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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H47 Ce2 N3 O21'
_chemical_formula_weight         1174.04

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'
Ce Ce -0.2486 2.6331 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   24.8443(7)
_cell_length_b                   12.8836(4)
_cell_length_c                   15.0538(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.709(3)
_cell_angle_gamma                90.00
_cell_volume                     4785.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4255
_cell_measurement_theta_min      2.2972
_cell_measurement_theta_max      29.0831

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2344
_exptl_absorpt_coefficient_mu    1.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7712
_exptl_absorpt_correction_T_max  0.8435
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
The structure contains disordered solvents.
Because it was difficult to refine a xonsisten disordered model, 
their contribution was subtracted from the observed structure factors
according to the BYPASS procedure, as implemented in PLATON.
van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. 
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.

(see more at the bottom of this .cif file)
 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13297
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5328
_reflns_number_gt                4260
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0503P)²+8.6734P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5328
_refine_ls_number_parameters     262
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.059
_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
Ce1 Ce 0.328806(8) 0.796964(17) 0.033831(15) 0.02430(9) Uani 1 1 d . . .
O1 O 0.30629(13) 0.7411(3) -0.1215(2) 0.0402(8) Uani 1 1 d . . .
O2 O 0.22817(13) 0.6557(3) -0.1516(2) 0.0485(9) Uani 1 1 d . . .
O3 O 0.20203(13) 0.4527(2) -0.4394(2) 0.0442(8) Uani 1 1 d . . .
O4 O 0.27345(12) 0.3606(2) -0.4633(2) 0.0338(7) Uani 1 1 d . . .
O5 O 0.59850(14) 0.6679(3) -0.4984(3) 0.0546(10) Uani 1 1 d . . .
O6 O 0.58481(14) 0.8293(3) -0.4597(3) 0.0519(10) Uani 1 1 d . . .
O7 O 0.3744(2) 0.9577(4) 0.1101(3) 0.0955(17) Uani 1 1 d . . .
O8 O 0.3761(2) 0.7321(5) 0.1791(3) 0.0979(18) Uani 1 1 d D . .
C1 C 0.27550(17) 0.6785(3) -0.1659(3) 0.0312(9) Uani 1 1 d . . .
C2 C 0.29716(16) 0.6278(3) -0.2451(3) 0.0286(9) Uani 1 1 d . . .
C3 C 0.26597(16) 0.5601(3) -0.2996(3) 0.0308(9) Uani 1 1 d . . .
H3 H 0.2302 0.5480 -0.2897 0.037 Uiso 1 1 calc R . .
C4 C 0.28700(16) 0.5097(3) -0.3689(3) 0.0289(9) Uani 1 1 d . . .
C5 C 0.25216(17) 0.4361(3) -0.4270(3) 0.0307(9) Uani 1 1 d . . .
C6 C 0.33989(17) 0.5306(3) -0.3856(3) 0.0325(10) Uani 1 1 d . . .
H6 H 0.3544 0.4953 -0.4312 0.039 Uiso 1 1 calc R . .
C7 C 0.37135(16) 0.6036(3) -0.3351(3) 0.0304(9) Uani 1 1 d . . .
C8 C 0.34965(17) 0.6505(3) -0.2635(3) 0.0332(10) Uani 1 1 d . . .
H8 H 0.3705 0.6976 -0.2275 0.040 Uiso 1 1 calc R . .
C9 C 0.42532(16) 0.6360(3) -0.3593(3) 0.0315(9) Uani 1 1 d . . .
C10 C 0.45978(19) 0.5653(4) -0.3928(4) 0.0450(13) Uani 1 1 d . . .
H10 H 0.4505 0.4953 -0.3956 0.054 Uiso 1 1 calc R . .
C11 C 0.50795(19) 0.5972(4) -0.4222(4) 0.0457(13) Uani 1 1 d . . .
H11 H 0.5308 0.5485 -0.4437 0.055 Uiso 1 1 calc R . .
C12 C 0.52220(17) 0.7007(3) -0.4200(3) 0.0331(10) Uani 1 1 d . . .
C13 C 0.57176(18) 0.7346(4) -0.4617(3) 0.0369(10) Uani 1 1 d . . .
C14 C 0.4897(2) 0.7697(4) -0.3838(4) 0.0457(13) Uani 1 1 d . . .
H14 H 0.4999 0.8391 -0.3792 0.055 Uiso 1 1 calc R . .
C15 C 0.4415(2) 0.7388(4) -0.3536(4) 0.0452(13) Uani 1 1 d . . .
H15 H 0.4198 0.7876 -0.3292 0.054 Uiso 1 1 calc R . .
N1 N 0.3921(7) 0.6575(15) 0.3165(7) 0.127(6) Uani 0.50 1 d PD . .
C16 C 0.3571(7) 0.6960(13) 0.2425(9) 0.110(6) Uani 0.50 1 d PDU . .
H16A H 0.3198 0.6934 0.2429 0.132 Uiso 0.50 1 calc PR . .
C17 C 0.3636(9) 0.6055(17) 0.3837(13) 0.166(9) Uani 0.50 1 d PDU . .
H17A H 0.3895 0.5768 0.4294 0.249 Uiso 0.50 1 calc PR . .
H17B H 0.3414 0.5509 0.3558 0.249 Uiso 0.50 1 calc PR . .
H17C H 0.3411 0.6548 0.4099 0.249 Uiso 0.50 1 calc PR . .
C18 C 0.4463(7) 0.6795(19) 0.3194(14) 0.151(9) Uani 0.50 1 d PDU . .
H18A H 0.4521 0.7241 0.2703 0.227 Uiso 0.50 1 calc PR . .
H18B H 0.4662 0.6162 0.3153 0.227 Uiso 0.50 1 calc PR . .
H18C H 0.4586 0.7137 0.3748 0.227 Uiso 0.50 1 calc PR . .
OW1 O 0.1281(4) 0.4412(8) -0.2801(6) 0.100(4) Uani 0.50 1 d P . .
H1A H 0.1576 0.4156 -0.2523 0.120 Uiso 0.50 1 d P . .
H1B H 0.1206 0.5049 -0.3077 0.120 Uiso 0.50 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
Ce1 O1 2.448(3) . ?
Ce1 O4 2.455(3) 6_566 ?
Ce1 O2 2.471(3) 7_565 ?
Ce1 O8 2.502(5) . ?
Ce1 O3 2.526(3) 4_554 ?
Ce1 O5 2.557(3) 2_654 ?
Ce1 O6 2.566(3) 2_654 ?
Ce1 O7 2.566(4) . ?
Ce1 O4 2.761(3) 4_554 ?
Ce1 C13 2.925(4) 2_654 ?
Ce1 C5 3.015(4) 4_554 ?
Ce1 Ce1 4.1113(4) 7_565 ?
O1 C1 1.250(5) . ?
O2 C1 1.255(5) . ?
O2 Ce1 2.471(3) 7_565 ?
O3 C5 1.256(5) . ?
O3 Ce1 2.526(3) 4_544 ?
O4 C5 1.262(5) . ?
O4 Ce1 2.455(3) 6_565 ?
O4 Ce1 2.761(3) 4_544 ?
O5 C13 1.253(6) . ?
O5 Ce1 2.557(3) 2_654 ?
O6 C13 1.262(6) . ?
O6 Ce1 2.566(3) 2_654 ?
O8 C16 1.205(13) . ?
C1 C2 1.513(5) . ?
C2 C3 1.372(6) . ?
C2 C8 1.395(5) . ?
C3 C4 1.382(5) . ?
C4 C6 1.393(5) . ?
C4 C5 1.496(6) . ?
C5 Ce1 3.015(4) 4_544 ?
C6 C7 1.391(6) . ?
C7 C8 1.397(5) . ?
C7 C9 1.490(5) . ?
C9 C15 1.383(6) . ?
C9 C10 1.385(6) . ?
C10 C11 1.386(6) . ?
C11 C12 1.379(6) . ?
C12 C14 1.356(6) . ?
C12 C13 1.511(6) . ?
C13 Ce1 2.925(4) 2_654 ?
C14 C15 1.389(6) . ?
N1 C18 1.372(15) . ?
N1 C16 1.420(14) . ?
N1 C17 1.463(15) . ?

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 Ce1 O4 73.00(11) . 6_566 ?
O1 Ce1 O2 132.20(11) . 7_565 ?
O4 Ce1 O2 79.78(11) 6_566 7_565 ?
O1 Ce1 O8 140.19(17) . . ?
O4 Ce1 O8 85.14(17) 6_566 . ?
O2 Ce1 O8 72.86(15) 7_565 . ?
O1 Ce1 O3 71.05(12) . 4_554 ?
O4 Ce1 O3 122.20(10) 6_566 4_554 ?
O2 Ce1 O3 92.66(12) 7_565 4_554 ?
O8 Ce1 O3 146.93(17) . 4_554 ?
O1 Ce1 O5 72.40(12) . 2_654 ?
O4 Ce1 O5 82.92(11) 6_566 2_654 ?
O2 Ce1 O5 142.02(12) 7_565 2_654 ?
O8 Ce1 O5 72.19(16) . 2_654 ?
O3 Ce1 O5 125.05(11) 4_554 2_654 ?
O1 Ce1 O6 75.05(12) . 2_654 ?
O4 Ce1 O6 129.84(10) 6_566 2_654 ?
O2 Ce1 O6 148.23(12) 7_565 2_654 ?
O8 Ce1 O6 95.92(17) . 2_654 ?
O3 Ce1 O6 80.81(11) 4_554 2_654 ?
O5 Ce1 O6 50.79(11) 2_654 2_654 ?
O1 Ce1 O7 134.76(15) . . ?
O4 Ce1 O7 151.44(13) 6_566 . ?
O2 Ce1 O7 74.91(14) 7_565 . ?
O8 Ce1 O7 75.0(2) . . ?
O3 Ce1 O7 72.54(16) 4_554 . ?
O5 Ce1 O7 109.42(16) 2_654 . ?
O6 Ce1 O7 73.47(14) 2_654 . ?
O1 Ce1 O4 67.84(10) . 4_554 ?
O4 Ce1 O4 76.11(9) 6_566 4_554 ?
O2 Ce1 O4 67.91(10) 7_565 4_554 ?
O8 Ce1 O4 138.77(15) . 4_554 ?
O3 Ce1 O4 48.92(9) 4_554 4_554 ?
O5 Ce1 O4 138.90(12) 2_654 4_554 ?
O6 Ce1 O4 124.31(11) 2_654 4_554 ?
O7 Ce1 O4 105.71(15) . 4_554 ?
O1 Ce1 C13 70.93(12) . 2_654 ?
O4 Ce1 C13 106.16(12) 6_566 2_654 ?
O2 Ce1 C13 156.02(13) 7_565 2_654 ?
O8 Ce1 C13 84.37(16) . 2_654 ?
O3 Ce1 C13 102.89(12) 4_554 2_654 ?
O5 Ce1 C13 25.30(12) 2_654 2_654 ?
O6 Ce1 C13 25.52(12) 2_654 2_654 ?
O7 Ce1 C13 92.29(16) . 2_654 ?
O4 Ce1 C13 135.90(11) 4_554 2_654 ?
O1 Ce1 C5 66.50(12) . 4_554 ?
O4 Ce1 C5 99.24(11) 6_566 4_554 ?
O2 Ce1 C5 80.42(12) 7_565 4_554 ?
O8 Ce1 C5 151.74(15) . 4_554 ?
O3 Ce1 C5 24.20(10) 4_554 4_554 ?
O5 Ce1 C5 135.95(12) 2_654 4_554 ?
O6 Ce1 C5 102.20(11) 2_654 4_554 ?
O7 Ce1 C5 89.50(16) . 4_554 ?
O4 Ce1 C5 24.75(9) 4_554 4_554 ?
C13 Ce1 C5 120.34(12) 2_654 4_554 ?
O1 Ce1 Ce1 64.66(7) . 7_565 ?
O4 Ce1 Ce1 40.68(7) 6_566 7_565 ?
O2 Ce1 Ce1 69.00(8) 7_565 7_565 ?
O8 Ce1 Ce1 117.03(15) . 7_565 ?
O3 Ce1 Ce1 82.93(7) 4_554 7_565 ?
O5 Ce1 Ce1 115.62(10) 2_654 7_565 ?
O6 Ce1 Ce1 139.55(9) 2_654 7_565 ?
O7 Ce1 Ce1 134.93(13) . 7_565 ?
O4 Ce1 Ce1 35.43(6) 4_554 7_565 ?
C13 Ce1 Ce1 130.42(10) 2_654 7_565 ?
C5 Ce1 Ce1 59.07(8) 4_554 7_565 ?
C1 O1 Ce1 139.2(3) . . ?
C1 O2 Ce1 133.8(3) . 7_565 ?
C5 O3 Ce1 100.3(3) . 4_544 ?
C5 O4 Ce1 155.3(3) . 6_565 ?
C5 O4 Ce1 89.0(2) . 4_544 ?
Ce1 O4 Ce1 103.89(9) 6_565 4_544 ?
C13 O5 Ce1 94.0(3) . 2_654 ?
C13 O6 Ce1 93.3(3) . 2_654 ?
C16 O8 Ce1 129.3(9) . . ?
O1 C1 O2 125.9(4) . . ?
O1 C1 C2 116.6(4) . . ?
O2 C1 C2 117.4(4) . . ?
C3 C2 C8 119.4(4) . . ?
C3 C2 C1 121.1(3) . . ?
C8 C2 C1 119.5(4) . . ?
C2 C3 C4 120.8(4) . . ?
C3 C4 C6 119.6(4) . . ?
C3 C4 C5 119.7(4) . . ?
C6 C4 C5 120.7(4) . . ?
O3 C5 O4 121.7(4) . . ?
O3 C5 C4 118.3(4) . . ?
O4 C5 C4 119.9(4) . . ?
O3 C5 Ce1 55.5(2) . 4_544 ?
O4 C5 Ce1 66.3(2) . 4_544 ?
C4 C5 Ce1 173.4(3) . 4_544 ?
C7 C6 C4 120.9(4) . . ?
C6 C7 C8 118.1(4) . . ?
C6 C7 C9 121.3(4) . . ?
C8 C7 C9 120.5(4) . . ?
C2 C8 C7 121.1(4) . . ?
C15 C9 C10 117.7(4) . . ?
C15 C9 C7 121.0(4) . . ?
C10 C9 C7 121.1(4) . . ?
C11 C10 C9 121.0(4) . . ?
C12 C11 C10 120.5(4) . . ?
C14 C12 C11 118.7(4) . . ?
C14 C12 C13 122.0(4) . . ?
C11 C12 C13 119.2(4) . . ?
O5 C13 O6 121.7(4) . . ?
O5 C13 C12 119.0(4) . . ?
O6 C13 C12 119.3(4) . . ?
O5 C13 Ce1 60.7(2) . 2_654 ?
O6 C13 Ce1 61.1(2) . 2_654 ?
C12 C13 Ce1 177.0(3) . 2_654 ?
C12 C14 C15 121.4(4) . . ?
C9 C15 C14 120.6(4) . . ?
C18 N1 C16 117.5(14) . . ?
C18 N1 C17 128.7(14) . . ?
C16 N1 C17 113.6(14) . . ?
O8 C16 N1 119.7(14) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.123



# 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 0.497 0.003 0.002 1071.0 152.3
_platon_squeeze_details          
;
;

# Start Validation Reply Form

_vrf_CHEMW03_1                   
;
PROBLEM:
The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          1174.04
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   33.00  396.36
           H         1.01   23.00   23.18
           O        16.00   17.00  271.98
           Ce      140.12    2.00  280.24
           N        14.01    1.00   14.01
           Calculated formula weight              985.78

RESPONSE:
The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modelled. Instead, the disordered solvent was accounted for using the SQUEEZE routine of PLATON. These additional solvent molecules were included in the chemical formula, leading the discrepancy between the formula calculated from the atoms in the CIF.
;

_vrf_PLAT215_1                   
;
PROBLEM:
Disordered N1        has ADP max/min Ratio .....        6.3   

RESPONSE: 
Rotational disorder on two positions.
;

_vrf_PLAT220_1                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        5.8 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;

_vrf_PLAT242_1                   
;
PROBLEM:
Low       Ueq as Compared to Neighbors for .....        Ce1 Check 

RESPONSE:
Static or dynamic disorder of a DMF molecule, described as a "false alarm" in the description of PLAT242
;

_vrf_PLAT222_1                   
;
PROBLEM:
Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        6.7 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents lead to this high value.
;

_vrf_PLAT241_1                   
;
PROBLEM:
High      Ueq as Compared to Neighbors for .....         O8 Check 

RESPONSE:
The disordered solvent attached to O8 leads to this high value.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 981948'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H47 N3 O21 Pr2'
_chemical_formula_weight         1175.62

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'
Pr Pr -0.2180 2.8214 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   24.7168(7)
_cell_length_b                   13.0121(4)
_cell_length_c                   14.9778(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.682(3)
_cell_angle_gamma                90.00
_cell_volume                     4784.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3554
_cell_measurement_theta_min      2.7329
_cell_measurement_theta_max      29.0136

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    2.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7583
_exptl_absorpt_correction_T_max  0.8341
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
The structure contains disordered solvents.
Because it was difficult to refine a xonsisten disordered model, 
their contribution was subtracted from the observed structure factors
according to the BYPASS procedure, as implemented in PLATON.
van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. 
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.

(see more at the bottom of this .cif file)
  
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10032
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5144
_reflns_number_gt                4070
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0492P)²+8.5170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5144
_refine_ls_number_parameters     262
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.073
_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
Pr1 Pr 0.328805(9) 0.795436(18) 0.032669(15) 0.02314(9) Uani 1 1 d . . .
O1 O 0.30531(14) 0.7384(3) -0.1216(2) 0.0371(8) Uani 1 1 d . . .
O2 O 0.22721(14) 0.6531(3) -0.1504(2) 0.0451(9) Uani 1 1 d . . .
O3 O 0.20146(13) 0.4491(3) -0.4389(3) 0.0419(9) Uani 1 1 d . . .
O4 O 0.27373(13) 0.3582(2) -0.4618(2) 0.0328(7) Uani 1 1 d . . .
O5 O 0.59904(15) 0.6671(3) -0.4982(3) 0.0507(11) Uani 1 1 d . . .
O6 O 0.58532(15) 0.8265(3) -0.4587(3) 0.0494(10) Uani 1 1 d . . .
O7 O 0.3755(2) 0.9525(4) 0.1080(3) 0.0866(16) Uani 1 1 d . . .
O8 O 0.3756(2) 0.7315(5) 0.1775(3) 0.0883(17) Uani 1 1 d D . .
C1 C 0.27477(19) 0.6762(4) -0.1653(3) 0.0303(10) Uani 1 1 d . . .
C2 C 0.29652(18) 0.6258(3) -0.2450(3) 0.0294(10) Uani 1 1 d . . .
C3 C 0.26524(18) 0.5577(3) -0.2990(3) 0.0304(10) Uani 1 1 d . . .
H3 H 0.2295 0.5451 -0.2886 0.036 Uiso 1 1 calc R . .
C4 C 0.28644(18) 0.5078(3) -0.3685(3) 0.0282(10) Uani 1 1 d . . .
C5 C 0.25179(18) 0.4338(3) -0.4257(3) 0.0289(10) Uani 1 1 d . . .
C6 C 0.33963(18) 0.5287(3) -0.3857(3) 0.0309(10) Uani 1 1 d . . .
H6 H 0.3544 0.4934 -0.4311 0.037 Uiso 1 1 calc R . .
C7 C 0.37055(18) 0.6017(3) -0.3356(3) 0.0291(10) Uani 1 1 d . . .
C8 C 0.34844(19) 0.6492(4) -0.2636(3) 0.0313(10) Uani 1 1 d . . .
H8 H 0.3691 0.6969 -0.2281 0.038 Uiso 1 1 calc R . .
C9 C 0.42481(18) 0.6341(4) -0.3598(3) 0.0323(11) Uani 1 1 d . . .
C10 C 0.4596(2) 0.5644(4) -0.3930(4) 0.0442(14) Uani 1 1 d . . .
H10 H 0.4504 0.4951 -0.3958 0.053 Uiso 1 1 calc R . .
C11 C 0.5081(2) 0.5962(4) -0.4220(4) 0.0445(14) Uani 1 1 d . . .
H11 H 0.5312 0.5480 -0.4433 0.053 Uiso 1 1 calc R . .
C12 C 0.52240(18) 0.6985(4) -0.4197(3) 0.0319(11) Uani 1 1 d . . .
C13 C 0.57224(19) 0.7329(4) -0.4606(4) 0.0366(11) Uani 1 1 d . . .
C14 C 0.4890(2) 0.7678(4) -0.3842(4) 0.0451(14) Uani 1 1 d . . .
H14 H 0.4990 0.8367 -0.3800 0.054 Uiso 1 1 calc R . .
C15 C 0.4406(2) 0.7365(4) -0.3545(4) 0.0463(14) Uani 1 1 d . . .
H15 H 0.4184 0.7846 -0.3309 0.056 Uiso 1 1 calc R . .
N1 N 0.3927(7) 0.6528(15) 0.3136(7) 0.123(6) Uani 0.50 1 d PD . .
C16 C 0.3582(7) 0.6986(13) 0.2414(9) 0.110(7) Uani 0.50 1 d PDU . .
H16A H 0.3209 0.7024 0.2449 0.132 Uiso 0.50 1 calc PR . .
C17 C 0.3640(9) 0.6021(16) 0.3817(12) 0.152(9) Uani 0.50 1 d PDU . .
H17A H 0.3901 0.5734 0.4275 0.228 Uiso 0.50 1 calc PR . .
H17B H 0.3414 0.5483 0.3541 0.228 Uiso 0.50 1 calc PR . .
H17C H 0.3419 0.6515 0.4082 0.228 Uiso 0.50 1 calc PR . .
C18 C 0.4472(8) 0.675(2) 0.3196(14) 0.145(9) Uani 0.50 1 d PDU . .
H18A H 0.4539 0.7199 0.2710 0.218 Uiso 0.50 1 calc PR . .
H18B H 0.4676 0.6129 0.3162 0.218 Uiso 0.50 1 calc PR . .
H18C H 0.4583 0.7089 0.3758 0.218 Uiso 0.50 1 calc PR . .
OW1 O 0.1256(6) 0.4409(9) -0.2794(8) 0.123(6) Uani 0.50 1 d P . .
H1A H 0.1576 0.4156 -0.2523 0.148 Uiso 0.50 1 d P . .
H1B H 0.1206 0.5049 -0.3077 0.148 Uiso 0.50 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
Pr1 O4 2.426(3) 6_566 ?
Pr1 O1 2.432(3) . ?
Pr1 O2 2.458(3) 7_565 ?
Pr1 O8 2.481(5) . ?
Pr1 O3 2.507(3) 4_554 ?
Pr1 O6 2.538(3) 2_654 ?
Pr1 O5 2.540(3) 2_654 ?
Pr1 O7 2.545(4) . ?
Pr1 O4 2.755(3) 4_554 ?
Pr1 C13 2.902(5) 2_654 ?
Pr1 C5 3.006(5) 4_554 ?
Pr1 Pr1 4.0797(5) 7_565 ?
O1 C1 1.240(6) . ?
O2 C1 1.258(5) . ?
O2 Pr1 2.458(3) 7_565 ?
O3 C5 1.252(5) . ?
O3 Pr1 2.507(3) 4_544 ?
O4 C5 1.273(5) . ?
O4 Pr1 2.426(3) 6_565 ?
O4 Pr1 2.755(3) 4_544 ?
O5 C13 1.256(6) . ?
O5 Pr1 2.540(3) 2_654 ?
O6 C13 1.260(6) . ?
O6 Pr1 2.538(3) 2_654 ?
O8 C16 1.175(14) . ?
C1 C2 1.513(6) . ?
C2 C3 1.376(6) . ?
C2 C8 1.379(6) . ?
C3 C4 1.381(6) . ?
C4 C6 1.396(6) . ?
C4 C5 1.491(6) . ?
C5 Pr1 3.006(5) 4_544 ?
C6 C7 1.385(6) . ?
C7 C8 1.407(6) . ?
C7 C9 1.490(6) . ?
C9 C10 1.381(6) . ?
C9 C15 1.388(7) . ?
C10 C11 1.384(6) . ?
C11 C12 1.376(6) . ?
C12 C14 1.371(6) . ?
C12 C13 1.507(6) . ?
C13 Pr1 2.902(4) 2_654 ?
C14 C15 1.387(7) . ?
N1 C18 1.371(15) . ?
N1 C16 1.428(14) . ?
N1 C17 1.465(15) . ?

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 Pr1 O1 73.02(11) 6_566 . ?
O4 Pr1 O2 80.49(11) 6_566 7_565 ?
O1 Pr1 O2 132.26(12) . 7_565 ?
O4 Pr1 O8 84.28(17) 6_566 . ?
O1 Pr1 O8 139.83(17) . . ?
O2 Pr1 O8 73.05(16) 7_565 . ?
O4 Pr1 O3 123.00(11) 6_566 4_554 ?
O1 Pr1 O3 71.86(12) . 4_554 ?
O2 Pr1 O3 91.62(13) 7_565 4_554 ?
O8 Pr1 O3 146.68(17) . 4_554 ?
O4 Pr1 O6 130.35(11) 6_566 2_654 ?
O1 Pr1 O6 75.73(13) . 2_654 ?
O2 Pr1 O6 147.03(13) 7_565 2_654 ?
O8 Pr1 O6 96.09(17) . 2_654 ?
O3 Pr1 O6 80.71(12) 4_554 2_654 ?
O4 Pr1 O5 82.82(11) 6_566 2_654 ?
O1 Pr1 O5 72.66(13) . 2_654 ?
O2 Pr1 O5 142.40(13) 7_565 2_654 ?
O8 Pr1 O5 71.94(16) . 2_654 ?
O3 Pr1 O5 125.56(11) 4_554 2_654 ?
O6 Pr1 O5 51.21(11) 2_654 2_654 ?
O4 Pr1 O7 150.90(14) 6_566 . ?
O1 Pr1 O7 135.43(15) . . ?
O2 Pr1 O7 74.17(14) 7_565 . ?
O8 Pr1 O7 74.9(2) . . ?
O3 Pr1 O7 72.46(17) 4_554 . ?
O6 Pr1 O7 72.93(15) 2_654 . ?
O5 Pr1 O7 108.97(16) 2_654 . ?
O4 Pr1 O4 76.29(10) 6_566 4_554 ?
O1 Pr1 O4 67.49(11) . 4_554 ?
O2 Pr1 O4 68.04(11) 7_565 4_554 ?
O8 Pr1 O4 138.69(15) . 4_554 ?
O3 Pr1 O4 49.19(10) 4_554 4_554 ?
O6 Pr1 O4 124.26(12) 2_654 4_554 ?
O5 Pr1 O4 138.84(12) 2_654 4_554 ?
O7 Pr1 O4 106.39(15) . 4_554 ?
O4 Pr1 C13 106.40(13) 6_566 2_654 ?
O1 Pr1 C13 71.31(13) . 2_654 ?
O2 Pr1 C13 155.85(14) 7_565 2_654 ?
O8 Pr1 C13 84.47(17) . 2_654 ?
O3 Pr1 C13 102.98(13) 4_554 2_654 ?
O6 Pr1 C13 25.67(13) 2_654 2_654 ?
O5 Pr1 C13 25.59(12) 2_654 2_654 ?
O7 Pr1 C13 91.82(16) . 2_654 ?
O4 Pr1 C13 135.80(12) 4_554 2_654 ?
O4 Pr1 C5 99.93(12) 6_566 4_554 ?
O1 Pr1 C5 66.82(12) . 4_554 ?
O2 Pr1 C5 79.95(12) 7_565 4_554 ?
O8 Pr1 C5 151.62(15) . 4_554 ?
O3 Pr1 C5 24.16(11) 4_554 4_554 ?
O6 Pr1 C5 102.00(12) 2_654 4_554 ?
O5 Pr1 C5 136.32(12) 2_654 4_554 ?
O7 Pr1 C5 89.64(16) . 4_554 ?
O4 Pr1 C5 25.06(10) 4_554 4_554 ?
C13 Pr1 C5 120.30(13) 2_654 4_554 ?
O4 Pr1 Pr1 41.00(7) 6_566 7_565 ?
O1 Pr1 Pr1 64.39(8) . 7_565 ?
O2 Pr1 Pr1 69.47(8) 7_565 7_565 ?
O8 Pr1 Pr1 116.62(15) . 7_565 ?
O3 Pr1 Pr1 83.25(8) 4_554 7_565 ?
O6 Pr1 Pr1 139.92(10) 2_654 7_565 ?
O5 Pr1 Pr1 115.73(10) 2_654 7_565 ?
O7 Pr1 Pr1 135.24(13) . 7_565 ?
O4 Pr1 Pr1 35.29(6) 4_554 7_565 ?
C13 Pr1 Pr1 130.70(11) 2_654 7_565 ?
C5 Pr1 Pr1 59.38(9) 4_554 7_565 ?
C1 O1 Pr1 139.8(3) . . ?
C1 O2 Pr1 132.7(3) . 7_565 ?
C5 O3 Pr1 100.8(3) . 4_544 ?
C5 O4 Pr1 156.9(3) . 6_565 ?
C5 O4 Pr1 88.5(3) . 4_544 ?
Pr1 O4 Pr1 103.71(10) 6_565 4_544 ?
C13 O5 Pr1 93.5(3) . 2_654 ?
C13 O6 Pr1 93.5(3) . 2_654 ?
C16 O8 Pr1 131.0(9) . . ?
O1 C1 O2 125.8(4) . . ?
O1 C1 C2 116.7(4) . . ?
O2 C1 C2 117.5(4) . . ?
C3 C2 C8 119.7(4) . . ?
C3 C2 C1 121.0(4) . . ?
C8 C2 C1 119.2(4) . . ?
C2 C3 C4 120.6(4) . . ?
C3 C4 C6 119.7(4) . . ?
C3 C4 C5 119.6(4) . . ?
C6 C4 C5 120.7(4) . . ?
O3 C5 O4 121.3(4) . . ?
O3 C5 C4 118.8(4) . . ?
O4 C5 C4 119.9(4) . . ?
O3 C5 Pr1 55.0(2) . 4_544 ?
O4 C5 Pr1 66.4(2) . 4_544 ?
C4 C5 Pr1 173.6(3) . 4_544 ?
C7 C6 C4 120.4(4) . . ?
C6 C7 C8 118.5(4) . . ?
C6 C7 C9 121.2(4) . . ?
C8 C7 C9 120.2(4) . . ?
C2 C8 C7 120.8(4) . . ?
C10 C9 C15 117.9(4) . . ?
C10 C9 C7 121.2(4) . . ?
C15 C9 C7 120.8(4) . . ?
C9 C10 C11 121.0(5) . . ?
C12 C11 C10 120.7(5) . . ?
C14 C12 C11 118.8(4) . . ?
C14 C12 C13 121.3(4) . . ?
C11 C12 C13 119.9(4) . . ?
O5 C13 O6 121.5(4) . . ?
O5 C13 C12 118.6(4) . . ?
O6 C13 C12 119.9(4) . . ?
O5 C13 Pr1 60.9(2) . 2_654 ?
O6 C13 Pr1 60.8(2) . 2_654 ?
C12 C13 Pr1 177.5(4) . 2_654 ?
C12 C14 C15 120.8(5) . . ?
C14 C15 C9 120.7(5) . . ?
C18 N1 C16 117.2(14) . . ?
C18 N1 C17 127.0(14) . . ?
C16 N1 C17 114.9(14) . . ?
O8 C16 N1 121.7(14) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.116
# 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 0.493 0.005 0.004 1081.8 63.4
_platon_squeeze_details          
;
;



# Start Validation Reply Form

_vrf_CHEMW03_2                   
;
PROBLEM:
The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          1175.62
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   33.00  396.36
           H         1.01   23.00   23.18
           O        16.00   17.00  271.98
           Pr      140.91    2.00  281.82
           N        14.01    1.00   14.01
           Calculated formula weight              987.35

RESPONSE:
The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modelled. Instead, the disordered solvent was accounted for using the SQUEEZE routine of PLATON. These additional solvent molecules were included in the chemical formula, leading the discrepancy between the formula calculated from the atoms in the CIF.
;

_vrf_PLAT215_2                   
;
PROBLEM:
Disordered N1        has ADP max/min Ratio .....        8.6   

RESPONSE: 
Rotational disorder on two positions.
;

_vrf_PLAT220_2                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        5.3 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;


_vrf_PLAT222_2                   
;
PROBLEM:
Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        6.3 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents lead to this high value.
;

# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 981949'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H47 Eu2 N3 O21'
_chemical_formula_weight         1197.72

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'
Eu Eu -0.1578 3.6682 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   ' C 1 2/c 1'

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

_cell_length_a                   24.5711(7)
_cell_length_b                   13.2963(4)
_cell_length_c                   14.7313(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.735(3)
_cell_angle_gamma                90.00
_cell_volume                     4779.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6114
_cell_measurement_theta_min      2.7790
_cell_measurement_theta_max      29.4512

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2384
_exptl_absorpt_coefficient_mu    2.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7054
_exptl_absorpt_correction_T_max  0.7945
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
The structure contains disordered solvents.
Because it was difficult to refine a xonsisten disordered model, 
their contribution was subtracted from the observed structure factors
according to the BYPASS procedure, as implemented in PLATON.
van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. 
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.

