 O28 64(3) . . ?
O29' La2 O30' 138(6) . . ?
O30 La2 O30' 24(5) . . ?
O28' La2 O30' 45(4) . . ?
O14 La2 O30' 69(4) . . ?
O27 La2 O30' 101(6) . . ?
O25 La2 O30' 120(5) . . ?
O28 La2 O30' 68(5) . . ?
O29' La2 O24 93(5) . . ?
O30 La2 O24 140(4) . . ?
O28' La2 O24 99(5) . . ?
O14 La2 O24 141(2) . . ?
O27 La2 O24 125(5) . . ?
O25 La2 O24 69(2) . . ?
O28 La2 O24 76(3) . . ?
O30' La2 O24 129(5) . . ?
O29' La2 O27' 67(6) . . ?
O30 La2 O27' 53(7) . . ?
O28' La2 O27' 119(7) . . ?
O14 La2 O27' 78(5) . . ?
O27 La2 O27' 29(6) . . ?
O25 La2 O27' 134(6) . . ?
O28 La2 O27' 144(6) . . ?
O30' La2 O27' 77(7) . . ?
O24 La2 O27' 136(5) . . ?
O29' La2 O26 141(4) . . ?
O30 La2 O26 69(4) . . ?
O28' La2 O26 72(5) . . ?
O14 La2 O26 133(2) . . ?
O27 La2 O26 124(5) . . ?
O25 La2 O26 127(3) . . ?
O28 La2 O26 73(3) . . ?
O30' La2 O26 64(5) . . ?
O24 La2 O26 71(3) . . ?
O27' La2 O26 99(6) . . ?
O29' La2 O23 70(4) . . ?
O30 La2 O23 98(5) . . ?
O28' La2 O23 143(5) . . ?
O14 La2 O23 141.2(18) . . ?
O27 La2 O23 69(5) . . ?
O25 La2 O23 123(2) . . ?
O28 La2 O23 135(2) . . ?
O30' La2 O23 116(4) . . ?
O24 La2 O23 69(2) . . ?
O27' La2 O23 67(5) . . ?
O26 La2 O23 71(2) . . ?
O35 Na O36 70(5) . . ?
O35 Na O15 76(3) . 3 ?
O36 Na O15 82.4(18) . 3 ?
O35 Na O15 76(3) . 8 ?
O36 Na O15 82.4(18) . 8 ?
O15 Na O15 151(5) 3 8 ?
O35 Na O11 137(4) . . ?
O36 Na O11 67(5) . . ?
O15 Na O11 98(2) 3 . ?
O15 Na O11 98(2) 8 . ?
O35 Na O20 70(3) . 5_667 ?
O36 Na O20 140(5) . 5_667 ?
O15 Na O20 88(2) 3 5_667 ?
O15 Na O20 88(2) 8 5_667 ?
O11 Na O20 153(3) . 5_667 ?
O1 S1 O1 113(4) . 6 ?
O1 S1 O2 110(2) . . ?
O1 S1 O2 110(2) 6 . ?
O1 S1 C16 107(2) . . ?
O1 S1 C16 107(2) 6 . ?
O2 S1 C16 108(4) . . ?
O3 S2 O5 108(4) . . ?
O3 S2 O4 116(4) . . ?
O5 S2 O4 110(3) . . ?
O3 S2 C8 107(3) . . ?
O5 S2 C8 107(2) . . ?
O4 S2 C8 109(3) . . ?
O6 S3 O6 109(6) . 6 ?
O6 S3 O7 115(3) . . ?
O6 S3 O7 115(3) 6 . ?
O6 S3 C1 107(3) . . ?
O6 S3 C1 107(3) 6 . ?
O7 S3 C1 104(4) . . ?
O12 S4 O12 115(6) . 6_565 ?
O12 S4 O11 110(4) . . ?
O12 S4 O11 110(4) 6_565 . ?
O12 S4 C32 108(3) . . ?
O12 S4 C32 108(3) 6_565 . ?
O11 S4 C32 106(5) . . ?
O13 S5 O15 111(6) . . ?
O13 S5 O14 113(4) . . ?
O15 S5 O14 109(4) . . ?
O13 S5 C24 109(3) . . ?
O15 S5 C24 107(3) . . ?
O14 S5 C24 108(3) . . ?
O16 S6 O16 118(7) 6_565 . ?
O16 S6 O17 106(5) 6_565 . ?
O16 S6 O17 106(5) . . ?
O16 S6 C17 111(3) 6_565 . ?
O16 S6 C17 111(3) . . ?
O17 S6 C17 103(6) . . ?
C2 C1 C2 120(7) 6 . ?
C2 C1 S3 120(4) 6 . ?
C2 C1 S3 120(4) . . ?
C1 C2 C3 121(5) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C4 118(5) . . ?
C2 C3 C5 118(5) . . ?
C4 C3 C5 124(5) . . ?
O10 C4 C3 119(3) . 6 ?
O10 C4 C3 119(3) . . ?
C3 C4 C3 122(7) 6 . ?
C6 C5 C3 111(4) . . ?
C6 C5 H5A 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C7 C6 C11 117(5) . . ?
C7 C6 C5 122(5) . . ?
C11 C6 C5 120(5) . . ?
C8 C7 C6 121(5) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 121(5) . . ?
C7 C8 S2 120(4) . . ?
C9 C8 S2 119(4) . . ?
C8 C9 C10 119(5) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 119(5) . . ?
C11 C10 C12 122(4) . . ?
C9 C10 C12 119(4) . . ?
O9 C11 C10 122(4) . . ?
O9 C11 C6 115(5) . . ?
C10 C11 C6 122(5) . . ?
C10 C12 C14 112(4) . . ?
C10 C12 H12A 109.1 . . ?
C14 C12 H12A 109.1 . . ?
C10 C12 H12B 109.1 . . ?
C14 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
O8 C13 C14 119(3) . . ?
O8 C13 C14 119(3) . 6 ?
C14 C13 C14 121(6) . 6 ?
C13 C14 C15 119(4) . . ?
C13 C14 C12 122(4) . . ?
C15 C14 C12 119(4) . . ?
C16 C15 C14 119(5) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C15 123(6) 6 . ?
C15 C16 S1 118(3) 6 . ?
C15 C16 S1 118(3) . . ?
C18 C17 C18 119(8) 6_565 . ?
C18 C17 S6 121(4) 6_565 . ?
C18 C17 S6 121(4) . . ?
C17 C18 C19 122(6) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C18 C19 C20 118(6) . . ?
C18 C19 C21 118(5) . . ?
C20 C19 C21 124(5) . . ?
O18 C20 C19 119(4) . . ?
O18 C20 C19 119(4) . 6_565 ?
C19 C20 C19 121(7) . 6_565 ?
C22 C21 C19 110(4) . . ?
C22 C21 H21A 109.6 . . ?
C19 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C19 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 C27 118(5) . . ?
C23 C22 C21 121(5) . . ?
C27 C22 C21 120(5) . . ?
C24 C23 C22 122(6) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 120(6) . . ?
C23 C24 S5 119(5) . . ?
C25 C24 S5 121(5) . . ?
C24 C25 C26 121(5) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C27 C26 C25 116(5) . . ?
C27 C26 C28 122(5) . . ?
C25 C26 C28 121(5) . . ?
O19 C27 C22 117(5) . . ?
O19 C27 C26 121(5) . . ?
C22 C27 C26 122(5) . . ?
C26 C28 C30 115(5) . . ?
C26 C28 H28A 108.6 . . ?
C30 C28 H28A 108.6 . . ?
C26 C28 H28B 108.6 . . ?
C30 C28 H28B 108.6 . . ?
H28A C28 H28B 107.5 . . ?
O20 C29 C30 119(3) . . ?
O20 C29 C30 119(3) . 6_565 ?
C30 C29 C30 121(7) . 6_565 ?
C31 C30 C29 119(5) . . ?
C31 C30 C28 119(5) . . ?
C29 C30 C28 122(5) . . ?
C30 C31 C32 120(5) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C31 121(7) . 6_565 ?
C31 C32 S4 120(4) . . ?
C31 C32 S4 120(4) 6_565 . ?
C33 C33 N2 121(5) 6_565 . ?
C33 C33 H33 119.7 6_565 . ?
N2 C33 H33 119.7 . . ?
C34 C34 N2 122(5) 6_565 . ?
C34 C34 H34 119.1 6_565 . ?
N2 C34 H34 119.1 . . ?
C35 C35 N1 122(4) 6 . ?
C35 C35 H35 119.1 6 . ?
N1 C35 H35 119.1 . . ?
N1 C36 C36 120(4) . 6 ?
N1 C36 H36 120.0 . . ?
C36 C36 H36 120.0 6 . ?
O22 N1 C35 122(6) . . ?
O22 N1 C36 120(6) . . ?
C35 N1 C36 118(6) . . ?
O21 N2 C34 122(8) . . ?
O21 N2 C33 121(8) . . ?
C34 N2 C33 117(7) . . ?
S2 O5 La1 148(2) . 7_656 ?
C13 O8 La1 138(4) . . ?
S4 O11 Na 169(7) . . ?
S5 O14 La2 158(3) . . ?
S5 O15 Na 148(6) . 3_445 ?
C29 O20 Na 119(5) . 5_667 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 S3 C1 C2 149(6) . . . 6 ?
O6 S3 C1 C2 33(7) 6 . . 6 ?
O7 S3 C1 C2 -89(6) . . . 6 ?
O6 S3 C1 C2 -33(7) . . . . ?
O6 S3 C1 C2 -149(6) 6 . . . ?
O7 S3 C1 C2 89(6) . . . . ?
C2 C1 C2 C3 3(11) 6 . . . ?
S3 C1 C2 C3 -175(5) . . . . ?
C1 C2 C3 C4 1(9) . . . . ?
C1 C2 C3 C5 -178(6) . . . . ?
C2 C3 C4 O10 177(6) . . . . ?
C5 C3 C4 O10 -4(9) . . . . ?
C2 C3 C4 C3 -6(10) . . . 6 ?
C5 C3 C4 C3 173(4) . . . 6 ?
C2 C3 C5 C6 69(6) . . . . ?
C4 C3 C5 C6 -110(6) . . . . ?
C3 C5 C6 C7 -103(6) . . . . ?
C3 C5 C6 C11 73(6) . . . . ?
C11 C6 C7 C8 0(7) . . . . ?
C5 C6 C7 C8 176(5) . . . . ?
C6 C7 C8 C9 0(8) . . . . ?
C6 C7 C8 S2 -178(4) . . . . ?
O3 S2 C8 C7 168(5) . . . . ?
O5 S2 C8 C7 -77(5) . . . . ?
O4 S2 C8 C7 42(5) . . . . ?
O3 S2 C8 C9 -10(5) . . . . ?
O5 S2 C8 C9 105(4) . . . . ?
O4 S2 C8 C9 -136(4) . . . . ?
C7 C8 C9 C10 0(7) . . . . ?
S2 C8 C9 C10 178(3) . . . . ?
C8 C9 C10 C11 -1(7) . . . . ?
C8 C9 C10 C12 -179(4) . . . . ?
C9 C10 C11 O9 -179(4) . . . . ?
C12 C10 C11 O9 -1(7) . . . . ?
C9 C10 C11 C6 1(7) . . . . ?
C12 C10 C11 C6 179(4) . . . . ?
C7 C6 C11 O9 179(4) . . . . ?
C5 C6 C11 O9 4(7) . . . . ?
C7 C6 C11 C10 -1(7) . . . . ?
