# 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
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#  data retrieval see:
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#  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            'C139 H58 O96 Tm12'
_chemical_formula_weight         5291.02

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/m

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

_cell_length_a                   27.7056(6)
_cell_length_b                   23.3950(6)
_cell_length_c                   21.0709(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.911(2)
_cell_angle_gamma                90.00
_cell_volume                     12485.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4383
_cell_measurement_theta_min      1.06
_cell_measurement_theta_max      28.35

_exptl_crystal_description       sheet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4983
_exptl_absorpt_coefficient_mu    4.287
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_T_max  0.424
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            46360
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.06
_diffrn_reflns_theta_max         28.35
_reflns_number_total             15921
_reflns_number_gt                11869
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0294P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15921
_refine_ls_number_parameters     572
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C34 C 1.0000 0.5000 1.0000 0.083(5) Uani 1 4 d S . .
C21 C 0.58963(16) 0.2731(2) 1.09724(19) 0.0270(10) Uani 1 1 d . . .
C17 C 0.54830(15) 0.31047(17) 0.84637(18) 0.0210(8) Uani 1 1 d . . .
C1 C 0.36007(16) 0.28862(18) 0.67741(19) 0.0257(9) Uani 1 1 d . . .
C3 C 0.26918(16) 0.30038(19) 0.58906(19) 0.0259(9) Uani 1 1 d . . .
H3 H 0.2534(16) 0.2748(18) 0.616(2) 0.031 Uiso 1 1 d . . .
C31 C 0.82786(16) 0.41941(18) 0.9770(2) 0.0263(9) Uani 1 1 d . . .
C28 C 0.86200(16) 0.28282(18) 1.17485(19) 0.0237(9) Uani 1 1 d . . .
C32 C 0.75416(16) 0.36707(18) 0.99251(19) 0.0252(9) Uani 1 1 d . . .
H11 H 0.7308 0.3847 0.9522 0.030 Uiso 1 1 calc R . .
C24 C 0.64012(15) 0.32227(18) 0.93855(18) 0.0243(9) Uani 1 1 d . . .
H7 H 0.6511 0.3321 0.9037 0.029 Uiso 1 1 calc R . .
C18 C 0.58713(15) 0.31003(17) 0.92108(18) 0.0217(8) Uani 1 1 d . . .
C2 C 0.32181(16) 0.31487(18) 0.61151(18) 0.0249(9) Uani 1 1 d . . .
C7 C 0.31557(16) 0.41708(19) 0.4700(2) 0.0263(9) Uani 1 1 d . . .
C29 C 0.84313(15) 0.35143(18) 1.07556(19) 0.0261(9) Uani 1 1 d . . .
H12 H 0.8791 0.3592 1.0921 0.031 Uiso 1 1 calc R . .
C25 C 0.73443(15) 0.33033(19) 1.02821(19) 0.0247(9) Uani 1 1 d . . .
C22 C 0.65900(16) 0.30682(19) 1.05859(19) 0.0283(10) Uani 1 1 d . . .
H9 H 0.6823 0.3080 1.1051 0.034 Uiso 1 1 calc R . .
C20 C 0.60654(16) 0.29188(19) 1.04153(19) 0.0271(9) Uani 1 1 d . . .
C4 C 0.23051(15) 0.32442(18) 0.52878(19) 0.0250(9) Uani 1 1 d . . .
C9 C 0.17405(16) 0.31036(19) 0.50810(19) 0.0251(9) Uani 1 1 d . . .
C12 C 0.08877(16) 0.2589(2) 0.5975(2) 0.0287(10) Uani 1 1 d . . .
C13 C 0.06870(16) 0.27804(19) 0.47255(19) 0.0282(10) Uani 1 1 d . . .
H6 H 0.0341 0.2660 0.4606 0.034 Uiso 1 1 calc R . .
C16 C 0.13741(15) 0.31108(18) 0.43860(18) 0.0241(9) Uani 1 1 d . . .
H5 H 0.1483 0.3220 0.4040 0.029 Uiso 1 1 calc R . .
C23 C 0.67749(15) 0.32009(18) 1.00766(19) 0.0237(9) Uani 1 1 d . . .
C30 C 0.80842(16) 0.37813(18) 1.01581(19) 0.0247(9) Uani 1 1 d . . .
C11 C 0.10444(16) 0.27863(19) 0.54176(19) 0.0271(10) Uani 1 1 d . . .
C26 C 0.77197(16) 0.30315(18) 1.08717(18) 0.0254(9) Uani 1 1 d . . .
H10 H 0.7602 0.2771 1.1110 0.031 Uiso 1 1 calc R . .
C19 C 0.57068(15) 0.29294(18) 0.97266(18) 0.0245(9) Uani 1 1 d . . .
H8 H 0.5358 0.2823 0.9609 0.029 Uiso 1 1 calc R . .
C14 C 0.08537(16) 0.29585(19) 0.42081(19) 0.0250(9) Uani 1 1 d . . .
C10 C 0.15602(16) 0.2957(2) 0.55843(19) 0.0284(10) Uani 1 1 d . . .
H4 H 0.1793 0.2975 0.6049 0.034 Uiso 1 1 calc R . .
C8 C 0.33807(16) 0.35304(18) 0.5730(2) 0.0288(10) Uani 1 1 d . . .
H1 H 0.3735 0.3630 0.5880 0.035 Uiso 1 1 calc R . .
C6 C 0.30094(16) 0.37583(19) 0.51235(19) 0.0282(10) Uani 1 1 d . . .
C5 C 0.24755(16) 0.36148(19) 0.49027(19) 0.0280(10) Uani 1 1 d . . .
H2 H 0.2230 0.3769 0.4492 0.034 Uiso 1 1 calc R . .
C15 C 0.04661(16) 0.29517(18) 0.34540(19) 0.0255(9) Uani 1 1 d . . .
C36 C 0.7606(3) 0.5000 0.7646(3) 0.0419(17) Uani 1 2 d S . .