(see more at the bottom of this .cif file)
 
;


_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24841
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5419
_reflns_number_gt                4071
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0704P)²+24.1862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5419
_refine_ls_number_parameters     262
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1476
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.078
_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
Eu1 Eu 0.328769(12) 0.79250(2) 0.030196(19) 0.02595(13) Uani 1 1 d . . .
O1 O 0.3045(2) 0.7343(4) -0.1206(3) 0.0385(11) Uani 1 1 d . . .
O2 O 0.22569(19) 0.6493(4) -0.1461(3) 0.0448(13) Uani 1 1 d . . .
O3 O 0.2016(2) 0.4396(4) -0.4376(4) 0.0415(12) Uani 1 1 d . . .
O4 O 0.2749(2) 0.3530(3) -0.4576(3) 0.0386(11) Uani 1 1 d . . .
O5 O 0.6006(2) 0.6660(4) -0.4993(4) 0.0524(14) Uani 1 1 d . . .
O6 O 0.5869(2) 0.8197(4) -0.4562(4) 0.0541(15) Uani 1 1 d . . .
O7 O 0.3767(3) 0.9397(6) 0.1038(5) 0.084(2) Uani 1 1 d . . .
O8 O 0.3738(3) 0.7318(6) 0.1759(5) 0.087(2) Uani 1 1 d D . .
C1 C 0.2731(3) 0.6724(5) -0.1635(4) 0.0327(14) Uani 1 1 d . . .
C2 C 0.2951(3) 0.6214(5) -0.2438(4) 0.0326(14) Uani 1 1 d . . .
C3 C 0.2642(3) 0.5519(5) -0.2976(4) 0.0329(14) Uani 1 1 d . . .
H3 H 0.2284 0.5384 -0.2867 0.039 Uiso 1 1 calc R . .
C4 C 0.2862(3) 0.5024(5) -0.3673(4) 0.0311(14) Uani 1 1 d . . .
C5 C 0.2520(3) 0.4264(5) -0.4232(4) 0.0297(13) Uani 1 1 d . . .
C6 C 0.3392(3) 0.5240(5) -0.3849(5) 0.0349(15) Uani 1 1 d . . .
H6 H 0.3545 0.4878 -0.4296 0.042 Uiso 1 1 calc R . .
C7 C 0.3700(3) 0.5991(5) -0.3366(5) 0.0337(15) Uani 1 1 d . . .
C8 C 0.3470(3) 0.6449(5) -0.2636(4) 0.0328(14) Uani 1 1 d . . .
H8 H 0.3675 0.6922 -0.2277 0.039 Uiso 1 1 calc R . .
C9 C 0.4240(3) 0.6311(5) -0.3613(5) 0.0348(15) Uani 1 1 d . . .
C10 C 0.4599(3) 0.5635(6) -0.3941(5) 0.0448(19) Uani 1 1 d . . .
H10 H 0.4507 0.4957 -0.3977 0.054 Uiso 1 1 calc R . .
C11 C 0.5089(3) 0.5944(6) -0.4216(5) 0.0451(18) Uani 1 1 d . . .
H11 H 0.5326 0.5470 -0.4416 0.054 Uiso 1 1 calc R . .
C12 C 0.5232(3) 0.6957(5) -0.4200(5) 0.0346(15) Uani 1 1 d . . .
C13 C 0.5737(3) 0.7281(5) -0.4610(5) 0.0365(16) Uani 1 1 d . . .
C14 C 0.4885(3) 0.7620(6) -0.3847(6) 0.052(2) Uani 1 1 d . . .
H14 H 0.4980 0.8297 -0.3806 0.062 Uiso 1 1 calc R . .
C15 C 0.4402(3) 0.7314(6) -0.3553(6) 0.051(2) Uani 1 1 d . . .
H15 H 0.4179 0.7784 -0.3309 0.062 Uiso 1 1 calc R . .
N1 N 0.3896(8) 0.6501(16) 0.3127(8) 0.105(8) Uani 0.50 1 d PD . .
C16 C 0.3546(8) 0.6970(15) 0.2395(10) 0.081(7) Uani 0.50 1 d PDU . .
H16A H 0.3170 0.7000 0.2419 0.098 Uiso 0.50 1 calc PR . .
C17 C 0.3616(10) 0.5969(19) 0.3822(15) 0.113(9) Uani 0.50 1 d PDU . .
H17A H 0.3884 0.5684 0.4276 0.169 Uiso 0.50 1 calc PR . .
H17B H 0.3390 0.5443 0.3534 0.169 Uiso 0.50 1 calc PR . .
H17C H 0.3391 0.6436 0.4108 0.169 Uiso 0.50 1 calc PR . .
C18 C 0.4467(8) 0.664(3) 0.3171(17) 0.118(9) Uani 0.50 1 d PDU . .
H18A H 0.4547 0.7080 0.2689 0.177 Uiso 0.50 1 calc PR . .
H18B H 0.4641 0.6000 0.3104 0.177 Uiso 0.50 1 calc PR . .
H18C H 0.4603 0.6926 0.3751 0.177 Uiso 0.50 1 calc PR . .
OW1 O 0.1218(12) 0.441(2) -0.2771(18) 0.218(17) Uani 0.50 1 d P . .
H1A H 0.1576 0.4156 -0.2523 0.262 Uiso 0.50 1 d P . .
H1B H 0.1206 0.5049 -0.3077 0.262 Uiso 0.50 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
Eu1 O1 2.361(5) . ?
Eu1 O4 2.362(5) 6_566 ?
Eu1 O2 2.417(4) 7_565 ?
Eu1 O8 2.435(7) . ?
Eu1 O3 2.450(5) 4_554 ?
Eu1 O7 2.469(6) . ?
Eu1 O6 2.478(5) 2_654 ?
Eu1 O5 2.496(5) 2_654 ?
Eu1 O4 2.765(5) 4_554 ?
Eu1 C13 2.845(7) 2_654 ?
Eu1 C5 2.978(6) 4_554 ?
Eu1 Eu1 4.0305(6) 7_565 ?
O1 C1 1.249(8) . ?
O2 C1 1.259(8) . ?
O2 Eu1 2.417(4) 7_565 ?
O3 C5 1.244(8) . ?
O3 Eu1 2.450(5) 4_544 ?
O4 C5 1.263(8) . ?
O4 Eu1 2.362(5) 6_565 ?
O4 Eu1 2.765(5) 4_544 ?
O5 C13 1.235(9) . ?
O5 Eu1 2.496(5) 2_654 ?
O6 C13 1.261(9) . ?
O6 Eu1 2.478(5) 2_654 ?
O8 C16 1.191(15) . ?
C1 C2 1.517(8) . ?
C2 C8 1.377(9) . ?
C2 C3 1.385(9) . ?
C3 C4 1.382(8) . ?
C4 C6 1.387(9) . ?
C4 C5 1.497(9) . ?
C5 Eu1 2.978(6) 4_544 ?
C6 C7 1.396(9) . ?
C7 C8 1.410(8) . ?
C7 C9 1.481(8) . ?
C9 C15 1.391(10) . ?
C9 C10 1.385(9) . ?
C10 C11 1.376(9) . ?
C11 C12 1.391(10) . ?
C12 C14 1.370(10) . ?
C12 C13 1.505(9) . ?
C13 Eu1 2.845(7) 2_654 ?
C14 C15 1.372(10) . ?
N1 C18 1.408(16) . ?
N1 C16 1.441(15) . ?
N1 C17 1.480(16) . ?

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 Eu1 O4 73.84(17) . 6_566 ?
O1 Eu1 O2 132.07(17) . 7_565 ?
O4 Eu1 O2 81.18(17) 6_566 7_565 ?
O1 Eu1 O8 139.4(2) . . ?
O4 Eu1 O8 82.1(3) 6_566 . ?
O2 Eu1 O8 73.5(2) 7_565 . ?
O1 Eu1 O3 73.22(18) . 4_554 ?
O4 Eu1 O3 124.00(16) 6_566 4_554 ?
O2 Eu1 O3 88.85(18) 7_565 4_554 ?
O8 Eu1 O3 146.4(2) . 4_554 ?
O1 Eu1 O7 136.7(2) . . ?
O4 Eu1 O7 149.1(2) 6_566 . ?
O2 Eu1 O7 73.2(2) 7_565 . ?
O8 Eu1 O7 74.4(3) . . ?
O3 Eu1 O7 73.2(2) 4_554 . ?
O1 Eu1 O6 76.44(19) . 2_654 ?
O4 Eu1 O6 131.13(17) 6_566 2_654 ?
O2 Eu1 O6 145.57(18) 7_565 2_654 ?
O8 Eu1 O6 96.9(3) . 2_654 ?
O3 Eu1 O6 81.63(18) 4_554 2_654 ?
O7 Eu1 O6 72.3(2) . 2_654 ?
O1 Eu1 O5 73.25(19) . 2_654 ?
O4 Eu1 O5 82.51(18) 6_566 2_654 ?
O2 Eu1 O5 143.00(18) 7_565 2_654 ?
O8 Eu1 O5 71.5(2) . 2_654 ?
O3 Eu1 O5 127.55(17) 4_554 2_654 ?
O7 Eu1 O5 107.9(2) . 2_654 ?
O6 Eu1 O5 51.95(18) 2_654 2_654 ?
O1 Eu1 O4 67.18(16) . 4_554 ?
O4 Eu1 O4 76.62(16) 6_566 4_554 ?
O2 Eu1 O4 67.60(16) 7_565 4_554 ?
O8 Eu1 O4 137.8(2) . 4_554 ?
O3 Eu1 O4 49.12(15) 4_554 4_554 ?
O7 Eu1 O4 108.1(2) . 4_554 ?
O6 Eu1 O4 124.56(17) 2_654 4_554 ?
O5 Eu1 O4 138.95(18) 2_654 4_554 ?
O1 Eu1 C13 72.2(2) . 2_654 ?
O4 Eu1 C13 106.49(19) 6_566 2_654 ?
O2 Eu1 C13 155.39(19) 7_565 2_654 ?
O8 Eu1 C13 84.3(2) . 2_654 ?
O3 Eu1 C13 104.81(19) 4_554 2_654 ?
O7 Eu1 C13 91.0(2) . 2_654 ?
O6 Eu1 C13 26.27(19) 2_654 2_654 ?
O5 Eu1 C13 25.70(19) 2_654 2_654 ?
O4 Eu1 C13 136.55(18) 4_554 2_654 ?
O1 Eu1 C5 67.62(18) . 4_554 ?
O4 Eu1 C5 100.69(17) 6_566 4_554 ?
O2 Eu1 C5 78.03(17) 7_565 4_554 ?
O8 Eu1 C5 150.6(2) . 4_554 ?
O3 Eu1 C5 24.08(16) 4_554 4_554 ?
O7 Eu1 C5 90.7(2) . 4_554 ?
O6 Eu1 C5 102.68(18) 2_654 4_554 ?
O5 Eu1 C5 137.83(18) 2_654 4_554 ?
O4 Eu1 C5 25.06(15) 4_554 4_554 ?
C13 Eu1 C5 121.88(19) 2_654 4_554 ?
O1 Eu1 Eu1 64.58(12) . 7_565 ?
O4 Eu1 Eu1 41.87(11) 6_566 7_565 ?
O2 Eu1 Eu1 69.43(11) 7_565 7_565 ?
O8 Eu1 Eu1 115.3(2) . 7_565 ?
O3 Eu1 Eu1 83.03(12) 4_554 7_565 ?
O7 Eu1 Eu1 135.73(19) . 7_565 ?
O6 Eu1 Eu1 140.77(15) 2_654 7_565 ?
O5 Eu1 Eu1 116.16(15) 2_654 7_565 ?
O4 Eu1 Eu1 34.76(10) 4_554 7_565 ?
C13 Eu1 Eu1 131.63(15) 2_654 7_565 ?
C5 Eu1 Eu1 59.15(13) 4_554 7_565 ?
C1 O1 Eu1 139.9(4) . . ?
C1 O2 Eu1 131.9(4) . 7_565 ?
C5 O3 Eu1 102.5(4) . 4_544 ?
C5 O4 Eu1 160.7(5) . 6_565 ?
C5 O4 Eu1 86.9(4) . 4_544 ?
Eu1 O4 Eu1 103.38(16) 6_565 4_544 ?
C13 O5 Eu1 93.1(4) . 2_654 ?
C13 O6 Eu1 93.3(4) . 2_654 ?
C16 O8 Eu1 129.9(10) . . ?
O1 C1 O2 126.1(6) . . ?
O1 C1 C2 115.7(6) . . ?
O2 C1 C2 118.2(6) . . ?
C8 C2 C3 119.3(6) . . ?
C8 C2 C1 119.1(6) . . ?
C3 C2 C1 121.5(6) . . ?
C4 C3 C2 120.4(6) . . ?
C3 C4 C6 119.9(6) . . ?
C3 C4 C5 119.1(6) . . ?
C6 C4 C5 121.0(6) . . ?
O3 C5 O4 121.4(6) . . ?
O3 C5 C4 118.8(6) . . ?
O4 C5 C4 119.7(6) . . ?
O3 C5 Eu1 53.5(3) . 4_544 ?
O4 C5 Eu1 68.0(3) . 4_544 ?
C4 C5 Eu1 172.3(5) . 4_544 ?
C4 C6 C7 121.1(6) . . ?
C6 C7 C8 117.2(6) . . ?
C6 C7 C9 121.9(6) . . ?
C8 C7 C9 120.9(6) . . ?
C2 C8 C7 121.8(6) . . ?
C15 C9 C10 117.1(6) . . ?
C15 C9 C7 121.2(6) . . ?
C10 C9 C7 121.7(6) . . ?
C11 C10 C9 121.5(7) . . ?
C10 C11 C12 120.8(7) . . ?
C14 C12 C11 117.5(7) . . ?
C14 C12 C13 123.1(6) . . ?
C11 C12 C13 119.3(6) . . ?
O5 C13 O6 121.5(7) . . ?
O5 C13 C12 120.2(6) . . ?
O6 C13 C12 118.3(6) . . ?
O5 C13 Eu1 61.2(4) . 2_654 ?
O6 C13 Eu1 60.4(4) . 2_654 ?
C12 C13 Eu1 177.3(5) . 2_654 ?
C15 C14 C12 121.9(7) . . ?
C14 C15 C9 121.0(7) . . ?
C18 N1 C16 118.9(16) . . ?
C18 N1 C17 124.9(15) . . ?
C16 N1 C17 116.0(15) . . ?
O8 C16 N1 120.0(16) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.683
_refine_diff_density_min         -2.440
_refine_diff_density_rms         0.171


# 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 0.475 0.020 0.008 1109.6 58.2
_platon_squeeze_details          
;
;



# Start Validation Reply Form

_vrf_CHEMW03_3                   
;
PROBLEM:
TThe ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          1197.72
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   33.00  396.36
           H         1.01   23.00   23.18
           O        16.00   17.00  271.98
           Eu      151.96    2.00  303.92
           N        14.01    1.00   14.01
           Calculated formula weight             1009.46

RESPONSE:
The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modelled. Instead, the disordered solvent was accounted for using the SQUEEZE routine of PLATON. These additional solvent molecules were included in the chemical formula, leading the discrepancy between the formula calculated from the atoms in the CIF.
;

_vrf_PLAT215_3                   
;
PROBLEM:
Disordered N1        has ADP max/min Ratio .....        5.2   

RESPONSE: 
Rotational disorder on two positions.
;

_vrf_PLAT220_3                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        4.0 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;


_vrf_PLAT222_3                   
;
PROBLEM:
Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        4.5 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents lead to this high value.
;

# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 981950'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H48.50 La2 N2.50 O20'
_chemical_formula_weight         1174.14

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'
La La -0.2871 2.4523 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   20.2686(3)
_cell_length_b                   18.9736(2)
_cell_length_c                   27.9855(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.6320(10)
_cell_angle_gamma                90.00
_cell_volume                     10256.7(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17105
_cell_measurement_theta_min      3.1700
_cell_measurement_theta_max      29.1570

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4688
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7253
_exptl_absorpt_correction_T_max  0.8206
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52229
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.10
_reflns_number_total             11283
_reflns_number_gt                9107
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0977P)²+555.6904P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11283
_refine_ls_number_parameters     873
_refine_ls_number_restraints     1008
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0819
_refine_ls_wR_factor_ref         0.2214
_refine_ls_wR_factor_gt          0.2049
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      0.975
_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 0.49073(2) 1.01748(2) 0.416370(18) 0.01908(15) Uani 1 1 d . . .
La2 La 0.45820(2) 0.43146(2) 0.440300(16) 0.01395(14) Uani 1 1 d . . .
O1 O 0.4029(3) 0.9242(3) 0.3688(2) 0.0239(13) Uani 1 1 d . A .
O2 O 0.4871(3) 0.8854(3) 0.4336(2) 0.0238(13) Uani 1 1 d . A .
O3 O 0.5055(4) 1.1305(3) 0.4668(3) 0.0339(16) Uani 1 1 d . A .
O4 O 0.557(3) 1.112(3) 0.3843(18) 0.105(18) Uani 0.50 1 d P A 1
O4B O 0.543(2) 1.116(3) 0.3731(10) 0.053(9) Uani 0.50 1 d P A 2
O6 O 0.0768(5) 0.7031(4) 0.1169(3) 0.057(3) Uani 1 1 d . . .
O7 O 0.1014(4) 0.5908(4) 0.1339(3) 0.043(2) Uani 1 1 d . . .
O8 O 0.4189(4) 0.5550(3) 0.4241(3) 0.0402(19) Uani 1 1 d . . .
O9 O 0.4851(4) 0.6298(4) 0.4802(2) 0.0385(18) Uani 1 1 d . . .
O10 O 0.4368(3) 0.4991(4) 0.5262(2) 0.0300(15) Uani 1 1 d . . .
O11 O 0.4664(4) 0.5327(6) 0.8516(3) 0.056(2) Uani 1 1 d U . .
O12 O 0.3656(4) 0.5730(4) 0.8552(3) 0.043(2) Uani 1 1 d . . .
O13 O 0.0806(4) 0.4981(4) 0.5299(4) 0.053(3) Uani 1 1 d . . .
O14 O 0.1150(3) 0.5038(5) 0.4605(3) 0.045(2) Uani 1 1 d . . .
O15 O 0.3533(3) 0.4452(4) 0.4685(3) 0.0289(15) Uani 1 1 d . . .
O16 O 0.3936(4) 0.3149(4) 0.4332(3) 0.0417(19) Uani 1 1 d . . .
O19 O 0.2337(7) 0.5859(15) 0.8607(5) 0.141(8) Uani 1 1 d D . .
H19G H 0.211(17) 0.560(14) 0.874(11) 0.212 Uiso 1 1 d D . .
H19H H 0.245(17) 0.627(8) 0.875(12) 0.212 Uiso 1 1 d D . .
C1 C 0.4323(4) 0.8745(5) 0.3966(3) 0.0212(17) Uani 1 1 d . A .
C2 C 0.4053(5) 0.8007(5) 0.3851(3) 0.0248(19) Uani 1 1 d . . .
C3 C 0.4336(5) 0.7453(5) 0.4174(4) 0.030(2) Uani 1 1 d . A .
H3 H 0.4690 0.7544 0.4479 0.036 Uiso 1 1 calc R . .
C4 C 0.4105(5) 0.6770(5) 0.4054(4) 0.032(2) Uani 1 1 d . . .
C5 C 0.4427(5) 0.6146(5) 0.4401(3) 0.0263(19) Uani 1 1 d . A .
C6 C 0.3587(6) 0.6638(5) 0.3598(4) 0.034(2) Uani 1 1 d . A .
H6 H 0.3438 0.6168 0.3511 0.041 Uiso 1 1 calc R . .
C7 C 0.3286(5) 0.7190(5) 0.3270(4) 0.032(2) Uani 1 1 d . . .
C8 C 0.3528(5) 0.7883(5) 0.3406(3) 0.0261(19) Uani 1 1 d . A .
H8 H 0.3330 0.8267 0.3192 0.031 Uiso 1 1 calc R . .
C9 C 0.2744(6) 0.7047(5) 0.2788(4) 0.036(2) Uani 1 1 d . A .
C10 C 0.2688(9) 0.6386(6) 0.2572(5) 0.046(4) Uani 0.91(3) 1 d PU A 1
H10 H 0.3013 0.6030 0.2725 0.056 Uiso 0.91(3) 1 calc PR A 1
C11 C 0.2167(8) 0.6238(6) 0.2135(5) 0.045(4) Uani 0.91(3) 1 d PU A 1
H11 H 0.2138 0.5782 0.1991 0.053 Uiso 0.91(3) 1 calc PR A 1
C14 C 0.1754(8) 0.7415(6) 0.2111(5) 0.041(4) Uani 0.91(3) 1 d PU A 1
H14 H 0.1442 0.7777 0.1950 0.049 Uiso 0.91(3) 1 calc PR A 1
C15 C 0.2273(8) 0.7559(6) 0.2549(5) 0.042(4) Uani 0.91(3) 1 d PU A 1
H15 H 0.2308 0.8018 0.2690 0.050 Uiso 0.91(3) 1 calc PR A 1
C10B C 0.237(9) 0.642(6) 0.273(6) 0.044(6) Uani 0.09(3) 1 d PU A 2
H10A H 0.2455 0.6087 0.2994 0.053 Uiso 0.09(3) 1 calc PR A 2
C11B C 0.188(9) 0.631(7) 0.227(5) 0.042(6) Uani 0.09(3) 1 d PU A 2
H11A H 0.1666 0.5857 0.2221 0.051 Uiso 0.09(3) 1 calc PR A 2
C14B C 0.199(8) 0.731(7) 0.194(6) 0.043(6) Uani 0.09(3) 1 d PU A 2
H14A H 0.1882 0.7627 0.1665 0.052 Uiso 0.09(3) 1 calc PR A 2
C15B C 0.251(8) 0.751(7) 0.241(6) 0.043(6) Uani 0.09(3) 1 d PU A 2
H15A H 0.2681 0.7977 0.2455 0.052 Uiso 0.09(3) 1 calc PR A 2
C12 C 0.1688(5) 0.6746(5) 0.1906(4) 0.033(2) Uani 1 1 d . . .
C13 C 0.1113(5) 0.6558(5) 0.1429(4) 0.030(2) Uani 1 1 d . A .
C20 C 0.3730(4) 0.4787(5) 0.5084(3) 0.0226(18) Uani 1 1 d . . .
C21 C 0.3234(5) 0.4930(5) 0.5368(3) 0.0217(17) Uani 1 1 d . . .
C22 C 0.2522(4) 0.4905(5) 0.5117(3) 0.0210(17) Uani 1 1 d . . .
H22 H 0.2368 0.4819 0.4766 0.025 Uiso 1 1 calc R . .
C23 C 0.2042(4) 0.5002(5) 0.5368(3) 0.0210(17) Uani 1 1 d . . .
C24 C 0.1284(4) 0.4994(5) 0.5068(4) 0.026(2) Uani 1 1 d . . .
C25 C 0.2274(4) 0.5099(4) 0.5893(3) 0.0189(16) Uani 1 1 d . . .
H25 H 0.1945 0.5146 0.6071 0.023 Uiso 1 1 calc R . .
C26 C 0.2976(4) 0.5128(5) 0.6152(3) 0.0211(17) Uani 1 1 d . B .
C27 C 0.3449(4) 0.5056(4) 0.5879(3) 0.0199(17) Uani 1 1 d . . .
H27 H 0.3931 0.5096 0.6050 0.024 Uiso 1 1 calc R . .
C28 C 0.3234(4) 0.5210(5) 0.6711(3) 0.0254(19) Uani 1 1 d D . .
C31 C 0.3749(4) 0.5373(5) 0.7756(3) 0.028(2) Uani 1 1 d D . .
C32 C 0.4043(5) 0.5496(6) 0.8311(3) 0.029(2) Uani 1 1 d . . .
C29 C 0.2808(17) 0.550(3) 0.6966(9) 0.034(4) Uani 0.748(18) 1 d PDU B 1
H29 H 0.2350 0.5648 0.6794 0.040 Uiso 0.748(18) 1 calc PR B 1
C30 C 0.3079(11) 0.557(3) 0.7482(9) 0.034(4) Uani 0.748(18) 1 d PDU B 1
H30 H 0.2788 0.5756 0.7660 0.041 Uiso 0.748(18) 1 calc PR B 1
C33 C 0.4113(6) 0.4993(9) 0.7493(4) 0.036(3) Uani 0.748(18) 1 d PDU B 1
H33 H 0.4550 0.4797 0.7670 0.044 Uiso 0.748(18) 1 calc PR B 1
C34 C 0.3856(6) 0.4894(10) 0.6978(4) 0.039(3) Uani 0.748(18) 1 d PDU B 1
H34 H 0.4102 0.4612 0.6810 0.047 Uiso 0.748(18) 1 calc PR B 1
C29B C 0.285(5) 0.546(9) 0.702(3) 0.035(5) Uani 0.252(18) 1 d PDU B 2
H29A H 0.2386 0.5594 0.6845 0.042 Uiso 0.252(18) 1 calc PR B 2
C30B C 0.303(4) 0.554(10) 0.751(3) 0.035(5) Uani 0.252(18) 1 d PU B 2
H30A H 0.2717 0.5690 0.7689 0.042 Uiso 0.252(18) 1 calc PR B 2
C33B C 0.418(2) 0.549(3) 0.7506(15) 0.037(5) Uani 0.252(18) 1 d PU B 2
H33A H 0.4646 0.5629 0.7663 0.044 Uiso 0.252(18) 1 calc PR B 2
C34B C 0.390(2) 0.541(3) 0.6966(15) 0.037(5) Uani 0.252(18) 1 d PU B 2
H34A H 0.4201 0.5498 0.6773 0.044 Uiso 0.252(18) 1 calc PR B 2
O17 O 0.5385(6) 0.3453(6) 0.4193(5) 0.074(3) Uani 1 1 d D . .
N2 N 0.6363(13) 0.3055(18) 0.4125(10) 0.053(6) Uani 0.326(13) 1 d PDU C 1
C35 C 0.5748(13) 0.326(2) 0.3914(9) 0.047(6) Uani 0.326(13) 1 d PDU C 1
C36 C 0.665(2) 0.314(4) 0.4685(11) 0.057(8) Uani 0.326(13) 1 d PDU C 1
H36A H 0.6794 0.2681 0.4840 0.085 Uiso 0.326(13) 1 calc PR C 1
H36B H 0.6301 0.3348 0.4816 0.085 Uiso 0.326(13) 1 calc PR C 1
H36C H 0.7058 0.3455 0.4761 0.085 Uiso 0.326(13) 1 calc PR C 1
C37 C 0.692(2) 0.284(2) 0.3902(15) 0.055(7) Uani 0.326(13) 1 d PDU C 1
H37A H 0.7373 0.2996 0.4120 0.083 Uiso 0.326(13) 1 calc PR C 1
H37B H 0.6833 0.3053 0.3570 0.083 Uiso 0.326(13) 1 calc PR C 1
H37C H 0.6924 0.2324 0.3870 0.083 Uiso 0.326(13) 1 calc PR C 1
C38 C 0.546(2) 0.316(2) 0.3326(10) 0.055(7) Uani 0.326(13) 1 d PDU C 1
H38A H 0.5046 0.3459 0.3194 0.083 Uiso 0.326(13) 1 calc PR C 1
H38B H 0.5337 0.2670 0.3246 0.083 Uiso 0.326(13) 1 calc PR C 1
H38C H 0.5814 0.3308 0.3173 0.083 Uiso 0.326(13) 1 calc PR C 1
N2B N 0.596(2) 0.302(3) 0.3739(18) 0.052(7) Uani 0.174(13) 1 d PDU C 2
C35B C 0.5972(14) 0.323(4) 0.4170(17) 0.048(7) Uani 0.174(13) 1 d PDU C 2
C36B C 0.538(3) 0.259(4) 0.338(3) 0.060(9) Uani 0.174(13) 1 d PDU C 2
H36D H 0.4934 0.2734 0.3419 0.090 Uiso 0.174(13) 1 calc PR C 2
H36E H 0.5456 0.2086 0.3468 0.090 Uiso 0.174(13) 1 calc PR C 2
H36F H 0.5383 0.2664 0.3039 0.090 Uiso 0.174(13) 1 calc PR C 2
C37B C 0.665(2) 0.279(4) 0.369(3) 0.050(8) Uani 0.174(13) 1 d PDU C 2
H37D H 0.7015 0.3100 0.3898 0.075 Uiso 0.174(13) 1 calc PR C 2
H37E H 0.6644 0.2818 0.3343 0.075 Uiso 0.174(13) 1 calc PR C 2
H37F H 0.6748 0.2302 0.3812 0.075 Uiso 0.174(13) 1 calc PR C 2
C38B C 0.655(4) 0.309(8) 0.469(2) 0.054(9) Uani 0.174(13) 1 d PDU C 2
H38D H 0.6389 0.3272 0.4961 0.081 Uiso 0.174(13) 1 calc PR C 2
H38E H 0.6975 0.3333 0.4688 0.081 Uiso 0.174(13) 1 calc PR C 2
H38F H 0.6635 0.2584 0.4732 0.081 Uiso 0.174(13) 1 calc PR C 2
O5 O 0.5354(5) 0.9670(6) 0.3506(3) 0.062(3) Uani 1 1 d D A .
N1 N 0.5834(13) 0.9620(13) 0.2866(8) 0.072(8) Uani 0.50 1 d PD A 1
C16 C 0.5663(15) 0.9368(13) 0.3227(9) 0.065(8) Uani 0.50 1 d PD A 1
C17 C 0.6173(16) 0.9232(16) 0.2534(11) 0.072(9) Uani 0.50 1 d PD A 1
H17A H 0.6194 0.8728 0.2614 0.108 Uiso 0.50 1 calc PR A 1
H17B H 0.6643 0.9414 0.2590 0.108 Uiso 0.50 1 calc PR A 1
H17C H 0.5902 0.9302 0.2183 0.108 Uiso 0.50 1 calc PR A 1
C18 C 0.5885(18) 1.0406(14) 0.2812(11) 0.073(9) Uani 0.50 1 d PD A 1
H18A H 0.5705 1.0643 0.3057 0.109 Uiso 0.50 1 calc PR A 1
H18B H 0.5613 1.0547 0.2472 0.109 Uiso 0.50 1 calc PR A 1
H18C H 0.6370 1.0538 0.2870 0.109 Uiso 0.50 1 calc PR A 1
C19 C 0.575(2) 0.8546(14) 0.3311(13) 0.077(10) Uani 0.50 1 d PD A 1
H19A H 0.5598 0.8413 0.3601 0.115 Uiso 0.50 1 calc PR A 1
H19B H 0.6231 0.8414 0.3372 0.115 Uiso 0.50 1 calc PR A 1
H19C H 0.5458 0.8301 0.3012 0.115 Uiso 0.50 1 calc PR A 1
O5B O 0.5318(15) 0.8219(16) 0.3252(10) 0.091(8) Uani 0.50 1 d PD D 2
C16B C 0.5599(16) 0.7830(16) 0.2993(12) 0.080(10) Uani 0.50 1 d PD D 2
N1B N 0.5244(15) 0.7315(14) 0.2764(11) 0.093(10) Uani 0.50 1 d PD . 2
C17B C 0.478(2) 0.690(2) 0.2998(14) 0.091(12) Uani 0.50 1 d PD . 2
H17D H 0.4673 0.7178 0.3255 0.136 Uiso 0.50 1 d PR . 2
H17E H 0.4356 0.6805 0.2734 0.136 Uiso 0.50 1 d PR . 2
H17F H 0.4998 0.6459 0.3137 0.136 Uiso 0.50 1 d PR . 2
C18B C 0.5577(19) 0.683(2) 0.2477(14) 0.090(12) Uani 0.50 1 d PD . 2
H18D H 0.5893 0.7136 0.2367 0.136 Uiso 0.50 1 d PR . 2
H18E H 0.5808 0.6393 0.2603 0.136 Uiso 0.50 1 d PR . 2
H18F H 0.5167 0.6738 0.2200 0.136 Uiso 0.50 1 d PR . 2
C19B C 0.6138(18) 0.819(2) 0.2767(14) 0.091(12) Uani 0.50 1 d PD D 2
H19D H 0.6254 0.8630 0.2950 0.136 Uiso 0.50 1 d PR D 2
H19E H 0.6558 0.7913 0.2807 0.136 Uiso 0.50 1 d PR D 2
H19F H 0.5924 0.8292 0.2417 0.136 Uiso 0.50 1 d PR D 2
O21 O 0.634(2) 1.029(2) 0.3316(14) 0.062(10) Uani 0.25 1 d P E 2
O22 O 0.6822(13) 1.1254(14) 0.4242(10) 0.030(6) Uani 0.25 1 d P F 2
O23 O 0.709(2) 1.074(3) 0.3932(17) 0.075(13) Uani 0.25 1 d P F 2
O24 O 0.7596(12) 1.0398(15) 0.3825(10) 0.028(6) Uani 0.25 1 d P F 2
O20 O 0.7570(8) 0.8042(7) 0.4310(10) 0.159(9) Uani 1 1 d D . .
N3 N 0.6673(8) 0.7555(8) 0.4441(8) 0.056(4) Uani 0.68(2) 1 d PDU G 1
C39 C 0.7189(10) 0.7497(8) 0.4281(10) 0.062(4) Uani 0.68(2) 1 d PDU G 1
C40 C 0.7385(14) 0.6784(11) 0.4069(12) 0.072(5) Uani 0.68(2) 1 d PDU G 1
H40A H 0.6996 0.6454 0.4008 0.107 Uiso 0.68(2) 1 calc PR G 1
H40B H 0.7793 0.6580 0.4314 0.107 Uiso 0.68(2) 1 calc PR G 1
H40C H 0.7488 0.6875 0.3755 0.107 Uiso 0.68(2) 1 calc PR G 1
C41 C 0.6150(15) 0.6969(12) 0.4350(14) 0.063(6) Uani 0.68(2) 1 d PDU G 1
H41A H 0.5796 0.7042 0.4027 0.095 Uiso 0.68(2) 1 calc PR G 1
H41B H 0.5932 0.6966 0.4619 0.095 Uiso 0.68(2) 1 calc PR G 1
H41C H 0.6383 0.6517 0.4346 0.095 Uiso 0.68(2) 1 calc PR G 1
C42 C 0.6457(15) 0.8216(13) 0.4588(13) 0.078(6) Uani 0.68(2) 1 d PDU G 1
H42A H 0.6844 0.8550 0.4664 0.116 Uiso 0.68(2) 1 calc PR G 1
H42B H 0.6308 0.8150 0.4888 0.116 Uiso 0.68(2) 1 calc PR G 1
H42C H 0.6070 0.8402 0.4315 0.116 Uiso 0.68(2) 1 calc PR G 1
N3B N 0.6692(19) 0.7260(17) 0.4189(18) 0.061(6) Uani 0.32(2) 1 d PDU G 2
C39B C 0.6950(13) 0.7867(19) 0.430(2) 0.064(6) Uani 0.32(2) 1 d PDU G 2
C40B C 0.663(3) 0.810(3) 0.472(2) 0.069(8) Uani 0.32(2) 1 d PDU G 2
H40D H 0.6219 0.7811 0.4696 0.103 Uiso 0.32(2) 1 calc PR G 2
H40E H 0.6501 0.8595 0.4678 0.103 Uiso 0.32(2) 1 calc PR G 2
H40F H 0.6973 0.8025 0.5049 0.103 Uiso 0.32(2) 1 calc PR G 2
C41B C 0.618(4) 0.680(4) 0.426(3) 0.065(8) Uani 0.32(2) 1 d PDU G 2
H41D H 0.6178 0.6361 0.4083 0.098 Uiso 0.32(2) 1 calc PR G 2
H41E H 0.5722 0.7029 0.4133 0.098 Uiso 0.32(2) 1 calc PR G 2
H41F H 0.6273 0.6708 0.4621 0.098 Uiso 0.32(2) 1 calc PR G 2
C42B C 0.707(3) 0.685(3) 0.382(2) 0.066(7) Uani 0.32(2) 1 d PDU G 2
H42D H 0.6861 0.6389 0.3733 0.099 Uiso 0.32(2) 1 calc PR G 2
H42E H 0.7566 0.6798 0.4002 0.099 Uiso 0.32(2) 1 calc PR G 2
H42F H 0.7015 0.7133 0.3519 0.099 Uiso 0.32(2) 1 calc PR G 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
La1 O13 2.398(11) 7_566 ?
La1 O7 2.410(7) 4 ?
La1 O14 2.460(7) 3 ?
La1 O5 2.477(8) . ?
La1 O3 2.535(7) . ?
La1 O4 2.56(4) . ?
La1 O2 2.558(6) . ?
La1 O1 2.576(6) . ?
La1 O4B 2.62(4) . ?
La1 C1 2.945(9) . ?
La2 O10 2.437(7) 5_666 ?
La2 O9 2.464(6) 5_666 ?
La2 O8 2.472(7) . ?
La2 O15 2.496(6) . ?
La2 O17 2.499(9) . ?
La2 O16 2.548(7) . ?
La2 O12 2.549(7) 6_565 ?
La2 O11 2.627(9) 6_565 ?
La2 O10 2.873(7) . ?
La2 C32 2.938(9) 6_565 ?
La2 C20 3.066(9) . ?
La2 La2 4.1679(9) 5_666 ?
O1 C1 1.253(10) . ?
O2 C1 1.284(10) . ?
O6 C13 1.232(12) . ?
O7 C13 1.261(11) . ?
O7 La1 2.410(7) 4_545 ?
O8 C5 1.257(11) . ?
O9 C5 1.224(11) . ?
O9 La2 2.464(6) 5_666 ?
O10 C20 1.295(10) . ?
O10 La2 2.437(7) 5_666 ?
O11 C32 1.258(13) . ?
O11 La2 2.627(9) 6_566 ?
O12 C32 1.259(12) . ?
O12 La2 2.549(7) 6_566 ?
O13 C24 1.320(14) . ?
O13 La1 2.398(11) 7_566 ?
O14 C24 1.244(13) . ?
O14 La1 2.460(6) 3_445 ?
O15 C20 1.240(11) . ?
O19 H19G 0.846(10) . ?
O19 H19H 0.871(11) . ?
C1 C2 1.502(12) . ?
C2 C3 1.390(12) . ?
C2 C8 1.393(12) . ?
C3 C4 1.384(13) . ?
C3 H3 0.9500 . ?
C4 C6 1.408(13) . ?
C4 C5 1.546(12) . ?
C6 C7 1.404(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.416(12) . ?
C7 C9 1.483(12) . ?
C8 H8 0.9500 . ?
C9 C15B 1.34(14) . ?
C9 C10 1.382(15) . ?
C9 C15 1.383(16) . ?
C9 C10B 1.39(14) . ?
C10 C11 1.380(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(15) . ?
C11 H11 0.9500 . ?
C14 C15 1.379(16) . ?
C14 C12 1.384(15) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C10B C11B 1.38(16) . ?
C10B H10A 0.9500 . ?
C11B C12 1.28(13) . ?
C11B H11A 0.9500 . ?
C14B C12 1.23(14) . ?
C14B C15B 1.46(17) . ?
C14B H14A 0.9500 . ?
C15B H15A 0.9500 . ?
C12 C13 1.524(12) . ?
C20 C21 1.484(12) . ?
C21 C27 1.386(11) . ?
C21 C22 1.401(12) . ?
C22 C23 1.374(12) . ?
C22 H22 0.9500 . ?
C23 C25 1.412(12) . ?
C23 C24 1.511(11) . ?
C25 C26 1.389(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.402(12) . ?
C26 C28 1.499(11) . ?
C27 H27 0.9500 . ?
C28 C34B 1.37(4) . ?
C28 C29 1.389(8) . ?
C28 C34 1.392(8) . ?
C28 C29B 1.409(10) . ?
C31 C33B 1.29(4) . ?
C31 C33 1.391(8) . ?
C31 C30 1.391(10) . ?
C31 C30B 1.45(6) . ?
C31 C32 1.506(13) . ?
C32 La2 2.938(9) 6_566 ?
C29 C30 1.386(10) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C33 C34 1.387(8) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C29B C30B 1.33(7) . ?
C29B H29A 0.9500 . ?
C30B H30A 0.9500 . ?
C33B C34B 1.45(5) . ?
C33B H33A 0.9500 . ?
C34B H34A 0.9500 . ?
O17 C35 1.280(15) . ?
O17 C35B 1.284(15) . ?
N2 C35 1.267(17) . ?
N2 C36 1.506(15) . ?
N2 C37 1.509(15) . ?
C35 C38 1.58(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N2B C35B 1.262(17) . ?
N2B C37B 1.518(15) . ?
N2B C36B 1.519(15) . ?
C35B C38B 1.58(2) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
O5 C16 1.276(15) . ?
N1 C16 1.257(17) . ?
N1 C17 1.503(15) . ?
N1 C18 1.505(15) . ?
C16 C19 1.58(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O5B C16B 1.282(15) . ?
C16B N1B 1.267(17) . ?
C16B C19B 1.57(2) . ?
N1B C18B 1.503(15) . ?
N1B N1B 1.51(6) 2_655 ?
N1B C17B 1.513(15) . ?
N1B C18B 1.84(5) 2_655 ?
C17B C18B 1.31(5) 2_655 ?
C17B H17D 0.9688 . ?
C17B H17E 0.9679 . ?
C17B H17F 0.9730 . ?
C18B C17B 1.31(5) 2_655 ?
C18B N1B 1.84(5) 2_655 ?
C18B H18D 0.9753 . ?
C18B H18E 0.9736 . ?
C18B H18F 0.9668 . ?
C19B H19D 0.9713 . ?
C19B H19E 0.9766 . ?
C19B H19F 0.9615 . ?
O22 O23 1.51(6) . ?
O23 O24 1.32(6) . ?
O20 C39 1.279(14) . ?
O20 C39B 1.288(15) . ?
N3 C39 1.261(16) . ?
N3 C42 1.43(3) . ?
N3 C41 1.503(15) . ?
C39 C40 1.58(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N3B C39B 1.263(17) . ?
N3B C41B 1.42(6) . ?
N3B C42B 1.65(6) . ?
C39B C40B 1.58(2) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