C5 C6 C11 C10 -176(4) . . . . ?
C11 C10 C12 C14 -76(6) . . . . ?
C9 C10 C12 C14 102(5) . . . . ?
O8 C13 C14 C15 179(5) . . . . ?
C14 C13 C14 C15 0(9) 6 . . . ?
O8 C13 C14 C12 0(8) . . . . ?
C14 C13 C14 C12 -179(4) 6 . . . ?
C10 C12 C14 C13 97(6) . . . . ?
C10 C12 C14 C15 -82(5) . . . . ?
C13 C14 C15 C16 1(8) . . . . ?
C12 C14 C15 C16 180(5) . . . . ?
C14 C15 C16 C15 -1(11) . . . 6 ?
C14 C15 C16 S1 -174(4) . . . . ?
O1 S1 C16 C15 155(5) . . . 6 ?
O1 S1 C16 C15 32(7) 6 . . 6 ?
O2 S1 C16 C15 -86(6) . . . 6 ?
O1 S1 C16 C15 -32(7) . . . . ?
O1 S1 C16 C15 -155(5) 6 . . . ?
O2 S1 C16 C15 86(6) . . . . ?
O16 S6 C17 C18 -156(8) 6_565 . . 6_565 ?
O16 S6 C17 C18 -23(10) . . . 6_565 ?
O17 S6 C17 C18 90(7) . . . 6_565 ?
O16 S6 C17 C18 23(10) 6_565 . . . ?
O16 S6 C17 C18 156(8) . . . . ?
O17 S6 C17 C18 -90(7) . . . . ?
C18 C17 C18 C19 0(13) 6_565 . . . ?
S6 C17 C18 C19 -179(5) . . . . ?
C17 C18 C19 C20 3(9) . . . . ?
C17 C18 C19 C21 -177(7) . . . . ?
C18 C19 C20 O18 176(6) . . . . ?
C21 C19 C20 O18 -4(10) . . . . ?
C18 C19 C20 C19 -6(10) . . . 6_565 ?
C21 C19 C20 C19 174(4) . . . 6_565 ?
C18 C19 C21 C22 72(7) . . . . ?
C20 C19 C21 C22 -108(6) . . . . ?
C19 C21 C22 C23 -104(6) . . . . ?
C19 C21 C22 C27 72(6) . . . . ?
C27 C22 C23 C24 2(8) . . . . ?
C21 C22 C23 C24 178(5) . . . . ?
C22 C23 C24 C25 -3(9) . . . . ?
C22 C23 C24 S5 180(4) . . . . ?
O13 S5 C24 C23 -170(6) . . . . ?
O15 S5 C24 C23 -50(7) . . . . ?
O14 S5 C24 C23 67(6) . . . . ?
O13 S5 C24 C25 12(7) . . . . ?
O15 S5 C24 C25 132(6) . . . . ?
O14 S5 C24 C25 -111(5) . . . . ?
C23 C24 C25 C26 1(8) . . . . ?
S5 C24 C25 C26 179(4) . . . . ?
C24 C25 C26 C27 1(8) . . . . ?
C24 C25 C26 C28 -179(5) . . . . ?
C23 C22 C27 O19 -178(5) . . . . ?
C21 C22 C27 O19 6(7) . . . . ?
C23 C22 C27 C26 0(8) . . . . ?
C21 C22 C27 C26 -176(5) . . . . ?
C25 C26 C27 O19 177(5) . . . . ?
C28 C26 C27 O19 -3(8) . . . . ?
C25 C26 C27 C22 -1(8) . . . . ?
C28 C26 C27 C22 179(5) . . . . ?
C27 C26 C28 C30 -78(6) . . . . ?
C25 C26 C28 C30 103(6) . . . . ?
O20 C29 C30 C31 179(6) . . . . ?
C30 C29 C30 C31 -2(11) 6_565 . . . ?
O20 C29 C30 C28 0(10) . . . . ?
C30 C29 C30 C28 180(5) 6_565 . . . ?
C26 C28 C30 C31 -86(6) . . . . ?
C26 C28 C30 C29 92(7) . . . . ?
C29 C30 C31 C32 2(9) . . . . ?
C28 C30 C31 C32 -179(6) . . . . ?
C30 C31 C32 C31 -2(12) . . . 6_565 ?
C30 C31 C32 S4 171(5) . . . . ?
O12 S4 C32 C31 31(9) . . . . ?
O12 S4 C32 C31 156(7) 6_565 . . . ?
O11 S4 C32 C31 -87(7) . . . . ?
O12 S4 C32 C31 -156(7) . . . 6_565 ?
O12 S4 C32 C31 -31(9) 6_565 . . 6_565 ?
O11 S4 C32 C31 87(6) . . . 6_565 ?
C35 C35 N1 O22 -178(6) 6 . . . ?
C35 C35 N1 C36 0(9) 6 . . . ?
C36 C36 N1 O22 178(6) 6 . . . ?
C36 C36 N1 C35 0(8) 6 . . . ?
C34 C34 N2 O21 -178(7) 6_565 . . . ?
C34 C34 N2 C33 7(12) 6_565 . . . ?
C33 C33 N2 O21 178(7) 6_565 . . . ?
C33 C33 N2 C34 -7(12) 6_565 . . . ?
O3 S2 O5 La1 -86(6) . . . 7_656 ?
O4 S2 O5 La1 41(6) . . . 7_656 ?
C8 S2 O5 La1 159(5) . . . 7_656 ?
C14 C13 O8 La1 90(5) . . . . ?
C14 C13 O8 La1 -90(5) 6 . . . ?
O5 La1 O8 C13 107.7(11) 4_646 . . . ?
O5 La1 O8 C13 -107.7(11) 7_656 . . . ?
O31 La1 O8 C13 64(2) . . . . ?
O31 La1 O8 C13 -64(2) 6 . . . ?
O34 La1 O8 C13 -29.6(12) 6 . . . ?
O34 La1 O8 C13 29.6(12) . . . . ?
O33 La1 O8 C13 180.000(16) . . . . ?
O32 La1 O8 C13 180.000(17) . . . . ?
O12 S4 O11 Na -116(3) . . . . ?
O12 S4 O11 Na 116(3) 6_565 . . . ?
C32 S4 O11 Na 0.00(11) . . . . ?
O35 Na O11 S4 180.00(7) . . . . ?
O36 Na O11 S4 180.00(8) . . . . ?
O15 Na O11 S4 -102(2) 3 . . . ?
O15 Na O11 S4 102(2) 8 . . . ?
O20 Na O11 S4 0.00(10) 5_667 . . . ?
O13 S5 O14 La2 118(9) . . . . ?
O15 S5 O14 La2 -7(10) . . . . ?
C24 S5 O14 La2 -122(8) . . . . ?
O29' La2 O14 S5 -54(9) . . . . ?
O30 La2 O14 S5 -177(10) . . . . ?
O28' La2 O14 S5 109(9) . . . . ?
O27 La2 O14 S5 -93(9) . . . . ?
O25 La2 O14 S5 23(8) . . . . ?
O28 La2 O14 S5 88(8) . . . . ?
O30' La2 O14 S5 157(10) . . . . ?
O24 La2 O14 S5 31(10) . . . . ?
O27' La2 O14 S5 -123(10) . . . . ?
O26 La2 O14 S5 147(8) . . . . ?
O23 La2 O14 S5 -97(9) . . . . ?
O13 S5 O15 Na -26(10) . . . 3_445 ?
O14 S5 O15 Na 100(10) . . . 3_445 ?
C24 S5 O15 Na -144(8) . . . 3_445 ?
C30 C29 O20 Na 90(6) . . . 5_667 ?
C30 C29 O20 Na -90(6) 6_565 . . 5_667 ?

_diffrn_measured_fraction_theta_max 0.932
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.932
_refine_diff_density_max         2.890
_refine_diff_density_min         -2.462
_refine_diff_density_rms         0.156


# Attachment 'Tb.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 682899'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H44 N2 Na2 O28.50 S4 Tb'
_chemical_formula_weight         1245.83

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'
Na Na 0.0362 0.0249 '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           Monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   31.59(3)
_cell_length_b                   17.867(11)
_cell_length_c                   22.10(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 134.057(17)
_cell_angle_gamma                90.00
_cell_volume                     8966(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       bolck
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5032
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            22619
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1049
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         25.45
_reflns_number_total             8119
_reflns_number_gt                5301
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

_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.

Some Q-peaks have large electron density due to the weak crystal diffraction
of the compound. It is chemical unreasonable to define a atom at the
position because the Q-peak has short distances with the neighboring
oxygen atoms.

;

_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)+(0.0949P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8119
_refine_ls_number_parameters     627
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1463
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_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
Tb Tb 0.666378(19) -0.27432(2) 0.16867(3) 0.01932(14) Uani 1 1 d . . .
Na1 Na 0.59073(16) 0.2977(2) 0.2196(2) 0.0363(10) Uani 1 1 d . . .
Na2 Na 0.99804(18) -0.0268(3) 0.6485(2) 0.0445(11) Uani 1 1 d . . .
S1 S 0.56313(10) 0.21668(13) 0.03006(15) 0.0304(6) Uani 1 1 d . . .
S2 S 0.60920(12) 0.16554(14) 0.39400(16) 0.0338(6) Uani 1 1 d . . .
S3 S 0.82840(10) -0.10895(13) 0.69230(14) 0.0267(5) Uani 1 1 d . . .
S4 S 0.85956(10) 0.07593(12) 0.42554(14) 0.0245(5) Uani 1 1 d . . .
C1 C 0.6228(4) 0.0084(5) 0.1213(5) 0.024(2) Uani 1 1 d . . .
C2 C 0.6161(4) 0.0796(5) 0.0925(5) 0.0221(19) Uani 1 1 d . . .
H2 H 0.6419 0.0965 0.0883 0.027 Uiso 1 1 calc R . .
C3 C 0.5728(4) 0.1267(5) 0.0697(6) 0.026(2) Uani 1 1 d . . .
C4 C 0.5347(4) 0.1020(5) 0.0776(5) 0.027(2) Uani 1 1 d . . .
H4 H 0.5056 0.1340 0.0632 0.033 Uiso 1 1 calc R . .
C5 C 0.5396(4) 0.0316(5) 0.1061(5) 0.0188(18) Uani 1 1 d . . .
C6 C 0.5845(4) -0.0154(5) 0.1283(5) 0.0203(19) Uani 1 1 d . . .
C7 C 0.5030(4) 0.0066(5) 0.1226(5) 0.025(2) Uani 1 1 d . . .
H7A H 0.4886 -0.0438 0.1011 0.030 Uiso 1 1 calc R . .
H7B H 0.4692 0.0394 0.0935 0.030 Uiso 1 1 calc R . .
C8 C 0.5390(4) 0.0079(5) 0.2159(5) 0.0217(19) Uani 1 1 d . . .
C9 C 0.5555(4) 0.0758(5) 0.2571(5) 0.024(2) Uani 1 1 d . . .
H9 H 0.5430 0.1200 0.2265 0.029 Uiso 1 1 calc R . .
C10 C 0.5902(4) 0.0794(5) 0.3434(6) 0.028(2) Uani 1 1 d . . .
C11 C 0.6089(4) 0.0135(5) 0.3881(6) 0.029(2) Uani 1 1 d . . .
H11 H 0.6333 0.0150 0.4461 0.035 Uiso 1 1 calc R . .
C12 C 0.5915(4) -0.0555(5) 0.3469(6) 0.026(2) Uani 1 1 d . . .