H14 H 0.7380 0.5000 0.7875 0.050 Uiso 1 2 calc SR . .
C35 C 0.9067(2) 0.6135(3) 0.8498(3) 0.0570(16) Uani 1 1 d . . .
H13 H 0.9431 0.6105 0.8747 0.068 Uiso 1 1 calc R . .
C33 C 0.8838(2) 0.1069(3) 1.3309(3) 0.0600(17) Uani 1 1 d . . .
H4A H 0.9180 0.1011 1.3638 0.072 Uiso 1 1 calc R . .
O11 O 0.95677(18) 0.5000 0.9709(3) 0.0530(14) Uani 1 2 d S . .
O13 O 0.80591(18) 0.5000 0.8022(2) 0.0444(13) Uani 1 2 d S . .
O4 O 0.50101(11) 0.29831(14) 0.83191(14) 0.0347(7) Uani 1 1 d . . .
O23 O 0.55112(11) 0.23942(13) 1.08306(13) 0.0300(7) Uani 1 1 d . . .
O7 O 0.84466(11) 0.24418(13) 1.20041(13) 0.0281(7) Uani 1 1 d . . .
O17 O 0.05404(12) 0.22150(13) 0.58593(13) 0.0314(7) Uani 1 1 d . . .
O1 O 0.34667(11) 0.24696(13) 0.70362(13) 0.0282(7) Uani 1 1 d . . .
O26 O 0.89412(12) 0.65567(13) 0.81052(14) 0.0345(7) Uani 1 1 d . . .
O8 O 0.91048(10) 0.29750(13) 1.20226(13) 0.0279(7) Uani 1 1 d . . .
O19 O 0.06272(11) 0.30956(13) 0.30015(13) 0.0306(7) Uani 1 1 d . . .
O22 O 0.56537(11) 0.32327(13) 0.80164(13) 0.0296(7) Uani 1 1 d . . .
O3 O 0.50884(11) 0.17703(13) 0.84217(14) 0.0337(7) Uani 1 1 d . . .
O16 O 0.11211(13) 0.28055(15) 0.65775(14) 0.0408(9) Uani 1 1 d . . .
O24 O 0.61503(13) 0.29024(16) 1.15925(14) 0.0424(9) Uani 1 1 d . . .
O10 O 0.87597(12) 0.43361(15) 1.00276(15) 0.0418(9) Uani 1 1 d . . .
O9 O 0.79734(12) 0.43941(15) 0.92086(16) 0.0455(9) Uani 1 1 d . . .
O2 O 0.40709(11) 0.30838(13) 0.70617(14) 0.0356(8) Uani 1 1 d . . .
O18 O 0.00061(12) 0.27966(15) 0.33227(15) 0.0434(9) Uani 1 1 d . . .
O5 O 0.87769(13) 0.14970(14) 1.29465(16) 0.0411(8) Uani 1 1 d . . .
O21 O 0.36311(12) 0.43222(16) 0.48725(16) 0.0497(10) Uani 1 1 d . . .
O25 O 0.85210(15) 0.07125(16) 1.33014(18) 0.0527(10) Uani 1 1 d . . .
O12 O 0.88387(16) 0.57701(16) 0.86259(19) 0.0610(11) Uani 1 1 d . . .
O15 O 0.73833(19) 0.5000 0.7028(2) 0.0459(13) Uani 1 2 d S . .
C27 C 0.82474(15) 0.31332(17) 1.11081(18) 0.0218(8) Uani 1 1 d . . .
O14 O 0.56927(19) 0.5000 0.5611(3) 0.0551(14) Uani 1 2 d S . .
O6 O 0.99731(16) 0.15531(17) 1.33989(16) 0.0638(12) Uani 1 1 d . . .
O20 O 0.28115(13) 0.43805(17) 0.41688(17) 0.0570(11) Uani 1 1 d . . .
Tm1 Tm 0.434082(6) 0.235533(8) 0.793775(8) 0.01822(5) Uani 1 1 d . . .
Tm2 Tm 0.930247(7) 0.222947(8) 1.289987(8) 0.02066(5) Uani 1 1 d . . .
Tm3 Tm 0.866180(9) 0.5000 0.913849(11) 0.01683(6) Uani 1 2 d S . .
Tm4 Tm 0.661179(10) 0.5000 0.607081(12) 0.02012(6) Uani 1 2 d S . .


_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
C34 O11 1.102(5) . ?
C34 O11 1.102(5) 5_767 ?
C21 O23 1.261(5) . ?
C21 O24 1.272(5) . ?
C21 C20 1.495(5) . ?
C21 Tm1 2.775(4) 2_657 ?
C17 O22 1.250(4) . ?
C17 O4 1.252(5) . ?
C17 C18 1.504(5) . ?
C1 O1 1.249(5) . ?
C1 O2 1.280(5) . ?
C1 C2 1.495(5) . ?
C3 C2 1.381(6) . ?
C3 C4 1.405(5) . ?
C3 H3 1.04(4) . ?
C31 O9 1.234(5) . ?
C31 O10 1.263(5) . ?
C31 C30 1.499(5) . ?
C28 O7 1.244(5) . ?
C28 O8 1.276(5) . ?
C28 C27 1.505(5) . ?
C32 C25 1.392(5) . ?
C32 C30 1.403(5) . ?
C32 H11 0.9300 . ?
C24 C18 1.391(5) . ?
C24 C23 1.405(5) . ?
C24 H7 0.9300 . ?
C18 C19 1.396(5) . ?
C2 C8 1.398(5) . ?
C7 O20 1.239(5) . ?
C7 O21 1.267(5) . ?
C7 C6 1.479(6) . ?
C7 Tm4 2.768(4) 5_666 ?
C29 C27 1.383(5) . ?
C29 C30 1.385(5) . ?
C29 H12 0.9300 . ?
C25 C26 1.408(5) . ?
C25 C23 1.476(5) . ?
C22 C20 1.393(5) . ?