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
O13 La1 O7 86.0(3) 7_566 4 ?
O13 La1 O14 113.1(3) 7_566 3 ?
O7 La1 O14 148.0(3) 4 3 ?
O13 La1 O5 147.5(3) 7_566 . ?
O7 La1 O5 100.5(3) 4 . ?
O14 La1 O5 77.5(3) 3 . ?
O13 La1 O3 75.3(3) 7_566 . ?
O7 La1 O3 77.1(2) 4 . ?
O14 La1 O3 83.1(3) 3 . ?
O5 La1 O3 137.1(3) . . ?
O13 La1 O4 141.9(13) 7_566 . ?
O7 La1 O4 77.8(13) 4 . ?
O14 La1 O4 71.5(13) 3 . ?
O5 La1 O4 70.1(13) . . ?
O3 La1 O4 67.6(13) . . ?
O13 La1 O2 72.8(2) 7_566 . ?
O7 La1 O2 127.9(2) 4 . ?
O14 La1 O2 83.5(3) 3 . ?
O5 La1 O2 78.4(3) . . ?
O3 La1 O2 136.8(2) . . ?
O4 La1 O2 143.0(14) . . ?
O13 La1 O1 77.7(2) 7_566 . ?
O7 La1 O1 78.7(2) 4 . ?
O14 La1 O1 129.0(3) 3 . ?
O5 La1 O1 72.6(3) . . ?
O3 La1 O1 144.6(2) . . ?
O4 La1 O1 130.8(12) . . ?
O2 La1 O1 50.90(18) . . ?
O13 La1 O4B 141.6(11) 7_566 . ?
O7 La1 O4B 70.8(9) 4 . ?
O14 La1 O4B 79.0(9) 3 . ?
O5 La1 O4B 68.9(11) . . ?
O3 La1 O4B 70.1(10) . . ?
O4 La1 O4B 7.9(17) . . ?
O2 La1 O4B 145.5(11) . . ?
O1 La1 O4B 124.3(7) . . ?
O13 La1 C1 73.7(2) 7_566 . ?
O7 La1 C1 103.1(2) 4 . ?
O14 La1 C1 106.8(3) 3 . ?
O5 La1 C1 73.8(3) . . ?
O3 La1 C1 149.0(2) . . ?
O4 La1 C1 143.3(13) . . ?
O2 La1 C1 25.8(2) . . ?
O1 La1 C1 25.1(2) . . ?
O4B La1 C1 140.0(9) . . ?
O10 La2 O9 78.1(2) 5_666 5_666 ?
O10 La2 O8 75.7(3) 5_666 . ?
O9 La2 O8 130.4(2) 5_666 . ?
O10 La2 O15 123.4(2) 5_666 . ?
O9 La2 O15 88.4(3) 5_666 . ?
O8 La2 O15 72.6(3) . . ?
O10 La2 O17 83.6(3) 5_666 . ?
O9 La2 O17 75.3(4) 5_666 . ?
O8 La2 O17 140.7(4) . . ?
O15 La2 O17 145.1(3) . . ?
O10 La2 O16 150.2(3) 5_666 . ?
O9 La2 O16 75.5(2) 5_666 . ?
O8 La2 O16 132.8(3) . . ?
O15 La2 O16 69.4(3) . . ?
O17 La2 O16 76.7(3) . . ?
O10 La2 O12 133.4(2) 5_666 6_565 ?
O9 La2 O12 147.0(2) 5_666 6_565 ?
O8 La2 O12 75.8(3) . 6_565 ?
O15 La2 O12 80.9(2) . 6_565 ?
O17 La2 O12 96.1(4) . 6_565 ?
O16 La2 O12 71.5(2) . 6_565 ?
O10 La2 O11 85.7(3) 5_666 6_565 ?
O9 La2 O11 146.0(3) 5_666 6_565 ?
O8 La2 O11 72.0(3) . 6_565 ?
O15 La2 O11 125.2(3) . 6_565 ?
O17 La2 O11 73.4(4) . 6_565 ?
O16 La2 O11 109.2(3) . 6_565 ?
O12 La2 O11 50.6(3) 6_565 6_565 ?
O10 La2 O10 76.9(2) 5_666 . ?
O9 La2 O10 66.6(2) 5_666 . ?
O8 La2 O10 66.9(2) . . ?
O15 La2 O10 47.87(19) . . ?
O17 La2 O10 139.8(3) . . ?
O16 La2 O10 104.4(2) . . ?
O12 La2 O10 122.8(2) 6_565 . ?
O11 La2 O10 138.1(3) 6_565 . ?
O10 La2 C32 109.9(3) 5_666 6_565 ?
O9 La2 C32 157.1(3) 5_666 6_565 ?
O8 La2 C32 72.3(3) . 6_565 ?
O15 La2 C32 103.4(2) . 6_565 ?
O17 La2 C32 84.2(3) . 6_565 ?
O16 La2 C32 90.3(3) . 6_565 ?
O12 La2 C32 25.3(2) 6_565 6_565 ?
O11 La2 C32 25.3(3) 6_565 6_565 ?
O10 La2 C32 135.5(2) . 6_565 ?
O10 La2 C20 101.2(2) 5_666 . ?
O9 La2 C20 76.9(3) 5_666 . ?
O8 La2 C20 68.0(3) . . ?
O15 La2 C20 23.0(2) . . ?
O17 La2 C20 150.1(3) . . ?
O16 La2 C20 86.0(3) . . ?
O12 La2 C20 101.3(3) 6_565 . ?
O11 La2 C20 136.1(3) 6_565 . ?
O10 La2 C20 24.9(2) . . ?
C32 La2 C20 120.5(2) 6_565 . ?
O10 La2 La2 42.16(15) 5_666 5_666 ?
O9 La2 La2 66.75(16) 5_666 5_666 ?
O8 La2 La2 65.51(16) . 5_666 ?
O15 La2 La2 81.94(14) . 5_666 ?
O17 La2 La2 117.5(3) . 5_666 ?
O16 La2 La2 132.75(18) . 5_666 ?
O12 La2 La2 140.8(2) 6_565 5_666 ?
O11 La2 La2 118.0(2) 6_565 5_666 ?
O10 La2 La2 34.70(13) . 5_666 ?
C32 La2 La2 133.6(2) 6_565 5_666 ?
C20 La2 La2 59.22(16) . 5_666 ?
C1 O1 La1 94.2(5) . . ?
C1 O2 La1 94.2(5) . . ?
C13 O7 La1 136.8(6) . 4_545 ?
C5 O8 La2 136.0(6) . . ?
C5 O9 La2 136.3(6) . 5_666 ?
C20 O10 La2 164.4(7) . 5_666 ?
C20 O10 La2 85.9(5) . . ?
La2 O10 La2 103.1(2) 5_666 . ?
C32 O11 La2 91.3(6) . 6_566 ?
C32 O12 La2 94.9(5) . 6_566 ?
C24 O13 La1 169.1(7) . 7_566 ?
C24 O14 La1 113.4(6) . 3_445 ?
C20 O15 La2 105.3(5) . . ?
H19G O19 H19H 115(2) . . ?
O1 C1 O2 120.7(8) . . ?
O1 C1 C2 119.7(7) . . ?
O2 C1 C2 119.5(7) . . ?
O1 C1 La1 60.7(4) . . ?
O2 C1 La1 60.0(4) . . ?
C2 C1 La1 176.9(6) . . ?
C3 C2 C8 120.5(8) . . ?
C3 C2 C1 120.9(8) . . ?
C8 C2 C1 118.6(8) . . ?
C4 C3 C2 120.5(8) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C6 119.4(8) . . ?
C3 C4 C5 121.2(8) . . ?
C6 C4 C5 119.3(8) . . ?
O9 C5 O8 128.7(9) . . ?
O9 C5 C4 116.2(8) . . ?
O8 C5 C4 115.0(8) . . ?
C7 C6 C4 121.1(9) . . ?
C7 C6 H6 119.4 . . ?
C4 C6 H6 119.4 . . ?
C6 C7 C8 118.1(8) . . ?
C6 C7 C9 120.9(8) . . ?
C8 C7 C9 121.0(8) . . ?
C2 C8 C7 120.3(8) . . ?
C2 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C15B C9 C10 107(6) . . ?
C15B C9 C15 30(8) . . ?
C10 C9 C15 118.2(10) . . ?
C15B C9 C10B 115(8) . . ?
C10 C9 C10B 37(8) . . ?
C15 C9 C10B 106(6) . . ?
C15B C9 C7 126(6) . . ?
C10 C9 C7 120.2(9) . . ?
C15 C9 C7 121.6(9) . . ?
C10B C9 C7 119(5) . . ?
C11 C10 C9 120.8(11) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 120.8(11) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C15 C14 C12 120.2(10) . . ?
C15 C14 H14 119.9 . . ?
C12 C14 H14 119.9 . . ?
C14 C15 C9 121.3(11) . . ?
C14 C15 H15 119.4 . . ?
C9 C15 H15 119.4 . . ?
C11B C10B C9 117(10) . . ?
C11B C10B H10A 121.4 . . ?
C9 C10B H10A 121.4 . . ?
C12 C11B C10B 127(10) . . ?
C12 C11B H11A 116.7 . . ?
C10B C11B H11A 116.7 . . ?
C12 C14B C15B 120(10) . . ?
C12 C14B H14A 120.0 . . ?
C15B C14B H14A 120.0 . . ?
C9 C15B C14B 122(10) . . ?
C9 C15B H15A 119.0 . . ?
C14B C15B H15A 119.0 . . ?
C14B C12 C11B 119(8) . . ?
C14B C12 C11 108(6) . . ?
C11B C12 C11 34(8) . . ?
C14B C12 C14 34(9) . . ?
C11B C12 C14 107(6) . . ?
C11 C12 C14 118.8(9) . . ?
C14B C12 C13 120(6) . . ?
C11B C12 C13 121(6) . . ?
C11 C12 C13 119.2(9) . . ?
C14 C12 C13 122.1(9) . . ?
O6 C13 O7 124.5(9) . . ?
O6 C13 C12 119.6(8) . . ?
O7 C13 C12 115.9(8) . . ?
O15 C20 O10 120.9(8) . . ?
O15 C20 C21 119.3(7) . . ?
O10 C20 C21 119.8(8) . . ?
O15 C20 La2 51.7(4) . . ?
O10 C20 La2 69.2(5) . . ?
C21 C20 La2 170.6(6) . . ?
C27 C21 C22 118.6(8) . . ?
C27 C21 C20 122.2(8) . . ?
C22 C21 C20 119.2(7) . . ?
C23 C22 C21 121.4(8) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C25 119.0(8) . . ?
C22 C23 C24 118.2(8) . . ?
C25 C23 C24 122.8(8) . . ?
O14 C24 O13 123.4(8) . . ?
O14 C24 C23 116.3(9) . . ?
O13 C24 C23 120.2(9) . . ?
C26 C25 C23 121.0(8) . . ?
C26 C25 H25 119.5 . . ?
C23 C25 H25 119.5 . . ?
C25 C26 C27 118.2(8) . . ?
C25 C26 C28 121.9(8) . . ?
C27 C26 C28 119.9(7) . . ?
C21 C27 C26 121.8(8) . . ?
C21 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
C34B C28 C29 107(3) . . ?
C34B C28 C34 42(2) . . ?
C29 C28 C34 119.8(14) . . ?
C34B C28 C29B 103(6) . . ?
C29 C28 C29B 7(6) . . ?
C34 C28 C29B 113(4) . . ?
C34B C28 C26 123.3(19) . . ?
C29 C28 C26 120.2(13) . . ?
C34 C28 C26 119.2(7) . . ?
C29B C28 C26 126(4) . . ?
C33B C31 C33 42(2) . . ?
C33B C31 C30 111(2) . . ?
C33 C31 C30 115.6(17) . . ?
C33B C31 C30B 117(5) . . ?
C33 C31 C30B 119(5) . . ?
C30 C31 C30B 6(7) . . ?
C33B C31 C32 114(2) . . ?
C33 C31 C32 121.3(9) . . ?
C30 C31 C32 122.9(14) . . ?
C30B C31 C32 118(4) . . ?
O11 C32 O12 123.1(9) . . ?
O11 C32 C31 117.4(9) . . ?
O12 C32 C31 119.4(8) . . ?
O11 C32 La2 63.3(5) . 6_566 ?
O12 C32 La2 59.8(5) . 6_566 ?
C31 C32 La2 177.6(7) . 6_566 ?
C30 C29 C28 117(2) . . ?
C30 C29 H29 121.3 . . ?
C28 C29 H29 121.3 . . ?
C29 C30 C31 124(3) . . ?
C29 C30 H30 117.9 . . ?
C31 C30 H30 117.9 . . ?
C34 C33 C31 121.7(10) . . ?
C34 C33 H33 119.1 . . ?
C31 C33 H33 119.1 . . ?
C33 C34 C28 119.6(10) . . ?
C33 C34 H34 120.2 . . ?
C28 C34 H34 120.2 . . ?
C30B C29B C28 130(9) . . ?
C30B C29B H29A 114.8 . . ?
C28 C29B H29A 114.8 . . ?
C29B C30B C31 112(9) . . ?
C29B C30B H30A 123.8 . . ?
C31 C30B H30A 123.8 . . ?
C31 C33B C34B 115(4) . . ?
C31 C33B H33A 122.4 . . ?
C34B C33B H33A 122.4 . . ?
C28 C34B C33B 126(4) . . ?
C28 C34B H34A 117.1 . . ?
C33B C34B H34A 117.1 . . ?
C35 O17 C35B 33(2) . . ?
C35 O17 La2 150.4(18) . . ?
C35B O17 La2 155(3) . . ?
C35 N2 C36 118(3) . . ?
C35 N2 C37 130(3) . . ?
C36 N2 C37 110.7(17) . . ?
N2 C35 O17 118(2) . . ?
N2 C35 C38 117(2) . . ?
O17 C35 C38 125(2) . . ?
C35B N2B C37B 115(4) . . ?
C35B N2B C36B 126(2) . . ?
C37B N2B C36B 110.0(17) . . ?
N2B C35B O17 113(3) . . ?
N2B C35B C38B 128(5) . . ?
O17 C35B C38B 117(5) . . ?
N2B C36B H36D 109.5 . . ?
N2B C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
N2B C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
N2B C37B H37D 109.5 . . ?
N2B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
N2B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35B C38B H38D 109.5 . . ?
C35B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C16 O5 La1 170.5(15) . . ?
C16 N1 C17 127(2) . . ?
C16 N1 C18 120(2) . . ?
C17 N1 C18 111.4(16) . . ?
N1 C16 O5 129(2) . . ?
N1 C16 C19 117(2) . . ?
O5 C16 C19 114(2) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1B C16B O5B 117(3) . . ?
N1B C16B C19B 119(3) . . ?
O5B C16B C19B 117(3) . . ?
C16B N1B C18B 117(3) . . ?
C16B N1B N1B 127(2) . 2_655 ?
C18B N1B N1B 75(2) . 2_655 ?
C16B N1B C17B 121(3) . . ?
C18B N1B C17B 110.8(17) . . ?
N1B N1B C17B 97(3) 2_655 . ?
C16B N1B C18B 152(2) . 2_655 ?
C18B N1B C18B 90(2) . 2_655 ?
N1B N1B C18B 52.3(15) 2_655 2_655 ?
C17B N1B C18B 44.9(19) . 2_655 ?
C18B C17B N1B 81(2) 2_655 . ?
C18B C17B H17D 128.7 2_655 . ?
N1B C17B H17D 110.6 . . ?
C18B C17B H17E 28.1 2_655 . ?
N1B C17B H17E 107.1 . . ?
H17D C17B H17E 108.7 . . ?
C18B C17B H17F 111.4 2_655 . ?
N1B C17B H17F 110.9 . . ?
H17D C17B H17F 110.2 . . ?
H17E C17B H17F 109.2 . . ?
C17B C18B N1B 106(3) 2_655 . ?
C17B C18B N1B 54.4(17) 2_655 2_655 ?
N1B C18B N1B 53(2) . 2_655 ?
C17B C18B H18D 80.7 2_655 . ?
N1B C18B H18D 105.0 . . ?
N1B C18B H18D 101.7 2_655 . ?
C17B C18B H18E 120.6 2_655 . ?
N1B C18B H18E 125.0 . . ?
N1B C18B H18E 147.5 2_655 . ?
H18D C18B H18E 109.2 . . ?
C17B C18B H18F 29.6 2_655 . ?
N1B C18B H18F 97.2 . . ?
N1B C18B H18F 48.4 2_655 . ?
H18D C18B H18F 110.2 . . ?
H18E C18B H18F 109.3 . . ?
C16B C19B H19D 104.3 . . ?
C16B C19B H19E 114.1 . . ?
H19D C19B H19E 109.6 . . ?
C16B C19B H19F 110.1 . . ?
H19D C19B H19F 109.0 . . ?
H19E C19B H19F 109.5 . . ?
O24 O23 O22 153(4) . . ?
C39 O20 C39B 39.2(18) . . ?
C39 N3 C42 122.6(17) . . ?
C39 N3 C41 119.5(18) . . ?
C42 N3 C41 115.9(17) . . ?
N3 C39 O20 117.2(16) . . ?
N3 C39 C40 122.7(16) . . ?
O20 C39 C40 120.1(17) . . ?
C39B N3B C41B 142(4) . . ?
C39B N3B C42B 110(4) . . ?
C41B N3B C42B 108(4) . . ?
N3B C39B O20 125(3) . . ?
N3B C39B C40B 101(4) . . ?
O20 C39B C40B 122(4) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
N3B C41B H41D 109.5 . . ?
N3B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
N3B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
N3B C42B H42D 109.5 . . ?
N3B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
N3B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         9.343
_refine_diff_density_min         -9.451
_refine_diff_density_rms         0.270

# Start Validation Reply Form
_vrf_PLAT215_4                   
;
PROBLEM:
Disordered O4        has ADP max/min Ratio .....        8.9   

RESPONSE:
Rotational disorder on two positions.
;

_vrf_PLAT220_4                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        4.1 Ratio 
Large Non-Solvent    O     Ueq(max)/Ueq(min) ...        4.2 Ratio

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;
_database_code_depnum_ccdc_archive 'CCDC 981951'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H48.50 N2.50 O20 Sm2'
_chemical_formula_weight         1197.02

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'
Sm Sm -0.1638 3.4418 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   19.8953(3)
_cell_length_b                   18.6848(2)
_cell_length_c                   27.9037(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.2660(10)
_cell_angle_gamma                90.00
_cell_volume                     9905.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18123
_cell_measurement_theta_min      3.0940
_cell_measurement_theta_max      29.1400