C13 C 0.5558(4) -0.0574(5) 0.2620(5) 0.0211(19) Uani 1 1 d . . .
C14 C 0.6154(4) -0.1283(6) 0.3995(6) 0.030(2) Uani 1 1 d . . .
H14A H 0.6085 -0.1272 0.4359 0.036 Uiso 1 1 calc R . .
H14B H 0.5944 -0.1709 0.3620 0.036 Uiso 1 1 calc R . .
C15 C 0.6803(4) -0.1374(5) 0.4522(5) 0.024(2) Uani 1 1 d . . .
C16 C 0.7212(4) -0.1219(5) 0.5369(6) 0.028(2) Uani 1 1 d . . .
H16 H 0.7085 -0.1078 0.5627 0.034 Uiso 1 1 calc R . .
C17 C 0.7808(4) -0.1270(5) 0.5841(5) 0.023(2) Uani 1 1 d . . .
C18 C 0.8002(4) -0.1489(5) 0.5475(5) 0.024(2) Uani 1 1 d . . .
H18 H 0.8403 -0.1541 0.5801 0.029 Uiso 1 1 calc R . .
C19 C 0.7600(4) -0.1634(5) 0.4618(5) 0.0196(19) Uani 1 1 d . . .
C20 C 0.7004(4) -0.1591(5) 0.4155(5) 0.023(2) Uani 1 1 d . . .
C21 C 0.7811(4) -0.1850(5) 0.4202(6) 0.024(2) Uani 1 1 d . . .
H21A H 0.7579 -0.2267 0.3823 0.029 Uiso 1 1 calc R . .
H21B H 0.8219 -0.2009 0.4629 0.029 Uiso 1 1 calc R . .
C22 C 0.7757(4) -0.1182(5) 0.3700(6) 0.023(2) Uani 1 1 d . . .
C23 C 0.8171(4) -0.0625(5) 0.4132(6) 0.027(2) Uani 1 1 d . . .
H23 H 0.8491 -0.0667 0.4711 0.032 Uiso 1 1 calc R . .
C24 C 0.8113(4) 0.0003(5) 0.3709(6) 0.024(2) Uani 1 1 d . . .
C25 C 0.7649(4) 0.0060(5) 0.2849(5) 0.0230(19) Uani 1 1 d . . .
H25 H 0.7617 0.0479 0.2571 0.028 Uiso 1 1 calc R . .
C26 C 0.7225(4) -0.0503(5) 0.2391(5) 0.0202(19) Uani 1 1 d . . .
C27 C 0.7282(4) -0.1140(4) 0.2829(5) 0.0165(18) Uani 1 1 d . . .
C28 C 0.6711(4) -0.0415(5) 0.1454(5) 0.0216(19) Uani 1 1 d . . .
H28A H 0.6853 -0.0210 0.1216 0.026 Uiso 1 1 calc R . .
H28B H 0.6547 -0.0905 0.1207 0.026 Uiso 1 1 calc R . .
C29 C 0.7781(5) 0.1655(7) 0.4947(7) 0.047(3) Uani 1 1 d . . .
H29 H 0.8038 0.1986 0.5393 0.056 Uiso 1 1 calc R . .
C30 C 0.7391(5) 0.1921(6) 0.4147(7) 0.040(3) Uani 1 1 d . . .
H30 H 0.7370 0.2432 0.4047 0.048 Uiso 1 1 calc R . .
C31 C 0.7406(8) 0.0460(7) 0.4409(13) 0.073(5) Uani 1 1 d . . .
H31 H 0.7401 -0.0051 0.4483 0.088 Uiso 1 1 calc R . .
C32 C 0.7050(7) 0.0731(7) 0.3669(10) 0.059(4) Uani 1 1 d . . .
H32 H 0.6784 0.0409 0.3218 0.071 Uiso 1 1 calc R . .
N1 N 0.7803(5) 0.0916(7) 0.5110(8) 0.063(3) Uani 1 1 d . . .
N2 N 0.7040(4) 0.1451(6) 0.3509(7) 0.050(3) Uani 1 1 d . . .
O1 O 0.5868(3) -0.0851(3) 0.1559(4) 0.0276(15) Uani 1 1 d . . .
H1 H 0.6193 -0.1037 0.1819 0.041 Uiso 1 1 calc R . .
O2 O 0.5369(3) -0.1262(3) 0.2239(4) 0.0302(15) Uani 1 1 d . . .
H2A H 0.5279 -0.1239 0.1791 0.045 Uiso 1 1 calc R . .
O3 O 0.6579(3) -0.1748(4) 0.3316(4) 0.0329(16) Uani 1 1 d . . .
H3 H 0.6723 -0.1993 0.3182 0.049 Uiso 1 1 calc R . .
O4 O 0.6871(3) -0.1673(3) 0.2401(3) 0.0229(13) Uani 1 1 d . . .
O5 O 0.5244(3) 0.2093(4) -0.0604(5) 0.047(2) Uani 1 1 d . . .
O6 O 0.6205(3) 0.2435(4) 0.0705(5) 0.052(2) Uani 1 1 d . . .
O7 O 0.5354(3) 0.2621(4) 0.0502(5) 0.0400(17) Uani 1 1 d . . .
O8 O 0.6039(4) 0.2214(4) 0.3424(5) 0.062(2) Uani 1 1 d . . .
O9 O 0.5679(3) 0.1792(5) 0.4029(5) 0.052(2) Uani 1 1 d . . .
O10 O 0.6692(3) 0.1593(4) 0.4740(5) 0.050(2) Uani 1 1 d . . .
O11 O 0.8873(3) -0.1263(4) 0.7317(4) 0.0414(18) Uani 1 1 d . . .
O12 O 0.8088(3) -0.1601(3) 0.7211(3) 0.0269(15) Uani 1 1 d . . .
O13 O 0.8199(3) -0.0327(4) 0.7023(4) 0.0446(19) Uani 1 1 d . . .
O14 O 0.8219(3) 0.1408(3) 0.4036(4) 0.0343(16) Uani 1 1 d . . .
O15 O 0.9018(3) 0.0571(4) 0.5129(4) 0.046(2) Uani 1 1 d . . .
O16 O 0.8842(3) 0.0935(4) 0.3896(4) 0.0387(17) Uani 1 1 d . . .
O17 O 0.8167(6) 0.0686(7) 0.5882(7) 0.111(5) Uani 1 1 d . . .
O18 O 0.6681(4) 0.1713(6) 0.2743(5) 0.076(3) Uani 1 1 d . . .
O19 O 0.5849(3) -0.2648(4) 0.1560(4) 0.0334(16) Uani 1 1 d . . .
O20 O 0.7004(3) -0.2003(3) 0.1196(4) 0.0296(15) Uani 1 1 d . . .
O21 O 0.5814(3) -0.2384(4) 0.0294(4) 0.0346(16) Uani 1 1 d . . .
O22 O 0.7709(3) -0.2880(4) 0.2655(4) 0.0350(16) Uani 1 1 d . . .
O23 O 0.7993(4) -0.1271(5) 0.1888(7) 0.083(3) Uani 1 1 d . . .
O24 O 0.9916(4) -0.0853(5) 0.5199(6) 0.071(3) Uani 1 1 d . . .
O25 O 1.0775(5) 0.0527(6) 0.6532(6) 0.101(4) Uani 1 1 d . . .
O26 O 0.9410(5) -0.1607(6) 0.6087(7) 0.094(3) Uani 1 1 d . . .
O27 O 0.9275(7) -0.0003(9) 0.6806(10) 0.152(6) Uiso 1 1 d . . .
O28 O 0.4798(5) 0.3365(6) 0.1606(9) 0.117(4) Uani 1 1 d . . .
O29 O 1.0000 -0.2445(18) 0.7500 0.053(15) Uiso 0.38(5) 2 d SP A 1
O30 O 1.0303(14) -0.2285(16) 0.7473(17) 0.061(11) Uiso 0.31(2) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb O4 2.267(6) . ?
Tb O12 2.296(6) 7_646 ?
Tb O21 2.367(6) . ?
Tb O20 2.387(6) . ?
Tb O22 2.390(6) . ?
Tb O19 2.393(7) . ?
Tb O14 2.410(6) 4_645 ?
Tb O16 2.631(7) 4_645 ?
Tb S4 3.129(3) 4_645 ?
Na1 O8 2.798(9) . ?
Na1 O28 2.848(13) . ?
Na1 O23 2.862(11) 4_655 ?
Na1 O7 2.894(9) . ?
Na1 O18 2.904(11) . ?
Na1 O25 2.937(12) 8_455 ?
Na2 O26 2.745(12) . ?
Na2 O27 2.769(16) 2_756 ?
Na2 O15 2.793(8) . ?
Na2 O27 2.810(16) . ?
Na2 O25 2.822(14) . ?
Na2 O24 2.901(11) . ?
S1 O6 1.437(7) . ?
S1 O5 1.452(8) . ?
S1 O7 1.471(7) . ?
S1 C3 1.754(9) . ?
S2 O8 1.435(8) . ?
S2 O10 1.439(8) . ?
S2 O9 1.470(7) . ?
S2 C10 1.745(9) . ?
S3 O13 1.434(7) . ?
S3 O11 1.436(7) . ?
S3 O12 1.473(6) . ?
S3 C17 1.755(9) . ?
S4 O15 1.427(7) . ?
S4 O16 1.480(7) . ?
S4 O14 1.480(7) . ?
S4 C24 1.745(9) . ?
S4 Tb 3.129(3) 4_655 ?
C1 C2 1.372(12) . ?
C1 C6 1.388(12) . ?
C1 C28 1.508(12) . ?
C2 C3 1.371(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.401(12) . ?
C4 C5 1.366(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(11) . ?
C5 C7 1.503(11) . ?
C6 O1 1.369(10) . ?
C7 C8 1.510(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.385(12) . ?
C8 C13 1.388(12) . ?
C9 C10 1.391(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.379(13) . ?
C11 C12 1.399(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.361(12) . ?
C12 C14 1.546(12) . ?
C13 O2 1.371(10) . ?
C14 C15 1.506(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.373(13) . ?
C15 C20 1.386(12) . ?
C16 C17 1.382(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(12) . ?
C18 C19 1.387(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(12) . ?
C19 C21 1.514(11) . ?
C20 O3 1.364(10) . ?
C21 C22 1.555(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.369(13) . ?
C22 C27 1.396(12) . ?
C23 C24 1.389(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.377(12) . ?
C25 C26 1.394(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.422(11) . ?
C26 C28 1.509(12) . ?
C27 O4 1.333(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.358(15) . ?
C29 N1 1.358(15) . ?
C29 H29 0.9300 . ?
C30 N2 1.322(14) . ?
C30 H30 0.9300 . ?
C31 C32 1.27(2) . ?
C31 N1 1.392(19) . ?
C31 H31 0.9300 . ?
C32 N2 1.330(16) . ?
C32 H32 0.9300 . ?
N1 O17 1.293(14) . ?
N2 O18 1.305(12) . ?
O1 H1 0.8200 . ?
O2 H2A 0.8200 . ?
O3 H3 0.8200 . ?
O12 Tb 2.296(6) 7_646 ?
O14 Tb 2.410(6) 4_655 ?
O16 Tb 2.631(7) 4_655 ?
O23 Na1 2.862(11) 4_645 ?
O25 Na1 2.937(12) 8_556 ?
O27 Na2 2.769(16) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb O12 88.4(2) . 7_646 ?
O4 Tb O21 101.2(2) . . ?
O12 Tb O21 139.5(2) 7_646 . ?