C22 C23 1.399(5) . ?
C22 H9 0.9300 . ?
C20 C19 1.387(5) . ?
C4 C5 1.394(5) . ?
C4 C9 1.481(5) . ?
C9 C10 1.386(5) . ?
C9 C16 1.404(5) . ?
C12 O17 1.249(5) . ?
C12 O16 1.273(5) . ?
C12 C11 1.482(5) . ?
C12 Tm2 2.759(4) 2_657 ?
C13 C11 1.392(5) . ?
C13 C14 1.408(5) . ?
C13 H6 0.9300 . ?
C16 C14 1.381(5) . ?
C16 H5 0.9300 . ?
C11 C10 1.385(5) . ?
C26 C27 1.361(5) . ?
C26 H10 0.9300 . ?
C19 H8 0.9300 . ?
C14 C15 1.515(5) . ?
C10 H4 0.9300 . ?
C8 C6 1.382(5) . ?
C8 H1 0.9300 . ?
C6 C5 1.400(6) . ?
C5 H2 0.9300 . ?
C15 O18 1.244(5) . ?
C15 O19 1.252(5) . ?
C36 O13 1.183(7) . ?
C36 O15 1.194(7) . ?
C36 H14 0.9300 . ?
C35 O12 1.158(6) . ?
C35 O26 1.244(6) . ?
C35 H13 0.9300 . ?
C33 O25 1.208(6) . ?
C33 O5 1.227(6) . ?
C33 H4A 0.9300 . ?
O11 Tm3 2.302(5) . ?
O13 Tm3 2.266(4) . ?
O4 Tm1 2.243(3) . ?
O23 Tm1 2.460(3) 2_657 ?
O7 Tm2 2.409(3) . ?
O17 Tm2 2.471(3) 2_657 ?
O1 Tm1 2.412(3) . ?
O26 Tm1 2.271(3) 3 ?
O8 Tm2 2.437(3) . ?
O19 Tm1 2.276(3) 7_556 ?
O22 Tm2 2.259(3) 7_657 ?
O3 Tm1 2.343(3) . ?
O16 Tm2 2.335(3) 2_657 ?
O24 Tm1 2.358(3) 2_657 ?
O10 Tm3 2.363(3) . ?
O9 Tm3 2.428(3) . ?
O2 Tm1 2.398(3) . ?
O18 Tm2 2.224(3) 1_454 ?
O5 Tm2 2.276(3) . ?
O21 Tm4 2.415(3) 5_666 ?
O25 Tm4 2.249(3) 7_657 ?
O12 Tm3 2.254(3) . ?
O15 Tm4 2.268(4) . ?
O14 Tm4 2.329(5) . ?
O6 Tm2 2.340(3) . ?
O20 Tm4 2.358(3) 5_666 ?
Tm1 O26 2.271(3) 3_445 ?
Tm1 O19 2.276(3) 7_556 ?
Tm1 O24 2.358(3) 2_657 ?
Tm1 O23 2.460(3) 2_657 ?
Tm1 C21 2.775(4) 2_657 ?
Tm2 O18 2.224(3) 1_656 ?
Tm2 O22 2.259(3) 7_657 ?
Tm2 O16 2.335(3) 2_657 ?
Tm2 O17 2.471(3) 2_657 ?
Tm2 C12 2.759(4) 2_657 ?
Tm3 O12 2.254(3) 6_565 ?
Tm3 O10 2.363(3) 6_565 ?
Tm3 O9 2.428(3) 6_565 ?
Tm3 C31 2.757(4) 6_565 ?
Tm4 O25 2.249(3) 7_657 ?
Tm4 O25 2.249(3) 4_657 ?
Tm4 O20 2.358(3) 2_656 ?
Tm4 O20 2.358(3) 5_666 ?
Tm4 O21 2.415(3) 2_656 ?
Tm4 O21 2.415(3) 5_666 ?
Tm4 C7 2.768(4) 2_656 ?
Tm4 C7 2.768(4) 5_666 ?

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
O11 C34 O11 180.0(3) . 5_767 ?
O23 C21 O24 120.2(4) . . ?
O23 C21 C20 120.1(3) . . ?
O24 C21 C20 119.7(4) . . ?
O23 C21 Tm1 62.4(2) . 2_657 ?
O24 C21 Tm1 57.8(2) . 2_657 ?
C20 C21 Tm1 175.7(3) . 2_657 ?
O22 C17 O4 123.3(3) . . ?
O22 C17 C18 117.5(3) . . ?
O4 C17 C18 119.1(3) . . ?
O1 C1 O2 120.0(3) . . ?
O1 C1 C2 120.4(4) . . ?
O2 C1 C2 119.6(4) . . ?
C2 C3 C4 121.6(4) . . ?
C2 C3 H3 125(2) . . ?
C4 C3 H3 113(2) . . ?
O9 C31 O10 120.4(4) . . ?
O9 C31 C30 120.6(4) . . ?
O10 C31 C30 119.0(3) . . ?
O7 C28 O8 121.3(3) . . ?
O7 C28 C27 119.2(4) . . ?
O8 C28 C27 119.5(4) . . ?
C25 C32 C30 121.6(4) . . ?
C25 C32 H11 119.2 . . ?
C30 C32 H11 119.2 . . ?
C18 C24 C23 121.5(3) . . ?
C18 C24 H7 119.3 . . ?
C23 C24 H7 119.3 . . ?
C24 C18 C19 119.7(3) . . ?
C24 C18 C17 120.4(3) . . ?
C19 C18 C17 119.7(3) . . ?
C3 C2 C8 120.1(4) . . ?
C3 C2 C1 118.0(4) . . ?
C8 C2 C1 121.8(4) . . ?
O20 C7 O21 118.6(4) . . ?
O20 C7 C6 120.3(4) . . ?
O21 C7 C6 121.1(4) . . ?
O20 C7 Tm4 58.0(2) . 5_666 ?
O21 C7 Tm4 60.7(2) . 5_666 ?