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4768
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_T_max  0.7597
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46443
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.10
_reflns_number_total             10875
_reflns_number_gt                8782
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0344P)²+72.6542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10875
_refine_ls_number_parameters     873
_refine_ls_number_restraints     1008
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0933
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.054
_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
Sm1 Sm 0.494510(12) 1.016220(11) 0.413610(8) 0.01627(7) Uani 1 1 d . . .
Sm2 Sm 0.456280(11) 0.431180(11) 0.441330(8) 0.01490(6) Uani 1 1 d . . .
O1 O 0.40771(17) 0.92582(16) 0.36681(11) 0.0232(7) Uani 1 1 d . A .
O2 O 0.48816(16) 0.88729(15) 0.43482(11) 0.0195(6) Uani 1 1 d . A .
O3 O 0.50925(18) 1.12886(17) 0.46477(11) 0.0263(7) Uani 1 1 d . A .
O4 O 0.5765(7) 1.1057(9) 0.3906(6) 0.049(3) Uani 0.50 1 d P A 1
O4B O 0.5496(7) 1.1123(10) 0.3754(5) 0.048(4) Uani 0.50 1 d P A 2
O6 O 0.0790(2) 0.7011(2) 0.11503(16) 0.0599(14) Uani 1 1 d . . .
O7 O 0.0918(2) 0.58898(19) 0.13871(14) 0.0472(11) Uani 1 1 d . . .
O8 O 0.4210(2) 0.55305(17) 0.42546(13) 0.0375(9) Uani 1 1 d . . .
O9 O 0.48797(19) 0.62949(17) 0.48147(12) 0.0316(8) Uani 1 1 d . . .
O10 O 0.43817(17) 0.50442(19) 0.52859(12) 0.0285(8) Uani 1 1 d . . .
O11 O 0.4681(2) 0.5355(4) 0.85656(15) 0.0741(16) Uani 1 1 d U . .
O12 O 0.3637(2) 0.5687(2) 0.85881(13) 0.0426(10) Uani 1 1 d . . .
O13 O 0.08292(16) 0.49177(19) 0.53744(12) 0.0269(7) Uani 1 1 d . . .
O14 O 0.10995(17) 0.5000(2) 0.46692(12) 0.0312(8) Uani 1 1 d . . .
O15 O 0.35508(17) 0.44660(18) 0.47122(11) 0.0254(7) Uani 1 1 d . . .
O16 O 0.3912(2) 0.31735(19) 0.43374(14) 0.0373(9) Uani 1 1 d . . .
O19 O 0.2297(4) 0.5694(7) 0.8654(3) 0.149(4) Uani 1 1 d D . .
H19G H 0.204(8) 0.541(7) 0.874(6) 0.224 Uiso 1 1 d D . .
H19H H 0.245(8) 0.602(6) 0.885(5) 0.224 Uiso 1 1 d D . .
C1 C 0.4353(2) 0.8762(2) 0.39653(16) 0.0184(9) Uani 1 1 d . A .
C2 C 0.4060(2) 0.8017(2) 0.38614(16) 0.0222(10) Uani 1 1 d . . .
C3 C 0.4351(3) 0.7458(2) 0.41837(17) 0.0253(10) Uani 1 1 d . A .
H3 H 0.4718 0.7550 0.4484 0.030 Uiso 1 1 calc R . .
C4 C 0.4106(3) 0.6765(2) 0.40682(17) 0.0272(11) Uani 1 1 d . . .
C5 C 0.4437(3) 0.6138(3) 0.44087(17) 0.0274(11) Uani 1 1 d . A .
C6 C 0.3568(3) 0.6632(3) 0.36272(18) 0.0320(12) Uani 1 1 d . A .
H6 H 0.3405 0.6156 0.3548 0.038 Uiso 1 1 calc R . .
C7 C 0.3263(3) 0.7192(3) 0.32968(18) 0.0299(11) Uani 1 1 d . . .
C8 C 0.3516(3) 0.7884(2) 0.34249(17) 0.0266(11) Uani 1 1 d . A .
H8 H 0.3314 0.8271 0.3210 0.032 Uiso 1 1 calc R . .
C9 C 0.2696(3) 0.7039(3) 0.28241(19) 0.0343(13) Uani 1 1 d . A .
C10 C 0.2618(6) 0.6356(4) 0.2614(4) 0.049(3) Uani 0.733(14) 1 d PU A 1
H10 H 0.2934 0.5987 0.2775 0.059 Uiso 0.733(14) 1 calc PR A 1
C11 C 0.2090(6) 0.6202(4) 0.2176(3) 0.044(3) Uani 0.733(14) 1 d PU A 1
H11 H 0.2040 0.5728 0.2047 0.053 Uiso 0.733(14) 1 calc PR A 1
C14 C 0.1731(6) 0.7423(5) 0.2114(4) 0.042(3) Uani 0.733(14) 1 d PU A 1
H14 H 0.1438 0.7797 0.1936 0.050 Uiso 0.733(14) 1 calc PR A 1
C15 C 0.2247(6) 0.7574(5) 0.2558(4) 0.041(2) Uani 0.733(14) 1 d PU A 1
H15 H 0.2296 0.8050 0.2685 0.049 Uiso 0.733(14) 1 calc PR A 1
C10B C 0.2298(16) 0.6413(12) 0.2786(10) 0.043(4) Uani 0.267(14) 1 d PU A 2
H10A H 0.2386 0.6090 0.3061 0.052 Uiso 0.267(14) 1 calc PR A 2
C11B C 0.1773(15) 0.6266(11) 0.2342(9) 0.038(4) Uani 0.267(14) 1 d PU A 2
H11A H 0.1498 0.5845 0.2319 0.045 Uiso 0.267(14) 1 calc PR A 2
C14B C 0.1977(16) 0.7348(14) 0.1990(11) 0.039(4) Uani 0.267(14) 1 d PU A 2
H14A H 0.1858 0.7696 0.1730 0.047 Uiso 0.267(14) 1 calc PR A 2
C15B C 0.2508(16) 0.7498(15) 0.2436(10) 0.041(4) Uani 0.267(14) 1 d PU A 2
H15A H 0.2746 0.7944 0.2466 0.050 Uiso 0.267(14) 1 calc PR A 2
C12 C 0.1637(3) 0.6726(3) 0.19237(18) 0.0307(12) Uani 1 1 d . . .
C13 C 0.1074(3) 0.6534(3) 0.14528(18) 0.0309(12) Uani 1 1 d . A .
C20 C 0.3757(2) 0.4816(2) 0.51112(17) 0.0216(9) Uani 1 1 d . . .
C21 C 0.3241(2) 0.4946(2) 0.54003(16) 0.0182(9) Uani 1 1 d . . .
C22 C 0.2526(2) 0.4897(2) 0.51515(16) 0.0184(9) Uani 1 1 d . . .
H22 H 0.2370 0.4805 0.4801 0.022 Uiso 1 1 calc R . .
C23 C 0.2038(2) 0.4984(2) 0.54163(16) 0.0185(9) Uani 1 1 d . . .
C24 C 0.1270(2) 0.4963(2) 0.51382(17) 0.0203(9) Uani 1 1 d . . .
C25 C 0.2271(2) 0.5087(3) 0.59306(17) 0.0237(10) Uani 1 1 d . . .
H25 H 0.1938 0.5124 0.6113 0.028 Uiso 1 1 calc R . .
C26 C 0.2996(2) 0.5138(3) 0.61887(16) 0.0232(10) Uani 1 1 d . B .
C27 C 0.3472(2) 0.5076(3) 0.59112(16) 0.0224(10) Uani 1 1 d . . .
H27 H 0.3962 0.5123 0.6075 0.027 Uiso 1 1 calc R . .
C28 C 0.3253(2) 0.5226(3) 0.67439(17) 0.0309(12) Uani 1 1 d D . .
C31 C 0.3757(3) 0.5383(3) 0.77895(18) 0.0378(13) Uani 1 1 d D . .
C32 C 0.4038(3) 0.5492(3) 0.83472(18) 0.0371(13) Uani 1 1 d . . .
C29 C 0.2793(6) 0.5440(14) 0.7001(5) 0.035(3) Uani 0.699(10) 1 d PDU B 1
H29 H 0.2312 0.5537 0.6832 0.043 Uiso 0.699(10) 1 calc PR B 1
C30 C 0.3069(7) 0.5507(11) 0.7517(5) 0.039(3) Uani 0.699(10) 1 d PDU B 1
H30 H 0.2755 0.5650 0.7698 0.046 Uiso 0.699(10) 1 calc PR B 1
C33 C 0.4161(4) 0.5010(6) 0.7532(2) 0.044(2) Uani 0.699(10) 1 d PDU B 1
H33 H 0.4604 0.4811 0.7713 0.053 Uiso 0.699(10) 1 calc PR B 1
C34 C 0.3908(4) 0.4934(6) 0.7014(2) 0.041(2) Uani 0.699(10) 1 d PDU B 1
H34 H 0.4180 0.4683 0.6840 0.049 Uiso 0.699(10) 1 calc PR B 1
C29B C 0.2894(18) 0.550(3) 0.7060(14) 0.037(5) Uani 0.301(10) 1 d PDU B 2
H29A H 0.2424 0.5633 0.6889 0.044 Uiso 0.301(10) 1 calc PR B 2
C30B C 0.3073(17) 0.561(3) 0.7575(13) 0.033(4) Uani 0.301(10) 1 d PU B 2
H30A H 0.2776 0.5816 0.7749 0.040 Uiso 0.301(10) 1 calc PR B 2
C33B C 0.4174(10) 0.5597(13) 0.7502(6) 0.041(4) Uani 0.301(10) 1 d PU B 2
H33A H 0.4621 0.5811 0.7650 0.049 Uiso 0.301(10) 1 calc PR B 2
C34B C 0.3920(10) 0.5487(13) 0.6988(6) 0.035(3) Uani 0.301(10) 1 d PU B 2
H34A H 0.4222 0.5598 0.6791 0.042 Uiso 0.301(10) 1 calc PR B 2
O17 O 0.5291(3) 0.3423(3) 0.4178(2) 0.0736(15) Uani 1 1 d D . .
N2 N 0.6302(7) 0.3007(9) 0.4119(6) 0.049(4) Uani 0.299(8) 1 d PDU C 1
C35 C 0.5637(7) 0.3171(11) 0.3917(5) 0.038(4) Uani 0.299(8) 1 d PDU C 1
C36 C 0.6596(16) 0.310(3) 0.4658(7) 0.054(6) Uani 0.299(8) 1 d PDU C 1
H36A H 0.6893 0.2694 0.4802 0.081 Uiso 0.299(8) 1 calc PR C 1
H36B H 0.6213 0.3144 0.4811 0.081 Uiso 0.299(8) 1 calc PR C 1
H36C H 0.6879 0.3543 0.4724 0.081 Uiso 0.299(8) 1 calc PR C 1
C37 C 0.6814(12) 0.2754(14) 0.3878(9) 0.057(5) Uani 0.299(8) 1 d PDU C 1
H37A H 0.7216 0.3082 0.3954 0.086 Uiso 0.299(8) 1 calc PR C 1
H37B H 0.6594 0.2734 0.3514 0.086 Uiso 0.299(8) 1 calc PR C 1
H37C H 0.6975 0.2274 0.4002 0.086 Uiso 0.299(8) 1 calc PR C 1
C38 C 0.5373(14) 0.3091(14) 0.3326(6) 0.065(6) Uani 0.299(8) 1 d PDU C 1
H38A H 0.4937 0.3364 0.3191 0.097 Uiso 0.299(8) 1 calc PR C 1
H38B H 0.5285 0.2584 0.3238 0.097 Uiso 0.299(8) 1 calc PR C 1
H38C H 0.5734 0.3273 0.3183 0.097 Uiso 0.299(8) 1 calc PR C 1
N2B N 0.5938(10) 0.2981(12) 0.3713(8) 0.045(4) Uani 0.201(8) 1 d PDU C 2
C35B C 0.5860(8) 0.3208(16) 0.4138(8) 0.041(5) Uani 0.201(8) 1 d PDU C 2
C36B C 0.5330(14) 0.270(2) 0.3324(12) 0.073(7) Uani 0.201(8) 1 d PDU C 2
H36D H 0.4897 0.2878 0.3382 0.109 Uiso 0.201(8) 1 calc PR C 2
H36E H 0.5337 0.2178 0.3336 0.109 Uiso 0.201(8) 1 calc PR C 2
H36F H 0.5349 0.2863 0.2994 0.109 Uiso 0.201(8) 1 calc PR C 2
C37B C 0.6595(12) 0.272(2) 0.3645(13) 0.046(6) Uani 0.201(8) 1 d PDU C 2
H37D H 0.6986 0.3018 0.3840 0.068 Uiso 0.201(8) 1 calc PR C 2
H37E H 0.6567 0.2745 0.3289 0.068 Uiso 0.201(8) 1 calc PR C 2
H37F H 0.6672 0.2223 0.3760 0.068 Uiso 0.201(8) 1 calc PR C 2
C38B C 0.646(2) 0.311(4) 0.4653(12) 0.055(7) Uani 0.201(8) 1 d PDU C 2
H38D H 0.6293 0.3298 0.4927 0.083 Uiso 0.201(8) 1 calc PR C 2
H38E H 0.6878 0.3382 0.4642 0.083 Uiso 0.201(8) 1 calc PR C 2
H38F H 0.6576 0.2606 0.4710 0.083 Uiso 0.201(8) 1 calc PR C 2
O5 O 0.5438(2) 0.9638(3) 0.35420(15) 0.0535(12) Uani 1 1 d D A .
N1 N 0.5807(7) 0.9618(7) 0.2841(4) 0.084(5) Uani 0.50 1 d PD A 1
C16 C 0.5629(7) 0.9373(7) 0.3212(4) 0.063(4) Uani 0.50 1 d PD A 1
C17 C 0.6077(8) 0.9239(9) 0.2488(5) 0.080(6) Uani 0.50 1 d PD A 1
H17A H 0.6101 0.8726 0.2566 0.120 Uiso 0.50 1 calc PR A 1
H17B H 0.6549 0.9416 0.2511 0.120 Uiso 0.50 1 calc PR A 1
H17C H 0.5765 0.9316 0.2147 0.120 Uiso 0.50 1 calc PR A 1
C18 C 0.5764(12) 1.0388(8) 0.2789(7) 0.096(6) Uani 0.50 1 d PD A 1
H18A H 0.5578 1.0590 0.3048 0.143 Uiso 0.50 1 calc PR A 1
H18B H 0.5451 1.0512 0.2457 0.143 Uiso 0.50 1 calc PR A 1
H18C H 0.6235 1.0583 0.2828 0.143 Uiso 0.50 1 calc PR A 1
C19 C 0.5760(10) 0.8542(9) 0.3270(8) 0.088(7) Uani 0.50 1 d PD A 1
H19A H 0.5621 0.8367 0.3558 0.132 Uiso 0.50 1 calc PR A 1
H19B H 0.6261 0.8442 0.3323 0.132 Uiso 0.50 1 calc PR A 1
H19C H 0.5481 0.8299 0.2964 0.132 Uiso 0.50 1 calc PR A 1
O5B O 0.5370(8) 0.8190(8) 0.3293(5) 0.087(4) Uani 0.50 1 d PD D 2
C16B C 0.5581(9) 0.7873(8) 0.2981(6) 0.084(6) Uani 0.50 1 d PD D 2
N1B N 0.5337(8) 0.7256(8) 0.2783(6) 0.104(6) Uani 0.50 1 d PD . 2
C17B C 0.4836(12) 0.6878(12) 0.2978(8) 0.105(7) Uani 0.50 1 d PD . 2
H17D H 0.4728 0.7154 0.3236 0.157 Uiso 0.50 1 d PR . 2
H17E H 0.4411 0.6780 0.2715 0.157 Uiso 0.50 1 d PR . 2
H17F H 0.5052 0.6435 0.3117 0.157 Uiso 0.50 1 d PR . 2
C18B C 0.5569(12) 0.6831(12) 0.2427(8) 0.112(8) Uani 0.50 1 d PD . 2
H18D H 0.5885 0.7132 0.2317 0.169 Uiso 0.50 1 d PR . 2
H18E H 0.5800 0.6389 0.2553 0.169 Uiso 0.50 1 d PR . 2
H18F H 0.5159 0.6735 0.2151 0.169 Uiso 0.50 1 d PR . 2
C19B C 0.6122(10) 0.8287(11) 0.2769(7) 0.105(7) Uani 0.50 1 d PD D 2
H19D H 0.6239 0.8727 0.2952 0.158 Uiso 0.50 1 d PR D 2
H19E H 0.6543 0.8011 0.2809 0.158 Uiso 0.50 1 d PR D 2
H19F H 0.5909 0.8389 0.2420 0.158 Uiso 0.50 1 d PR D 2
O21 O 0.6387(12) 1.0280(14) 0.3288(9) 0.081(7) Uani 0.25 1 d P E 2
O22 O 0.6848(11) 1.1242(11) 0.4281(9) 0.089(9) Uani 0.25 1 d P F 2
O23 O 0.7104(11) 1.0721(13) 0.3938(8) 0.063(6) Uani 0.25 1 d P F 2
O24 O 0.7546(11) 1.0469(12) 0.3909(8) 0.069(6) Uani 0.25 1 d P F 2
O20 O 0.7516(3) 0.8100(3) 0.4272(4) 0.127(3) Uani 1 1 d D . .
N3 N 0.6660(4) 0.7545(5) 0.4424(4) 0.046(2) Uani 0.590(12) 1 d PDU G 1
C39 C 0.7180(6) 0.7537(5) 0.4227(5) 0.057(3) Uani 0.590(12) 1 d PDU G 1
C40 C 0.7316(10) 0.6835(10) 0.3958(8) 0.078(5) Uani 0.590(12) 1 d PDU G 1
H40A H 0.6924 0.6757 0.3653 0.117 Uiso 0.590(12) 1 calc PR G 1
H40B H 0.7354 0.6426 0.4184 0.117 Uiso 0.590(12) 1 calc PR G 1
H40C H 0.7754 0.6886 0.3868 0.117 Uiso 0.590(12) 1 calc PR G 1
C41 C 0.6154(10) 0.6969(8) 0.4374(8) 0.054(4) Uani 0.590(12) 1 d PDU G 1
H41A H 0.5777 0.7023 0.4057 0.082 Uiso 0.590(12) 1 calc PR G 1
H41B H 0.5954 0.6987 0.4655 0.082 Uiso 0.590(12) 1 calc PR G 1
H41C H 0.6390 0.6508 0.4376 0.082 Uiso 0.590(12) 1 calc PR G 1
C42 C 0.6493(12) 0.8187(11) 0.4659(9) 0.072(6) Uani 0.590(12) 1 d PDU G 1
H42A H 0.6872 0.8538 0.4699 0.108 Uiso 0.590(12) 1 calc PR G 1
H42B H 0.6446 0.8066 0.4989 0.108 Uiso 0.590(12) 1 calc PR G 1
H42C H 0.6050 0.8390 0.4448 0.108 Uiso 0.590(12) 1 calc PR G 1
N3B N 0.6740(7) 0.7218(6) 0.4188(6) 0.049(3) Uani 0.410(12) 1 d PDU G 2
C39B C 0.6974(8) 0.7856(8) 0.4346(8) 0.067(4) Uani 0.410(12) 1 d PDU G 2
C40B C 0.6634(18) 0.8129(19) 0.4758(11) 0.068(7) Uani 0.410(12) 1 d PDU G 2
H40D H 0.6214 0.7845 0.4741 0.103 Uiso 0.410(12) 1 calc PR G 2
H40E H 0.6503 0.8634 0.4697 0.103 Uiso 0.410(12) 1 calc PR G 2
H40F H 0.6975 0.8078 0.5091 0.103 Uiso 0.410(12) 1 calc PR G 2
C41B C 0.6163(15) 0.6793(14) 0.4252(13) 0.062(6) Uani 0.410(12) 1 d PDU G 2
H41D H 0.6144 0.6335 0.4078 0.093 Uiso 0.410(12) 1 calc PR G 2
H41E H 0.5719 0.7051 0.4111 0.093 Uiso 0.410(12) 1 calc PR G 2
H41F H 0.6236 0.6706 0.4610 0.093 Uiso 0.410(12) 1 calc PR G 2
C42B C 0.7084(13) 0.6908(16) 0.3846(11) 0.067(6) Uani 0.410(12) 1 d PDU G 2
H42D H 0.6889 0.6432 0.3742 0.101 Uiso 0.410(12) 1 calc PR G 2
H42E H 0.7591 0.6868 0.4014 0.101 Uiso 0.410(12) 1 calc PR G 2
H42F H 0.7006 0.7215 0.3550 0.101 Uiso 0.410(12) 1 calc PR G 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
Sm1 O7 2.333(3) 4 ?
Sm1 O13 2.347(3) 7_566 ?
Sm1 O14 2.356(3) 3 ?
Sm1 O5 2.374(4) . ?
Sm1 O1 2.490(3) . ?
Sm1 O2 2.493(3) . ?
Sm1 O4B 2.501(16) . ?
Sm1 O3 2.511(3) . ?
Sm1 O4 2.547(16) . ?
Sm1 C1 2.851(4) . ?
Sm2 O10 2.349(3) 5_666 ?
Sm2 O8 2.385(3) . ?
Sm2 O9 2.395(3) 5_666 ?
Sm2 O15 2.414(3) . ?
Sm2 O17 2.420(4) . ?
Sm2 O16 2.466(3) . ?
Sm2 O12 2.485(3) 6_565 ?
Sm2 O11 2.523(4) 6_565 ?
Sm2 C32 2.869(5) 6_565 ?
Sm2 O10 2.907(3) . ?
Sm2 C20 3.017(5) . ?
O1 C1 1.256(5) . ?
O2 C1 1.275(5) . ?
O6 C13 1.241(6) . ?
O7 C13 1.243(6) . ?
O7 Sm1 2.333(3) 4_545 ?
O8 C5 1.250(6) . ?
O9 C5 1.246(5) . ?
O9 Sm2 2.395(3) 5_666 ?
O10 C20 1.267(5) . ?
O10 Sm2 2.349(3) 5_666 ?
O11 C32 1.269(7) . ?
O11 Sm2 2.523(4) 6_566 ?
O12 C32 1.240(7) . ?
O12 Sm2 2.485(3) 6_566 ?
O13 C24 1.246(6) . ?
O13 Sm1 2.347(3) 7_566 ?
O14 C24 1.253(6) . ?
O14 Sm1 2.356(3) 3_445 ?
O15 C20 1.250(5) . ?
O19 H19G 0.822(10) . ?
O19 H19H 0.823(10) . ?
C1 C2 1.503(6) . ?
C2 C3 1.388(6) . ?
C2 C8 1.390(6) . ?
C3 C4 1.387(6) . ?
C3 H3 0.9500 . ?
C4 C6 1.392(6) . ?
C4 C5 1.528(6) . ?
C6 C7 1.406(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(6) . ?
C7 C9 1.487(6) . ?
C8 H8 0.9500 . ?
C9 C15B 1.34(3) . ?
C9 C10 1.394(10) . ?
C9 C10B 1.40(2) . ?
C9 C15 1.399(10) . ?
C10 C11 1.385(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(9) . ?
C11 H11 0.9500 . ?
C14 C15 1.385(12) . ?
C14 C12 1.398(11) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C10B C11B 1.39(3) . ?
C10B H10A 0.9500 . ?
C11B C12 1.41(2) . ?
C11B H11A 0.9500 . ?
C14B C12 1.33(3) . ?
C14B C15B 1.40(3) . ?
C14B H14A 0.9500 . ?
C15B H15A 0.9500 . ?
C12 C13 1.496(6) . ?
C20 C21 1.503(6) . ?
C21 C27 1.383(6) . ?
C21 C22 1.387(6) . ?
C22 C23 1.393(6) . ?
C22 H22 0.9500 . ?
C23 C25 1.384(6) . ?
C23 C24 1.496(6) . ?
C25 C26 1.411(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.394(6) . ?
C26 C28 1.489(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.379(6) . ?
C28 C29B 1.386(8) . ?
C28 C34B 1.388(19) . ?
C28 C34 1.407(6) . ?
C31 C30 1.373(8) . ?
C31 C33B 1.37(2) . ?
C31 C30B 1.38(3) . ?
C31 C33 1.412(6) . ?
C31 C32 1.503(7) . ?
C32 Sm2 2.869(5) 6_566 ?
C29 C30 1.388(8) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C33 C34 1.391(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C29B C30B 1.39(3) . ?
C29B H29A 0.9500 . ?
C30B H30A 0.9500 . ?
C33B C34B 1.39(2) . ?
C33B H33A 0.9500 . ?
C34B H34A 0.9500 . ?
O17 C35 1.234(9) . ?
O17 C35B 1.236(10) . ?
N2 C35 1.311(10) . ?
N2 C36 1.454(10) . ?
N2 C37 1.457(9) . ?
C35 C38 1.582(14) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N2B C35B 1.313(10) . ?
N2B C37B 1.457(10) . ?
N2B C36B 1.460(10) . ?
C35B C38B 1.582(15) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
O5 C16 1.203(8) . ?
N1 C16 1.274(10) . ?
N1 C17 1.442(9) . ?
N1 C18 1.445(9) . ?
C16 C19 1.575(14) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 H19D 1.5645 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 H19D 1.5209 . ?
O5B C16B 1.225(9) . ?
C16B N1B 1.307(10) . ?
C16B C19B 1.577(14) . ?
N1B C18B 1.449(9) . ?
N1B C17B 1.453(10) . ?
N1B N1B 1.74(3) 2_655 ?
N1B C18B 1.90(3) 2_655 ?
C17B C18B 1.18(3) 2_655 ?
C17B H17D 0.9600 . ?
C17B H17E 0.9599 . ?
C17B H17F 0.9601 . ?
C18B C17B 1.18(3) 2_655 ?
C18B N1B 1.90(3) 2_655 ?
C18B H18D 0.9597 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9596 . ?
C19B H19D 0.9601 . ?
C19B H19E 0.9598 . ?
C19B H19F 0.9599 . ?
O22 O23 1.55(3) . ?
O23 O24 1.02(3) . ?
O20 C39 1.233(8) . ?
O20 C39B 1.242(9) . ?
N3 C39 1.306(9) . ?
N3 C41 1.453(9) . ?
N3 C42 1.453(17) . ?
C39 C40 1.574(14) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N3B C39B 1.309(10) . ?
N3B C41B 1.45(3) . ?
N3B C42B 1.45(3) . ?
C39B C40B 1.581(15) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

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
O7 Sm1 O13 85.00(15) 4 7_566 ?
O7 Sm1 O14 150.32(14) 4 3 ?
O13 Sm1 O14 108.03(12) 7_566 3 ?
O7 Sm1 O5 100.58(16) 4 . ?
O13 Sm1 O5 149.15(14) 7_566 . ?
O14 Sm1 O5 81.98(14) 3 . ?
O7 Sm1 O1 78.46(11) 4 . ?
O13 Sm1 O1 77.84(11) 7_566 . ?
O14 Sm1 O1 129.65(11) 3 . ?
O5 Sm1 O1 73.72(14) . . ?
O7 Sm1 O2 129.20(12) 4 . ?
O13 Sm1 O2 73.27(11) 7_566 . ?
O14 Sm1 O2 80.46(11) 3 . ?
O5 Sm1 O2 80.06(14) . . ?
O1 Sm1 O2 52.62(9) . . ?
O7 Sm1 O4B 69.5(3) 4 . ?
O13 Sm1 O4B 137.7(5) 7_566 . ?
O14 Sm1 O4B 83.8(3) 3 . ?
O5 Sm1 O4B 71.0(5) . . ?
O1 Sm1 O4B 125.9(4) . . ?
O2 Sm1 O4B 148.7(5) . . ?
O7 Sm1 O3 78.89(11) 4 . ?
O13 Sm1 O3 73.06(11) 7_566 . ?
O14 Sm1 O3 79.72(12) 3 . ?
O5 Sm1 O3 137.76(14) . . ?
O1 Sm1 O3 144.33(11) . . ?
O2 Sm1 O3 132.89(10) . . ?
O4B Sm1 O3 69.4(5) . . ?
O7 Sm1 O4 82.4(3) 4 . ?
O13 Sm1 O4 140.2(4) 7_566 . ?
O14 Sm1 O4 70.5(3) 3 . ?
O5 Sm1 O4 70.5(4) . . ?
O1 Sm1 O4 135.2(4) . . ?
O2 Sm1 O4 140.8(4) . . ?
O4B Sm1 O4 13.3(3) . . ?
O3 Sm1 O4 67.5(4) . . ?
O7 Sm1 C1 103.83(13) 4 . ?
O13 Sm1 C1 74.26(12) 7_566 . ?
O14 Sm1 C1 105.35(13) 3 . ?
O5 Sm1 C1 74.95(14) . . ?
O1 Sm1 C1 26.10(11) . . ?
O2 Sm1 C1 26.53(11) . . ?
O4B Sm1 C1 143.1(5) . . ?
O3 Sm1 C1 146.82(12) . . ?
O4 Sm1 C1 145.5(4) . . ?
O10 Sm2 O8 76.12(13) 5_666 . ?
O10 Sm2 O9 78.16(12) 5_666 5_666 ?
O8 Sm2 O9 130.62(11) . 5_666 ?
O10 Sm2 O15 124.35(11) 5_666 . ?
O8 Sm2 O15 73.76(13) . . ?
O9 Sm2 O15 87.53(12) 5_666 . ?
O10 Sm2 O17 84.53(16) 5_666 . ?
O8 Sm2 O17 140.52(17) . . ?
O9 Sm2 O17 76.39(17) 5_666 . ?
O15 Sm2 O17 143.50(16) . . ?
O10 Sm2 O16 149.71(13) 5_666 . ?
O8 Sm2 O16 133.56(13) . . ?
O9 Sm2 O16 76.13(12) 5_666 . ?
O15 Sm2 O16 70.26(12) . . ?
O17 Sm2 O16 74.11(16) . . ?
O10 Sm2 O12 131.97(12) 5_666 6_565 ?
O8 Sm2 O12 74.37(13) . 6_565 ?
O9 Sm2 O12 148.40(12) 5_666 6_565 ?
O15 Sm2 O12 81.68(12) . 6_565 ?
O17 Sm2 O12 95.04(18) . 6_565 ?
O16 Sm2 O12 72.27(12) . 6_565 ?
O10 Sm2 O11 83.49(14) 5_666 6_565 ?
O8 Sm2 O11 72.24(17) . 6_565 ?
O9 Sm2 O11 144.35(14) 5_666 6_565 ?
O15 Sm2 O11 127.85(13) . 6_565 ?
O17 Sm2 O11 71.61(19) . 6_565 ?
O16 Sm2 O11 108.94(17) . 6_565 ?
O12 Sm2 O11 51.74(14) 6_565 6_565 ?
O10 Sm2 C32 108.47(15) 5_666 6_565 ?
O8 Sm2 C32 71.88(14) . 6_565 ?
O9 Sm2 C32 157.21(14) 5_666 6_565 ?
O15 Sm2 C32 104.99(14) . 6_565 ?
O17 Sm2 C32 82.48(18) . 6_565 ?
O16 Sm2 C32 90.05(16) . 6_565 ?
O12 Sm2 C32 25.52(14) 6_565 6_565 ?
O11 Sm2 C32 26.23(16) 6_565 6_565 ?
O10 Sm2 O10 77.26(11) 5_666 . ?
O8 Sm2 O10 66.62(11) . . ?
O9 Sm2 O10 66.98(11) 5_666 . ?
O15 Sm2 O10 48.02(10) . . ?
O17 Sm2 O10 141.60(16) . . ?
O16 Sm2 O10 106.59(11) . . ?
O12 Sm2 O10 122.24(12) 6_565 . ?
O11 Sm2 O10 137.59(16) 6_565 . ?
C32 Sm2 O10 135.30(13) 6_565 . ?
O10 Sm2 C20 101.50(12) 5_666 . ?
O8 Sm2 C20 68.79(13) . . ?
O9 Sm2 C20 76.12(13) 5_666 . ?
O15 Sm2 C20 23.43(11) . . ?
O17 Sm2 C20 149.92(16) . . ?
O16 Sm2 C20 87.63(13) . . ?
O12 Sm2 C20 102.02(13) 6_565 . ?
O11 Sm2 C20 138.02(15) 6_565 . ?
C32 Sm2 C20 121.99(14) 6_565 . ?
O10 Sm2 C20 24.60(10) . . ?
C1 O1 Sm1 93.2(2) . . ?
C1 O2 Sm1 92.6(2) . . ?
C13 O7 Sm1 139.6(3) . 4_545 ?
C5 O8 Sm2 138.3(3) . . ?
C5 O9 Sm2 136.0(3) . 5_666 ?
C20 O10 Sm2 168.9(3) . 5_666 ?
C20 O10 Sm2 82.5(3) . . ?
Sm2 O10 Sm2 102.74(11) 5_666 . ?
C32 O11 Sm2 92.3(3) . 6_566 ?
C32 O12 Sm2 94.8(3) . 6_566 ?
C24 O13 Sm1 176.6(3) . 7_566 ?
C24 O14 Sm1 125.3(3) . 3_445 ?
C20 O15 Sm2 106.4(3) . . ?
H19G O19 H19H 115(2) . . ?
O1 C1 O2 121.5(4) . . ?
O1 C1 C2 119.2(4) . . ?
O2 C1 C2 119.2(4) . . ?
O1 C1 Sm1 60.7(2) . . ?
O2 C1 Sm1 60.9(2) . . ?
C2 C1 Sm1 177.6(3) . . ?
C3 C2 C8 119.9(4) . . ?
C3 C2 C1 120.6(4) . . ?
C8 C2 C1 119.4(4) . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C6 119.7(4) . . ?
C3 C4 C5 120.9(4) . . ?
C6 C4 C5 119.3(4) . . ?
O9 C5 O8 127.8(4) . . ?
O9 C5 C4 116.3(4) . . ?
O8 C5 C4 115.9(4) . . ?
C4 C6 C7 121.1(4) . . ?
C4 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 117.9(4) . . ?
C8 C7 C9 121.8(4) . . ?
C6 C7 C9 120.3(4) . . ?
C2 C8 C7 121.2(4) . . ?
C2 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C15B C9 C10 106.0(13) . . ?
C15B C9 C10B 117.1(15) . . ?
C10 C9 C10B 38.0(12) . . ?
C15B C9 C15 30.2(13) . . ?
C10 C9 C15 117.3(6) . . ?
C10B C9 C15 107.5(11) . . ?
C15B C9 C7 123.2(12) . . ?
C10 C9 C7 120.6(5) . . ?
C10B C9 C7 119.5(10) . . ?
C15 C9 C7 122.0(5) . . ?
C11 C10 C9 121.4(7) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C12 C11 C10 120.9(7) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C15 C14 C12 120.6(8) . . ?
C15 C14 H14 119.7 . . ?
C12 C14 H14 119.7 . . ?
C14 C15 C9 121.1(8) . . ?
C14 C15 H15 119.5 . . ?
C9 C15 H15 119.5 . . ?
C11B C10B C9 119.4(19) . . ?
C11B C10B H10A 120.3 . . ?
C9 C10B H10A 120.3 . . ?
C10B C11B C12 121.8(19) . . ?
C10B C11B H11A 119.1 . . ?
C12 C11B H11A 119.1 . . ?
C12 C14B C15B 121(2) . . ?
C12 C14B H14A 119.5 . . ?
C15B C14B H14A 119.5 . . ?
C9 C15B C14B 123(2) . . ?
C9 C15B H15A 118.5 . . ?
C14B C15B H15A 118.5 . . ?
C14B C12 C11 108.9(13) . . ?
C14B C12 C14 29.3(13) . . ?
C11 C12 C14 118.5(6) . . ?
C14B C12 C11B 117.0(15) . . ?
C11 C12 C11B 37.5(11) . . ?
C14 C12 C11B 106.5(10) . . ?
C14B C12 C13 123.3(12) . . ?
C11 C12 C13 119.0(5) . . ?
C14 C12 C13 122.5(5) . . ?
C11B C12 C13 119.4(10) . . ?
O6 C13 O7 123.5(4) . . ?
O6 C13 C12 119.8(4) . . ?
O7 C13 C12 116.8(4) . . ?
O15 C20 O10 123.0(4) . . ?
O15 C20 C21 117.8(4) . . ?
O10 C20 C21 119.2(4) . . ?
O15 C20 Sm2 50.1(2) . . ?
O10 C20 Sm2 72.9(3) . . ?
C21 C20 Sm2 167.4(3) . . ?
C27 C21 C22 120.3(4) . . ?
C27 C21 C20 120.7(4) . . ?
C22 C21 C20 118.9(4) . . ?
C21 C22 C23 119.9(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C25 C23 C22 119.6(4) . . ?
C25 C23 C24 121.2(4) . . ?
C22 C23 C24 119.2(4) . . ?
O13 C24 O14 122.8(4) . . ?
O13 C24 C23 119.9(4) . . ?
O14 C24 C23 117.3(4) . . ?
C23 C25 C26 121.0(4) . . ?
C23 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C27 C26 C25 118.1(4) . . ?
C27 C26 C28 120.4(4) . . ?
C25 C26 C28 121.5(4) . . ?
C21 C27 C26 120.9(4) . . ?
C21 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C29 C28 C29B 10(2) . . ?
C29 C28 C34B 109.2(11) . . ?
C29B C28 C34B 99(2) . . ?
C29 C28 C34 119.1(8) . . ?
C29B C28 C34 111.8(19) . . ?
C34B C28 C34 43.6(9) . . ?
C29 C28 C26 119.7(7) . . ?
C29B C28 C26 128.3(18) . . ?
C34B C28 C26 122.2(8) . . ?
C34 C28 C26 119.4(4) . . ?
C30 C31 C33B 107.7(13) . . ?
C30 C31 C30B 11(2) . . ?
C33B C31 C30B 110(2) . . ?
C30 C31 C33 115.3(8) . . ?
C33B C31 C33 46.5(9) . . ?
C30B C31 C33 124.7(17) . . ?
C30 C31 C32 123.6(7) . . ?
C33B C31 C32 117.5(8) . . ?
C30B C31 C32 115.1(18) . . ?
C33 C31 C32 120.0(5) . . ?
O12 C32 O11 121.2(5) . . ?
O12 C32 C31 119.9(5) . . ?
O11 C32 C31 118.8(5) . . ?
O12 C32 Sm2 59.7(3) . 6_566 ?
O11 C32 Sm2 61.5(3) . 6_566 ?
C31 C32 Sm2 179.4(4) . 6_566 ?
C28 C29 C30 116.5(12) . . ?
C28 C29 H29 121.7 . . ?
C30 C29 H29 121.7 . . ?
C31 C30 C29 125.5(13) . . ?
C31 C30 H30 117.2 . . ?
C29 C30 H30 117.2 . . ?
C34 C33 C31 119.6(6) . . ?
C34 C33 H33 120.2 . . ?
C31 C33 H33 120.2 . . ?
C33 C34 C28 120.6(6) . . ?
C33 C34 H34 119.7 . . ?
C28 C34 H34 119.7 . . ?
C28 C29B C30B 134(3) . . ?
C28 C29B H29A 113.1 . . ?
C30B C29B H29A 113.1 . . ?
C31 C30B C29B 109(3) . . ?
C31 C30B H30A 125.7 . . ?
C29B C30B H30A 125.7 . . ?
C31 C33B C34B 117.6(16) . . ?
C31 C33B H33A 121.2 . . ?
C34B C33B H33A 121.2 . . ?
C33B C34B C28 124.2(16) . . ?
C33B C34B H34A 117.9 . . ?
C28 C34B H34A 117.9 . . ?
C35 O17 C35B 30.4(12) . . ?
C35 O17 Sm2 154.9(10) . . ?
C35B O17 Sm2 152.3(13) . . ?
C35 N2 C36 117.4(15) . . ?
C35 N2 C37 129.1(15) . . ?
C36 N2 C37 113.4(13) . . ?
O17 C35 N2 120.2(13) . . ?
O17 C35 C38 125.5(13) . . ?
N2 C35 C38 114.0(13) . . ?
C35B N2B C37B 125.2(18) . . ?
C35B N2B C36B 119.5(13) . . ?
C37B N2B C36B 111.1(12) . . ?
O17 C35B N2B 123.0(15) . . ?
O17 C35B C38B 115(2) . . ?
N2B C35B C38B 122(2) . . ?
N2B C36B H36D 109.5 . . ?
N2B C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
N2B C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
N2B C37B H37D 109.5 . . ?
N2B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
N2B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35B C38B H38D 109.5 . . ?
C35B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C16 O5 Sm1 174.2(8) . . ?
C16 N1 C17 128.9(12) . . ?
C16 N1 C18 114.7(12) . . ?
C17 N1 C18 116.4(11) . . ?
O5 C16 N1 134.5(13) . . ?
O5 C16 C19 114.1(12) . . ?
N1 C16 C19 111.2(12) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C17 H19D 76.2 . . ?
H17A C17 H19D 40.1 . . ?
H17B C17 H19D 101.2 . . ?
H17C C17 H19D 144.0 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C19 H19D 80.2 . . ?
H19A C19 H19D 158.7 . . ?
H19B C19 H19D 49.3 . . ?
H19C C19 H19D 83.7 . . ?
O5B C16B N1B 124.3(15) . . ?
O5B C16B C19B 116.5(14) . . ?
N1B C16B C19B 118.9(13) . . ?
C16B N1B C18B 128.2(15) . . ?
C16B N1B C17B 118.7(14) . . ?
C18B N1B C17B 112.6(11) . . ?
C16B N1B N1B 118.2(13) . 2_655 ?
C18B N1B N1B 72.3(13) . 2_655 ?
C17B N1B N1B 84.9(14) . 2_655 ?
C16B N1B C18B 134.4(15) . 2_655 ?
C18B N1B C18B 91.5(14) . 2_655 ?
C17B N1B C18B 38.5(10) . 2_655 ?
N1B N1B C18B 46.7(7) 2_655 2_655 ?
C18B C17B N1B 91.5(16) 2_655 . ?
C18B C17B H17D 121.1 2_655 . ?
N1B C17B H17D 110.6 . . ?
C18B C17B H17E 19.3 2_655 . ?
N1B C17B H17E 110.5 . . ?
H17D C17B H17E 109.5 . . ?
C18B C17B H17F 114.8 2_655 . ?
N1B C17B H17F 107.2 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C17B C18B N1B 110(2) 2_655 . ?
C17B C18B N1B 50.0(11) 2_655 2_655 ?
N1B C18B N1B 61.0(14) . 2_655 ?
C17B C18B H18D 88.6 2_655 . ?
N1B C18B H18D 105.7 . . ?
N1B C18B H18D 108.0 2_655 . ?
C17B C18B H18E 122.1 2_655 . ?
N1B C18B H18E 115.8 . . ?
N1B C18B H18E 141.4 2_655 . ?
H18D C18B H18E 109.5 . . ?
C17B C18B H18F 21.2 2_655 . ?
N1B C18B H18F 106.6 . . ?
N1B C18B H18F 47.7 2_655 . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C16B C19B H19D 107.7 . . ?
C16B C19B H19E 111.2 . . ?
H19D C19B H19E 109.5 . . ?
C16B C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
O24 O23 O22 142(3) . . ?
C39 O20 C39B 40.0(8) . . ?
C39 N3 C41 124.3(10) . . ?
C39 N3 C42 121.0(11) . . ?
C41 N3 C42 114.2(11) . . ?
O20 C39 N3 114.8(9) . . ?
O20 C39 C40 126.5(12) . . ?
N3 C39 C40 118.7(11) . . ?
C39B N3B C41B 132.3(15) . . ?
C39B N3B C42B 113.3(16) . . ?
C41B N3B C42B 114.1(16) . . ?
O20 C39B N3B 121.1(13) . . ?
O20 C39B C40B 125.6(18) . . ?
N3B C39B C40B 110.7(17) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
N3B C41B H41D 109.5 . . ?
N3B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
N3B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
N3B C42B H42D 109.5 . . ?
N3B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
N3B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.138