O4 Tb O20 81.1(2) . . ?
O12 Tb O20 146.7(2) 7_646 . ?
O21 Tb O20 73.8(2) . . ?
O4 Tb O22 85.0(2) . . ?
O12 Tb O22 76.0(2) 7_646 . ?
O21 Tb O22 143.5(2) . . ?
O20 Tb O22 71.7(2) . . ?
O4 Tb O19 77.8(2) . . ?
O12 Tb O19 72.9(2) 7_646 . ?
O21 Tb O19 71.0(2) . . ?
O20 Tb O19 134.0(2) . . ?
O22 Tb O19 144.6(2) . . ?
O4 Tb O14 152.7(2) . 4_645 ?
O12 Tb O14 106.6(2) 7_646 4_645 ?
O21 Tb O14 82.3(2) . 4_645 ?
O20 Tb O14 73.9(2) . 4_645 ?
O22 Tb O14 77.1(2) . 4_645 ?
O19 Tb O14 127.9(2) . 4_645 ?
O4 Tb O16 151.8(2) . 4_645 ?
O12 Tb O16 72.8(2) 7_646 4_645 ?
O21 Tb O16 81.5(2) . 4_645 ?
O20 Tb O16 125.9(2) . 4_645 ?
O22 Tb O16 109.7(2) . 4_645 ?
O19 Tb O16 76.7(2) . 4_645 ?
O14 Tb O16 55.3(2) 4_645 4_645 ?
O4 Tb S4 178.53(17) . 4_645 ?
O12 Tb S4 90.47(17) 7_646 4_645 ?
O21 Tb S4 80.26(18) . 4_645 ?
O20 Tb S4 99.43(16) . 4_645 ?
O22 Tb S4 93.91(17) . 4_645 ?
O19 Tb S4 102.71(17) . 4_645 ?
O14 Tb S4 27.24(16) 4_645 4_645 ?
O16 Tb S4 28.10(14) 4_645 4_645 ?
O8 Na1 O28 82.4(4) . . ?
O8 Na1 O23 104.7(3) . 4_655 ?
O28 Na1 O23 135.4(3) . 4_655 ?
O8 Na1 O7 134.1(3) . . ?
O28 Na1 O7 91.0(3) . . ?
O23 Na1 O7 111.2(3) 4_655 . ?
O8 Na1 O18 72.7(3) . . ?
O28 Na1 O18 142.4(3) . . ?
O23 Na1 O18 79.3(3) 4_655 . ?
O7 Na1 O18 86.8(2) . . ?
O8 Na1 O25 143.3(3) . 8_455 ?
O28 Na1 O25 81.2(4) . 8_455 ?
O23 Na1 O25 66.9(3) 4_655 8_455 ?
O7 Na1 O25 78.8(3) . 8_455 ?
O18 Na1 O25 134.6(3) . 8_455 ?
O26 Na2 O27 109.4(4) . 2_756 ?
O26 Na2 O15 98.2(3) . . ?
O27 Na2 O15 129.1(4) 2_756 . ?
O26 Na2 O27 76.6(4) . . ?
O27 Na2 O27 72.4(6) 2_756 . ?
O15 Na2 O27 73.6(4) . . ?
O26 Na2 O25 145.0(4) . . ?
O27 Na2 O25 88.5(4) 2_756 . ?
O15 Na2 O25 92.6(3) . . ?
O27 Na2 O25 138.4(4) . . ?
O26 Na2 O24 77.8(3) . . ?
O27 Na2 O24 144.4(4) 2_756 . ?
O15 Na2 O24 81.9(3) . . ?
O27 Na2 O24 141.4(4) . . ?
O25 Na2 O24 70.8(3) . . ?
O6 S1 O5 112.2(5) . . ?
O6 S1 O7 112.8(5) . . ?
O5 S1 O7 110.9(4) . . ?
O6 S1 C3 106.9(4) . . ?
O5 S1 C3 107.0(4) . . ?
O7 S1 C3 106.7(4) . . ?
O8 S2 O10 110.9(5) . . ?
O8 S2 O9 111.6(5) . . ?
O10 S2 O9 112.5(5) . . ?
O8 S2 C10 107.8(5) . . ?
O10 S2 C10 106.9(5) . . ?
O9 S2 C10 106.9(4) . . ?
O13 S3 O11 114.4(5) . . ?
O13 S3 O12 110.1(4) . . ?
O11 S3 O12 111.1(4) . . ?
O13 S3 C17 108.0(4) . . ?
O11 S3 C17 108.0(4) . . ?
O12 S3 C17 104.8(4) . . ?
O15 S4 O16 115.4(5) . . ?
O15 S4 O14 114.2(4) . . ?
O16 S4 O14 105.1(4) . . ?
O15 S4 C24 107.4(4) . . ?
O16 S4 C24 109.0(4) . . ?
O14 S4 C24 105.3(4) . . ?
O15 S4 Tb 131.8(3) . 4_655 ?
O16 S4 Tb 56.9(3) . 4_655 ?
O14 S4 Tb 48.2(3) . 4_655 ?
C24 S4 Tb 120.2(3) . 4_655 ?
C2 C1 C6 118.1(8) . . ?
C2 C1 C28 120.2(8) . . ?
C6 C1 C28 121.7(8) . . ?
C3 C2 C1 122.1(8) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 119.1(8) . . ?
C2 C3 S1 121.9(7) . . ?
C4 C3 S1 119.1(7) . . ?
C5 C4 C3 121.1(8) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 118.1(8) . . ?
C4 C5 C7 121.8(8) . . ?
C6 C5 C7 119.8(8) . . ?
O1 C6 C1 123.3(8) . . ?
O1 C6 C5 115.1(7) . . ?
C1 C6 C5 121.6(8) . . ?
C5 C7 C8 110.5(7) . . ?
C5 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C5 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C13 118.4(8) . . ?
C9 C8 C7 119.6(8) . . ?
C13 C8 C7 122.0(8) . . ?
C8 C9 C10 121.3(8) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C11 C10 C9 118.7(8) . . ?
C11 C10 S2 120.6(7) . . ?
C9 C10 S2 120.8(7) . . ?
C10 C11 C12 120.5(8) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.5(8) . . ?
C13 C12 C14 121.3(8) . . ?
C11 C12 C14 119.2(8) . . ?
C12 C13 O2 117.3(8) . . ?
C12 C13 C8 121.3(8) . . ?
O2 C13 C8 121.4(7) . . ?
C15 C14 C12 111.3(7) . . ?
C15 C14 H14A 109.4 . . ?
C12 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C12 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 118.4(9) . . ?
C16 C15 C14 121.1(8) . . ?
C20 C15 C14 120.5(8) . . ?
C15 C16 C17 120.8(8) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 120.4(8) . . ?
C18 C17 S3 123.1(7) . . ?
C16 C17 S3 116.4(7) . . ?
C17 C18 C19 120.0(9) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 118.7(8) . . ?
C20 C19 C21 120.9(8) . . ?
C18 C19 C21 120.4(8) . . ?
O3 C20 C15 115.9(8) . . ?
O3 C20 C19 122.5(7) . . ?
C15 C20 C19 121.5(8) . . ?
C19 C21 C22 111.3(7) . . ?
C19 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
C19 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C23 C22 C27 120.8(8) . . ?
C23 C22 C21 118.8(8) . . ?
C27 C22 C21 120.3(8) . . ?
C22 C23 C24 120.2(9) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 120.2(8) . . ?
C25 C24 S4 118.5(7) . . ?
C23 C24 S4 121.1(7) . . ?
C24 C25 C26 120.8(8) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 118.7(8) . . ?
C25 C26 C28 119.7(8) . . ?
C27 C26 C28 121.6(8) . . ?
O4 C27 C22 121.5(7) . . ?
O4 C27 C26 119.3(7) . . ?
C22 C27 C26 119.2(8) . . ?
C1 C28 C26 113.9(7) . . ?
C1 C28 H28A 108.8 . . ?
C26 C28 H28A 108.8 . . ?
C1 C28 H28B 108.8 . . ?
C26 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C30 C29 N1 121.3(11) . . ?
C30 C29 H29 119.4 . . ?
N1 C29 H29 119.4 . . ?
N2 C30 C29 119.7(11) . . ?
N2 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 N1 121.1(13) . . ?
C32 C31 H31 119.5 . . ?
N1 C31 H31 119.5 . . ?
C31 C32 N2 123.1(14) . . ?
C31 C32 H32 118.4 . . ?
N2 C32 H32 118.4 . . ?
O17 N1 C29 119.6(14) . . ?
O17 N1 C31 124.6(14) . . ?
C29 N1 C31 115.7(12) . . ?
O18 N2 C30 119.0(11) . . ?
O18 N2 C32 122.0(12) . . ?
C30 N2 C32 119.0(11) . . ?
C6 O1 H1 109.5 . . ?
C13 O2 H2A 109.5 . . ?
C20 O3 H3 109.5 . . ?
C27 O4 Tb 139.8(5) . . ?
S1 O7 Na1 124.2(4) . . ?
S2 O8 Na1 165.1(5) . . ?
S3 O12 Tb 147.1(4) . 7_646 ?
S4 O14 Tb 104.6(3) . 4_655 ?
S4 O15 Na2 151.0(5) . . ?
S4 O16 Tb 95.0(3) . 4_655 ?
N2 O18 Na1 122.6(7) . . ?
Na2 O25 Na1 106.9(4) . 8_556 ?
Na2 O27 Na2 104.2(5) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.9(13) . . . . ?
C28 C1 C2 C3 179.8(8) . . . . ?
C1 C2 C3 C4 1.3(13) . . . . ?
C1 C2 C3 S1 -178.1(7) . . . . ?
O6 S1 C3 C2 -32.7(9) . . . . ?
O5 S1 C3 C2 87.6(8) . . . . ?
O7 S1 C3 C2 -153.6(8) . . . . ?
O6 S1 C3 C4 147.9(8) . . . . ?
O5 S1 C3 C4 -91.7(8) . . . . ?
O7 S1 C3 C4 27.0(9) . . . . ?
C2 C3 C4 C5 -1.1(13) . . . . ?
S1 C3 C4 C5 178.3(7) . . . . ?
C3 C4 C5 C6 0.6(13) . . . . ?
C3 C4 C5 C7 174.2(8) . . . . ?
C2 C1 C6 O1 179.8(8) . . . . ?
C28 C1 C6 O1 -0.9(13) . . . . ?
C2 C1 C6 C5 0.3(13) . . . . ?
C28 C1 C6 C5 179.6(8) . . . . ?
C4 C5 C6 O1 -179.7(7) . . . . ?
C7 C5 C6 O1 6.5(11) . . . . ?
C4 C5 C6 C1 -0.2(12) . . . . ?
C7 C5 C6 C1 -174.0(8) . . . . ?
C4 C5 C7 C8 -102.1(10) . . . . ?
C6 C5 C7 C8 71.4(10) . . . . ?
C5 C7 C8 C9 70.4(10) . . . . ?
C5 C7 C8 C13 -110.5(9) . . . . ?
C13 C8 C9 C10 2.9(13) . . . . ?
C7 C8 C9 C10 -177.9(8) . . . . ?
C8 C9 C10 C11 0.7(13) . . . . ?
C8 C9 C10 S2 -178.5(7) . . . . ?
O8 S2 C10 C11 158.7(8) . . . . ?
O10 S2 C10 C11 39.5(9) . . . . ?
O9 S2 C10 C11 -81.2(8) . . . . ?