C6 C7 Tm4 176.0(3) . 5_666 ?
C27 C29 C30 120.5(4) . . ?
C27 C29 H12 119.8 . . ?
C30 C29 H12 119.8 . . ?
C32 C25 C26 116.4(4) . . ?
C32 C25 C23 123.3(3) . . ?
C26 C25 C23 120.3(4) . . ?
C20 C22 C23 121.7(4) . . ?
C20 C22 H9 119.1 . . ?
C23 C22 H9 119.1 . . ?
C19 C20 C22 119.7(4) . . ?
C19 C20 C21 120.5(4) . . ?
C22 C20 C21 119.8(3) . . ?
C5 C4 C3 117.5(4) . . ?
C5 C4 C9 122.2(3) . . ?
C3 C4 C9 120.3(4) . . ?
C10 C9 C16 118.0(4) . . ?
C10 C9 C4 119.7(3) . . ?
C16 C9 C4 122.4(3) . . ?
O17 C12 O16 120.9(4) . . ?
O17 C12 C11 120.9(4) . . ?
O16 C12 C11 118.2(4) . . ?
O17 C12 Tm2 63.5(2) . 2_657 ?
O16 C12 Tm2 57.4(2) . 2_657 ?
C11 C12 Tm2 174.5(3) . 2_657 ?
C11 C13 C14 119.4(4) . . ?
C11 C13 H6 120.3 . . ?
C14 C13 H6 120.3 . . ?
C14 C16 C9 120.9(4) . . ?
C14 C16 H5 119.5 . . ?
C9 C16 H5 119.5 . . ?
C22 C23 C24 117.3(4) . . ?
C22 C23 C25 119.4(3) . . ?
C24 C23 C25 123.3(3) . . ?
C29 C30 C32 119.1(4) . . ?
C29 C30 C31 121.0(4) . . ?
C32 C30 C31 119.9(3) . . ?
C10 C11 C13 119.4(4) . . ?
C10 C11 C12 119.5(3) . . ?
C13 C11 C12 121.0(4) . . ?
C27 C26 C25 122.9(4) . . ?
C27 C26 H10 118.5 . . ?
C25 C26 H10 118.5 . . ?
C20 C19 C18 119.9(4) . . ?
C20 C19 H8 120.1 . . ?
C18 C19 H8 120.1 . . ?
C16 C14 C13 120.0(3) . . ?
C16 C14 C15 120.4(3) . . ?
C13 C14 C15 119.6(4) . . ?
C11 C10 C9 122.1(4) . . ?
C11 C10 H4 118.9 . . ?
C9 C10 H4 118.9 . . ?
C6 C8 C2 119.3(4) . . ?
C6 C8 H1 120.4 . . ?
C2 C8 H1 120.4 . . ?
C8 C6 C5 120.3(4) . . ?
C8 C6 C7 121.8(4) . . ?
C5 C6 C7 117.9(3) . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H2 119.4 . . ?
C6 C5 H2 119.4 . . ?
O18 C15 O19 124.0(4) . . ?
O18 C15 C14 117.6(4) . . ?
O19 C15 C14 118.4(4) . . ?
O13 C36 O15 132.0(7) . . ?
O13 C36 H14 114.0 . . ?
O15 C36 H14 114.0 . . ?
O12 C35 O26 135.0(6) . . ?
O12 C35 H13 112.5 . . ?
O26 C35 H13 112.5 . . ?
O25 C33 O5 129.7(5) . . ?
O25 C33 H4A 115.1 . . ?
O5 C33 H4A 115.1 . . ?
C34 O11 Tm3 177.9(4) . . ?
C36 O13 Tm3 146.2(5) . . ?
C17 O4 Tm1 150.2(3) . . ?
C21 O23 Tm1 90.6(2) . 2_657 ?
C28 O7 Tm2 93.4(2) . . ?
C12 O17 Tm2 89.5(2) . 2_657 ?
C1 O1 Tm1 92.9(2) . . ?
C35 O26 Tm1 137.1(3) . 3 ?
C28 O8 Tm2 91.3(2) . . ?
C15 O19 Tm1 133.6(3) . 7_556 ?
C17 O22 Tm2 134.2(3) . 7_657 ?
C12 O16 Tm2 95.2(3) . 2_657 ?
C21 O24 Tm1 95.0(2) . 2_657 ?
C31 O10 Tm3 94.0(2) . . ?
C31 O9 Tm3 91.7(3) . . ?
C1 O2 Tm1 92.7(2) . . ?
C15 O18 Tm2 156.3(3) . 1_454 ?
C33 O5 Tm2 135.3(4) . . ?
C7 O21 Tm4 92.1(2) . 5_666 ?
C33 O25 Tm4 142.8(4) . 7_657 ?
C35 O12 Tm3 161.1(4) . . ?
C36 O15 Tm4 148.7(5) . . ?
C26 C27 C29 119.4(3) . . ?
C26 C27 C28 119.3(4) . . ?
C29 C27 C28 121.3(4) . . ?
C7 O20 Tm4 95.5(3) . 5_666 ?
O4 Tm1 O26 150.13(10) . 3_445 ?
O4 Tm1 O19 107.28(11) . 7_556 ?
O26 Tm1 O19 86.96(11) 3_445 7_556 ?
O4 Tm1 O3 76.71(11) . . ?
O26 Tm1 O3 81.51(11) 3_445 . ?
O19 Tm1 O3 76.62(10) 7_556 . ?
O4 Tm1 O24 91.61(13) . 2_657 ?
O26 Tm1 O24 88.89(12) 3_445 2_657 ?
O19 Tm1 O24 148.11(10) 7_556 2_657 ?
O3 Tm1 O24 133.86(10) . 2_657 ?
O4 Tm1 O2 76.41(10) . . ?
O26 Tm1 O2 133.20(10) 3_445 . ?
O19 Tm1 O2 76.70(11) 7_556 . ?
O3 Tm1 O2 134.02(11) . . ?