# Start Validation Reply Form
_vrf_PLAT220_5                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        5.2 Ratio 
Large Non-Solvent    O     Ueq(max)/Ueq(min) ...        4.2 Ratio

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;
_database_code_depnum_ccdc_archive 'CCDC 981952'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H48.50 Eu2 N2.50 O20'
_chemical_formula_weight         1200.24

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'
Eu Eu -0.1578 3.6682 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   ' C 1 2/c 1'

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

_cell_length_a                   19.8267(3)
_cell_length_b                   18.6253(2)
_cell_length_c                   27.8685(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1000(10)
_cell_angle_gamma                90.00
_cell_volume                     9836.3(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17256
_cell_measurement_theta_min      3.3070
_cell_measurement_theta_max      29.3870

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4784
_exptl_absorpt_coefficient_mu    2.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49468
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.10
_reflns_number_total             10816
_reflns_number_gt                8429
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0610P)²+339.6226P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10816
_refine_ls_number_parameters     873
_refine_ls_number_restraints     1014
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1611
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.49451(2) 1.01622(2) 0.413610(13) 0.01625(11) Uani 1 1 d . . .
Eu2 Eu 0.45628(2) 0.43118(2) 0.441330(12) 0.01489(11) Uani 1 1 d . . .
O1 O 0.4077(3) 0.9258(3) 0.36681(19) 0.0231(12) Uani 1 1 d . A .
O2 O 0.4882(3) 0.8873(3) 0.43482(18) 0.0194(11) Uani 1 1 d . A .
O3 O 0.5092(3) 1.1289(3) 0.4648(2) 0.0263(13) Uani 1 1 d . A .
O4 O 0.5765(14) 1.1057(15) 0.3906(9) 0.049(6) Uani 0.50 1 d P A 1
O4B O 0.5496(12) 1.1123(18) 0.3754(9) 0.047(6) Uani 0.50 1 d P A 2
O6 O 0.0790(5) 0.7011(4) 0.1150(3) 0.060(3) Uani 1 1 d . . .
O7 O 0.0918(4) 0.5890(3) 0.1387(2) 0.047(2) Uani 1 1 d . . .
O8 O 0.4210(4) 0.5531(3) 0.4255(2) 0.0375(17) Uani 1 1 d . . .
O9 O 0.4880(3) 0.6295(3) 0.4815(2) 0.0315(15) Uani 1 1 d . . .
O10 O 0.4382(3) 0.5044(4) 0.5286(2) 0.0284(13) Uani 1 1 d . . .
O11 O 0.4681(4) 0.5355(7) 0.8566(3) 0.074(3) Uani 1 1 d U . .
O12 O 0.3637(4) 0.5687(4) 0.8588(2) 0.0426(19) Uani 1 1 d . . .
O13 O 0.0829(3) 0.4918(3) 0.5374(2) 0.0269(13) Uani 1 1 d . . .
O14 O 0.1100(3) 0.5000(4) 0.4669(2) 0.0311(14) Uani 1 1 d . . .
O15 O 0.3551(3) 0.4466(3) 0.4712(2) 0.0254(13) Uani 1 1 d . . .
O16 O 0.3912(4) 0.3174(3) 0.4337(2) 0.0373(16) Uani 1 1 d . . .
O19 O 0.2297(7) 0.5694(14) 0.8654(5) 0.149(8) Uani 1 1 d D . .
H19G H 0.204(16) 0.541(14) 0.874(11) 0.224 Uiso 1 1 d D . .
H19H H 0.245(15) 0.602(11) 0.885(9) 0.224 Uiso 1 1 d D . .
C1 C 0.4353(4) 0.8762(4) 0.3965(3) 0.0184(15) Uani 1 1 d . A .
C2 C 0.4060(4) 0.8017(4) 0.3861(3) 0.0222(17) Uani 1 1 d . . .
C3 C 0.4351(5) 0.7458(4) 0.4184(3) 0.0252(18) Uani 1 1 d . A .
H3 H 0.4718 0.7550 0.4484 0.030 Uiso 1 1 calc R . .
C4 C 0.4106(5) 0.6765(4) 0.4068(3) 0.0271(19) Uani 1 1 d . . .
C5 C 0.4437(5) 0.6138(5) 0.4409(3) 0.0274(19) Uani 1 1 d . A .
C6 C 0.3568(5) 0.6632(5) 0.3627(3) 0.032(2) Uani 1 1 d . A .
H6 H 0.3405 0.6155 0.3548 0.038 Uiso 1 1 calc R . .
C7 C 0.3263(5) 0.7192(5) 0.3297(3) 0.030(2) Uani 1 1 d . . .
C8 C 0.3516(5) 0.7884(4) 0.3425(3) 0.0266(18) Uani 1 1 d . A .
H8 H 0.3314 0.8273 0.3210 0.032 Uiso 1 1 calc R . .
C9 C 0.2696(5) 0.7039(5) 0.2824(3) 0.034(2) Uani 1 1 d . A .
C10 C 0.2618(10) 0.6356(8) 0.2614(6) 0.049(4) Uani 0.73(2) 1 d PU A 1
H10 H 0.2934 0.5986 0.2775 0.059 Uiso 0.73(2) 1 calc PR A 1
C11 C 0.2090(10) 0.6202(7) 0.2176(6) 0.044(4) Uani 0.73(2) 1 d PU A 1
H11 H 0.2040 0.5726 0.2047 0.053 Uiso 0.73(2) 1 calc PR A 1
C14 C 0.1731(10) 0.7423(9) 0.2114(6) 0.042(4) Uani 0.73(2) 1 d PU A 1
H14 H 0.1438 0.7799 0.1936 0.050 Uiso 0.73(2) 1 calc PR A 1
C15 C 0.2247(10) 0.7574(8) 0.2558(6) 0.040(4) Uani 0.73(2) 1 d PU A 1
H15 H 0.2296 0.8051 0.2685 0.048 Uiso 0.73(2) 1 calc PR A 1
C10B C 0.230(3) 0.641(2) 0.2786(16) 0.043(5) Uani 0.27(2) 1 d PU A 2
H10A H 0.2385 0.6089 0.3061 0.052 Uiso 0.27(2) 1 calc PR A 2
C11B C 0.177(3) 0.627(2) 0.2342(15) 0.038(5) Uani 0.27(2) 1 d PU A 2
H11A H 0.1497 0.5843 0.2320 0.045 Uiso 0.27(2) 1 calc PR A 2
C14B C 0.198(3) 0.735(2) 0.1990(17) 0.039(5) Uani 0.27(2) 1 d PU A 2
H14A H 0.1859 0.7698 0.1730 0.047 Uiso 0.27(2) 1 calc PR A 2
C15B C 0.251(3) 0.750(2) 0.2436(17) 0.041(5) Uani 0.27(2) 1 d PU A 2
H15A H 0.2746 0.7946 0.2466 0.049 Uiso 0.27(2) 1 calc PR A 2
C12 C 0.1637(5) 0.6726(5) 0.1924(3) 0.031(2) Uani 1 1 d . . .
C13 C 0.1074(5) 0.6534(5) 0.1453(3) 0.031(2) Uani 1 1 d . A .
C20 C 0.3757(4) 0.4816(4) 0.5111(3) 0.0216(16) Uani 1 1 d . . .
C21 C 0.3241(4) 0.4946(4) 0.5400(3) 0.0182(15) Uani 1 1 d . . .
C22 C 0.2526(4) 0.4897(4) 0.5152(3) 0.0183(15) Uani 1 1 d . . .
H22 H 0.2371 0.4805 0.4801 0.022 Uiso 1 1 calc R . .
C23 C 0.2038(4) 0.4984(4) 0.5416(3) 0.0185(15) Uani 1 1 d . . .
C24 C 0.1270(4) 0.4963(4) 0.5138(3) 0.0203(16) Uani 1 1 d . . .
C25 C 0.2271(4) 0.5087(5) 0.5931(3) 0.0237(17) Uani 1 1 d . . .
H25 H 0.1936 0.5124 0.6113 0.028 Uiso 1 1 calc R . .
C26 C 0.2996(4) 0.5138(5) 0.6189(3) 0.0232(17) Uani 1 1 d . B .
C27 C 0.3472(4) 0.5076(5) 0.5911(3) 0.0224(17) Uani 1 1 d . . .
H27 H 0.3963 0.5123 0.6075 0.027 Uiso 1 1 calc R . .
C28 C 0.3253(4) 0.5226(5) 0.6744(3) 0.031(2) Uani 1 1 d D . .
C31 C 0.3757(5) 0.5383(6) 0.7789(3) 0.038(2) Uani 1 1 d D . .
C32 C 0.4038(5) 0.5492(6) 0.8347(3) 0.037(2) Uani 1 1 d . . .
C29 C 0.2793(9) 0.544(2) 0.7001(6) 0.035(4) Uani 0.699(16) 1 d PDU B 1
H29 H 0.2311 0.5537 0.6833 0.043 Uiso 0.699(16) 1 calc PR B 1
C30 C 0.3069(10) 0.5507(17) 0.7517(7) 0.038(4) Uani 0.699(16) 1 d PDU B 1
H30 H 0.2754 0.5651 0.7699 0.046 Uiso 0.699(16) 1 calc PR B 1
C33 C 0.4161(7) 0.5010(10) 0.7532(4) 0.044(3) Uani 0.699(16) 1 d PDU B 1
H33 H 0.4605 0.4811 0.7712 0.053 Uiso 0.699(16) 1 calc PR B 1
C34 C 0.3908(6) 0.4934(10) 0.7014(3) 0.041(3) Uani 0.699(16) 1 d PDU B 1
H34 H 0.4182 0.4682 0.6840 0.049 Uiso 0.699(16) 1 calc PR B 1
C29B C 0.289(2) 0.550(5) 0.7060(19) 0.037(5) Uani 0.301(16) 1 d PDU B 2
H29A H 0.2423 0.5634 0.6889 0.044 Uiso 0.301(16) 1 calc PR B 2
C30B C 0.307(3) 0.561(4) 0.7575(18) 0.033(5) Uani 0.301(16) 1 d PU B 2
H30A H 0.2774 0.5816 0.7749 0.040 Uiso 0.301(16) 1 calc PR B 2
C33B C 0.4174(18) 0.560(2) 0.7502(11) 0.041(5) Uani 0.301(16) 1 d PU B 2
H33A H 0.4622 0.5812 0.7649 0.049 Uiso 0.301(16) 1 calc PR B 2
C34B C 0.3920(17) 0.549(2) 0.6988(10) 0.035(4) Uani 0.301(16) 1 d PU B 2
H34A H 0.4223 0.5599 0.6791 0.042 Uiso 0.301(16) 1 calc PR B 2
O17 O 0.5291(5) 0.3423(5) 0.4178(4) 0.074(3) Uani 1 1 d D . .
N2 N 0.6302(12) 0.3007(16) 0.4119(10) 0.049(5) Uani 0.299(13) 1 d PDU C 1
C35 C 0.5637(12) 0.3171(19) 0.3917(9) 0.038(5) Uani 0.299(13) 1 d PDU C 1
C36 C 0.660(2) 0.310(4) 0.4658(11) 0.054(8) Uani 0.299(13) 1 d PDU C 1
H36A H 0.6893 0.2692 0.4801 0.081 Uiso 0.299(13) 1 calc PR C 1
H36B H 0.6211 0.3145 0.4811 0.081 Uiso 0.299(13) 1 calc PR C 1
H36C H 0.6880 0.3544 0.4724 0.081 Uiso 0.299(13) 1 calc PR C 1
C37 C 0.681(2) 0.275(2) 0.3878(15) 0.057(7) Uani 0.299(13) 1 d PDU C 1
H37A H 0.7217 0.3082 0.3954 0.086 Uiso 0.299(13) 1 calc PR C 1
H37B H 0.6594 0.2735 0.3513 0.086 Uiso 0.299(13) 1 calc PR C 1
H37C H 0.6975 0.2272 0.4002 0.086 Uiso 0.299(13) 1 calc PR C 1
C38 C 0.537(2) 0.309(2) 0.3326(10) 0.065(7) Uani 0.299(13) 1 d PDU C 1
H38A H 0.4936 0.3365 0.3191 0.097 Uiso 0.299(13) 1 calc PR C 1
H38B H 0.5284 0.2583 0.3238 0.097 Uiso 0.299(13) 1 calc PR C 1
H38C H 0.5735 0.3274 0.3182 0.097 Uiso 0.299(13) 1 calc PR C 1
N2B N 0.5938(18) 0.298(2) 0.3713(13) 0.045(6) Uani 0.201(13) 1 d PDU C 2
C35B C 0.5860(12) 0.321(3) 0.4138(13) 0.041(6) Uani 0.201(13) 1 d PDU C 2
C36B C 0.533(2) 0.270(4) 0.332(2) 0.073(9) Uani 0.201(13) 1 d PDU C 2
H36D H 0.4895 0.2878 0.3382 0.109 Uiso 0.201(13) 1 calc PR C 2
H36E H 0.5337 0.2176 0.3335 0.109 Uiso 0.201(13) 1 calc PR C 2
H36F H 0.5351 0.2864 0.2994 0.109 Uiso 0.201(13) 1 calc PR C 2
C37B C 0.659(2) 0.272(3) 0.365(2) 0.046(7) Uani 0.201(13) 1 d PDU C 2
H37D H 0.6987 0.3018 0.3841 0.068 Uiso 0.201(13) 1 calc PR C 2
H37E H 0.6569 0.2746 0.3289 0.068 Uiso 0.201(13) 1 calc PR C 2
H37F H 0.6671 0.2222 0.3760 0.068 Uiso 0.201(13) 1 calc PR C 2
C38B C 0.646(3) 0.311(6) 0.4653(19) 0.055(9) Uani 0.201(13) 1 d PDU C 2
H38D H 0.6291 0.3299 0.4927 0.083 Uiso 0.201(13) 1 calc PR C 2
H38E H 0.6879 0.3382 0.4642 0.083 Uiso 0.201(13) 1 calc PR C 2
H38F H 0.6577 0.2605 0.4710 0.083 Uiso 0.201(13) 1 calc PR C 2
O5 O 0.5438(4) 0.9638(5) 0.3542(3) 0.054(2) Uani 1 1 d D A .
N1 N 0.5807(13) 0.9618(13) 0.2841(8) 0.084(8) Uani 0.50 1 d PD A 1
C16 C 0.5629(13) 0.9373(12) 0.3212(7) 0.063(8) Uani 0.50 1 d PD A 1
C17 C 0.6077(15) 0.9239(17) 0.2488(9) 0.080(10) Uani 0.50 1 d PD A 1
H17A H 0.6101 0.8724 0.2566 0.120 Uiso 0.50 1 calc PR A 1
H17B H 0.6550 0.9417 0.2510 0.120 Uiso 0.50 1 calc PR A 1
H17C H 0.5764 0.9316 0.2147 0.120 Uiso 0.50 1 calc PR A 1
C18 C 0.576(2) 1.0388(14) 0.2789(12) 0.096(11) Uani 0.50 1 d PD A 1
H18A H 0.5578 1.0591 0.3049 0.143 Uiso 0.50 1 calc PR A 1
H18B H 0.5450 1.0513 0.2457 0.143 Uiso 0.50 1 calc PR A 1
H18C H 0.6236 1.0584 0.2827 0.143 Uiso 0.50 1 calc PR A 1
C19 C 0.5760(19) 0.8542(14) 0.3270(14) 0.088(12) Uani 0.50 1 d PD A 1
H19A H 0.5621 0.8367 0.3558 0.132 Uiso 0.50 1 calc PR A 1
H19B H 0.6262 0.8442 0.3322 0.132 Uiso 0.50 1 calc PR A 1
H19C H 0.5480 0.8298 0.2965 0.132 Uiso 0.50 1 calc PR A 1
O5B O 0.5370(14) 0.8190(14) 0.3293(8) 0.087(7) Uani 0.50 1 d PD D 2
C16B C 0.5581(16) 0.7873(15) 0.2981(11) 0.084(10) Uani 0.50 1 d PD D 2
N1B N 0.5337(16) 0.7256(14) 0.2783(11) 0.104(10) Uani 0.50 1 d PD . 2
C17B C 0.484(2) 0.688(2) 0.2978(15) 0.105(13) Uani 0.50 1 d PD . 2
H17D H 0.4728 0.7154 0.3236 0.157 Uiso 0.50 1 d PR . 2
H17E H 0.4411 0.6780 0.2715 0.157 Uiso 0.50 1 d PR . 2
H17F H 0.5052 0.6435 0.3117 0.157 Uiso 0.50 1 d PR . 2
C18B C 0.557(2) 0.683(2) 0.2427(15) 0.112(15) Uani 0.50 1 d PD . 2
H18D H 0.5885 0.7132 0.2317 0.169 Uiso 0.50 1 d PR . 2
H18E H 0.5800 0.6389 0.2553 0.169 Uiso 0.50 1 d PR . 2
H18F H 0.5159 0.6735 0.2151 0.169 Uiso 0.50 1 d PR . 2
C19B C 0.6122(18) 0.829(2) 0.2769(14) 0.105(13) Uani 0.50 1 d PD D 2
H19D H 0.6239 0.8727 0.2952 0.158 Uiso 0.50 1 d PR D 2
H19E H 0.6543 0.8011 0.2809 0.158 Uiso 0.50 1 d PR D 2
H19F H 0.5909 0.8389 0.2420 0.158 Uiso 0.50 1 d PR D 2
O21 O 0.639(2) 1.028(3) 0.3288(16) 0.081(12) Uani 0.25 1 d P E 2
O22 O 0.685(2) 1.124(2) 0.4281(17) 0.089(16) Uani 0.25 1 d P F 2
O23 O 0.710(2) 1.072(2) 0.3938(14) 0.063(11) Uani 0.25 1 d P F 2
O24 O 0.755(2) 1.047(2) 0.3909(15) 0.069(12) Uani 0.25 1 d P F 2
O20 O 0.7516(6) 0.8100(6) 0.4272(7) 0.127(6) Uani 1 1 d D . .
N3 N 0.6660(8) 0.7545(8) 0.4424(7) 0.046(4) Uani 0.590(18) 1 d PDU G 1
C39 C 0.7180(10) 0.7537(8) 0.4227(9) 0.057(4) Uani 0.590(18) 1 d PDU G 1
C40 C 0.7316(17) 0.6835(16) 0.3958(14) 0.078(6) Uani 0.590(18) 1 d PDU G 1
H40A H 0.6923 0.6758 0.3653 0.117 Uiso 0.590(18) 1 calc PR G 1
H40B H 0.7353 0.6424 0.4184 0.117 Uiso 0.590(18) 1 calc PR G 1
H40C H 0.7756 0.6885 0.3868 0.117 Uiso 0.590(18) 1 calc PR G 1
C41 C 0.6154(14) 0.6969(12) 0.4374(12) 0.054(5) Uani 0.590(18) 1 d PDU G 1
H41A H 0.5777 0.7023 0.4057 0.082 Uiso 0.590(18) 1 calc PR G 1
H41B H 0.5952 0.6987 0.4655 0.082 Uiso 0.590(18) 1 calc PR G 1
H41C H 0.6391 0.6506 0.4376 0.082 Uiso 0.590(18) 1 calc PR G 1
C42 C 0.6493(17) 0.8187(15) 0.4659(14) 0.072(7) Uani 0.590(18) 1 d PDU G 1
H42A H 0.6873 0.8539 0.4699 0.108 Uiso 0.590(18) 1 calc PR G 1
H42B H 0.6445 0.8066 0.4989 0.108 Uiso 0.590(18) 1 calc PR G 1
H42C H 0.6049 0.8391 0.4448 0.108 Uiso 0.590(18) 1 calc PR G 1
N3B N 0.6740(12) 0.7218(11) 0.4188(10) 0.049(5) Uani 0.410(18) 1 d PDU G 2
C39B C 0.6974(13) 0.7856(14) 0.4346(14) 0.067(5) Uani 0.410(18) 1 d PDU G 2
C40B C 0.663(3) 0.813(3) 0.4758(16) 0.068(8) Uani 0.410(18) 1 d PDU G 2
H40D H 0.6212 0.7845 0.4741 0.102 Uiso 0.410(18) 1 calc PR G 2
H40E H 0.6503 0.8636 0.4697 0.102 Uiso 0.410(18) 1 calc PR G 2
H40F H 0.6976 0.8077 0.5091 0.102 Uiso 0.410(18) 1 calc PR G 2
C41B C 0.616(2) 0.679(2) 0.425(2) 0.062(7) Uani 0.410(18) 1 d PDU G 2
H41D H 0.6144 0.6333 0.4077 0.093 Uiso 0.410(18) 1 calc PR G 2
H41E H 0.5718 0.7052 0.4112 0.093 Uiso 0.410(18) 1 calc PR G 2
H41F H 0.6235 0.6705 0.4610 0.093 Uiso 0.410(18) 1 calc PR G 2
C42B C 0.708(2) 0.691(2) 0.3846(18) 0.067(7) Uani 0.410(18) 1 d PDU G 2
H42D H 0.6888 0.6430 0.3742 0.101 Uiso 0.410(18) 1 calc PR G 2
H42E H 0.7592 0.6868 0.4014 0.101 Uiso 0.410(18) 1 calc PR G 2
H42F H 0.7006 0.7217 0.3550 0.101 Uiso 0.410(18) 1 calc PR G 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
Eu1 O7 2.329(6) 4 ?
Eu1 O13 2.339(6) 7_566 ?
Eu1 O14 2.353(6) 3 ?
Eu1 O5 2.367(7) . ?
Eu1 O2 2.485(5) . ?
Eu1 O1 2.486(5) . ?
Eu1 O4B 2.49(3) . ?
Eu1 O3 2.505(5) . ?
Eu1 O4 2.54(3) . ?
Eu1 C1 2.843(8) . ?
Eu1 C24 3.244(8) 3 ?
Eu2 O10 2.343(6) 5_666 ?
Eu2 O8 2.378(6) . ?
Eu2 O9 2.394(5) 5_666 ?
Eu2 O15 2.405(6) . ?
Eu2 O17 2.411(8) . ?
Eu2 O16 2.458(6) . ?
Eu2 O12 2.485(6) 6_565 ?
Eu2 O11 2.519(8) 6_565 ?
Eu2 C32 2.868(8) 6_565 ?
Eu2 O10 2.901(6) . ?
Eu2 C20 3.007(8) . ?
Eu2 Eu2 4.1155(7) 5_666 ?
O1 C1 1.254(9) . ?
O2 C1 1.274(9) . ?
O6 C13 1.239(11) . ?
O7 C13 1.240(11) . ?
O7 Eu1 2.329(6) 4_545 ?
O8 C5 1.247(10) . ?
O9 C5 1.246(9) . ?
O9 Eu2 2.394(5) 5_666 ?
O10 C20 1.264(10) . ?
O10 Eu2 2.343(6) 5_666 ?
O11 C32 1.267(13) . ?
O11 Eu2 2.519(8) 6_566 ?
O12 C32 1.236(12) . ?
O12 Eu2 2.485(6) 6_566 ?
O13 C24 1.242(10) . ?
O13 Eu1 2.339(6) 7_566 ?
O14 C24 1.252(10) . ?
O14 Eu1 2.353(6) 3_445 ?
O15 C20 1.249(9) . ?
O19 H19G 0.819(10) . ?
O19 H19H 0.821(11) . ?
C1 C2 1.498(11) . ?
C2 C3 1.386(11) . ?
C2 C8 1.390(11) . ?
C3 C4 1.383(11) . ?
C3 H3 0.9500 . ?
C4 C6 1.392(11) . ?
C4 C5 1.526(11) . ?
C6 C7 1.404(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(12) . ?
C7 C9 1.487(11) . ?
C8 H8 0.9500 . ?
C9 C15B 1.34(4) . ?
C9 C10 1.390(17) . ?
C9 C10B 1.39(4) . ?
C9 C15 1.396(17) . ?
C10 C11 1.385(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.371(16) . ?
C11 H11 0.9500 . ?
C14 C15 1.384(19) . ?
C14 C12 1.394(18) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C10B C11B 1.39(5) . ?
C10B H10A 0.9500 . ?
C11B C12 1.41(4) . ?
C11B H11A 0.9500 . ?
C14B C12 1.32(5) . ?
C14B C15B 1.40(5) . ?
C14B H14A 0.9500 . ?
C15B H15A 0.9500 . ?
C12 C13 1.495(11) . ?
C20 C21 1.497(11) . ?
C21 C27 1.383(10) . ?
C21 C22 1.385(11) . ?
C22 C23 1.388(11) . ?
C22 H22 0.9500 . ?
C23 C25 1.384(11) . ?
C23 C24 1.493(11) . ?
C24 Eu1 3.244(8) 3_445 ?
C25 C26 1.408(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.389(12) . ?
C26 C28 1.489(10) . ?
C27 H27 0.9500 . ?
C28 C29 1.374(8) . ?
C28 C29B 1.382(9) . ?
C28 C34B 1.39(3) . ?
C28 C34 1.405(8) . ?
C31 C33B 1.37(4) . ?
C31 C30 1.371(9) . ?
C31 C30B 1.38(5) . ?
C31 C33 1.407(8) . ?
C31 C32 1.503(11) . ?
C32 Eu2 2.868(8) 6_566 ?
C29 C30 1.388(9) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C33 C34 1.391(8) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C29B C30B 1.39(5) . ?
C29B H29A 0.9500 . ?
C30B H30A 0.9500 . ?
C33B C34B 1.39(4) . ?
C33B H33A 0.9500 . ?
C34B H34A 0.9500 . ?
O17 C35 1.230(13) . ?
O17 C35B 1.231(14) . ?
N2 C35 1.308(16) . ?
N2 C37 1.452(14) . ?
N2 C36 1.454(14) . ?
C35 C38 1.58(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N2B C35B 1.310(16) . ?
N2B C37B 1.452(14) . ?
N2B C36B 1.459(14) . ?
C35B C38B 1.58(2) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
O5 C16 1.199(13) . ?
N1 C16 1.271(16) . ?
N1 C17 1.438(13) . ?
N1 C18 1.441(14) . ?
C16 C19 1.57(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 H19D 1.5622 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 H19D 1.5157 . ?
O5B C16B 1.222(13) . ?
C16B N1B 1.304(16) . ?
C16B C19B 1.57(2) . ?
N1B C18B 1.445(14) . ?
N1B C17B 1.448(14) . ?
N1B N1B 1.74(6) 2_655 ?
N1B C18B 1.89(5) 2_655 ?
C17B C18B 1.18(5) 2_655 ?
C17B H17D 0.9576 . ?
C17B H17E 0.9592 . ?
C17B H17F 0.9576 . ?
C18B C17B 1.18(5) 2_655 ?
C18B N1B 1.89(5) 2_655 ?
C18B H18D 0.9562 . ?
C18B H18E 0.9576 . ?
C18B H18F 0.9591 . ?
C19B H19D 0.9578 . ?
C19B H19E 0.9568 . ?
C19B H19F 0.9596 . ?
O22 O23 1.55(6) . ?
O23 O24 1.02(5) . ?
O20 C39 1.229(13) . ?
O20 C39B 1.238(13) . ?
N3 C39 1.301(15) . ?
N3 C41 1.448(13) . ?
N3 C42 1.45(3) . ?
C39 C40 1.57(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N3B C39B 1.305(16) . ?
N3B C41B 1.44(4) . ?
N3B C42B 1.45(5) . ?
C39B C40B 1.58(2) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