O8 S2 C10 C9 -22.0(9) . . . . ?
O10 S2 C10 C9 -141.3(8) . . . . ?
O9 S2 C10 C9 98.0(8) . . . . ?
C9 C10 C11 C12 -2.2(13) . . . . ?
S2 C10 C11 C12 177.1(7) . . . . ?
C10 C11 C12 C13 0.0(13) . . . . ?
C10 C11 C12 C14 177.4(8) . . . . ?
C11 C12 C13 O2 -175.9(7) . . . . ?
C14 C12 C13 O2 6.8(12) . . . . ?
C11 C12 C13 C8 3.8(13) . . . . ?
C14 C12 C13 C8 -173.5(8) . . . . ?
C9 C8 C13 C12 -5.2(12) . . . . ?
C7 C8 C13 C12 175.6(8) . . . . ?
C9 C8 C13 O2 174.5(8) . . . . ?
C7 C8 C13 O2 -4.7(12) . . . . ?
C13 C12 C14 C15 108.5(10) . . . . ?
C11 C12 C14 C15 -68.9(10) . . . . ?
C12 C14 C15 C16 102.5(10) . . . . ?
C12 C14 C15 C20 -75.3(11) . . . . ?
C20 C15 C16 C17 0.8(13) . . . . ?
C14 C15 C16 C17 -177.0(8) . . . . ?
C15 C16 C17 C18 -1.2(13) . . . . ?
C15 C16 C17 S3 -177.8(7) . . . . ?
O13 S3 C17 C18 120.3(8) . . . . ?
O11 S3 C17 C18 -3.9(9) . . . . ?
O12 S3 C17 C18 -122.4(8) . . . . ?
O13 S3 C17 C16 -63.1(8) . . . . ?
O11 S3 C17 C16 172.7(7) . . . . ?
O12 S3 C17 C16 54.2(8) . . . . ?
C16 C17 C18 C19 2.5(13) . . . . ?
S3 C17 C18 C19 178.9(7) . . . . ?
C17 C18 C19 C20 -3.4(13) . . . . ?
C17 C18 C19 C21 177.8(8) . . . . ?
C16 C15 C20 O3 179.2(8) . . . . ?
C14 C15 C20 O3 -3.0(12) . . . . ?
C16 C15 C20 C19 -1.8(13) . . . . ?
C14 C15 C20 C19 176.0(8) . . . . ?
C18 C19 C20 O3 -177.9(8) . . . . ?
C21 C19 C20 O3 0.9(13) . . . . ?
C18 C19 C20 C15 3.1(13) . . . . ?
C21 C19 C20 C15 -178.1(8) . . . . ?
C20 C19 C21 C22 77.5(10) . . . . ?
C18 C19 C21 C22 -103.7(9) . . . . ?
C19 C21 C22 C23 77.7(10) . . . . ?
C19 C21 C22 C27 -99.7(9) . . . . ?
C27 C22 C23 C24 1.8(13) . . . . ?
C21 C22 C23 C24 -175.6(8) . . . . ?
C22 C23 C24 C25 -1.8(13) . . . . ?
C22 C23 C24 S4 174.2(7) . . . . ?
O15 S4 C24 C25 177.8(7) . . . . ?
O16 S4 C24 C25 -56.5(8) . . . . ?
O14 S4 C24 C25 55.7(8) . . . . ?
Tb S4 C24 C25 5.6(8) 4_655 . . . ?
O15 S4 C24 C23 1.8(9) . . . . ?
O16 S4 C24 C23 127.4(8) . . . . ?
O14 S4 C24 C23 -120.3(8) . . . . ?
Tb S4 C24 C23 -170.5(6) 4_655 . . . ?
C23 C24 C25 C26 1.0(13) . . . . ?
S4 C24 C25 C26 -175.1(6) . . . . ?
C24 C25 C26 C27 -0.2(12) . . . . ?
C24 C25 C26 C28 178.1(8) . . . . ?
C23 C22 C27 O4 -179.0(8) . . . . ?
C21 C22 C27 O4 -1.6(12) . . . . ?
C23 C22 C27 C26 -1.0(12) . . . . ?
C21 C22 C27 C26 176.4(7) . . . . ?
C25 C26 C27 O4 178.2(7) . . . . ?
C28 C26 C27 O4 0.0(11) . . . . ?
C25 C26 C27 C22 0.2(11) . . . . ?
C28 C26 C27 C22 -178.1(7) . . . . ?
C2 C1 C28 C26 104.8(9) . . . . ?
C6 C1 C28 C26 -74.5(11) . . . . ?
C25 C26 C28 C1 -79.4(10) . . . . ?
C27 C26 C28 C1 98.9(9) . . . . ?
N1 C29 C30 N2 -2.6(16) . . . . ?
N1 C31 C32 N2 2(2) . . . . ?
C30 C29 N1 O17 -177.7(11) . . . . ?
C30 C29 N1 C31 0.3(16) . . . . ?
C32 C31 N1 O17 178.0(12) . . . . ?
C32 C31 N1 C29 0.1(18) . . . . ?
C29 C30 N2 O18 -177.8(10) . . . . ?
C29 C30 N2 C32 4.4(15) . . . . ?
C31 C32 N2 O18 178.1(12) . . . . ?
C31 C32 N2 C30 -4.2(19) . . . . ?
C22 C27 O4 Tb -93.0(9) . . . . ?
C26 C27 O4 Tb 89.0(9) . . . . ?
O12 Tb O4 C27 106.9(8) 7_646 . . . ?
O21 Tb O4 C27 -112.8(8) . . . . ?
O20 Tb O4 C27 -41.4(8) . . . . ?
O22 Tb O4 C27 30.8(8) . . . . ?
O19 Tb O4 C27 179.8(8) . . . . ?
O14 Tb O4 C27 -17.8(10) 4_645 . . . ?
O16 Tb O4 C27 154.2(7) 4_645 . . . ?
S4 Tb O4 C27 70(6) 4_645 . . . ?
O6 S1 O7 Na1 -52.8(6) . . . . ?
O5 S1 O7 Na1 -179.7(4) . . . . ?
C3 S1 O7 Na1 64.2(5) . . . . ?
O8 Na1 O7 S1 -81.8(6) . . . . ?
O28 Na1 O7 S1 -162.2(5) . . . . ?
O23 Na1 O7 S1 57.4(5) 4_655 . . . ?
O18 Na1 O7 S1 -19.8(5) . . . . ?
O25 Na1 O7 S1 117.0(5) 8_455 . . . ?
O10 S2 O8 Na1 106(2) . . . . ?
O9 S2 O8 Na1 -128(2) . . . . ?
C10 S2 O8 Na1 -11(3) . . . . ?
O28 Na1 O8 S2 110(2) . . . . ?
O23 Na1 O8 S2 -115(2) 4_655 . . . ?
O7 Na1 O8 S2 26(3) . . . . ?
O18 Na1 O8 S2 -41(2) . . . . ?
O25 Na1 O8 S2 174(2) 8_455 . . . ?
O13 S3 O12 Tb -89.5(8) . . . 7_646 ?
O11 S3 O12 Tb 38.3(8) . . . 7_646 ?
C17 S3 O12 Tb 154.6(7) . . . 7_646 ?
O15 S4 O14 Tb 125.4(4) . . . 4_655 ?
O16 S4 O14 Tb -2.1(4) . . . 4_655 ?
C24 S4 O14 Tb -117.1(4) . . . 4_655 ?
O16 S4 O15 Na2 -51.8(10) . . . . ?
O14 S4 O15 Na2 -173.7(8) . . . . ?
C24 S4 O15 Na2 69.9(10) . . . . ?
Tb S4 O15 Na2 -119.1(7) 4_655 . . . ?
O26 Na2 O15 S4 -73.0(9) . . . . ?
O27 Na2 O15 S4 163.8(9) 2_756 . . . ?
O27 Na2 O15 S4 -146.4(10) . . . . ?
O25 Na2 O15 S4 73.6(9) . . . . ?
O24 Na2 O15 S4 3.4(9) . . . . ?
O15 S4 O16 Tb -124.9(4) . . . 4_655 ?
O14 S4 O16 Tb 1.8(4) . . . 4_655 ?
C24 S4 O16 Tb 114.2(4) . . . 4_655 ?
C30 N2 O18 Na1 -50.1(12) . . . . ?
C32 N2 O18 Na1 127.6(10) . . . . ?
O8 Na1 O18 N2 -32.0(8) . . . . ?
O28 Na1 O18 N2 -83.0(10) . . . . ?
O23 Na1 O18 N2 77.3(8) 4_655 . . . ?
O7 Na1 O18 N2 -170.4(8) . . . . ?
O25 Na1 O18 N2 118.9(8) 8_455 . . . ?
O26 Na2 O25 Na1 -179.7(5) . . . 8_556 ?
O27 Na2 O25 Na1 -57.0(5) 2_756 . . 8_556 ?
O15 Na2 O25 Na1 72.0(3) . . . 8_556 ?
O27 Na2 O25 Na1 3.9(7) . . . 8_556 ?
O24 Na2 O25 Na1 152.5(4) . . . 8_556 ?
O26 Na2 O27 Na2 95.5(5) . . . 2_756 ?
O27 Na2 O27 Na2 -20.2(7) 2_756 . . 2_756 ?
O15 Na2 O27 Na2 -161.7(6) . . . 2_756 ?
O25 Na2 O27 Na2 -86.7(7) . . . 2_756 ?
O24 Na2 O27 Na2 145.4(4) . . . 2_756 ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.45
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         9.188
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.177

# Attachment 'Eu.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 682900'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H44 Eu N2 Na2 O28.50 S4'
_chemical_formula_weight         1238.87

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'
Na Na 0.0362 0.0249 '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           Monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   31.695(3)
_cell_length_b                   17.9061(12)
_cell_length_c                   22.221(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 133.979(2)
_cell_angle_gamma                90.00
_cell_volume                     9074.9(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       bolck
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5016
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25738
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0966
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         26.85
_reflns_number_total             9603
_reflns_number_gt                6193
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

_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.

Some Q-peaks have large electron density due to the weak crystal diffraction
of these compounds. It is chemical unreasonable to define a atom at the
position because the Q-peak has short distance with the neighboring
oxygen atoms.
;

_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)+(0.0876P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9603
_refine_ls_number_parameters     632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1622
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Eu Eu 0.666182(16) -0.275119(19) 0.16818(2) 0.01875(12) Uani 1 1 d . . .
Na1 Na 0.59054(14) 0.29801(19) 0.2195(2) 0.0383(8) Uani 1 1 d . . .
Na2 Na 0.99847(15) -0.0285(2) 0.6489(2) 0.0448(9) Uani 1 1 d . . .
S1 S 0.56344(9) 0.21572(11) 0.02969(13) 0.0308(5) Uani 1 1 d . . .
S2 S 0.60876(9) 0.16551(12) 0.39360(14) 0.0336(5) Uani 1 1 d . . .
S3 S 0.82830(9) -0.10855(10) 0.69155(12) 0.0265(4) Uani 1 1 d . . .
S4 S 0.85985(8) 0.07509(10) 0.42602(12) 0.0244(4) Uani 1 1 d . . .
C1 C 0.6231(3) 0.0086(4) 0.1216(4) 0.0210(15) Uani 1 1 d . . .
C2 C 0.6162(3) 0.0794(4) 0.0923(4) 0.0238(16) Uani 1 1 d . . .
H2 H 0.6413 0.0963 0.0871 0.029 Uiso 1 1 calc R . .