O24 Tm1 O2 83.36(11) 2_657 . ?
O4 Tm1 O1 129.04(10) . . ?
O26 Tm1 O1 79.42(10) 3_445 . ?
O19 Tm1 O1 75.35(10) 7_556 . ?
O3 Tm1 O1 146.70(11) . . ?
O24 Tm1 O1 72.81(10) 2_657 . ?
O2 Tm1 O1 54.17(9) . . ?
O4 Tm1 O23 80.66(10) . 2_657 ?
O26 Tm1 O23 75.51(10) 3_445 2_657 ?
O19 Tm1 O23 152.39(10) 7_556 2_657 ?
O3 Tm1 O23 79.77(10) . 2_657 ?
O24 Tm1 O23 54.18(9) 2_657 2_657 ?
O2 Tm1 O23 130.73(11) . 2_657 ?
O1 Tm1 O23 120.78(9) . 2_657 ?
O4 Tm1 C21 86.27(12) . 2_657 ?
O26 Tm1 C21 80.68(12) 3_445 2_657 ?
O19 Tm1 C21 166.44(12) 7_556 2_657 ?
O3 Tm1 C21 106.79(11) . 2_657 ?
O24 Tm1 C21 27.17(10) 2_657 2_657 ?
O2 Tm1 C21 107.90(12) . 2_657 ?
O1 Tm1 C21 96.76(11) . 2_657 ?
O23 Tm1 C21 27.02(10) 2_657 2_657 ?
O18 Tm2 O22 106.61(12) 1_656 7_657 ?
O18 Tm2 O5 154.68(11) 1_656 . ?
O22 Tm2 O5 86.19(11) 7_657 . ?
O18 Tm2 O16 89.61(13) 1_656 2_657 ?
O22 Tm2 O16 152.97(10) 7_657 2_657 ?
O5 Tm2 O16 87.80(13) . 2_657 ?
O18 Tm2 O6 79.41(15) 1_656 . ?
O22 Tm2 O6 75.67(11) 7_657 . ?
O5 Tm2 O6 82.92(14) . . ?
O16 Tm2 O6 129.60(11) 2_657 . ?
O18 Tm2 O7 127.98(11) 1_656 . ?
O22 Tm2 O7 78.81(10) 7_657 . ?
O5 Tm2 O7 75.25(10) . . ?
O16 Tm2 O7 74.18(10) 2_657 . ?
O6 Tm2 O7 147.29(12) . . ?
O18 Tm2 O8 76.58(10) 1_656 . ?
O22 Tm2 O8 76.57(10) 7_657 . ?
O5 Tm2 O8 128.35(10) . . ?
O16 Tm2 O8 86.75(10) 2_657 . ?
O6 Tm2 O8 135.90(12) . . ?
O7 Tm2 O8 53.91(9) . . ?
O18 Tm2 O17 80.47(11) 1_656 2_657 ?
O22 Tm2 O17 148.28(10) 7_657 2_657 ?
O5 Tm2 O17 77.61(11) . 2_657 ?
O16 Tm2 O17 54.23(10) 2_657 2_657 ?
O6 Tm2 O17 75.40(10) . 2_657 ?
O7 Tm2 O17 121.82(10) . 2_657 ?
O8 Tm2 O17 134.55(10) . 2_657 ?
O18 Tm2 C12 85.16(12) 1_656 2_657 ?
O22 Tm2 C12 167.22(12) 7_657 2_657 ?
O5 Tm2 C12 81.04(13) . 2_657 ?
O16 Tm2 C12 27.34(11) 2_657 2_657 ?
O6 Tm2 C12 102.32(12) . 2_657 ?
O7 Tm2 C12 98.05(11) . 2_657 ?
O8 Tm2 C12 111.77(12) . 2_657 ?
O17 Tm2 C12 26.91(11) 2_657 2_657 ?
O12 Tm3 O12 106.1(2) 6_565 . ?
O12 Tm3 O13 73.42(12) 6_565 . ?
O12 Tm3 O13 73.42(12) . . ?
O12 Tm3 O11 81.22(13) 6_565 . ?
O12 Tm3 O11 81.22(13) . . ?
O13 Tm3 O11 136.94(18) . . ?
O12 Tm3 O10 158.09(12) 6_565 6_565 ?
O12 Tm3 O10 82.94(14) . 6_565 ?
O13 Tm3 O10 128.48(10) . 6_565 ?
O11 Tm3 O10 80.54(12) . 6_565 ?
O12 Tm3 O10 82.94(14) 6_565 . ?
O12 Tm3 O10 158.09(12) . . ?
O13 Tm3 O10 128.48(10) . . ?
O11 Tm3 O10 80.54(12) . . ?
O10 Tm3 O10 82.19(17) 6_565 . ?
O12 Tm3 O9 145.52(12) 6_565 6_565 ?
O12 Tm3 O9 83.76(15) . 6_565 ?
O13 Tm3 O9 78.27(12) . 6_565 ?
O11 Tm3 O9 133.26(11) . 6_565 ?
O10 Tm3 O9 53.75(10) 6_565 6_565 ?
O10 Tm3 O9 100.14(12) . 6_565 ?
O12 Tm3 O9 83.76(15) 6_565 . ?
O12 Tm3 O9 145.52(12) . . ?
O13 Tm3 O9 78.27(12) . . ?
O11 Tm3 O9 133.26(11) . . ?
O10 Tm3 O9 100.14(12) 6_565 . ?
O10 Tm3 O9 53.75(10) . . ?
O9 Tm3 O9 71.43(18) 6_565 . ?
O12 Tm3 C31 168.25(15) 6_565 6_565 ?
O12 Tm3 C31 83.44(14) . 6_565 ?
O13 Tm3 C31 103.60(12) . 6_565 ?
O11 Tm3 C31 107.44(12) . 6_565 ?
O10 Tm3 C31 27.20(10) 6_565 6_565 ?
O10 Tm3 C31 90.55(12) . 6_565 ?