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
O7 Eu1 O13 85.1(3) 4 7_566 ?
O7 Eu1 O14 150.4(2) 4 3 ?
O13 Eu1 O14 107.9(2) 7_566 3 ?
O7 Eu1 O5 100.4(3) 4 . ?
O13 Eu1 O5 149.1(3) 7_566 . ?
O14 Eu1 O5 82.2(3) 3 . ?
O7 Eu1 O2 129.2(2) 4 . ?
O13 Eu1 O2 73.3(2) 7_566 . ?
O14 Eu1 O2 80.4(2) 3 . ?
O5 Eu1 O2 80.1(2) . . ?
O7 Eu1 O1 78.3(2) 4 . ?
O13 Eu1 O1 77.9(2) 7_566 . ?
O14 Eu1 O1 129.7(2) 3 . ?
O5 Eu1 O1 73.6(3) . . ?
O2 Eu1 O1 52.74(16) . . ?
O7 Eu1 O4B 69.4(5) 4 . ?
O13 Eu1 O4B 137.7(8) 7_566 . ?
O14 Eu1 O4B 83.9(5) 3 . ?
O5 Eu1 O4B 71.0(8) . . ?
O2 Eu1 O4B 148.7(8) . . ?
O1 Eu1 O4B 125.8(6) . . ?
O7 Eu1 O3 79.1(2) 4 . ?
O13 Eu1 O3 73.0(2) 7_566 . ?
O14 Eu1 O3 79.6(2) 3 . ?
O5 Eu1 O3 137.8(3) . . ?
O2 Eu1 O3 132.81(17) . . ?
O1 Eu1 O3 144.4(2) . . ?
O4B Eu1 O3 69.5(8) . . ?
O7 Eu1 O4 82.4(6) 4 . ?
O13 Eu1 O4 140.2(7) 7_566 . ?
O14 Eu1 O4 70.6(5) 3 . ?
O5 Eu1 O4 70.6(7) . . ?
O2 Eu1 O4 140.8(6) . . ?
O1 Eu1 O4 135.1(6) . . ?
O4B Eu1 O4 13.4(5) . . ?
O3 Eu1 O4 67.5(7) . . ?
O7 Eu1 C1 103.7(2) 4 . ?
O13 Eu1 C1 74.3(2) 7_566 . ?
O14 Eu1 C1 105.4(2) 3 . ?
O5 Eu1 C1 74.9(3) . . ?
O2 Eu1 C1 26.60(19) . . ?
O1 Eu1 C1 26.14(19) . . ?
O4B Eu1 C1 143.0(7) . . ?
O3 Eu1 C1 146.8(2) . . ?
O4 Eu1 C1 145.5(7) . . ?
O7 Eu1 C24 149.9(2) 4 3 ?
O13 Eu1 C24 89.7(2) 7_566 3 ?
O14 Eu1 C24 18.3(2) 3 3 ?
O5 Eu1 C24 99.1(3) . 3 ?
O2 Eu1 C24 76.68(18) . 3 ?
O1 Eu1 C24 129.40(18) . 3 ?
O4B Eu1 C24 96.0(4) . 3 ?
O3 Eu1 C24 71.12(19) . 3 ?
O4 Eu1 C24 82.9(5) . 3 ?
C1 Eu1 C24 103.3(2) . 3 ?
O10 Eu2 O8 76.2(2) 5_666 . ?
O10 Eu2 O9 78.0(2) 5_666 5_666 ?
O8 Eu2 O9 130.6(2) . 5_666 ?
O10 Eu2 O15 124.3(2) 5_666 . ?
O8 Eu2 O15 73.8(2) . . ?
O9 Eu2 O15 87.5(2) 5_666 . ?
O10 Eu2 O17 84.6(3) 5_666 . ?
O8 Eu2 O17 140.5(3) . . ?
O9 Eu2 O17 76.4(3) 5_666 . ?
O15 Eu2 O17 143.5(3) . . ?
O10 Eu2 O16 149.7(2) 5_666 . ?
O8 Eu2 O16 133.5(2) . . ?
O9 Eu2 O16 76.2(2) 5_666 . ?
O15 Eu2 O16 70.3(2) . . ?
O17 Eu2 O16 74.1(3) . . ?
O10 Eu2 O12 132.0(2) 5_666 6_565 ?
O8 Eu2 O12 74.3(2) . 6_565 ?
O9 Eu2 O12 148.5(2) 5_666 6_565 ?
O15 Eu2 O12 81.7(2) . 6_565 ?
O17 Eu2 O12 95.0(3) . 6_565 ?
O16 Eu2 O12 72.2(2) . 6_565 ?
O10 Eu2 O11 83.7(3) 5_666 6_565 ?
O8 Eu2 O11 72.2(3) . 6_565 ?
O9 Eu2 O11 144.4(3) 5_666 6_565 ?
O15 Eu2 O11 127.8(2) . 6_565 ?
O17 Eu2 O11 71.7(4) . 6_565 ?
O16 Eu2 O11 108.8(3) . 6_565 ?
O12 Eu2 O11 51.6(2) 6_565 6_565 ?
O10 Eu2 C32 108.6(3) 5_666 6_565 ?
O8 Eu2 C32 71.8(3) . 6_565 ?
O9 Eu2 C32 157.3(3) 5_666 6_565 ?
O15 Eu2 C32 104.9(2) . 6_565 ?
O17 Eu2 C32 82.5(3) . 6_565 ?
O16 Eu2 C32 90.0(3) . 6_565 ?
O12 Eu2 C32 25.4(3) 6_565 6_565 ?
O11 Eu2 C32 26.2(3) 6_565 6_565 ?
O10 Eu2 O10 77.1(2) 5_666 . ?
O8 Eu2 O10 66.7(2) . . ?
O9 Eu2 O10 66.8(2) 5_666 . ?
O15 Eu2 O10 48.10(17) . . ?
O17 Eu2 O10 141.5(3) . . ?
O16 Eu2 O10 106.6(2) . . ?
O12 Eu2 O10 122.4(2) 6_565 . ?
O11 Eu2 O10 137.6(3) 6_565 . ?
C32 Eu2 O10 135.4(2) 6_565 . ?
O10 Eu2 C20 101.4(2) 5_666 . ?
O8 Eu2 C20 68.8(2) . . ?
O9 Eu2 C20 76.0(2) 5_666 . ?
O15 Eu2 C20 23.5(2) . . ?
O17 Eu2 C20 149.9(3) . . ?
O16 Eu2 C20 87.7(2) . . ?
O12 Eu2 C20 102.1(2) 6_565 . ?
O11 Eu2 C20 138.0(3) 6_565 . ?
C32 Eu2 C20 122.0(2) 6_565 . ?
O10 Eu2 C20 24.62(19) . . ?
O10 Eu2 Eu2 43.41(15) 5_666 5_666 ?
O8 Eu2 Eu2 65.51(14) . 5_666 ?
O9 Eu2 Eu2 66.71(14) 5_666 5_666 ?
O15 Eu2 Eu2 81.36(13) . 5_666 ?
O17 Eu2 Eu2 119.9(3) . 5_666 ?
O16 Eu2 Eu2 133.90(15) . 5_666 ?
O12 Eu2 Eu2 139.35(18) 6_565 5_666 ?
O11 Eu2 Eu2 117.3(3) 6_565 5_666 ?
C32 Eu2 Eu2 133.1(2) 6_565 5_666 ?
O10 Eu2 Eu2 33.71(11) . 5_666 ?
C20 Eu2 Eu2 58.09(15) . 5_666 ?
C1 O1 Eu1 93.0(4) . . ?
C1 O2 Eu1 92.5(4) . . ?
C13 O7 Eu1 139.6(6) . 4_545 ?
C5 O8 Eu2 138.2(6) . . ?
C5 O9 Eu2 136.2(5) . 5_666 ?
C20 O10 Eu2 168.9(6) . 5_666 ?
C20 O10 Eu2 82.4(5) . . ?
Eu2 O10 Eu2 102.9(2) 5_666 . ?
C32 O11 Eu2 92.5(6) . 6_566 ?
C32 O12 Eu2 94.9(5) . 6_566 ?
C24 O13 Eu1 176.6(5) . 7_566 ?
C24 O14 Eu1 125.4(5) . 3_445 ?
C20 O15 Eu2 106.4(5) . . ?
H19G O19 H19H 115(2) . . ?
O1 C1 O2 121.7(7) . . ?
O1 C1 C2 119.1(7) . . ?
O2 C1 C2 119.2(7) . . ?
O1 C1 Eu1 60.8(4) . . ?
O2 C1 Eu1 60.9(4) . . ?
C2 C1 Eu1 177.6(6) . . ?
C3 C2 C8 120.1(7) . . ?
C3 C2 C1 120.5(7) . . ?
C8 C2 C1 119.4(7) . . ?
C4 C3 C2 120.0(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C6 119.7(7) . . ?
C3 C4 C5 120.8(7) . . ?
C6 C4 C5 119.4(7) . . ?
O9 C5 O8 127.8(8) . . ?
O9 C5 C4 116.4(7) . . ?
O8 C5 C4 115.8(7) . . ?
C4 C6 C7 121.2(8) . . ?
C4 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 117.8(7) . . ?
C8 C7 C9 121.8(7) . . ?
C6 C7 C9 120.5(8) . . ?
C2 C8 C7 121.2(7) . . ?
C2 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C15B C9 C10 106(2) . . ?
C15B C9 C10B 117(3) . . ?
C10 C9 C10B 38(2) . . ?
C15B C9 C15 30(2) . . ?
C10 C9 C15 117.1(10) . . ?
C10B C9 C15 107(2) . . ?
C15B C9 C7 123(2) . . ?
C10 C9 C7 120.7(9) . . ?
C10B C9 C7 119.5(17) . . ?
C15 C9 C7 122.1(9) . . ?
C11 C10 C9 121.5(12) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C12 C11 C10 121.1(12) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C15 C14 C12 120.7(13) . . ?
C15 C14 H14 119.7 . . ?
C12 C14 H14 119.7 . . ?
C14 C15 C9 121.2(13) . . ?
C14 C15 H15 119.4 . . ?
C9 C15 H15 119.4 . . ?
C11B C10B C9 119(3) . . ?
C11B C10B H10A 120.3 . . ?
C9 C10B H10A 120.3 . . ?
C10B C11B C12 122(3) . . ?
C10B C11B H11A 119.0 . . ?
C12 C11B H11A 119.0 . . ?
C12 C14B C15B 121(4) . . ?
C12 C14B H14A 119.5 . . ?
C15B C14B H14A 119.5 . . ?
C9 C15B C14B 123(4) . . ?
C9 C15B H15A 118.4 . . ?
C14B C15B H15A 118.4 . . ?
C14B C12 C11 109(2) . . ?
C14B C12 C14 29(2) . . ?
C11 C12 C14 118.4(10) . . ?
C14B C12 C11B 117(2) . . ?
C11 C12 C11B 37(2) . . ?
C14 C12 C11B 106.3(18) . . ?
C14B C12 C13 123(2) . . ?
C11 C12 C13 119.1(9) . . ?
C14 C12 C13 122.5(9) . . ?
C11B C12 C13 119.5(17) . . ?
O6 C13 O7 123.3(8) . . ?
O6 C13 C12 119.9(8) . . ?
O7 C13 C12 116.8(7) . . ?
O15 C20 O10 123.1(8) . . ?
O15 C20 C21 117.8(7) . . ?
O10 C20 C21 119.1(7) . . ?
O15 C20 Eu2 50.1(4) . . ?
O10 C20 Eu2 73.0(5) . . ?
C21 C20 Eu2 167.4(5) . . ?
C27 C21 C22 120.5(7) . . ?
C27 C21 C20 120.7(7) . . ?
C22 C21 C20 118.7(7) . . ?
C21 C22 C23 119.8(7) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C25 C23 C22 119.6(7) . . ?
C25 C23 C24 121.3(7) . . ?
C22 C23 C24 119.0(7) . . ?
O13 C24 O14 122.8(7) . . ?
O13 C24 C23 119.8(7) . . ?
O14 C24 C23 117.5(7) . . ?
O13 C24 Eu1 86.9(5) . 3_445 ?
O14 C24 Eu1 36.2(4) . 3_445 ?
C23 C24 Eu1 152.7(5) . 3_445 ?
C23 C25 C26 121.2(7) . . ?
C23 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C27 C26 C25 117.9(7) . . ?
C27 C26 C28 120.4(7) . . ?
C25 C26 C28 121.6(7) . . ?
C21 C27 C26 120.9(7) . . ?
C21 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C29 C28 C29B 10(3) . . ?
C29 C28 C34B 109.0(17) . . ?
C29B C28 C34B 99(3) . . ?
C29 C28 C34 119.0(12) . . ?
C29B C28 C34 112(3) . . ?
C34B C28 C34 43.5(16) . . ?
C29 C28 C26 119.7(9) . . ?
C29B C28 C26 128(3) . . ?
C34B C28 C26 122.4(14) . . ?
C34 C28 C26 119.6(7) . . ?
C33B C31 C30 108(2) . . ?
C33B C31 C30B 110(3) . . ?
C30 C31 C30B 11(3) . . ?
C33B C31 C33 46.5(17) . . ?
C30 C31 C33 115.1(11) . . ?
C30B C31 C33 125(2) . . ?
C33B C31 C32 117.5(15) . . ?
C30 C31 C32 123.8(10) . . ?
C30B C31 C32 115(2) . . ?
C33 C31 C32 120.0(9) . . ?
O12 C32 O11 121.0(8) . . ?
O12 C32 C31 119.9(8) . . ?
O11 C32 C31 119.0(9) . . ?
O12 C32 Eu2 59.7(4) . 6_566 ?
O11 C32 Eu2 61.3(5) . 6_566 ?
C31 C32 Eu2 179.4(8) . 6_566 ?
C28 C29 C30 116.5(16) . . ?
C28 C29 H29 121.7 . . ?
C30 C29 H29 121.7 . . ?
C31 C30 C29 125.7(17) . . ?
C31 C30 H30 117.2 . . ?
C29 C30 H30 117.2 . . ?
C34 C33 C31 119.6(10) . . ?
C34 C33 H33 120.2 . . ?
C31 C33 H33 120.2 . . ?
C33 C34 C28 120.7(10) . . ?
C33 C34 H34 119.6 . . ?
C28 C34 H34 119.6 . . ?
C28 C29B C30B 134(5) . . ?
C28 C29B H29A 113.1 . . ?
C30B C29B H29A 113.1 . . ?
C31 C30B C29B 109(5) . . ?
C31 C30B H30A 125.6 . . ?
C29B C30B H30A 125.6 . . ?
C31 C33B C34B 118(3) . . ?
C31 C33B H33A 121.2 . . ?
C34B C33B H33A 121.2 . . ?
C28 C34B C33B 124(3) . . ?
C28 C34B H34A 117.8 . . ?
C33B C34B H34A 117.8 . . ?
C35 O17 C35B 31(2) . . ?
C35 O17 Eu2 154.9(18) . . ?
C35B O17 Eu2 152(2) . . ?
C35 N2 C37 129(2) . . ?
C35 N2 C36 118(3) . . ?
C37 N2 C36 113.4(17) . . ?
O17 C35 N2 120(2) . . ?
O17 C35 C38 125(2) . . ?
N2 C35 C38 114(2) . . ?
C35B N2B C37B 125(3) . . ?
C35B N2B C36B 119.6(18) . . ?
C37B N2B C36B 111.1(16) . . ?
O17 C35B N2B 123(3) . . ?
O17 C35B C38B 115(4) . . ?
N2B C35B C38B 122(4) . . ?
N2B C36B H36D 109.5 . . ?
N2B C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
N2B C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
N2B C37B H37D 109.5 . . ?
N2B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
N2B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35B C38B H38D 109.5 . . ?
C35B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C16 O5 Eu1 174.2(14) . . ?
C16 N1 C17 129(2) . . ?
C16 N1 C18 115(2) . . ?
C17 N1 C18 116.3(17) . . ?
O5 C16 N1 135(2) . . ?
O5 C16 C19 114(2) . . ?
N1 C16 C19 111(2) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C17 H19D 76.1 . . ?
H17A C17 H19D 40.2 . . ?
H17B C17 H19D 101.2 . . ?
H17C C17 H19D 144.0 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C19 H19D 80.2 . . ?
H19A C19 H19D 158.6 . . ?
H19B C19 H19D 49.3 . . ?
H19C C19 H19D 83.8 . . ?
O5B C16B N1B 124(3) . . ?
O5B C16B C19B 116(2) . . ?
N1B C16B C19B 119(2) . . ?
C16B N1B C18B 128(3) . . ?
C16B N1B C17B 119(2) . . ?
C18B N1B C17B 112.5(16) . . ?
C16B N1B N1B 118(2) . 2_655 ?
C18B N1B N1B 72(3) . 2_655 ?
C17B N1B N1B 85(3) . 2_655 ?
C16B N1B C18B 134(3) . 2_655 ?
C18B N1B C18B 91(2) . 2_655 ?
C17B N1B C18B 38.7(19) . 2_655 ?
N1B N1B C18B 46.6(13) 2_655 2_655 ?
C18B C17B N1B 91(3) 2_655 . ?
C18B C17B H17D 121.2 2_655 . ?
N1B C17B H17D 110.6 . . ?
C18B C17B H17E 19.2 2_655 . ?
N1B C17B H17E 110.4 . . ?
H17D C17B H17E 109.6 . . ?
C18B C17B H17F 114.9 2_655 . ?
N1B C17B H17F 107.3 . . ?
H17D C17B H17F 109.3 . . ?
H17E C17B H17F 109.6 . . ?
C17B C18B N1B 111(4) 2_655 . ?
C17B C18B N1B 50(2) 2_655 2_655 ?
N1B C18B N1B 61(3) . 2_655 ?
C17B C18B H18D 88.6 2_655 . ?
N1B C18B H18D 105.7 . . ?
N1B C18B H18D 107.9 2_655 . ?
C17B C18B H18E 122.1 2_655 . ?
N1B C18B H18E 115.7 . . ?
N1B C18B H18E 141.4 2_655 . ?
H18D C18B H18E 109.5 . . ?
C17B C18B H18F 21.1 2_655 . ?
N1B C18B H18F 106.7 . . ?
N1B C18B H18F 47.6 2_655 . ?
H18D C18B H18F 109.4 . . ?
H18E C18B H18F 109.6 . . ?
C16B C19B H19D 107.7 . . ?
C16B C19B H19E 111.1 . . ?
H19D C19B H19E 109.4 . . ?
C16B C19B H19F 109.5 . . ?
H19D C19B H19F 109.6 . . ?
H19E C19B H19F 109.6 . . ?
O24 O23 O22 142(5) . . ?
C39 O20 C39B 40.0(14) . . ?
C39 N3 C41 124.3(17) . . ?
C39 N3 C42 121.0(17) . . ?
C41 N3 C42 114.3(17) . . ?
O20 C39 N3 114.8(14) . . ?
O20 C39 C40 127(2) . . ?
N3 C39 C40 118.7(18) . . ?
C39B N3B C41B 132(3) . . ?
C39B N3B C42B 113(3) . . ?
C41B N3B C42B 114(3) . . ?
O20 C39B N3B 121(2) . . ?
O20 C39B C40B 126(3) . . ?
N3B C39B C40B 111(3) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
N3B C41B H41D 109.5 . . ?
N3B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
N3B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
N3B C42B H42D 109.5 . . ?
N3B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
N3B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         9.836
_refine_diff_density_min         -8.182
_refine_diff_density_rms         0.237


# Start Validation Reply Form

_vrf_PLAT220_6                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        5.2 Ratio 
Large Non-Solvent    O     Ueq(max)/Ueq(min) ...        4.2 Ratio

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;
_database_code_depnum_ccdc_archive 'CCDC 981953'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H48.50 N2.50 O20 Tb2'
_chemical_formula_weight         1214.16

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'
Tb Tb -0.1723 4.1537 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   19.7427(3)
_cell_length_b                   18.4330(2)
_cell_length_c                   27.8981(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.3330(10)
_cell_angle_gamma                90.00
_cell_volume                     9691.6(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18376
_cell_measurement_theta_min      3.1790
_cell_measurement_theta_max      29.2340