C3 C 0.5729(3) 0.1257(4) 0.0706(5) 0.0240(16) Uani 1 1 d . . .
C4 C 0.5350(3) 0.1014(4) 0.0774(5) 0.0230(16) Uani 1 1 d . . .
H4 H 0.5056 0.1330 0.0620 0.028 Uiso 1 1 calc R . .
C5 C 0.5403(3) 0.0314(4) 0.1065(4) 0.0221(15) Uani 1 1 d . . .
C6 C 0.5843(3) -0.0145(4) 0.1284(4) 0.0225(15) Uani 1 1 d . . .
C7 C 0.5029(3) 0.0076(4) 0.1223(4) 0.0225(15) Uani 1 1 d . . .
H7A H 0.4875 -0.0421 0.0997 0.027 Uiso 1 1 calc R . .
H7B H 0.4700 0.0415 0.0939 0.027 Uiso 1 1 calc R . .
C8 C 0.5388(3) 0.0075(4) 0.2158(4) 0.0227(15) Uani 1 1 d . . .
C9 C 0.5556(3) 0.0760(4) 0.2571(4) 0.0224(15) Uani 1 1 d . . .
H9 H 0.5434 0.1202 0.2270 0.027 Uiso 1 1 calc R . .
C10 C 0.5903(3) 0.0788(4) 0.3431(5) 0.0279(17) Uani 1 1 d . . .
C11 C 0.6089(3) 0.0122(4) 0.3874(5) 0.0270(17) Uani 1 1 d . . .
H11 H 0.6335 0.0139 0.4451 0.032 Uiso 1 1 calc R . .
C12 C 0.5918(3) -0.0569(4) 0.3479(5) 0.0255(16) Uani 1 1 d . . .
C13 C 0.5558(3) -0.0578(4) 0.2614(5) 0.0231(16) Uani 1 1 d . . .
C14 C 0.6151(3) -0.1274(4) 0.3989(5) 0.0264(17) Uani 1 1 d . . .
H14A H 0.5944 -0.1700 0.3617 0.032 Uiso 1 1 calc R . .
H14B H 0.6078 -0.1264 0.4347 0.032 Uiso 1 1 calc R . .
C15 C 0.6803(3) -0.1365(4) 0.4522(5) 0.0262(17) Uani 1 1 d . . .
C16 C 0.7206(3) -0.1211(4) 0.5363(5) 0.0253(16) Uani 1 1 d . . .
H16 H 0.7078 -0.1066 0.5616 0.030 Uiso 1 1 calc R . .
C17 C 0.7809(3) -0.1271(4) 0.5845(5) 0.0243(16) Uani 1 1 d . . .
C18 C 0.8002(3) -0.1488(4) 0.5479(5) 0.0253(17) Uani 1 1 d . . .
H18 H 0.8402 -0.1537 0.5804 0.030 Uiso 1 1 calc R . .
C19 C 0.7602(3) -0.1638(4) 0.4617(5) 0.0211(15) Uani 1 1 d . . .
C20 C 0.6997(3) -0.1585(4) 0.4147(5) 0.0240(16) Uani 1 1 d . . .
C21 C 0.7807(3) -0.1846(4) 0.4196(5) 0.0218(15) Uani 1 1 d . . .
H21A H 0.7576 -0.2262 0.3820 0.026 Uiso 1 1 calc R . .
H21B H 0.8213 -0.2006 0.4617 0.026 Uiso 1 1 calc R . .
C22 C 0.7753(3) -0.1192(4) 0.3705(5) 0.0202(15) Uani 1 1 d . . .
C23 C 0.8172(3) -0.0624(4) 0.4138(5) 0.0254(16) Uani 1 1 d . . .
H23 H 0.8489 -0.0661 0.4714 0.030 Uiso 1 1 calc R . .
C24 C 0.8118(3) -0.0003(4) 0.3713(5) 0.0233(16) Uani 1 1 d . . .
C25 C 0.7650(3) 0.0055(4) 0.2855(5) 0.0225(15) Uani 1 1 d . . .
H25 H 0.7615 0.0477 0.2580 0.027 Uiso 1 1 calc R . .
C26 C 0.7229(3) -0.0508(4) 0.2396(5) 0.0217(15) Uani 1 1 d . . .
C27 C 0.7287(3) -0.1145(3) 0.2836(4) 0.0183(14) Uani 1 1 d . . .
C28 C 0.6713(3) -0.0415(4) 0.1461(4) 0.0216(15) Uani 1 1 d . . .
H28A H 0.6855 -0.0213 0.1223 0.026 Uiso 1 1 calc R . .
H28B H 0.6548 -0.0904 0.1215 0.026 Uiso 1 1 calc R . .
C29 C 0.7778(4) 0.1660(5) 0.4938(7) 0.046(2) Uani 1 1 d . . .
H29 H 0.8031 0.1998 0.5372 0.055 Uiso 1 1 calc R . .
C30 C 0.7393(4) 0.1912(5) 0.4152(6) 0.036(2) Uani 1 1 d . . .
H30 H 0.7371 0.2421 0.4051 0.043 Uiso 1 1 calc R . .
C31 C 0.7412(6) 0.0465(6) 0.4429(11) 0.074(4) Uani 1 1 d . . .
H31 H 0.7404 -0.0040 0.4518 0.088 Uiso 1 1 calc R . .
C32 C 0.7054(6) 0.0720(6) 0.3670(9) 0.062(3) Uani 1 1 d . . .
H32 H 0.6803 0.0390 0.3226 0.074 Uiso 1 1 calc R . .
N1 N 0.7812(4) 0.0937(6) 0.5121(7) 0.062(3) Uani 1 1 d . . .
N2 N 0.7038(4) 0.1442(5) 0.3509(6) 0.051(2) Uani 1 1 d . . .
O1 O 0.5874(2) -0.0847(3) 0.1570(4) 0.0297(13) Uani 1 1 d . . .
H1 H 0.6160 -0.1070 0.1721 0.045 Uiso 1 1 calc R . .
O2 O 0.5372(2) -0.1256(3) 0.2237(3) 0.0298(12) Uani 1 1 d . . .
H2A H 0.5371 -0.1265 0.1866 0.045 Uiso 1 1 calc R . .
O3 O 0.6579(2) -0.1737(3) 0.3317(3) 0.0313(13) Uani 1 1 d . . .
H3 H 0.6727 -0.1967 0.3182 0.047 Uiso 1 1 calc R . .
O4 O 0.6868(2) -0.1674(2) 0.2397(3) 0.0217(11) Uani 1 1 d . . .
O5 O 0.5245(3) 0.2077(3) -0.0603(4) 0.0446(16) Uani 1 1 d . . .
O6 O 0.6201(2) 0.2419(3) 0.0691(4) 0.0492(18) Uani 1 1 d . . .
O7 O 0.5351(3) 0.2613(3) 0.0484(4) 0.0403(15) Uani 1 1 d . . .
O8 O 0.6033(4) 0.2215(3) 0.3419(5) 0.063(2) Uani 1 1 d . . .
O9 O 0.5681(3) 0.1780(4) 0.4030(4) 0.0522(18) Uani 1 1 d . . .
O10 O 0.6685(3) 0.1583(4) 0.4741(4) 0.0498(17) Uani 1 1 d . . .
O11 O 0.8870(2) -0.1269(3) 0.7303(4) 0.0392(14) Uani 1 1 d . . .
O12 O 0.8086(2) -0.1596(3) 0.7198(3) 0.0281(12) Uani 1 1 d . . .
O13 O 0.8204(3) -0.0329(3) 0.7018(4) 0.0474(16) Uani 1 1 d . . .
O14 O 0.8232(2) 0.1401(3) 0.4072(4) 0.0328(13) Uani 1 1 d . . .
O15 O 0.9029(3) 0.0563(3) 0.5132(4) 0.0443(16) Uani 1 1 d . . .
O16 O 0.8841(2) 0.0933(3) 0.3903(4) 0.0339(13) Uani 1 1 d . . .
O17 O 0.8174(5) 0.0705(6) 0.5891(7) 0.116(4) Uani 1 1 d . . .
O18 O 0.6683(3) 0.1702(6) 0.2740(5) 0.078(3) Uani 1 1 d . . .
O19 O 0.5841(2) -0.2653(3) 0.1557(4) 0.0340(13) Uani 1 1 d . . .
O20 O 0.6998(3) -0.2003(3) 0.1183(4) 0.0310(13) Uani 1 1 d . . .
O21 O 0.5806(2) -0.2379(3) 0.0279(4) 0.0345(13) Uani 1 1 d . . .
O22 O 0.7720(2) -0.2884(3) 0.2662(4) 0.0391(14) Uani 1 1 d . . .
O23 O 0.8002(3) -0.1264(4) 0.1902(6) 0.083(3) Uani 1 1 d . . .
O24 O 0.9916(3) -0.0858(4) 0.5192(5) 0.068(2) Uani 1 1 d . . .
O25 O 1.0768(4) 0.0519(5) 0.6523(6) 0.098(3) Uani 1 1 d . . .
O26 O 0.9403(5) -0.1620(5) 0.6070(7) 0.099(3) Uani 1 1 d . . .
O27 O 0.9266(5) -0.0015(10) 0.6788(8) 0.168(6) Uani 1 1 d . . .
O28 O 0.4789(5) 0.3360(6) 0.1584(7) 0.115(4) Uani 1 1 d . . .
O29 O 1.0000 -0.2448(13) 0.7500 0.054(11) Uiso 0.42(4) 2 d SP A 1
O30 O 1.0327(12) -0.2270(14) 0.7519(17) 0.065(10) Uiso 0.29(2) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu O4 2.286(5) . ?
Eu O12 2.332(5) 7_646 ?
Eu O21 2.403(5) . ?
Eu O20 2.408(5) . ?
Eu O19 2.424(5) . ?
Eu O22 2.430(5) . ?
Eu O14 2.451(5) 4_645 ?
Eu O16 2.628(6) 4_645 ?
Eu S4 3.1398(18) 4_645 ?
Na1 O8 2.812(7) . ?
Na1 O28 2.856(11) . ?
Na1 O23 2.863(9) 4_655 ?
Na1 O18 2.937(10) . ?
Na1 O7 2.948(7) . ?
Na1 O25 2.956(10) 8_455 ?
Na2 O26 2.757(10) . ?
Na2 O15 2.808(7) . ?
Na2 O27 2.812(13) 2_756 ?
Na2 O27 2.822(13) . ?
Na2 O25 2.825(11) . ?
Na2 O24 2.920(9) . ?
S1 O6 1.424(6) . ?
S1 O5 1.455(6) . ?
S1 O7 1.472(6) . ?
S1 C3 1.771(7) . ?
S2 O8 1.442(7) . ?
S2 O10 1.448(7) . ?
S2 O9 1.459(6) . ?
S2 C10 1.762(8) . ?
S3 O13 1.424(6) . ?
S3 O11 1.444(6) . ?
S3 O12 1.471(5) . ?
S3 C17 1.750(8) . ?
S4 O15 1.434(6) . ?
S4 O16 1.474(5) . ?
S4 O14 1.484(5) . ?
S4 C24 1.746(7) . ?
S4 Eu 3.1398(18) 4_655 ?
C1 C2 1.372(10) . ?
C1 C6 1.401(10) . ?
C1 C28 1.509(10) . ?
C2 C3 1.372(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(10) . ?
C4 C5 1.366(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(10) . ?
C5 C7 1.512(10) . ?
C6 O1 1.382(8) . ?
C7 C8 1.525(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.387(10) . ?