O9 Tm3 C31 26.58(10) 6_565 6_565 ?
O9 Tm3 C31 84.50(13) . 6_565 ?
O25 Tm4 O25 95.7(2) 7_657 4_657 ?
O25 Tm4 O15 78.27(12) 7_657 . ?
O25 Tm4 O15 78.27(12) 4_657 . ?
O25 Tm4 O14 80.37(13) 7_657 . ?
O25 Tm4 O14 80.37(13) 4_657 . ?
O15 Tm4 O14 147.94(19) . . ?
O25 Tm4 O20 87.53(15) 7_657 2_656 ?
O25 Tm4 O20 150.21(12) 4_657 2_656 ?
O15 Tm4 O20 73.40(12) . 2_656 ?
O14 Tm4 O20 129.23(11) . 2_656 ?
O25 Tm4 O20 150.21(12) 7_657 5_666 ?
O25 Tm4 O20 87.53(15) 4_657 5_666 ?
O15 Tm4 O20 73.40(12) . 5_666 ?
O14 Tm4 O20 129.23(11) . 5_666 ?
O20 Tm4 O20 75.8(2) 2_656 5_666 ?
O25 Tm4 O21 86.56(14) 7_657 2_656 ?
O25 Tm4 O21 155.95(12) 4_657 2_656 ?
O15 Tm4 O21 125.44(11) . 2_656 ?
O14 Tm4 O21 76.39(12) . 2_656 ?
O20 Tm4 O21 53.66(10) 2_656 2_656 ?
O20 Tm4 O21 102.38(14) 5_666 2_656 ?
O25 Tm4 O21 155.95(12) 7_657 5_666 ?
O25 Tm4 O21 86.56(14) 4_657 5_666 ?
O15 Tm4 O21 125.44(11) . 5_666 ?
O14 Tm4 O21 76.39(12) . 5_666 ?
O20 Tm4 O21 102.38(14) 2_656 5_666 ?
O20 Tm4 O21 53.66(10) 5_666 5_666 ?
O21 Tm4 O21 82.07(18) 2_656 5_666 ?
O25 Tm4 C7 87.59(13) 7_657 2_656 ?
O25 Tm4 C7 175.44(14) 4_657 2_656 ?
O15 Tm4 C7 99.33(12) . 2_656 ?
O14 Tm4 C7 103.37(13) . 2_656 ?
O20 Tm4 C7 26.47(10) 2_656 2_656 ?
O20 Tm4 C7 88.07(14) 5_666 2_656 ?
O21 Tm4 C7 27.22(10) 2_656 2_656 ?
O21 Tm4 C7 91.78(12) 5_666 2_656 ?
O25 Tm4 C7 175.44(14) 7_657 5_666 ?
O25 Tm4 C7 87.59(13) 4_657 5_666 ?
O15 Tm4 C7 99.33(12) . 5_666 ?
O14 Tm4 C7 103.37(13) . 5_666 ?
O20 Tm4 C7 88.07(14) 2_656 5_666 ?
O20 Tm4 C7 26.47(10) 5_666 5_666 ?
O21 Tm4 C7 91.78(12) 2_656 5_666 ?
O21 Tm4 C7 27.22(10) 5_666 5_666 ?
C7 Tm4 C7 88.99(18) 2_656 5_666 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.804
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.151
# SQUEEZE RESULTS 
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 -0.007 -0.015 -0.011 6050.8 1051.2
2 0.000 0.356 0.000 39.9 16.4
3 0.000 0.644 0.000 40.5 17.0
4 0.500 0.144 0.000 40.5 17.0
5 0.500 0.856 0.000 39.9 16.4
_platon_squeeze_details          
;
;
#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939025'
#######################################################################
#
#                 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          'not measured'
_chemical_formula_moiety         'C16 H6 Nd O10'
_chemical_formula_sum            'C16 H6 Nd O10 '
_chemical_formula_weight         502.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   c2/c

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

_cell_length_a                   12.143(2)
_cell_length_b                   24.875(5)
_cell_length_c                   19.669(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.90(3)
_cell_angle_gamma                90.00
_cell_volume                     5791(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4383
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.50

_exptl_crystal_description       sheet
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_T_max  0.634
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6601
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6601
_reflns_number_gt                5339
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0882P)²+19.8408P] 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         6601
_refine_ls_number_parameters     244
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1536
_refine_ls_wR_factor_gt          0.1486
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.442
_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
C16 C 0.5375(13) 0.3738(6) 0.0325(10) 0.129(8) Uani 1 1 d D . .
C12 C 0.2730(13) 0.2818(6) 0.0115(10) 0.109(5) Uani 1 1 d DU . .
C1 C -0.2028(5) 0.4673(3) 0.1621(3) 0.0235(13) Uani 1 1 d . . .
C2 C -0.2636(5) 0.4818(3) 0.2185(3) 0.0232(13) Uani 1 1 d . . .
C3 C -0.3807(5) 0.4821(3) 0.2052(3) 0.0264(14) Uani 1 1 d . . .
H3 H -0.4221 0.4732 0.1609 0.032 Uiso 1 1 calc R . .
C4 C -0.4377(5) 0.4955(3) 0.2574(3) 0.0227(13) Uani 1 1 d . . .
C8 C -0.1913(5) 0.5186(3) 0.4101(3) 0.0245(14) Uani 1 1 d . . .
C9 C 0.1123(7) 0.4120(3) -0.0355(5) 0.0413(19) Uani 1 1 d . . .
C5 C -0.3735(5) 0.5083(3) 0.3233(3) 0.0224(13) Uani 1 1 d . . .
H5 H -0.4096 0.5184 0.3583 0.027 Uiso 1 1 calc R . .
C7 C -0.2006(5) 0.4931(3) 0.2853(3) 0.0245(13) Uani 1 1 d . . .
H7 H -0.1221 0.4919 0.2948 0.029 Uiso 1 1 calc R . .
C6 C -0.2562(5) 0.5061(3) 0.3375(3) 0.0228(13) Uani 1 1 d . . .