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4816
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_T_max  0.7169
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46707
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.10
_reflns_number_total             10637
_reflns_number_gt                8802
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0779P)²+294.5078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10637
_refine_ls_number_parameters     850
_refine_ls_number_restraints     1008
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1681
_refine_ls_wR_factor_gt          0.1556
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.002
_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
Tb1 Tb 0.496630(19) 1.018390(18) 0.413300(12) 0.01675(11) Uani 1 1 d . . .
Tb2 Tb 0.453370(19) 0.428540(19) 0.441710(12) 0.01615(11) Uani 1 1 d . . .
O1 O 0.4118(3) 0.9280(3) 0.36643(19) 0.0220(12) Uani 1 1 d . A .
O2 O 0.4908(3) 0.8896(3) 0.43520(18) 0.0212(11) Uani 1 1 d . A .
O3 O 0.5096(3) 1.1306(3) 0.4642(2) 0.0266(13) Uani 1 1 d . A .
O4 O 0.5817(13) 1.1100(15) 0.3958(8) 0.047(6) Uani 0.50 1 d P A 1
O4B O 0.5566(10) 1.1096(13) 0.3787(6) 0.031(4) Uani 0.50 1 d P A 2
O6 O 0.0890(6) 0.6990(4) 0.1111(3) 0.081(4) Uani 1 1 d . . .
O7 O 0.0869(4) 0.5897(3) 0.1401(2) 0.044(2) Uani 1 1 d . . .
O8 O 0.4267(4) 0.5499(3) 0.4250(2) 0.0422(18) Uani 1 1 d . . .
O9 O 0.4945(4) 0.6272(3) 0.4807(2) 0.0332(15) Uani 1 1 d . . .
O10 O 0.4377(3) 0.5162(4) 0.5314(2) 0.0336(15) Uani 1 1 d . . .
O11 O 0.4672(4) 0.5487(7) 0.8577(3) 0.075(3) Uani 1 1 d U . .
O12 O 0.3601(4) 0.5683(4) 0.8609(2) 0.048(2) Uani 1 1 d . . .
O13 O 0.0826(3) 0.4886(3) 0.5409(2) 0.0276(13) Uani 1 1 d . . .
O14 O 0.1071(3) 0.5018(3) 0.4694(2) 0.0263(12) Uani 1 1 d . . .
O15 O 0.3571(3) 0.4527(3) 0.4739(2) 0.0256(12) Uani 1 1 d . . .
O16 O 0.3828(4) 0.3187(3) 0.4358(2) 0.0396(16) Uani 1 1 d . . .
O19 O 0.2229(7) 0.5574(11) 0.8679(6) 0.144(7) Uani 1 1 d D . .
H19G H 0.221(13) 0.599(6) 0.878(11) 0.216 Uiso 1 1 d D . .
H19H H 0.262(6) 0.538(13) 0.877(11) 0.216 Uiso 1 1 d D . .
C1 C 0.4388(4) 0.8776(4) 0.3967(3) 0.0220(16) Uani 1 1 d . A .
C2 C 0.4091(5) 0.8022(4) 0.3861(3) 0.0254(17) Uani 1 1 d . . .
C3 C 0.4385(5) 0.7450(4) 0.4187(3) 0.0271(19) Uani 1 1 d . A .
H3 H 0.4753 0.7547 0.4488 0.033 Uiso 1 1 calc R . .
C4 C 0.4149(5) 0.6747(4) 0.4075(3) 0.0294(19) Uani 1 1 d . . .
C5 C 0.4487(5) 0.6130(4) 0.4404(3) 0.0271(19) Uani 1 1 d . A .
C6 C 0.3584(5) 0.6614(5) 0.3628(3) 0.036(2) Uani 1 1 d . A .
H6 H 0.3421 0.6132 0.3545 0.044 Uiso 1 1 calc R . .
C7 C 0.3270(5) 0.7181(5) 0.3312(3) 0.036(2) Uani 1 1 d . . .
C8 C 0.3532(6) 0.7882(5) 0.3435(3) 0.036(2) Uani 1 1 d . A .
H8 H 0.3322 0.8274 0.3220 0.043 Uiso 1 1 calc R . .
C9 C 0.2691(6) 0.7038(5) 0.2835(4) 0.042(3) Uani 1 1 d . A .
C10 C 0.2578(11) 0.6346(10) 0.2645(7) 0.032(4) Uani 0.526(15) 1 d PU A 1
H10 H 0.2857 0.5960 0.2827 0.038 Uiso 0.526(15) 1 calc PR A 1
C11 C 0.2067(11) 0.6200(10) 0.2194(7) 0.031(3) Uani 0.526(15) 1 d PU A 1
H11 H 0.2014 0.5718 0.2068 0.037 Uiso 0.526(15) 1 calc PR A 1
C14 C 0.1679(13) 0.7425(10) 0.2112(7) 0.041(4) Uani 0.526(15) 1 d PU A 1
H14 H 0.1358 0.7788 0.1939 0.049 Uiso 0.526(15) 1 calc PR A 1
C15 C 0.2207(12) 0.7585(10) 0.2562(7) 0.037(4) Uani 0.526(15) 1 d PU A 1
H15 H 0.2246 0.8066 0.2690 0.044 Uiso 0.526(15) 1 calc PR A 1
C10B C 0.2302(15) 0.6404(13) 0.2797(9) 0.043(4) Uani 0.474(15) 1 d PU A 2
H10A H 0.2392 0.6072 0.3069 0.052 Uiso 0.474(15) 1 calc PR A 2
C11B C 0.1771(15) 0.6267(12) 0.2345(9) 0.044(4) Uani 0.474(15) 1 d PU A 2
H11A H 0.1488 0.5843 0.2321 0.053 Uiso 0.474(15) 1 calc PR A 2
C14B C 0.2050(12) 0.7353(11) 0.1997(8) 0.034(4) Uani 0.474(15) 1 d PU A 2
H14A H 0.1964 0.7691 0.1728 0.041 Uiso 0.474(15) 1 calc PR A 2
C15B C 0.2581(13) 0.7510(11) 0.2439(7) 0.033(4) Uani 0.474(15) 1 d PU A 2
H15A H 0.2863 0.7935 0.2465 0.040 Uiso 0.474(15) 1 calc PR A 2
C12 C 0.1638(6) 0.6730(5) 0.1927(3) 0.037(2) Uani 1 1 d . . .
C13 C 0.1079(6) 0.6542(5) 0.1450(3) 0.037(2) Uani 1 1 d . A .
C20 C 0.3765(4) 0.4903(5) 0.5139(3) 0.0232(17) Uani 1 1 d . . .
C21 C 0.3242(4) 0.5006(4) 0.5423(3) 0.0195(15) Uani 1 1 d . . .
C22 C 0.2521(4) 0.4931(4) 0.5172(3) 0.0188(15) Uani 1 1 d . . .
H22 H 0.2370 0.4830 0.4822 0.023 Uiso 1 1 calc R . .
C23 C 0.2025(4) 0.5003(4) 0.5431(3) 0.0182(15) Uani 1 1 d . . .
C24 C 0.1256(4) 0.4972(4) 0.5161(3) 0.0194(15) Uani 1 1 d . . .
C25 C 0.2264(4) 0.5117(4) 0.5957(3) 0.0211(16) Uani 1 1 d . . .
H25 H 0.1929 0.5151 0.6140 0.025 Uiso 1 1 calc R . .
C26 C 0.2985(4) 0.5180(5) 0.6209(3) 0.0236(17) Uani 1 1 d . B .
C27 C 0.3467(4) 0.5141(5) 0.5936(3) 0.0242(17) Uani 1 1 d . . .
H27 H 0.3958 0.5208 0.6102 0.029 Uiso 1 1 calc R . .
C28 C 0.3248(4) 0.5285(5) 0.6765(3) 0.0291(19) Uani 1 1 d D . .
C31 C 0.3740(5) 0.5442(6) 0.7807(3) 0.037(2) Uani 1 1 d D . .
C32 C 0.4012(6) 0.5549(5) 0.8367(3) 0.036(2) Uani 1 1 d . . .
C29 C 0.2741(11) 0.5339(12) 0.7034(7) 0.034(4) Uani 0.520(15) 1 d PDU B 1
H29 H 0.2247 0.5336 0.6862 0.040 Uiso 0.520(15) 1 calc PR B 1
C30 C 0.2992(7) 0.5399(15) 0.7567(7) 0.033(4) Uani 0.520(15) 1 d PDU B 1
H30 H 0.2668 0.5411 0.7760 0.040 Uiso 0.520(15) 1 calc PR B 1
C33 C 0.4166(8) 0.5049(11) 0.7559(4) 0.033(3) Uani 0.520(15) 1 d PDU B 1
H33 H 0.4601 0.4832 0.7747 0.039 Uiso 0.520(15) 1 calc PR B 1
C34 C 0.3927(7) 0.4988(12) 0.7024(4) 0.034(3) Uani 0.520(15) 1 d PDU B 1
H34 H 0.4210 0.4758 0.6847 0.041 Uiso 0.520(15) 1 calc PR B 1
C29B C 0.2839(11) 0.5563(14) 0.7063(8) 0.032(4) Uani 0.480(15) 1 d PDU B 2
H29A H 0.2363 0.5707 0.6902 0.038 Uiso 0.480(15) 1 calc PR B 2
C30B C 0.3085(14) 0.5630(14) 0.7541(9) 0.031(4) Uani 0.480(15) 1 d PU B 2
H30A H 0.2780 0.5824 0.7716 0.038 Uiso 0.480(15) 1 calc PR B 2
C33B C 0.4141(11) 0.5649(13) 0.7528(7) 0.038(4) Uani 0.480(15) 1 d PU B 2
H33A H 0.4593 0.5854 0.7687 0.045 Uiso 0.480(15) 1 calc PR B 2
C34B C 0.3922(10) 0.5575(12) 0.7008(6) 0.034(3) Uani 0.480(15) 1 d PU B 2
H34A H 0.4225 0.5720 0.6818 0.040 Uiso 0.480(15) 1 calc PR B 2
O17 O 0.5210(5) 0.3296(5) 0.4230(4) 0.071(3) Uani 1 1 d D . .
N2 N 0.6241(11) 0.2924(16) 0.4111(10) 0.061(6) Uani 0.351(16) 1 d PDU C 1
C35 C 0.5548(12) 0.309(2) 0.3948(9) 0.060(6) Uani 0.351(16) 1 d PDU C 1
C36 C 0.662(2) 0.303(3) 0.4661(11) 0.058(7) Uani 0.351(16) 1 d PDU C 1
H36A H 0.6789 0.2559 0.4815 0.088 Uiso 0.351(16) 1 calc PR C 1
H36B H 0.6291 0.3241 0.4826 0.088 Uiso 0.351(16) 1 calc PR C 1
H36C H 0.7024 0.3356 0.4700 0.088 Uiso 0.351(16) 1 calc PR C 1
C37 C 0.6650(18) 0.2668(18) 0.3769(13) 0.057(7) Uani 0.351(16) 1 d PDU C 1
H37A H 0.7036 0.3009 0.3782 0.086 Uiso 0.351(16) 1 calc PR C 1
H37B H 0.6333 0.2640 0.3424 0.086 Uiso 0.351(16) 1 calc PR C 1
H37C H 0.6849 0.2186 0.3876 0.086 Uiso 0.351(16) 1 calc PR C 1
C38 C 0.519(2) 0.284(2) 0.3368(11) 0.069(8) Uani 0.351(16) 1 d PDU C 1
H38A H 0.4681 0.2775 0.3301 0.103 Uiso 0.351(16) 1 calc PR C 1
H38B H 0.5404 0.2373 0.3313 0.103 Uiso 0.351(16) 1 calc PR C 1
H38C H 0.5285 0.3203 0.3140 0.103 Uiso 0.351(16) 1 calc PR C 1
N2B N 0.577(3) 0.289(4) 0.369(2) 0.066(7) Uani 0.149(16) 1 d PDU C 2
C35B C 0.5768(17) 0.317(5) 0.413(2) 0.064(7) Uani 0.149(16) 1 d PDU C 2
C36B C 0.516(4) 0.253(5) 0.330(3) 0.068(10) Uani 0.149(16) 1 d PDU C 2
H36D H 0.4710 0.2688 0.3339 0.103 Uiso 0.149(16) 1 calc PR C 2
H36E H 0.5206 0.2001 0.3339 0.103 Uiso 0.149(16) 1 calc PR C 2
H36F H 0.5181 0.2661 0.2961 0.103 Uiso 0.149(16) 1 calc PR C 2
C37B C 0.650(3) 0.281(6) 0.363(3) 0.061(9) Uani 0.149(16) 1 d PDU C 2
H37D H 0.6821 0.3151 0.3853 0.092 Uiso 0.149(16) 1 calc PR C 2
H37E H 0.6476 0.2915 0.3280 0.092 Uiso 0.149(16) 1 calc PR C 2
H37F H 0.6664 0.2313 0.3713 0.092 Uiso 0.149(16) 1 calc PR C 2
C38B C 0.646(5) 0.316(6) 0.463(3) 0.064(9) Uani 0.149(16) 1 d PDU C 2
H38D H 0.6320 0.3336 0.4922 0.096 Uiso 0.149(16) 1 calc PR C 2
H38E H 0.6831 0.3469 0.4580 0.096 Uiso 0.149(16) 1 calc PR C 2
H38F H 0.6634 0.2660 0.4698 0.096 Uiso 0.149(16) 1 calc PR C 2
O5 O 0.5499(4) 0.9642(4) 0.3567(2) 0.0451(18) Uani 1 1 d D A .
N1 N 0.5735(12) 0.9629(13) 0.2825(7) 0.19(3) Uani 0.50 1 d PD A 1
C16 C 0.5613(13) 0.9318(14) 0.3220(8) 0.13(2) Uani 0.50 1 d PD A 1
C17 C 0.5989(12) 0.9215(13) 0.2455(7) 0.049(6) Uani 0.50 1 d PD A 1
H17A H 0.6010 0.8697 0.2539 0.073 Uiso 0.50 1 calc PR A 1
H17B H 0.6464 0.9385 0.2465 0.073 Uiso 0.50 1 calc PR A 1
H17C H 0.5662 0.9288 0.2118 0.073 Uiso 0.50 1 calc PR A 1
C18 C 0.5503(19) 1.0404(14) 0.2756(11) 0.084(11) Uani 0.50 1 d PD A 1
H18A H 0.5317 1.0549 0.3030 0.126 Uiso 0.50 1 calc PR A 1
H18B H 0.5132 1.0459 0.2435 0.126 Uiso 0.50 1 calc PR A 1
H18C H 0.5909 1.0711 0.2758 0.126 Uiso 0.50 1 calc PR A 1
C19 C 0.5841(19) 0.8471(15) 0.3214(14) 0.096(13) Uani 0.50 1 d PD A 1
H19A H 0.5732 0.8213 0.3489 0.144 Uiso 0.50 1 calc PR A 1
H19B H 0.6351 0.8439 0.3257 0.144 Uiso 0.50 1 calc PR A 1
H19C H 0.5577 0.8251 0.2893 0.144 Uiso 0.50 1 calc PR A 1
O5B O 0.5455(11) 0.8239(12) 0.3326(7) 0.071(6) Uani 0.50 1 d PD D 2
C16B C 0.5617(15) 0.7921(10) 0.2991(8) 0.059(7) Uani 0.50 1 d PD D 2
N1B N 0.5393(12) 0.7280(10) 0.2776(8) 0.069(6) Uani 0.50 1 d PD . 2
C17B C 0.481(2) 0.6893(18) 0.2906(16) 0.100(13) Uani 0.50 1 d PD . 2
H17D H 0.4698 0.7169 0.3164 0.149 Uiso 0.50 1 d PR . 2
H17E H 0.4381 0.6795 0.2643 0.149 Uiso 0.50 1 d PR . 2
H17F H 0.5022 0.6450 0.3045 0.149 Uiso 0.50 1 d PR . 2
C18B C 0.567(2) 0.699(3) 0.2372(15) 0.16(3) Uani 0.50 1 d PD . 2
H18D H 0.5987 0.7288 0.2261 0.241 Uiso 0.50 1 d PR . 2
H18E H 0.5902 0.6545 0.2498 0.241 Uiso 0.50 1 d PR . 2
H18F H 0.5260 0.6890 0.2095 0.241 Uiso 0.50 1 d PR . 2
C19B C 0.6186(14) 0.8353(14) 0.2778(10) 0.071(8) Uani 0.50 1 d PD D 2
H19D H 0.6302 0.8794 0.2961 0.106 Uiso 0.50 1 d PR D 2
H19E H 0.6606 0.8078 0.2818 0.106 Uiso 0.50 1 d PR D 2
H19F H 0.5973 0.8456 0.2428 0.106 Uiso 0.50 1 d PR D 2
O20 O 0.7414(7) 0.8180(6) 0.4246(7) 0.128(6) Uani 1 1 d D . .
N3 N 0.6639(18) 0.7546(16) 0.4414(14) 0.057(5) Uani 0.321(18) 1 d PDU E 1
C39 C 0.714(2) 0.7574(12) 0.4182(17) 0.067(6) Uani 0.321(18) 1 d PDU E 1
C40 C 0.716(5) 0.679(2) 0.391(3) 0.065(8) Uani 0.321(18) 1 d PDU E 1
H40A H 0.6770 0.6766 0.3600 0.098 Uiso 0.321(18) 1 calc PR E 1
H40B H 0.7108 0.6402 0.4139 0.098 Uiso 0.321(18) 1 calc PR E 1
H40C H 0.7614 0.6737 0.3841 0.098 Uiso 0.321(18) 1 calc PR E 1
C41 C 0.639(3) 0.6783(18) 0.443(2) 0.065(8) Uani 0.321(18) 1 d PDU E 1
H41A H 0.6190 0.6599 0.4090 0.098 Uiso 0.321(18) 1 calc PR E 1
H41B H 0.6027 0.6771 0.4607 0.098 Uiso 0.321(18) 1 calc PR E 1
H41C H 0.6792 0.6478 0.4613 0.098 Uiso 0.321(18) 1 calc PR E 1
C42 C 0.655(4) 0.817(2) 0.460(2) 0.068(8) Uani 0.321(18) 1 d PDU E 1
H42A H 0.7007 0.8418 0.4718 0.102 Uiso 0.321(18) 1 calc PR E 1
H42B H 0.6352 0.8097 0.4877 0.102 Uiso 0.321(18) 1 calc PR E 1
H42C H 0.6221 0.8460 0.4336 0.102 Uiso 0.321(18) 1 calc PR E 1
N3B N 0.6736(8) 0.7206(7) 0.4180(6) 0.054(4) Uani 0.679(18) 1 d PDU E 2
C39B C 0.6933(9) 0.7871(8) 0.4360(8) 0.060(4) Uani 0.679(18) 1 d PDU E 2
C40B C 0.6555(16) 0.8161(11) 0.4769(9) 0.063(6) Uani 0.679(18) 1 d PDU E 2
H40D H 0.6132 0.7869 0.4746 0.094 Uiso 0.679(18) 1 calc PR E 2
H40E H 0.6418 0.8670 0.4699 0.094 Uiso 0.679(18) 1 calc PR E 2
H40F H 0.6888 0.8119 0.5107 0.094 Uiso 0.679(18) 1 calc PR E 2
C41B C 0.6121(13) 0.6838(11) 0.4269(10) 0.066(5) Uani 0.679(18) 1 d PDU E 2
H41D H 0.6057 0.6362 0.4105 0.099 Uiso 0.679(18) 1 calc PR E 2
H41E H 0.5694 0.7132 0.4129 0.099 Uiso 0.679(18) 1 calc PR E 2
H41F H 0.6204 0.6776 0.4631 0.099 Uiso 0.679(18) 1 calc PR E 2
C42B C 0.713(2) 0.6922(14) 0.3852(14) 0.071(6) Uani 0.679(18) 1 d PDU E 2
H42D H 0.6953 0.6437 0.3735 0.107 Uiso 0.679(18) 1 calc PR E 2
H42E H 0.7635 0.6893 0.4038 0.107 Uiso 0.679(18) 1 calc PR E 2
H42F H 0.7064 0.7245 0.3563 0.107 Uiso 0.679(18) 1 calc PR E 2
O21 O 0.6787(4) 0.1457(4) 0.4198(3) 0.0500(19) Uani 1 1 d . . .
O22 O 0.7123(4) 0.0672(4) 0.3894(3) 0.0500(19) Uiso 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
Tb1 O7 2.282(6) 4 ?
Tb1 O14 2.295(5) 3 ?
Tb1 O13 2.300(6) 7_566 ?
Tb1 O5 2.364(7) . ?
Tb1 O4B 2.42(2) . ?
Tb1 O1 2.447(5) . ?
Tb1 O2 2.462(5) . ?
Tb1 O3 2.478(5) . ?
Tb1 O4 2.53(3) . ?
Tb1 C1 2.819(8) . ?
Tb2 O10 2.294(6) 5_666 ?
Tb2 O8 2.313(6) . ?
Tb2 O9 2.339(5) 5_666 ?
Tb2 O15 2.374(6) . ?
Tb2 O17 2.407(7) . ?
Tb2 O16 2.434(6) . ?
Tb2 O12 2.450(6) 6_565 ?
Tb2 O11 2.476(7) 6_565 ?
Tb2 C32 2.818(8) 6_565 ?
O1 C1 1.263(9) . ?
O2 C1 1.266(9) . ?
O6 C13 1.229(11) . ?
O7 C13 1.253(11) . ?
O7 Tb1 2.282(6) 4_545 ?
O8 C5 1.271(10) . ?
O9 C5 1.243(9) . ?
O9 Tb2 2.339(5) 5_666 ?
O10 C20 1.256(10) . ?
O10 Tb2 2.294(6) 5_666 ?
O11 C32 1.264(13) . ?
O11 Tb2 2.476(7) 6_566 ?
O12 C32 1.227(12) . ?
O12 Tb2 2.450(6) 6_566 ?
O13 C24 1.253(10) . ?
O13 Tb1 2.300(6) 7_566 ?
O14 C24 1.248(9) . ?
O14 Tb1 2.295(5) 3_445 ?
O15 C20 1.272(9) . ?
O19 H19G 0.823(10) . ?
O19 H19H 0.821(10) . ?
C1 C2 1.502(11) . ?
C2 C8 1.384(11) . ?
C2 C3 1.401(11) . ?
C3 C4 1.382(11) . ?
C3 H3 0.9500 . ?
C4 C6 1.425(11) . ?
C4 C5 1.489(11) . ?
C6 C7 1.390(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(13) . ?
C7 C9 1.495(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.37(2) . ?
C9 C15B 1.37(2) . ?
C9 C10B 1.39(3) . ?
C9 C15 1.44(2) . ?
C10 C11 1.38(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.36(2) . ?
C11 H11 0.9500 . ?
C14 C12 1.37(2) . ?
C14 C15 1.40(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C10B C11B 1.40(3) . ?
C10B H10A 0.9500 . ?
C11B C12 1.41(3) . ?
C11B H11A 0.9500 . ?
C14B C12 1.39(2) . ?
C14B C15B 1.39(3) . ?
C14B H14A 0.9500 . ?
C15B H15A 0.9500 . ?
C12 C13 1.494(11) . ?
C20 C21 1.489(11) . ?
C21 C27 1.389(10) . ?
C21 C22 1.392(11) . ?
C22 C23 1.389(11) . ?
C22 H22 0.9500 . ?
C23 C25 1.417(10) . ?
C23 C24 1.481(11) . ?
C25 C26 1.393(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(11) . ?
C26 C28 1.494(10) . ?
C27 H27 0.9500 . ?
C28 C34B 1.41(2) . ?
C28 C29B 1.416(9) . ?
C28 C29 1.421(9) . ?
C28 C34 1.429(9) . ?
C31 C33B 1.32(2) . ?
C31 C30B 1.33(3) . ?
C31 C30 1.430(9) . ?
C31 C33 1.436(9) . ?
C31 C32 1.505(11) . ?
C32 Tb2 2.818(8) 6_566 ?
C29 C30 1.427(10) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C33 C34 1.428(9) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C29B C30B 1.28(3) . ?
C29B H29A 0.9500 . ?
C30B H30A 0.9500 . ?
C33B C34B 1.39(2) . ?
C33B H33A 0.9500 . ?
C34B H34A 0.9500 . ?
O17 C35 1.230(15) . ?
O17 C35B 1.232(15) . ?
N2 C35 1.345(16) . ?
N2 C37 1.499(14) . ?
N2 C36 1.505(14) . ?
C35 C38 1.63(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N2B C35B 1.348(17) . ?
N2B C37B 1.505(14) . ?
N2B C36B 1.509(14) . ?
C35B C38B 1.63(2) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
O5 C16 1.216(15) . ?
N1 C16 1.326(16) . ?
N1 C17 1.485(13) . ?
N1 C18 1.494(14) . ?
C16 C19 1.62(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 H19D 1.5660 . ?
C17 H19F 1.4003 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 H19D 1.4377 . ?
O5B C16B 1.226(15) . ?
C16B N1B 1.337(16) . ?
C16B C19B 1.63(2) . ?
N1B C17B 1.495(14) . ?
N1B C18B 1.496(14) . ?
N1B N1B 1.83(5) 2_655 ?
N1B C17B 1.96(5) 2_655 ?
C17B C18B 1.04(5) 2_655 ?
C17B N1B 1.96(5) 2_655 ?
C17B H17D 0.9556 . ?
C17B H17E 0.9544 . ?
C17B H17F 0.9492 . ?
C18B C17B 1.04(5) 2_655 ?
C18B H18D 0.9517 . ?
C18B H18E 0.9490 . ?
C18B H18F 0.9546 . ?
C19B H19D 0.9503 . ?
C19B H19E 0.9506 . ?
C19B H19F 0.9582 . ?
O20 C39B 1.229(14) . ?
O20 C39 1.229(15) . ?
N3 C42 1.29(4) . ?
N3 C39 1.338(16) . ?
N3 C41 1.496(14) . ?
C39 C40 1.63(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N3B C39B 1.338(15) . ?
N3B C42B 1.46(3) . ?
N3B C41B 1.47(2) . ?
C39B C40B 1.63(2) . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

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
O7 Tb1 O14 151.3(2) 4 3 ?
O7 Tb1 O13 85.2(3) 4 7_566 ?
O14 Tb1 O13 106.2(2) 3 7_566 ?
O7 Tb1 O5 100.7(3) 4 . ?
O14 Tb1 O5 83.0(2) 3 . ?
O13 Tb1 O5 149.3(2) 7_566 . ?
O7 Tb1 O4B 71.5(5) 4 . ?
O14 Tb1 O4B 83.4(5) 3 . ?
O13 Tb1 O4B 139.1(6) 7_566 . ?
O5 Tb1 O4B 70.0(6) . . ?
O7 Tb1 O1 78.3(2) 4 . ?
O14 Tb1 O1 129.37(19) 3 . ?
O13 Tb1 O1 77.78(19) 7_566 . ?
O5 Tb1 O1 74.1(2) . . ?
O4B Tb1 O1 126.8(4) . . ?
O7 Tb1 O2 129.8(2) 4 . ?
O14 Tb1 O2 78.91(19) 3 . ?
O13 Tb1 O2 73.7(2) 7_566 . ?
O5 Tb1 O2 79.7(2) . . ?
O4B Tb1 O2 146.5(6) . . ?
O1 Tb1 O2 53.21(16) . . ?
O7 Tb1 O3 79.9(2) 4 . ?
O14 Tb1 O3 78.8(2) 3 . ?
O13 Tb1 O3 72.5(2) 7_566 . ?
O5 Tb1 O3 138.1(2) . . ?
O4B Tb1 O3 70.7(5) . . ?
O1 Tb1 O3 144.3(2) . . ?
O2 Tb1 O3 131.81(17) . . ?
O7 Tb1 O4 83.2(6) 4 . ?
O14 Tb1 O4 70.7(5) 3 . ?
O13 Tb1 O4 138.2(7) 7_566 . ?
O5 Tb1 O4 72.5(7) . . ?
O4B Tb1 O4 13.2(5) . . ?
O1 Tb1 O4 137.7(5) . . ?
O2 Tb1 O4 140.7(7) . . ?
O3 Tb1 O4 65.9(7) . . ?
O7 Tb1 C1 104.2(2) 4 . ?
O14 Tb1 C1 104.2(2) 3 . ?
O13 Tb1 C1 74.4(2) 7_566 . ?
O5 Tb1 C1 75.0(2) . . ?
O4B Tb1 C1 142.9(5) . . ?
O1 Tb1 C1 26.56(19) . . ?
O2 Tb1 C1 26.65(19) . . ?
O3 Tb1 C1 146.1(2) . . ?
O4 Tb1 C1 147.5(7) . . ?
O10 Tb2 O8 76.8(3) 5_666 . ?
O10 Tb2 O9 77.4(2) 5_666 5_666 ?
O8 Tb2 O9 128.5(2) . 5_666 ?
O10 Tb2 O15 124.8(2) 5_666 . ?
O8 Tb2 O15 74.7(3) . . ?
O9 Tb2 O15 85.0(2) 5_666 . ?
O10 Tb2 O17 83.2(3) 5_666 . ?
O8 Tb2 O17 142.8(3) . . ?
O9 Tb2 O17 75.4(3) 5_666 . ?
O15 Tb2 O17 141.5(3) . . ?
O10 Tb2 O16 148.5(2) 5_666 . ?
O8 Tb2 O16 134.4(3) . . ?
O9 Tb2 O16 77.4(2) 5_666 . ?
O15 Tb2 O16 71.1(2) . . ?
O17 Tb2 O16 72.4(3) . . ?
O10 Tb2 O12 131.7(2) 5_666 6_565 ?
O8 Tb2 O12 74.3(2) . 6_565 ?
O9 Tb2 O12 149.8(2) 5_666 6_565 ?
O15 Tb2 O12 82.9(2) . 6_565 ?
O17 Tb2 O12 97.6(3) . 6_565 ?
O16 Tb2 O12 72.5(2) . 6_565 ?
O10 Tb2 O11 83.0(3) 5_666 6_565 ?
O8 Tb2 O11 74.2(3) . 6_565 ?
O9 Tb2 O11 144.0(3) 5_666 6_565 ?
O15 Tb2 O11 130.8(2) . 6_565 ?
O17 Tb2 O11 72.4(4) . 6_565 ?
O16 Tb2 O11 107.4(3) . 6_565 ?
O12 Tb2 O11 52.4(3) 6_565 6_565 ?
O10 Tb2 C32 108.0(3) 5_666 6_565 ?
O8 Tb2 C32 72.2(2) . 6_565 ?
O9 Tb2 C32 159.0(2) 5_666 6_565 ?
O15 Tb2 C32 106.7(3) . 6_565 ?
O17 Tb2 C32 84.9(3) . 6_565 ?
O16 Tb2 C32 89.7(3) . 6_565 ?
O12 Tb2 C32 25.7(3) 6_565 6_565 ?
O11 Tb2 C32 26.6(3) 6_565 6_565 ?
C1 O1 Tb1 93.4(4) . . ?
C1 O2 Tb1 92.6(4) . . ?
C13 O7 Tb1 140.3(6) . 4_545 ?
C5 O8 Tb2 141.5(6) . . ?
C5 O9 Tb2 138.1(5) . 5_666 ?
C20 O10 Tb2 175.0(6) . 5_666 ?
C32 O11 Tb2 92.0(6) . 6_566 ?
C32 O12 Tb2 94.1(6) . 6_566 ?
C24 O13 Tb1 175.9(6) . 7_566 ?
C24 O14 Tb1 130.1(5) . 3_445 ?
C20 O15 Tb2 111.7(5) . . ?
H19G O19 H19H 115(2) . . ?
O1 C1 O2 120.8(7) . . ?
O1 C1 C2 119.1(7) . . ?
O2 C1 C2 120.0(7) . . ?
O1 C1 Tb1 60.1(4) . . ?
O2 C1 Tb1 60.8(4) . . ?
C2 C1 Tb1 177.7(6) . . ?
C8 C2 C3 119.2(7) . . ?
C8 C2 C1 120.4(7) . . ?
C3 C2 C1 120.4(7) . . ?
C4 C3 C2 120.9(7) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C6 118.8(7) . . ?
C3 C4 C5 121.2(7) . . ?
C6 C4 C5 119.9(7) . . ?
O9 C5 O8 125.6(7) . . ?
O9 C5 C4 117.9(7) . . ?
O8 C5 C4 116.4(7) . . ?
C7 C6 C4 120.8(8) . . ?
C7 C6 H6 119.6 . . ?
C4 C6 H6 119.6 . . ?
C6 C7 C8 118.5(8) . . ?
C6 C7 C9 120.6(8) . . ?
C8 C7 C9 120.7(7) . . ?
C2 C8 C7 121.7(8) . . ?
C2 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C15B 108.0(13) . . ?
C10 C9 C10B 33.3(12) . . ?
C15B C9 C10B 121.4(14) . . ?
C10 C9 C15 116.1(11) . . ?
C15B C9 C15 37.8(11) . . ?
C10B C9 C15 106.5(14) . . ?
C10 C9 C7 120.0(10) . . ?
C15B C9 C7 120.0(12) . . ?
C10B C9 C7 118.5(12) . . ?
C15 C9 C7 123.8(10) . . ?
C9 C10 C11 121.5(15) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C12 C11 C10 121.6(16) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C12 C14 C15 118.5(17) . . ?
C12 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C9 121.6(16) . . ?
C14 C15 H15 119.2 . . ?
C9 C15 H15 119.2 . . ?
C9 C10B C11B 118.1(19) . . ?
C9 C10B H10A 120.9 . . ?
C11B C10B H10A 120.9 . . ?
C10B C11B C12 123(2) . . ?
C10B C11B H11A 118.6 . . ?
C12 C11B H11A 118.6 . . ?
C12 C14B C15B 123.5(17) . . ?
C12 C14B H14A 118.3 . . ?
C15B C14B H14A 118.3 . . ?
C9 C15B C14B 118.7(18) . . ?
C9 C15B H15A 120.7 . . ?
C14B C15B H15A 120.7 . . ?
C11 C12 C14 120.4(12) . . ?
C11 C12 C14B 106.0(13) . . ?
C14 C12 C14B 37.7(12) . . ?
C11 C12 C11B 34.7(12) . . ?
C14 C12 C11B 106.2(14) . . ?
C14B C12 C11B 115.5(14) . . ?
C11 C12 C13 119.7(10) . . ?
C14 C12 C13 119.7(11) . . ?
C14B C12 C13 124.3(11) . . ?
C11B C12 C13 120.2(12) . . ?
O6 C13 O7 122.6(8) . . ?
O6 C13 C12 120.3(8) . . ?
O7 C13 C12 116.7(8) . . ?
O10 C20 O15 123.5(7) . . ?
O10 C20 C21 119.0(7) . . ?
O15 C20 C21 117.5(7) . . ?
C27 C21 C22 120.1(7) . . ?
C27 C21 C20 120.7(7) . . ?
C22 C21 C20 119.0(6) . . ?
C23 C22 C21 120.1(6) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C25 119.0(7) . . ?
C22 C23 C24 120.4(6) . . ?
C25 C23 C24 120.5(7) . . ?
O14 C24 O13 123.3(8) . . ?
O14 C24 C23 117.7(7) . . ?
O13 C24 C23 119.0(6) . . ?
C26 C25 C23 120.7(7) . . ?
C26 C25 H25 119.6 . . ?
C23 C25 H25 119.6 . . ?
C27 C26 C25 118.9(7) . . ?
C27 C26 C28 119.7(7) . . ?
C25 C26 C28 121.4(7) . . ?
C26 C27 C21 121.0(7) . . ?
C26 C27 H27 119.5 . . ?
C21 C27 H27 119.5 . . ?
C34B C28 C29B 101.7(14) . . ?
C34B C28 C29 115.7(13) . . ?
C29B C28 C29 18.4(13) . . ?
C34B C28 C34 44.9(12) . . ?
C29B C28 C34 117.1(12) . . ?
C29 C28 C34 117.6(13) . . ?
C34B C28 C26 122.3(10) . . ?
C29B C28 C26 125.0(12) . . ?
C29 C28 C26 118.4(11) . . ?
C34 C28 C26 117.3(8) . . ?
C33B C31 C30B 104.5(16) . . ?
C33B C31 C30 117.2(13) . . ?
C30B C31 C30 19.5(15) . . ?
C33B C31 C33 47.2(12) . . ?
C30B C31 C33 118.3(14) . . ?
C30 C31 C33 114.8(13) . . ?
C33B C31 C32 118.8(11) . . ?
C30B C31 C32 122.2(15) . . ?
C30 C31 C32 119.5(11) . . ?
C33 C31 C32 119.1(9) . . ?
O12 C32 O11 121.5(8) . . ?
O12 C32 C31 120.5(9) . . ?
O11 C32 C31 118.0(9) . . ?
O12 C32 Tb2 60.1(4) . 6_566 ?
O11 C32 Tb2 61.4(5) . 6_566 ?
C31 C32 Tb2 178.7(8) . 6_566 ?
C28 C29 C30 118.4(18) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C29 C30 C31 118.7(18) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C34 C33 C31 119.0(11) . . ?
C34 C33 H33 120.5 . . ?
C31 C33 H33 120.5 . . ?
C33 C34 C28 117.8(10) . . ?
C33 C34 H34 121.1 . . ?
C28 C34 H34 121.1 . . ?
C30B C29B C28 123(2) . . ?
C30B C29B H29A 118.7 . . ?
C28 C29B H29A 118.7 . . ?
C29B C30B C31 124(2) . . ?
C29B C30B H30A 118.0 . . ?
C31 C30B H30A 118.0 . . ?
C31 C33B C34B 122.1(17) . . ?
C31 C33B H33A 118.9 . . ?
C34B C33B H33A 118.9 . . ?
C33B C34B C28 119.7(17) . . ?
C33B C34B H34A 120.2 . . ?
C28 C34B H34A 120.2 . . ?
C35 O17 C35B 28(3) . . ?
C35 O17 Tb2 144.0(19) . . ?
C35B O17 Tb2 141(4) . . ?
C35 N2 C37 123(2) . . ?
C35 N2 C36 117(2) . . ?
C37 N2 C36 119.5(17) . . ?
O17 C35 N2 123(2) . . ?
O17 C35 C38 125(3) . . ?
N2 C35 C38 111(2) . . ?
C35B N2B C37B 114(4) . . ?
C35B N2B C36B 128(2) . . ?
C37B N2B C36B 116.9(18) . . ?
O17 C35B N2B 121(4) . . ?
O17 C35B C38B 113(6) . . ?
N2B C35B C38B 124(5) . . ?
N2B C36B H36D 109.5 . . ?
N2B C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
N2B C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
N2B C37B H37D 109.5 . . ?
N2B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
N2B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35B C38B H38D 109.5 . . ?
C35B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C16 O5 Tb1 164.9(12) . . ?
C16 N1 C17 122.4(17) . . ?
C16 N1 C18 113.3(19) . . ?
C17 N1 C18 123.8(17) . . ?
O5 C16 N1 125(2) . . ?
O5 C16 C19 127(3) . . ?
N1 C16 C19 106.8(19) . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C17 H19D 75.8 . . ?
H17A C17 H19D 47.6 . . ?
H17B C17 H19D 90.9 . . ?
H17C C17 H19D 154.7 . . ?
N1 C17 H19F 122.9 . . ?
H17A C17 H19F 16.2 . . ?
H17B C17 H19F 109.2 . . ?
H17C C17 H19F 95.0 . . ?
H19D C17 H19F 63.3 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C19 H19D 79.9 . . ?
H19A C19 H19D 154.9 . . ?
H19B C19 H19D 46.0 . . ?
H19C C19 H19D 87.9 . . ?
O5B C16B N1B 130(2) . . ?
O5B C16B C19B 114.3(19) . . ?
N1B C16B C19B 116.2(18) . . ?
C16B N1B C17B 119(2) . . ?
C16B N1B C18B 121(2) . . ?
C17B N1B C18B 119.7(17) . . ?
C16B N1B N1B 117.4(16) . 2_655 ?
C17B N1B N1B 71(2) . 2_655 ?
C18B N1B N1B 77(2) . 2_655 ?
C16B N1B C17B 134.4(19) . 2_655 ?
C17B N1B C17B 96.7(19) . 2_655 ?
C18B N1B C17B 32(2) . 2_655 ?
N1B N1B C17B 46.2(10) 2_655 2_655 ?
C18B C17B N1B 110(4) 2_655 . ?
C18B C17B N1B 49(2) 2_655 2_655 ?
N1B C17B N1B 62(2) . 2_655 ?
C18B C17B H17D 96.7 2_655 . ?
N1B C17B H17D 107.0 . . ?
N1B C17B H17D 120.8 2_655 . ?
C18B C17B H17E 20.6 2_655 . ?
N1B C17B H17E 118.1 . . ?
N1B C17B H17E 56.2 2_655 . ?
H17D C17B H17E 109.7 . . ?
C18B C17B H17F 130.2 2_655 . ?
N1B C17B H17F 102.9 . . ?
N1B C17B H17F 130.2 2_655 . ?
H17D C17B H17F 108.9 . . ?
H17E C17B H17F 109.8 . . ?
C17B C18B N1B 100(3) 2_655 . ?
C17B C18B H18D 113.0 2_655 . ?
N1B C18B H18D 117.1 . . ?
C17B C18B H18E 111.2 2_655 . ?
N1B C18B H18E 105.9 . . ?
H18D C18B H18E 109.3 . . ?
C17B C18B H18F 5.6 2_655 . ?
N1B C18B H18F 105.3 . . ?
H18D C18B H18F 109.1 . . ?
H18E C18B H18F 109.8 . . ?
C16B C19B H19D 107.7 . . ?
C16B C19B H19E 111.6 . . ?
H19D C19B H19E 109.3 . . ?
C16B C19B H19F 109.1 . . ?
H19D C19B H19F 109.9 . . ?
H19E C19B H19F 109.2 . . ?
C39B O20 C39 43.7(18) . . ?
C42 N3 C39 112(4) . . ?
C42 N3 C41 137(4) . . ?
C39 N3 C41 111(3) . . ?
O20 C39 N3 109(2) . . ?
O20 C39 C40 143(4) . . ?
N3 C39 C40 108(3) . . ?
C39B N3B C42B 114.4(17) . . ?
C39B N3B C41B 121.4(17) . . ?
C42B N3B C41B 123.9(18) . . ?
O20 C39B N3B 119.3(15) . . ?
O20 C39B C40B 125.5(17) . . ?
N3B C39B C40B 114.8(15) . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
N3B C41B H41D 109.5 . . ?
N3B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
N3B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
N3B C42B H42D 109.5 . . ?
N3B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
N3B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.799
_refine_diff_density_min         -7.796
_refine_diff_density_rms         0.232


# Start Validation Reply Form

_vrf_PLAT215_7                   
;
PROBLEM:
Disordered N1        has ADP max/min Ratio .....        6.9
Disordered C16       has ADP max/min Ratio .....       10.7      

RESPONSE: 
Rotational disorder on two positions.
;

_vrf_PLAT220_7                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       7.1 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents and disordered anions lead to this high value.
;
_database_code_depnum_ccdc_archive 'CCDC 981954'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H21 O9 S2 Sm'
_chemical_formula_weight         607.83

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'
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   24.8112(8)
_cell_length_b                   13.7461(4)
_cell_length_c                   13.6627(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.153(3)
_cell_angle_gamma                90.00
_cell_volume                     4600.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3792
_cell_measurement_theta_min      2.3544
_cell_measurement_theta_max      29.1210

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2408
_exptl_absorpt_coefficient_mu    2.780
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_T_max  0.8082
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
The structure contains disordered solvents.
Because it was difficult to refine a xonsisten disordered model, 
their contribution was subtracted from the observed structure factors
according to the BYPASS procedure, as implemented in PLATON.
van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. 
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.