C8 C9 1.399(10) . ?
C9 C10 1.393(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.390(11) . ?
C11 C12 1.392(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.397(10) . ?
C12 C14 1.504(10) . ?
C13 O2 1.356(8) . ?
C14 C15 1.517(10) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.373(10) . ?
C15 C20 1.394(10) . ?
C16 C17 1.403(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.372(10) . ?
C18 C19 1.405(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.411(10) . ?
C19 C21 1.510(9) . ?
C20 O3 1.355(9) . ?
C21 C22 1.528(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.397(10) . ?
C22 C27 1.400(10) . ?
C23 C24 1.389(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.385(10) . ?
C25 C26 1.395(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.429(9) . ?
C26 C28 1.517(10) . ?
C27 O4 1.346(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.335(13) . ?
C29 N1 1.339(13) . ?
C29 H29 0.9300 . ?
C30 N2 1.336(12) . ?
C30 H30 0.9300 . ?
C31 C32 1.298(17) . ?
C31 N1 1.406(17) . ?
C31 H31 0.9300 . ?
C32 N2 1.332(14) . ?
C32 H32 0.9300 . ?
N1 O17 1.300(12) . ?
N2 O18 1.315(11) . ?
O1 H1 0.8200 . ?
O2 H2A 0.8200 . ?
O3 H3 0.8200 . ?
O12 Eu 2.332(5) 7_646 ?
O14 Eu 2.451(5) 4_655 ?
O16 Eu 2.628(6) 4_655 ?
O23 Na1 2.863(9) 4_645 ?
O25 Na1 2.956(10) 8_556 ?
O27 Na2 2.812(13) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Eu O12 87.75(17) . 7_646 ?
O4 Eu O21 100.85(18) . . ?
O12 Eu O21 139.90(18) 7_646 . ?
O4 Eu O20 81.14(17) . . ?
O12 Eu O20 146.83(19) 7_646 . ?
O21 Eu O20 73.17(19) . . ?
O4 Eu O19 77.59(18) . . ?
O12 Eu O19 72.75(18) 7_646 . ?
O21 Eu O19 71.12(19) . . ?
O20 Eu O19 133.63(18) . . ?
O4 Eu O22 84.76(19) . . ?
O12 Eu O22 75.97(19) 7_646 . ?
O21 Eu O22 143.32(19) . . ?
O20 Eu O22 72.0(2) . . ?
O19 Eu O22 144.4(2) . . ?
O4 Eu O14 152.69(17) . 4_645 ?
O12 Eu O14 108.10(18) 7_646 4_645 ?
O21 Eu O14 81.51(19) . 4_645 ?
O20 Eu O14 73.47(17) . 4_645 ?
O19 Eu O14 127.78(18) . 4_645 ?
O22 Eu O14 78.04(19) . 4_645 ?
O4 Eu O16 151.99(16) . 4_645 ?
O12 Eu O16 73.69(18) 7_646 4_645 ?
O21 Eu O16 81.73(18) . 4_645 ?
O20 Eu O16 125.53(17) . 4_645 ?
O19 Eu O16 76.95(17) . 4_645 ?
O22 Eu O16 109.96(18) . 4_645 ?
O14 Eu O16 55.26(16) 4_645 4_645 ?
O4 Eu S4 178.67(14) . 4_645 ?
O12 Eu S4 91.15(13) 7_646 4_645 ?
O21 Eu S4 80.48(14) . 4_645 ?
O20 Eu S4 99.41(13) . 4_645 ?
O19 Eu S4 102.79(14) . 4_645 ?
O22 Eu S4 94.25(14) . 4_645 ?
O14 Eu S4 27.41(12) 4_645 4_645 ?
O16 Eu S4 27.85(12) 4_645 4_645 ?
O8 Na1 O28 82.8(3) . . ?
O8 Na1 O23 105.1(3) . 4_655 ?
O28 Na1 O23 135.8(3) . 4_655 ?
O8 Na1 O18 72.8(2) . . ?
O28 Na1 O18 142.1(3) . . ?
O23 Na1 O18 79.6(2) 4_655 . ?
O8 Na1 O7 134.0(2) . . ?
O28 Na1 O7 90.4(3) . . ?
O23 Na1 O7 110.9(3) 4_655 . ?
O18 Na1 O7 86.3(2) . . ?
O8 Na1 O25 143.5(3) . 8_455 ?
O28 Na1 O25 81.0(3) . 8_455 ?
O23 Na1 O25 66.8(3) 4_655 8_455 ?
O18 Na1 O25 134.7(3) . 8_455 ?
O7 Na1 O25 78.7(2) . 8_455 ?
O26 Na2 O15 97.9(3) . . ?
O26 Na2 O27 110.1(4) . 2_756 ?
O15 Na2 O27 129.1(4) . 2_756 ?
O26 Na2 O27 76.6(4) . . ?
O15 Na2 O27 73.5(3) . . ?
O27 Na2 O27 72.9(4) 2_756 . ?
O26 Na2 O25 145.1(3) . . ?
O15 Na2 O25 91.5(2) . . ?
O27 Na2 O25 88.9(4) 2_756 . ?
O27 Na2 O25 138.1(4) . . ?
O26 Na2 O24 77.7(3) . . ?
O15 Na2 O24 81.1(2) . . ?
O27 Na2 O24 144.9(3) 2_756 . ?
O27 Na2 O24 140.6(4) . . ?
O25 Na2 O24 70.6(3) . . ?
O6 S1 O5 112.5(4) . . ?
O6 S1 O7 113.6(4) . . ?
O5 S1 O7 110.0(4) . . ?
O6 S1 C3 107.0(3) . . ?
O5 S1 C3 107.1(4) . . ?
O7 S1 C3 106.2(3) . . ?
O8 S2 O10 112.1(4) . . ?
O8 S2 O9 112.3(5) . . ?
O10 S2 O9 111.4(4) . . ?
O8 S2 C10 107.5(4) . . ?
O10 S2 C10 106.2(4) . . ?
O9 S2 C10 106.9(4) . . ?
O13 S3 O11 114.7(4) . . ?
O13 S3 O12 110.4(3) . . ?
O11 S3 O12 110.9(3) . . ?
O13 S3 C17 108.5(4) . . ?
O11 S3 C17 107.6(4) . . ?
O12 S3 C17 104.1(3) . . ?
O15 S4 O16 114.6(4) . . ?
O15 S4 O14 112.9(4) . . ?
O16 S4 O14 105.9(3) . . ?
O15 S4 C24 108.1(3) . . ?
O16 S4 C24 109.0(3) . . ?
O14 S4 C24 106.0(3) . . ?
O15 S4 Eu 131.6(2) . 4_655 ?
O16 S4 Eu 56.4(2) . 4_655 ?
O14 S4 Eu 49.5(2) . 4_655 ?
C24 S4 Eu 119.9(3) . 4_655 ?
C2 C1 C6 117.5(7) . . ?
C2 C1 C28 120.6(6) . . ?
C6 C1 C28 122.0(6) . . ?
C1 C2 C3 121.1(7) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C2 C3 C4 120.3(7) . . ?
C2 C3 S1 120.2(5) . . ?
C4 C3 S1 119.5(6) . . ?
C5 C4 C3 120.7(7) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.2(6) . . ?
C4 C5 C7 120.7(6) . . ?
C6 C5 C7 120.8(6) . . ?
O1 C6 C5 115.7(6) . . ?
O1 C6 C1 122.1(6) . . ?
C5 C6 C1 122.2(7) . . ?
C5 C7 C8 110.6(6) . . ?
C5 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C13 C8 C9 118.8(7) . . ?
C13 C8 C7 122.7(7) . . ?
C9 C8 C7 118.5(6) . . ?
C10 C9 C8 120.6(7) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 119.0(7) . . ?
C11 C10 S2 120.9(6) . . ?
C9 C10 S2 120.1(6) . . ?
C10 C11 C12 121.8(7) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C13 117.8(7) . . ?
C11 C12 C14 119.9(7) . . ?
C13 C12 C14 122.1(7) . . ?
O2 C13 C8 121.4(7) . . ?
O2 C13 C12 116.7(7) . . ?
C8 C13 C12 121.8(7) . . ?
C12 C14 C15 111.6(6) . . ?
C12 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
C12 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 119.4(7) . . ?
C16 C15 C14 121.1(7) . . ?
C20 C15 C14 119.4(7) . . ?
C15 C16 C17 120.6(7) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 120.1(7) . . ?
C18 C17 S3 123.0(6) . . ?
C16 C17 S3 116.9(5) . . ?
C17 C18 C19 120.7(7) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 118.2(6) . . ?
C18 C19 C21 121.4(6) . . ?
C20 C19 C21 120.4(6) . . ?
O3 C20 C15 116.8(7) . . ?
O3 C20 C19 122.3(6) . . ?
C15 C20 C19 120.9(7) . . ?
C19 C21 C22 111.8(5) . . ?
C19 C21 H21A 109.3 . . ?
C22 C21 H21A 109.3 . . ?
C19 C21 H21B 109.3 . . ?
C22 C21 H21B 109.3 . . ?
H21A C21 H21B 107.9 . . ?
C23 C22 C27 119.7(6) . . ?
C23 C22 C21 119.0(7) . . ?
C27 C22 C21 121.3(6) . . ?
C24 C23 C22 120.3(7) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 120.3(7) . . ?
C25 C24 S4 118.9(5) . . ?
C23 C24 S4 120.6(6) . . ?
C24 C25 C26 121.3(7) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C27 118.2(7) . . ?
C25 C26 C28 119.8(6) . . ?
C27 C26 C28 121.9(6) . . ?
O4 C27 C22 121.5(6) . . ?
O4 C27 C26 118.2(6) . . ?
C22 C27 C26 120.2(6) . . ?
C1 C28 C26 114.7(6) . . ?
C1 C28 H28A 108.6 . . ?
C26 C28 H28A 108.6 . . ?
C1 C28 H28B 108.6 . . ?
C26 C28 H28B 108.6 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 N1 122.1(10) . . ?
C30 C29 H29 119.0 . . ?
N1 C29 H29 119.0 . . ?
C29 C30 N2 120.8(9) . . ?
C29 C30 H30 119.6 . . ?
N2 C30 H30 119.6 . . ?
C32 C31 N1 121.3(10) . . ?
C32 C31 H31 119.4 . . ?
N1 C31 H31 119.4 . . ?
C31 C32 N2 121.8(11) . . ?
C31 C32 H32 119.1 . . ?
N2 C32 H32 119.1 . . ?
O17 N1 C29 121.3(12) . . ?
O17 N1 C31 123.2(11) . . ?
C29 N1 C31 115.4(10) . . ?
O18 N2 C32 122.1(10) . . ?
O18 N2 C30 119.4(9) . . ?
C32 N2 C30 118.5(10) . . ?
C6 O1 H1 109.5 . . ?
C13 O2 H2A 109.5 . . ?
C20 O3 H3 109.5 . . ?
C27 O4 Eu 139.4(4) . . ?
S1 O7 Na1 123.6(3) . . ?
S2 O8 Na1 165.1(4) . . ?
S3 O12 Eu 146.6(3) . 7_646 ?
S4 O14 Eu 103.1(3) . 4_655 ?
S4 O15 Na2 151.9(4) . . ?
S4 O16 Eu 95.8(3) . 4_655 ?
N2 O18 Na1 121.9(6) . . ?
Na2 O25 Na1 107.2(4) . 8_556 ?
Na2 O27 Na2 103.6(4) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.1(11) . . . . ?