C10 C 0.2063(11) 0.3708(4) -0.0213(11) 0.114(7) Uani 1 1 d . . .
C11 C 0.1827(11) 0.3172(4) -0.0136(10) 0.122(8) Uani 1 1 d D . .
H11 H 0.1086 0.3047 -0.0247 0.146 Uiso 1 1 calc R . .
C14 C 0.4158(10) 0.3562(6) 0.0237(11) 0.108(6) Uani 1 1 d D . .
C15 C 0.3246(9) 0.3898(4) -0.0024(7) 0.066(3) Uani 1 1 d . . .
H15 H 0.3388 0.4261 -0.0082 0.079 Uiso 1 1 calc R . .
Nd1 Nd -0.07944(2) 0.449539(14) 0.055232(16) 0.02063(15) Uani 1 1 d . . .
O4 O -0.2369(4) 0.5457(2) 0.4496(3) 0.0355(13) Uani 1 1 d . . .
O9 O 0.0597(6) 0.3899(3) 0.1368(4) 0.071(2) Uani 1 1 d . . .
O3 O -0.0917(4) 0.5013(2) 0.4297(2) 0.0313(11) Uani 1 1 d . . .
O5 O 0.0250(4) 0.3993(2) -0.0162(3) 0.0378(12) Uani 1 1 d . . .
O2 O -0.2582(4) 0.4532(2) 0.1030(3) 0.0366(13) Uani 1 1 d . . .
O1 O -0.0972(4) 0.4686(3) 0.1757(3) 0.0377(13) Uani 1 1 d . . .
O6 O 0.1360(5) 0.4565(2) -0.0571(3) 0.0368(13) Uani 1 1 d . . .
O10 O -0.1618(5) 0.3588(3) 0.0485(4) 0.0567(17) Uani 1 1 d . . .
O8 O 0.5349(11) 0.4206(6) 0.0375(6) 0.124(4) Uani 1 1 d . . .
O7 O 0.6105(7) 0.3411(4) 0.0463(7) 0.108(4) Uani 1 1 d . . .
C13 C 0.3911(13) 0.3019(6) 0.0311(9) 0.100(4) Uani 1 1 d U . .
H13 H 0.4494 0.2780 0.0486 0.120 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C16 O8 1.169(17) . ?
C16 O7 1.189(15) . ?
C16 C14 1.513(17) . ?
C12 C11 1.407(16) . ?
C12 C13 1.49(2) . ?
C12 C12 1.71(3) 7 ?
C1 O1 1.251(8) . ?
C1 O2 1.257(8) . ?
C1 C2 1.506(8) . ?
C2 C3 1.388(8) . ?
C2 C7 1.393(9) . ?
C3 C4 1.400(9) . ?
C4 C5 1.392(9) . ?
C4 C4 1.476(11) 2_455 ?
C8 O4 1.248(8) . ?
C8 O3 1.261(8) . ?
C8 C6 1.500(9) . ?
C8 Nd1 2.983(6) 6_566 ?
C9 O6 1.242(9) . ?
C9 O5 1.244(9) . ?
C9 C10 1.512(13) . ?
C5 C6 1.390(8) . ?
C7 C6 1.387(9) . ?
C10 C11 1.379(13) . ?
C10 C15 1.479(17) . ?
C14 C15 1.391(16) . ?
C14 C13 1.398(19) . ?
Nd1 O3 2.406(5) 2 ?
Nd1 O5 2.438(5) . ?
Nd1 O6 2.439(5) 5_565 ?
Nd1 O10 2.459(6) . ?
Nd1 O1 2.473(5) . ?
Nd1 O4 2.493(5) 6_565 ?
Nd1 O9 2.533(7) . ?
Nd1 O2 2.552(5) . ?
Nd1 O3 2.730(5) 6_565 ?
Nd1 C8 2.983(6) 6_565 ?
Nd1 Nd1 4.0765(10) 5_565 ?
O4 Nd1 2.493(5) 6_566 ?
O3 Nd1 2.406(5) 2 ?
O3 Nd1 2.730(5) 6_566 ?
O6 Nd1 2.439(5) 5_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 C16 O7 134.0(16) . . ?
O8 C16 C14 104.7(14) . . ?
O7 C16 C14 119.2(14) . . ?
C11 C12 C13 120.8(13) . . ?
C11 C12 C12 107.7(16) . 7 ?
C13 C12 C12 128.4(14) . 7 ?
O1 C1 O2 121.1(6) . . ?
O1 C1 C2 119.0(6) . . ?
O2 C1 C2 119.9(6) . . ?
C3 C2 C7 120.0(6) . . ?
C3 C2 C1 120.8(6) . . ?
C7 C2 C1 119.1(5) . . ?
C2 C3 C4 121.1(6) . . ?
C5 C4 C3 118.1(5) . . ?
C5 C4 C4 121.3(7) . 2_455 ?
C3 C4 C4 120.6(7) . 2_455 ?
O4 C8 O3 121.5(6) . . ?
O4 C8 C6 119.5(6) . . ?
O3 C8 C6 119.0(6) . . ?
O4 C8 Nd1 55.3(3) . 6_566 ?
O3 C8 Nd1 66.2(3) . 6_566 ?
C6 C8 Nd1 174.7(5) . 6_566 ?
O6 C9 O5 127.4(7) . . ?
O6 C9 C10 116.4(7) . . ?
O5 C9 C10 115.6(8) . . ?
C6 C5 C4 121.0(6) . . ?
C6 C7 C2 119.3(6) . . ?
C7 C6 C5 120.4(6) . . ?
C7 C6 C8 120.9(5) . . ?
C5 C6 C8 118.7(6) . . ?
C11 C10 C15 119.7(12) . . ?
C11 C10 C9 120.5(10) . . ?
C15 C10 C9 118.7(9) . . ?
C10 C11 C12 118.6(13) . . ?
C15 C14 C13 116.5(12) . . ?