(see more at the bottom of this .cif file)
 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9536
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4282
_reflns_number_gt                3645
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0630P)²+22.0125P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4282
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.003

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
Sm1 Sm 0.170233(5) 0.215478(8) 0.461044(8) 0.01288(3) Uani 1 1 d . . .
C1 C 0.07530(10) 0.28048(17) 0.53748(18) 0.0207(7) Uani 1 1 d . . .
C2 C 0.02402(10) 0.31182(19) 0.57474(18) 0.0216(6) Uani 1 1 d . . .
C3 C -0.01422(12) 0.2436(2) 0.5932(3) 0.0406(8) Uani 1 1 d . . .
H3 H -0.0068 0.1776 0.5886 0.049 Uiso 1 1 calc R . .
C4 C -0.06371(13) 0.2737(2) 0.6185(3) 0.0480(10) Uani 1 1 d . . .
H4 H -0.0893 0.2272 0.6298 0.058 Uiso 1 1 calc R . .
C5 C -0.07590(10) 0.37206(18) 0.62747(18) 0.0237(7) Uani 1 1 d . . .
C6 C -0.03678(11) 0.4398(2) 0.6107(2) 0.0290(7) Uani 1 1 d . . .
H6 H -0.0436 0.5060 0.6157 0.035 Uiso 1 1 calc R . .
C7 C 0.01269(11) 0.4080(2) 0.5862(2) 0.0303(7) Uani 1 1 d . . .
H7 H 0.0390 0.4539 0.5774 0.036 Uiso 1 1 calc R . .
C8 C -0.13064(10) 0.39993(18) 0.65019(19) 0.0226(7) Uani 1 1 d . . .
C9 C -0.15381(10) 0.34657(19) 0.71914(18) 0.0237(7) Uani 1 1 d . . .
H9 H -0.1332 0.2982 0.7550 0.028 Uiso 1 1 calc R . .
C10 C -0.20665(10) 0.36301(17) 0.73630(17) 0.0198(6) Uani 1 1 d . . .
C11 C -0.23812(10) 0.43346(17) 0.67997(18) 0.0215(6) Uani 1 1 d . . .
H11 H -0.2746 0.4421 0.6864 0.026 Uiso 1 1 calc R . .
C12 C -0.21438(10) 0.49103(16) 0.61371(17) 0.0177(6) Uani 1 1 d . . .
C13 C -0.16114(10) 0.47529(17) 0.60036(17) 0.0200(6) Uani 1 1 d . . .
H13 H -0.1454 0.5153 0.5578 0.024 Uiso 1 1 calc R . .
C14 C -0.22871(10) 0.30712(18) 0.81685(18) 0.0192(6) Uani 1 1 d . . .
C15 C -0.24922(10) 0.56970(16) 0.55873(16) 0.0160(6) Uani 1 1 d . . .
C16 C 0.0575(3) 0.3373(8) 0.1609(7) 0.162(3) Uani 0.771(3) 1 d P A 1
H16A H 0.0271 0.3038 0.1810 0.243 Uiso 0.771(3) 1 calc PR A 1
H16B H 0.0537 0.3372 0.0898 0.243 Uiso 0.771(3) 1 calc PR A 1
H16C H 0.0583 0.4032 0.1844 0.243 Uiso 0.771(3) 1 calc PR A 1
C17 C 0.1585(3) 0.3514(7) 0.1867(7) 0.162(3) Uani 0.771(3) 1 d P A 1
H17A H 0.1944 0.3252 0.2078 0.243 Uiso 0.771(3) 1 calc PR A 1
H17B H 0.1547 0.4112 0.2212 0.243 Uiso 0.771(3) 1 calc PR A 1
H17C H 0.1534 0.3634 0.1167 0.243 Uiso 0.771(3) 1 calc PR A 1
C18 C 0.18057(19) -0.0663(3) 0.3271(3) 0.0754(15) Uani 1 1 d . . .
H18A H 0.2154 -0.0377 0.3513 0.113 Uiso 1 1 calc R . .
H18B H 0.1846 -0.1138 0.2773 0.113 Uiso 1 1 calc R . .
H18C H 0.1666 -0.0972 0.3809 0.113 Uiso 1 1 calc R . .
C19 C 0.0770(2) -0.0459(3) 0.2372(4) 0.0826(16) Uani 1 1 d . . .
H19A H 0.0643 -0.0717 0.2948 0.124 Uiso 1 1 calc R . .
H19B H 0.0869 -0.0984 0.1974 0.124 Uiso 1 1 calc R . .
H19C H 0.0485 -0.0082 0.1992 0.124 Uiso 1 1 calc R . .
O1 O 0.10696(7) 0.34308(13) 0.51399(15) 0.0334(5) Uani 1 1 d . . .
O2 O 0.08439(7) 0.18995(13) 0.52822(14) 0.0287(5) Uani 1 1 d . . .
O3 O -0.22727(7) 0.64462(11) 0.53041(12) 0.0215(4) Uani 1 1 d . . .
O4 O -0.30037(7) 0.55892(12) 0.54345(13) 0.0242(5) Uani 1 1 d . . .
O5 O -0.27694(7) 0.32743(14) 0.83011(13) 0.0275(5) Uani 1 1 d . . .
O6 O -0.19809(7) 0.24671(13) 0.86404(12) 0.0214(4) Uani 1 1 d . . .
O7 O 0.12500(11) 0.29888(16) 0.31574(17) 0.0527(8) Uani 1 1 d . . .
O8 O 0.12079(8) 0.08572(14) 0.36104(15) 0.0355(6) Uani 1 1 d . . .
S1 S 0.11667(7) 0.28005(10) 0.20949(9) 0.0672(5) Uani 0.771(3) 1 d P A 1
S2 S 0.13348(4) 0.02764(7) 0.27387(7) 0.0546(3) Uani 1 1 d . A .


_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
Sm1 O3 2.3795(16) 5_566 ?
Sm1 O7 2.410(2) . ?
Sm1 O6 2.4182(16) 2_556 ?
Sm1 O5 2.4519(18) 8 ?
Sm1 O8 2.4536(19) . ?
Sm1 O2 2.4747(19) . ?
Sm1 O4 2.4839(16) 3_545 ?
Sm1 O1 2.5348(19) . ?
Sm1 O3 2.7472(17) 3_545 ?
Sm1 C1 2.867(3) . ?
Sm1 C15 2.990(2) 3_545 ?
Sm1 Sm1 4.0449(3) 7_556 ?
C1 O1 1.241(3) . ?
C1 O2 1.275(3) . ?
C1 C2 1.507(4) . ?
C2 C7 1.366(4) . ?
C2 C3 1.385(4) . ?
C3 C4 1.391(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(4) . ?
C5 C8 1.491(4) . ?
C6 C7 1.393(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.389(4) . ?
C8 C13 1.395(3) . ?
C9 C10 1.387(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(3) . ?
C10 C14 1.514(4) . ?
C11 C12 1.401(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(4) . ?
C12 C15 1.508(3) . ?
C13 H13 0.9300 . ?
C14 O6 1.236(3) . ?
C14 O5 1.270(3) . ?
C15 O3 1.255(3) . ?
C15 O4 1.262(3) . ?
C15 Sm1 2.990(2) 3_455 ?
C16 S1 1.705(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 S1 1.496(10) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 S2 1.814(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 S2 1.736(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O3 Sm1 2.3795(16) 5_566 ?
O3 Sm1 2.7472(17) 3_455 ?
O4 Sm1 2.4839(16) 3_455 ?
O5 Sm1 2.4519(18) 8_456 ?
O6 Sm1 2.4182(16) 2_556 ?
O7 S1 1.457(3) . ?
O8 S2 1.508(2) . ?

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
O3 Sm1 O7 81.45(7) 5_566 . ?
O3 Sm1 O6 74.56(6) 5_566 2_556 ?
O7 Sm1 O6 138.78(7) . 2_556 ?
O3 Sm1 O5 81.23(6) 5_566 8 ?
O7 Sm1 O5 75.30(8) . 8 ?
O6 Sm1 O5 131.44(6) 2_556 8 ?
O3 Sm1 O8 148.83(6) 5_566 . ?
O7 Sm1 O8 76.17(7) . . ?
O6 Sm1 O8 135.92(6) 2_556 . ?
O5 Sm1 O8 72.35(6) 8 . ?
O3 Sm1 O2 129.54(6) 5_566 . ?
O7 Sm1 O2 93.29(8) . . ?
O6 Sm1 O2 77.66(6) 2_556 . ?
O5 Sm1 O2 145.89(6) 8 . ?
O8 Sm1 O2 73.73(7) . . ?
O3 Sm1 O4 123.26(6) 5_566 3_545 ?
O7 Sm1 O4 148.25(7) . 3_545 ?
O6 Sm1 O4 71.86(6) 2_556 3_545 ?
O5 Sm1 O4 88.27(6) 8 3_545 ?
O8 Sm1 O4 72.98(6) . 3_545 ?
O2 Sm1 O4 85.24(6) . 3_545 ?
O3 Sm1 O1 79.47(6) 5_566 . ?
O7 Sm1 O1 71.18(8) . . ?
O6 Sm1 O1 71.81(6) 2_556 . ?
O5 Sm1 O1 143.30(6) 8 . ?
O8 Sm1 O1 112.61(6) . . ?
O2 Sm1 O1 51.95(6) . . ?
O4 Sm1 O1 128.37(6) 3_545 . ?
O3 Sm1 O3 76.05(5) 5_566 3_545 ?
O7 Sm1 O3 137.49(8) . 3_545 ?
O6 Sm1 O3 67.58(6) 2_556 3_545 ?
O5 Sm1 O3 66.01(5) 8 3_545 ?
O8 Sm1 O3 106.72(6) . 3_545 ?
O2 Sm1 O3 128.75(6) . 3_545 ?
O4 Sm1 O3 49.27(5) 3_545 3_545 ?
O1 Sm1 O3 136.73(5) . 3_545 ?
O3 Sm1 C1 104.29(6) 5_566 . ?
O7 Sm1 C1 81.36(8) . . ?
O6 Sm1 C1 72.96(6) 2_556 . ?
O5 Sm1 C1 154.99(6) 8 . ?
O8 Sm1 C1 93.58(7) . . ?
O2 Sm1 C1 26.32(6) . . ?
O4 Sm1 C1 107.69(7) 3_545 . ?
O1 Sm1 C1 25.63(6) . . ?
O3 Sm1 C1 138.93(6) 3_545 . ?
O3 Sm1 C15 99.77(6) 5_566 3_545 ?
O7 Sm1 C15 151.30(8) . 3_545 ?
O6 Sm1 C15 67.18(6) 2_556 3_545 ?
O5 Sm1 C15 76.56(6) 8 3_545 ?
O8 Sm1 C15 90.05(6) . 3_545 ?
O2 Sm1 C15 107.04(6) . 3_545 ?
O4 Sm1 C15 24.48(6) 3_545 3_545 ?
O1 Sm1 C15 137.44(6) . 3_545 ?
O3 Sm1 C15 24.80(6) 3_545 3_545 ?
C1 Sm1 C15 125.15(7) . 3_545 ?
O3 Sm1 Sm1 41.23(4) 5_566 7_556 ?
O7 Sm1 Sm1 114.41(7) . 7_556 ?
O6 Sm1 Sm1 65.44(4) 2_556 7_556 ?
O5 Sm1 Sm1 68.54(4) 8 7_556 ?
O8 Sm1 Sm1 134.33(5) . 7_556 ?
O2 Sm1 Sm1 143.10(4) . 7_556 ?
O4 Sm1 Sm1 83.08(4) 3_545 7_556 ?
O1 Sm1 Sm1 112.77(4) . 7_556 ?
O3 Sm1 Sm1 34.81(3) 3_545 7_556 ?
C1 Sm1 Sm1 131.09(5) . 7_556 ?
C15 Sm1 Sm1 58.88(4) 3_545 7_556 ?
O1 C1 O2 121.5(2) . . ?
O1 C1 C2 119.5(2) . . ?
O2 C1 C2 119.0(2) . . ?
O1 C1 Sm1 62.06(14) . . ?
O2 C1 Sm1 59.40(13) . . ?
C2 C1 Sm1 177.64(17) . . ?
C7 C2 C3 118.3(3) . . ?
C7 C2 C1 121.1(2) . . ?
C3 C2 C1 120.5(2) . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 121.5(3) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 117.9(3) . . ?
C6 C5 C8 123.0(2) . . ?
C4 C5 C8 119.0(2) . . ?
C5 C6 C7 119.6(2) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C2 C7 C6 122.5(3) . . ?
C2 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C9 C8 C13 118.2(2) . . ?
C9 C8 C5 119.7(2) . . ?
C13 C8 C5 122.1(2) . . ?
C10 C9 C8 122.2(2) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C11 118.7(2) . . ?
C9 C10 C14 120.1(2) . . ?
C11 C10 C14 121.2(2) . . ?
C10 C11 C12 119.5(2) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 C15 122.1(2) . . ?
C11 C12 C15 117.4(2) . . ?
C12 C13 C8 120.6(2) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
O6 C14 O5 126.1(2) . . ?
O6 C14 C10 117.2(2) . . ?
O5 C14 C10 116.7(2) . . ?
O3 C15 O4 121.3(2) . . ?
O3 C15 C12 120.0(2) . . ?
O4 C15 C12 118.7(2) . . ?
O3 C15 Sm1 66.69(12) . 3_455 ?
O4 C15 Sm1 54.66(11) . 3_455 ?
C12 C15 Sm1 172.86(17) . 3_455 ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S1 C17 H17A 109.5 . . ?
S1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
S1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S2 C18 H18A 109.5 . . ?
S2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S2 C19 H19A 109.5 . . ?
S2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C1 O1 Sm1 92.31(15) . . ?
C1 O2 Sm1 94.28(15) . . ?
C15 O3 Sm1 158.78(15) . 5_566 ?
C15 O3 Sm1 88.51(14) . 3_455 ?
Sm1 O3 Sm1 103.95(5) 5_566 3_455 ?
C15 O4 Sm1 100.85(14) . 3_455 ?
C14 O5 Sm1 132.58(15) . 8_456 ?
C14 O6 Sm1 133.66(16) . 2_556 ?
S1 O7 Sm1 135.26(15) . . ?
S2 O8 Sm1 132.53(12) . . ?
O7 S1 C17 95.6(4) . . ?
O7 S1 C16 106.5(4) . . ?
C17 S1 C16 101.5(5) . . ?
O8 S2 C19 106.01(19) . . ?
O8 S2 C18 105.20(17) . . ?
C19 S2 C18 98.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.038
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.158

# 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 0.003 -0.009 -0.014 663.8 1.1
_platon_squeeze_details          
;
;

# Start Validation Reply Form

_vrf_PLAT222_8                   
;
PROBLEM:
Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       10.0 Ratio  

RESPONSE: 
Disordered solvents lead to this high value.
;



_vrf_CHEMW03_8                   
;
PROBLEM:
The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.95 <> 1.05
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight           607.83
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   18.54  222.71
           H         1.01   17.63   17.77
           O        16.00    8.00  127.99
           S        32.07    1.77   56.79
           Sm      150.36    1.00  150.36
           Calculated formula weight              575.62

RESPONSE:

The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modelled. Instead, the disordered solvent was accounted for using the SQUEEZE routine of PLATON. These additional solvent molecules were included in the chemical formula, leading the discrepancy between the formula calculated from the atoms in the CIF.
;


_vrf_PLAT220_8                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       10.0 Ratio

RESPONSE:
Disordered solvents and disordered anions lead to this high value.
;

_vrf_PLAT230_8                   
;
PROBLEM:
Hirshfeld Test Diff for    S2     --  O8      ..       11.0 su

RESPONSE:
Caused by vibration of terminal DMSO molecules.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 981955'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H21 Nd O9 S2'
_chemical_formula_weight         601.72

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   ' C 1 2/c 1'

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

_cell_length_a                   24.8718(8)
_cell_length_b                   13.7591(4)
_cell_length_c                   13.6832(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.949(3)
_cell_angle_gamma                90.00
_cell_volume                     4625.6(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4187
_cell_measurement_theta_min      2.3484
_cell_measurement_theta_max      29.0184

_exptl_crystal_description       block
_exptl_crystal_colour            lavender
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2392
_exptl_absorpt_coefficient_mu    2.471
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6932
_exptl_absorpt_correction_T_max  0.8268
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
; 
The structure contains disordered solvents.
Because it was difficult to refine a xonsisten disordered model, 
their contribution was subtracted from the observed structure factors
according to the BYPASS procedure, as implemented in PLATON.
van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. 
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.

(see more at the bottom of this .cif file)
 
;


_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8860
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         25.49
_reflns_number_total             4316
_reflns_number_gt                3705
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0666P)²+10.4074P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4316
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1085
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.007

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
Nd1 Nd 0.169935(4) 0.215976(8) 0.461143(7) 0.01360(3) Uani 1 1 d . . .
C1 C 0.07445(8) 0.28171(17) 0.53794(17) 0.0219(6) Uani 1 1 d . . .
C2 C 0.02339(8) 0.31325(18) 0.57545(16) 0.0223(6) Uani 1 1 d . . .
C3 C -0.01509(9) 0.2441(2) 0.5928(2) 0.0417(8) Uani 1 1 d . . .
H3 H -0.0079 0.1780 0.5880 0.050 Uiso 1 1 calc R . .
C4 C -0.06421(10) 0.2756(2) 0.6174(2) 0.0461(8) Uani 1 1 d . . .
H4 H -0.0901 0.2296 0.6279 0.055 Uiso 1 1 calc R . .
C5 C -0.07611(8) 0.37343(18) 0.62696(16) 0.0237(6) Uani 1 1 d . . .
C6 C -0.03703(8) 0.4411(2) 0.61123(18) 0.0316(7) Uani 1 1 d . . .
H6 H -0.0438 0.5072 0.6169 0.038 Uiso 1 1 calc R . .
C7 C 0.01210(9) 0.40952(19) 0.58702(18) 0.0321(7) Uani 1 1 d . . .
H7 H 0.0384 0.4554 0.5783 0.038 Uiso 1 1 calc R . .
C8 C -0.13128(8) 0.40076(18) 0.64894(16) 0.0233(6) Uani 1 1 d . . .
C9 C -0.15327(8) 0.34646(18) 0.71905(16) 0.0244(6) Uani 1 1 d . . .
H9 H -0.1322 0.2991 0.7553 0.029 Uiso 1 1 calc R . .
C10 C -0.20685(8) 0.36262(17) 0.73541(15) 0.0197(5) Uani 1 1 d . . .
C11 C -0.23788(8) 0.43227(18) 0.67891(15) 0.0213(6) Uani 1 1 d . . .
H11 H -0.2743 0.4402 0.6852 0.026 Uiso 1 1 calc R . .
C12 C -0.21507(7) 0.49013(17) 0.61314(14) 0.0179(5) Uani 1 1 d . . .
C13 C -0.16117(8) 0.47531(17) 0.59998(15) 0.0197(5) Uani 1 1 d . . .
H13 H -0.1454 0.5159 0.5581 0.024 Uiso 1 1 calc R . .
C14 C -0.22852(8) 0.30586(17) 0.81514(16) 0.0187(5) Uani 1 1 d . . .
C15 C -0.24955(8) 0.56796(15) 0.55919(14) 0.0150(5) Uani 1 1 d . . .
C16 C 0.0602(3) 0.3410(7) 0.1628(5) 0.148(2) Uani 0.780(2) 1 d P A 1
H16A H 0.0291 0.3089 0.1819 0.223 Uiso 0.780(2) 1 calc PR A 1
H16B H 0.0567 0.3423 0.0919 0.223 Uiso 0.780(2) 1 calc PR A 1
H16C H 0.0622 0.4063 0.1878 0.223 Uiso 0.780(2) 1 calc PR A 1
C17 C 0.1597(3) 0.3526(7) 0.1840(6) 0.148(2) Uani 0.780(2) 1 d P A 1
H17A H 0.1952 0.3257 0.2052 0.223 Uiso 0.780(2) 1 calc PR A 1
H17B H 0.1564 0.4132 0.2172 0.223 Uiso 0.780(2) 1 calc PR A 1
H17C H 0.1546 0.3632 0.1138 0.223 Uiso 0.780(2) 1 calc PR A 1
C18 C 0.18028(13) -0.0667(3) 0.3259(3) 0.0643(11) Uani 1 1 d . . .
H18A H 0.2144 -0.0376 0.3531 0.096 Uiso 1 1 calc R . .
H18B H 0.1859 -0.1122 0.2753 0.096 Uiso 1 1 calc R . .
H18C H 0.1654 -0.0999 0.3772 0.096 Uiso 1 1 calc R . .
C19 C 0.07698(14) -0.0466(3) 0.2355(3) 0.0719(12) Uani 1 1 d . . .
H19A H 0.0646 -0.0739 0.2926 0.108 Uiso 1 1 calc R . .
H19B H 0.0868 -0.0980 0.1942 0.108 Uiso 1 1 calc R . .
H19C H 0.0484 -0.0083 0.1990 0.108 Uiso 1 1 calc R . .
O1 O 0.10647(6) 0.34469(13) 0.51580(13) 0.0348(5) Uani 1 1 d . . .
O2 O 0.08320(6) 0.19170(13) 0.52801(13) 0.0297(5) Uani 1 1 d . . .
O3 O -0.22779(5) 0.64288(11) 0.52902(11) 0.0212(4) Uani 1 1 d . . .
O4 O -0.30057(5) 0.55746(12) 0.54456(12) 0.0246(4) Uani 1 1 d . . .
O5 O -0.27723(5) 0.32574(14) 0.82768(11) 0.0283(5) Uani 1 1 d . . .
O6 O -0.19849(6) 0.24627(13) 0.86159(11) 0.0234(4) Uani 1 1 d . . .
O7 O 0.12417(9) 0.30138(17) 0.31511(15) 0.0544(7) Uani 1 1 d . . .
O8 O 0.12051(6) 0.08501(14) 0.36065(12) 0.0361(5) Uani 1 1 d . . .
S1 S 0.11625(6) 0.28143(10) 0.20900(8) 0.0661(4) Uani 0.780(2) 1 d P A 1
S2 S 0.13352(3) 0.02684(6) 0.27314(5) 0.0466(2) Uani 1 1 d . A .


_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
Nd1 O3 2.4083(15) 5_566 ?
Nd1 O7 2.442(2) . ?
Nd1 O6 2.4548(15) 2_556 ?
Nd1 O8 2.4744(18) . ?
Nd1 O5 2.4775(15) 8 ?
Nd1 O2 2.4934(16) . ?
Nd1 O4 2.5174(16) 3_545 ?
Nd1 O1 2.5602(17) . ?
Nd1 O3 2.7585(13) 3_545 ?
Nd1 C1 2.888(2) . ?
Nd1 C15 3.0201(19) 3_545 ?
Nd1 Nd1 4.0684(2) 7_556 ?
C1 O1 1.246(3) . ?
C1 O2 1.268(3) . ?
C1 C2 1.506(3) . ?
C2 C7 1.368(4) . ?
C2 C3 1.396(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(3) . ?
C5 C8 1.498(3) . ?
C6 C7 1.385(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C13 1.378(3) . ?
C8 C9 1.393(3) . ?
C9 C10 1.403(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.388(3) . ?
C10 C14 1.508(3) . ?
C11 C12 1.387(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.395(3) . ?
C12 C15 1.494(3) . ?
C13 H13 0.9300 . ?
C14 O6 1.219(3) . ?
C14 O5 1.279(3) . ?
C15 O3 1.263(3) . ?
C15 O4 1.262(2) . ?
C15 Nd1 3.0201(19) 3_455 ?
C16 S1 1.656(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 S1 1.536(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 S2 1.808(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 S2 1.743(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O3 Nd1 2.4083(15) 5_566 ?
O3 Nd1 2.7585(13) 3_455 ?
O4 Nd1 2.5174(16) 3_455 ?
O5 Nd1 2.4775(15) 8_456 ?
O6 Nd1 2.4548(15) 2_556 ?
O7 S1 1.460(2) . ?
O8 S2 1.5164(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
O3 Nd1 O7 81.73(6) 5_566 . ?
O3 Nd1 O6 74.29(5) 5_566 2_556 ?
O7 Nd1 O6 138.88(7) . 2_556 ?
O3 Nd1 O8 149.22(5) 5_566 . ?
O7 Nd1 O8 76.56(7) . . ?
O6 Nd1 O8 135.65(6) 2_556 . ?
O3 Nd1 O5 81.21(5) 5_566 8 ?
O7 Nd1 O5 75.02(7) . 8 ?
O6 Nd1 O5 131.50(5) 2_556 8 ?
O8 Nd1 O5 72.32(5) . 8 ?
O3 Nd1 O2 129.13(5) 5_566 . ?
O7 Nd1 O2 92.57(7) . . ?
O6 Nd1 O2 78.11(5) 2_556 . ?
O8 Nd1 O2 73.92(6) . . ?
O5 Nd1 O2 145.88(5) 8 . ?
O3 Nd1 O4 122.95(5) 5_566 3_545 ?
O7 Nd1 O4 148.64(6) . 3_545 ?
O6 Nd1 O4 71.33(5) 2_556 3_545 ?
O8 Nd1 O4 72.88(5) . 3_545 ?
O5 Nd1 O4 89.03(6) 8 3_545 ?
O2 Nd1 O4 85.71(5) . 3_545 ?
O3 Nd1 O1 79.40(5) 5_566 . ?
O7 Nd1 O1 71.10(7) . . ?
O6 Nd1 O1 71.98(5) 2_556 . ?
O8 Nd1 O1 112.98(5) . . ?
O5 Nd1 O1 142.88(6) 8 . ?
O2 Nd1 O1 51.50(6) . . ?
O4 Nd1 O1 128.04(5) 3_545 . ?
O3 Nd1 O3 76.32(5) 5_566 3_545 ?
O7 Nd1 O3 137.65(6) . 3_545 ?
O6 Nd1 O3 67.62(5) 2_556 3_545 ?
O8 Nd1 O3 105.90(5) . 3_545 ?
O5 Nd1 O3 66.21(4) 8 3_545 ?
O2 Nd1 O3 129.26(5) . 3_545 ?
O4 Nd1 O3 48.94(4) 3_545 3_545 ?
O1 Nd1 O3 137.06(5) . 3_545 ?
O3 Nd1 C1 104.19(6) 5_566 . ?
O7 Nd1 C1 80.91(7) . . ?
O6 Nd1 C1 73.45(6) 2_556 . ?
O8 Nd1 C1 93.71(6) . . ?
O5 Nd1 C1 154.34(5) 8 . ?
O2 Nd1 C1 25.96(6) . . ?
O4 Nd1 C1 107.72(6) 3_545 . ?
O1 Nd1 C1 25.54(6) . . ?
O3 Nd1 C1 139.39(5) 3_545 . ?
O3 Nd1 C15 99.78(5) 5_566 3_545 ?
O7 Nd1 C15 151.71(7) . 3_545 ?
O6 Nd1 C15 66.77(5) 2_556 3_545 ?
O8 Nd1 C15 89.63(6) . 3_545 ?
O5 Nd1 C15 77.30(5) 8 3_545 ?
O2 Nd1 C15 107.36(5) . 3_545 ?
O4 Nd1 C15 24.23(5) 3_545 3_545 ?
O1 Nd1 C15 137.14(5) . 3_545 ?
O3 Nd1 C15 24.72(5) 3_545 3_545 ?
C1 Nd1 C15 125.14(6) . 3_545 ?
O3 Nd1 Nd1 41.21(3) 5_566 7_556 ?
O7 Nd1 Nd1 114.58(6) . 7_556 ?
O6 Nd1 Nd1 65.27(4) 2_556 7_556 ?
O8 Nd1 Nd1 133.97(4) . 7_556 ?
O5 Nd1 Nd1 68.66(3) 8 7_556 ?
O2 Nd1 Nd1 143.38(4) . 7_556 ?
O4 Nd1 Nd1 82.91(3) 3_545 7_556 ?
O1 Nd1 Nd1 112.80(4) . 7_556 ?
O3 Nd1 Nd1 35.11(3) 3_545 7_556 ?
C1 Nd1 Nd1 131.29(4) . 7_556 ?
C15 Nd1 Nd1 58.98(4) 3_545 7_556 ?
O1 C1 O2 121.8(2) . . ?
O1 C1 C2 119.2(2) . . ?
O2 C1 C2 119.1(2) . . ?
O1 C1 Nd1 62.37(12) . . ?
O2 C1 Nd1 59.38(11) . . ?
C2 C1 Nd1 177.83(16) . . ?
C7 C2 C3 118.8(2) . . ?
C7 C2 C1 121.2(2) . . ?
C3 C2 C1 119.9(2) . . ?
C4 C3 C2 118.7(2) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 122.3(2) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 118.1(2) . . ?
C6 C5 C8 123.3(2) . . ?
C4 C5 C8 118.5(2) . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C2 C7 C6 122.4(2) . . ?
C2 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C13 C8 C9 119.61(19) . . ?
C13 C8 C5 122.1(2) . . ?
C9 C8 C5 118.3(2) . . ?
C8 C9 C10 120.6(2) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 118.7(2) . . ?
C11 C10 C14 122.03(18) . . ?
C9 C10 C14 119.25(19) . . ?
C12 C11 C10 120.63(18) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.87(19) . . ?
C11 C12 C15 118.08(17) . . ?
C13 C12 C15 122.04(19) . . ?
C8 C13 C12 120.2(2) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
O6 C14 O5 126.2(2) . . ?
O6 C14 C10 117.81(19) . . ?
O5 C14 C10 116.03(18) . . ?
O3 C15 O4 120.87(18) . . ?
O3 C15 C12 120.29(17) . . ?
O4 C15 C12 118.84(18) . . ?
O3 C15 Nd1 65.97(10) . 3_455 ?
O4 C15 Nd1 54.96(10) . 3_455 ?
C12 C15 Nd1 173.32(14) . 3_455 ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S1 C17 H17A 109.5 . . ?
S1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
S1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S2 C18 H18A 109.5 . . ?
S2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S2 C19 H19A 109.5 . . ?
S2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C1 O1 Nd1 92.09(14) . . ?
C1 O2 Nd1 94.66(13) . . ?
C15 O3 Nd1 157.29(12) . 5_566 ?
C15 O3 Nd1 89.31(11) . 3_455 ?
Nd1 O3 Nd1 103.68(5) 5_566 3_455 ?
C15 O4 Nd1 100.81(13) . 3_455 ?
C14 O5 Nd1 132.17(14) . 8_456 ?
C14 O6 Nd1 133.54(15) . 2_556 ?
S1 O7 Nd1 134.16(15) . . ?
S2 O8 Nd1 132.43(10) . . ?
O7 S1 C17 96.4(3) . . ?
O7 S1 C16 105.2(3) . . ?
C17 S1 C16 100.3(4) . . ?
O8 S2 C19 106.13(15) . . ?
O8 S2 C18 105.29(14) . . ?
C19 S2 C18 98.31(17) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.353
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.147

# 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 0.003 -0.009 -0.014 663.8 1.1
_platon_squeeze_details          
;
;

# Start Validation Reply Form

_vrf_CHEMW03_9                   
;
PROBLEM:
The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.95 <> 1.05
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight           601.72
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   18.56  222.92
           H         1.01   17.68   17.82
           O        16.00    8.00  127.99
           S        32.07    1.78   57.08
           Nd      144.24    1.00  144.24
           Calculated formula weight              570.06

RESPONSE:

The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modelled. Instead, the disordered solvent was accounted for using the SQUEEZE routine of PLATON. These additional solvent molecules were included in the chemical formula, leading the discrepancy between the formula calculated from the atoms in the CIF.
;

_vrf_PLAT220_9                   
;
PROBLEM:
Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       9.9 Ratio

RESPONSE:
Disordered solvents and disordered anions lead to this high value.
;

_vrf_PLAT222_9                   
;
PROBLEM:
Large Non-Solvent    H    Uiso(max)/Uiso(min) ..        9.3 Ratio 

RESPONSE:
Many crystals tried and the best presented - disordered solvents lead to this high value.
;

_vrf_PLAT230_9                   
;
PROBLEM:
Hirshfeld Test Diff for    S2     --  O8      ..       9.0 su

RESPONSE:
Caused by vibration of terminal DMSO molecules.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 981956'