C28 C1 C2 C3 -179.4(7) . . . . ?
C1 C2 C3 C4 -0.4(11) . . . . ?
C1 C2 C3 S1 -178.0(6) . . . . ?
O6 S1 C3 C2 -33.4(8) . . . . ?
O5 S1 C3 C2 87.4(7) . . . . ?
O7 S1 C3 C2 -155.1(6) . . . . ?
O6 S1 C3 C4 149.0(7) . . . . ?
O5 S1 C3 C4 -90.1(7) . . . . ?
O7 S1 C3 C4 27.4(7) . . . . ?
C2 C3 C4 C5 0.6(11) . . . . ?
S1 C3 C4 C5 178.2(6) . . . . ?
C3 C4 C5 C6 -0.4(11) . . . . ?
C3 C4 C5 C7 173.8(7) . . . . ?
C4 C5 C6 O1 -179.7(6) . . . . ?
C7 C5 C6 O1 6.1(10) . . . . ?
C4 C5 C6 C1 0.1(11) . . . . ?
C7 C5 C6 C1 -174.1(7) . . . . ?
C2 C1 C6 O1 179.8(6) . . . . ?
C28 C1 C6 O1 -0.7(11) . . . . ?
C2 C1 C6 C5 0.1(11) . . . . ?
C28 C1 C6 C5 179.6(7) . . . . ?
C4 C5 C7 C8 -104.1(8) . . . . ?
C6 C5 C7 C8 69.9(9) . . . . ?
C5 C7 C8 C13 -108.2(7) . . . . ?
C5 C7 C8 C9 71.1(8) . . . . ?
C13 C8 C9 C10 1.9(10) . . . . ?
C7 C8 C9 C10 -177.5(6) . . . . ?
C8 C9 C10 C11 1.0(11) . . . . ?
C8 C9 C10 S2 -177.5(5) . . . . ?
O8 S2 C10 C11 158.9(7) . . . . ?
O10 S2 C10 C11 38.8(7) . . . . ?
O9 S2 C10 C11 -80.2(7) . . . . ?
O8 S2 C10 C9 -22.5(7) . . . . ?
O10 S2 C10 C9 -142.7(6) . . . . ?
O9 S2 C10 C9 98.3(7) . . . . ?
C9 C10 C11 C12 -2.7(11) . . . . ?
S2 C10 C11 C12 175.9(6) . . . . ?
C10 C11 C12 C13 1.3(11) . . . . ?
C10 C11 C12 C14 177.3(7) . . . . ?
C9 C8 C13 O2 175.0(6) . . . . ?
C7 C8 C13 O2 -5.7(10) . . . . ?
C9 C8 C13 C12 -3.4(10) . . . . ?
C7 C8 C13 C12 175.9(6) . . . . ?
C11 C12 C13 O2 -176.6(6) . . . . ?
C14 C12 C13 O2 7.4(10) . . . . ?
C11 C12 C13 C8 1.8(10) . . . . ?
C14 C12 C13 C8 -174.1(6) . . . . ?
C11 C12 C14 C15 -67.8(9) . . . . ?
C13 C12 C14 C15 108.1(8) . . . . ?
C12 C14 C15 C16 102.5(8) . . . . ?
C12 C14 C15 C20 -75.4(9) . . . . ?
C20 C15 C16 C17 0.2(11) . . . . ?
C14 C15 C16 C17 -177.7(7) . . . . ?
C15 C16 C17 C18 -0.3(11) . . . . ?
C15 C16 C17 S3 -178.4(6) . . . . ?
O13 S3 C17 C18 119.5(6) . . . . ?
O11 S3 C17 C18 -5.1(7) . . . . ?
O12 S3 C17 C18 -122.9(6) . . . . ?
O13 S3 C17 C16 -62.4(6) . . . . ?
O11 S3 C17 C16 172.9(6) . . . . ?
O12 S3 C17 C16 55.2(6) . . . . ?
C16 C17 C18 C19 1.3(10) . . . . ?
S3 C17 C18 C19 179.3(5) . . . . ?
C17 C18 C19 C20 -2.3(10) . . . . ?
C17 C18 C19 C21 177.4(6) . . . . ?
C16 C15 C20 O3 179.3(7) . . . . ?
C14 C15 C20 O3 -2.7(10) . . . . ?
C16 C15 C20 C19 -1.2(11) . . . . ?
C14 C15 C20 C19 176.7(6) . . . . ?
C18 C19 C20 O3 -178.3(6) . . . . ?
C21 C19 C20 O3 1.9(10) . . . . ?
C18 C19 C20 C15 2.2(10) . . . . ?
C21 C19 C20 C15 -177.5(6) . . . . ?
C18 C19 C21 C22 -103.3(8) . . . . ?
C20 C19 C21 C22 76.4(8) . . . . ?
C19 C21 C22 C23 77.6(8) . . . . ?
C19 C21 C22 C27 -100.9(8) . . . . ?
C27 C22 C23 C24 2.0(10) . . . . ?
C21 C22 C23 C24 -176.6(6) . . . . ?
C22 C23 C24 C25 -0.5(11) . . . . ?
C22 C23 C24 S4 173.8(5) . . . . ?
O15 S4 C24 C25 178.2(6) . . . . ?
O16 S4 C24 C25 -56.7(7) . . . . ?
O14 S4 C24 C25 56.8(6) . . . . ?
Eu S4 C24 C25 4.8(7) 4_655 . . . ?
O15 S4 C24 C23 3.8(7) . . . . ?
O16 S4 C24 C23 128.9(6) . . . . ?
O14 S4 C24 C23 -117.5(6) . . . . ?
Eu S4 C24 C23 -169.6(5) 4_655 . . . ?
C23 C24 C25 C26 -1.0(11) . . . . ?
S4 C24 C25 C26 -175.4(5) . . . . ?
C24 C25 C26 C27 1.0(10) . . . . ?
C24 C25 C26 C28 178.2(6) . . . . ?
C23 C22 C27 O4 -178.8(6) . . . . ?
C21 C22 C27 O4 -0.2(10) . . . . ?
C23 C22 C27 C26 -2.0(10) . . . . ?
C21 C22 C27 C26 176.6(6) . . . . ?
C25 C26 C27 O4 177.4(6) . . . . ?
C28 C26 C27 O4 0.3(10) . . . . ?
C25 C26 C27 C22 0.5(10) . . . . ?
C28 C26 C27 C22 -176.6(6) . . . . ?
C2 C1 C28 C26 105.2(8) . . . . ?
C6 C1 C28 C26 -74.3(9) . . . . ?
C25 C26 C28 C1 -78.3(8) . . . . ?
C27 C26 C28 C1 98.8(8) . . . . ?
N1 C29 C30 N2 -2.8(13) . . . . ?
N1 C31 C32 N2 -1.7(18) . . . . ?
C30 C29 N1 O17 -177.3(9) . . . . ?
C30 C29 N1 C31 -0.3(13) . . . . ?
C32 C31 N1 O17 179.4(10) . . . . ?
C32 C31 N1 C29 2.5(15) . . . . ?
C31 C32 N2 O18 178.9(10) . . . . ?
C31 C32 N2 C30 -1.4(15) . . . . ?
C29 C30 N2 O18 -176.7(8) . . . . ?
C29 C30 N2 C32 3.6(13) . . . . ?
C22 C27 O4 Eu -93.1(8) . . . . ?
C26 C27 O4 Eu 90.1(8) . . . . ?
O12 Eu O4 C27 105.6(7) 7_646 . . . ?
O21 Eu O4 C27 -113.9(7) . . . . ?
O20 Eu O4 C27 -43.1(6) . . . . ?
O19 Eu O4 C27 178.4(7) . . . . ?
O22 Eu O4 C27 29.5(7) . . . . ?
O14 Eu O4 C27 -21.4(9) 4_645 . . . ?
O16 Eu O4 C27 153.3(6) 4_645 . . . ?
S4 Eu O4 C27 72(6) 4_645 . . . ?
O6 S1 O7 Na1 -53.2(5) . . . . ?
O5 S1 O7 Na1 179.7(3) . . . . ?
C3 S1 O7 Na1 64.1(4) . . . . ?
O8 Na1 O7 S1 -81.6(5) . . . . ?
O28 Na1 O7 S1 -162.0(4) . . . . ?
O23 Na1 O7 S1 57.6(4) 4_655 . . . ?
O18 Na1 O7 S1 -19.8(4) . . . . ?
O25 Na1 O7 S1 117.2(4) 8_455 . . . ?
O10 S2 O8 Na1 105(2) . . . . ?
O9 S2 O8 Na1 -128.9(19) . . . . ?
C10 S2 O8 Na1 -11(2) . . . . ?
O28 Na1 O8 S2 110(2) . . . . ?
O23 Na1 O8 S2 -114(2) 4_655 . . . ?
O18 Na1 O8 S2 -40(2) . . . . ?
O7 Na1 O8 S2 27(2) . . . . ?
O25 Na1 O8 S2 174.5(18) 8_455 . . . ?
O13 S3 O12 Eu -88.1(6) . . . 7_646 ?
O11 S3 O12 Eu 40.1(7) . . . 7_646 ?
C17 S3 O12 Eu 155.6(6) . . . 7_646 ?
O15 S4 O14 Eu 125.9(3) . . . 4_655 ?
O16 S4 O14 Eu -0.2(4) . . . 4_655 ?
C24 S4 O14 Eu -115.9(3) . . . 4_655 ?
O16 S4 O15 Na2 -54.9(8) . . . . ?
O14 S4 O15 Na2 -176.2(6) . . . . ?
C24 S4 O15 Na2 66.9(8) . . . . ?
Eu S4 O15 Na2 -120.8(6) 4_655 . . . ?
O26 Na2 O15 S4 -70.0(8) . . . . ?
O27 Na2 O15 S4 166.1(7) 2_756 . . . ?
O27 Na2 O15 S4 -143.4(9) . . . . ?
O25 Na2 O15 S4 76.3(8) . . . . ?
O24 Na2 O15 S4 6.2(8) . . . . ?
O15 S4 O16 Eu -124.9(3) . . . 4_655 ?
O14 S4 O16 Eu 0.1(3) . . . 4_655 ?
C24 S4 O16 Eu 113.8(3) . . . 4_655 ?
C32 N2 O18 Na1 128.8(8) . . . . ?
C30 N2 O18 Na1 -50.8(9) . . . . ?
O8 Na1 O18 N2 -31.6(7) . . . . ?
O28 Na1 O18 N2 -84.0(9) . . . . ?
O23 Na1 O18 N2 77.9(7) 4_655 . . . ?
O7 Na1 O18 N2 -170.0(7) . . . . ?
O25 Na1 O18 N2 119.8(7) 8_455 . . . ?
O26 Na2 O25 Na1 178.6(4) . . . 8_556 ?
O15 Na2 O25 Na1 72.6(3) . . . 8_556 ?
O27 Na2 O25 Na1 -56.5(4) 2_756 . . 8_556 ?
O27 Na2 O25 Na1 6.0(6) . . . 8_556 ?
O24 Na2 O25 Na1 152.6(4) . . . 8_556 ?
O26 Na2 O27 Na2 96.0(5) . . . 2_756 ?
O15 Na2 O27 Na2 -161.4(6) . . . 2_756 ?
O27 Na2 O27 Na2 -20.2(8) 2_756 . . 2_756 ?
O25 Na2 O27 Na2 -88.3(7) . . . 2_756 ?
O24 Na2 O27 Na2 146.7(3) . . . 2_756 ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.85
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         8.900
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.170