C15 C14 C16 123.1(12) . . ?
C13 C14 C16 119.6(12) . . ?
C14 C15 C10 123.3(10) . . ?
O3 Nd1 O5 78.38(17) 2 . ?
O3 Nd1 O6 73.98(18) 2 5_565 ?
O5 Nd1 O6 133.19(18) . 5_565 ?
O3 Nd1 O10 145.78(19) 2 . ?
O5 Nd1 O10 75.9(2) . . ?
O6 Nd1 O10 140.1(2) 5_565 . ?
O3 Nd1 O1 92.13(18) 2 . ?
O5 Nd1 O1 144.94(19) . . ?
O6 Nd1 O1 73.6(2) 5_565 . ?
O10 Nd1 O1 96.1(2) . . ?
O3 Nd1 O4 123.91(16) 2 6_565 ?
O5 Nd1 O4 86.84(19) . 6_565 ?
O6 Nd1 O4 78.5(2) 5_565 6_565 ?
O10 Nd1 O4 76.8(2) . 6_565 ?
O1 Nd1 O4 125.12(17) . 6_565 ?
O3 Nd1 O9 78.4(2) 2 . ?
O5 Nd1 O9 72.9(2) . . ?
O6 Nd1 O9 134.6(2) 5_565 . ?
O10 Nd1 O9 72.7(2) . . ?
O1 Nd1 O9 72.1(2) . . ?
O4 Nd1 O9 146.6(2) 6_565 . ?
O3 Nd1 O2 135.87(17) 2 . ?
O5 Nd1 O2 145.66(17) . . ?
O6 Nd1 O2 72.20(18) 5_565 . ?
O10 Nd1 O2 71.58(19) . . ?
O1 Nd1 O2 51.49(16) . . ?
O4 Nd1 O2 75.39(17) 6_565 . ?
O9 Nd1 O2 106.8(2) . . ?
O3 Nd1 O3 75.10(16) 2 6_565 ?
O5 Nd1 O3 68.81(18) . 6_565 ?
O6 Nd1 O3 67.99(18) 5_565 6_565 ?
O10 Nd1 O3 115.0(2) . 6_565 ?
O1 Nd1 O3 141.47(19) . 6_565 ?
O4 Nd1 O3 49.29(15) 6_565 6_565 ?
O9 Nd1 O3 136.8(2) . 6_565 ?
O2 Nd1 O3 115.94(16) . 6_565 ?
O3 Nd1 C8 99.91(17) 2 6_565 ?
O5 Nd1 C8 76.64(19) . 6_565 ?
O6 Nd1 C8 71.9(2) 5_565 6_565 ?
O10 Nd1 C8 95.7(2) . 6_565 ?
O1 Nd1 C8 138.43(18) . 6_565 ?
O4 Nd1 C8 24.29(17) 6_565 6_565 ?
O9 Nd1 C8 149.2(2) . 6_565 ?
O2 Nd1 C8 95.70(17) . 6_565 ?
O3 Nd1 C8 25.00(15) 6_565 6_565 ?
O3 Nd1 Nd1 40.33(12) 2 5_565 ?
O5 Nd1 Nd1 68.84(13) . 5_565 ?
O6 Nd1 Nd1 65.56(12) 5_565 5_565 ?
O10 Nd1 Nd1 140.48(17) . 5_565 ?
O1 Nd1 Nd1 123.09(15) . 5_565 ?
O4 Nd1 Nd1 83.83(12) 6_565 5_565 ?
O9 Nd1 Nd1 111.7(2) . 5_565 ?
O2 Nd1 Nd1 135.77(14) . 5_565 ?
O3 Nd1 Nd1 34.77(10) 6_565 5_565 ?
C8 Nd1 Nd1 59.64(13) 6_565 5_565 ?
C8 O4 Nd1 100.4(4) . 6_566 ?
C8 O3 Nd1 164.6(5) . 2 ?
C8 O3 Nd1 88.8(4) . 6_566 ?
Nd1 O3 Nd1 104.90(16) 2 6_566 ?
C9 O5 Nd1 129.4(5) . . ?
C1 O2 Nd1 91.5(4) . . ?
C1 O1 Nd1 95.4(4) . . ?
C9 O6 Nd1 139.6(5) . 5_565 ?
C14 C13 C12 121.0(13) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         3.297
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.164
# 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 -0.082 0.250 0.011 1450.9 45.8
2 0.020 0.750 0.062 1450.9 45.8
_platon_squeeze_details          
;
;
#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939026'
#######################################################################
#
#                 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          'not measured '
_chemical_formula_moiety         'C48 H18 Eu3 O26'
_chemical_formula_sum            'C48 H18 Eu3 O26'
_chemical_formula_weight         1440.38

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.660(2)
_cell_length_b                   12.245(2)
_cell_length_c                   13.568(3)
_cell_angle_alpha                64.88(3)
_cell_angle_beta                 68.25(3)
_cell_angle_gamma                88.14(3)
_cell_volume                     1611.1(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4838
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.47

_exptl_crystal_description       sheet
_exptl_crystal_colour            coloress
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             681
_exptl_absorpt_coefficient_mu    2.952
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7269
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7269
_reflns_number_gt                6152
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0374P)²+6.8670P] 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         7269
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.005
_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 0.0000 0.0000 0.0000 0.00916(8) Uani 1 2 d S . .
Eu2 Eu 0.07117(2) 0.17060(2) 0.17231(2) 0.01055(8) Uani 1 1 d . . .
O1 O 0.2100(3) 0.1936(3) -0.0201(3) 0.0209(8) Uani 1 1 d . . .
O3 O 0.0281(3) -0.0299(3) 0.1863(3) 0.0169(7) Uani 1 1 d . . .
O5 O 0.9343(3) 0.1573(3) 0.0559(3) 0.0134(7) Uani 1 1 d . . .
O6 O -0.0593(4) -0.1287(3) 0.6286(3) 0.0213(8) Uani 1 1 d . . .
O9 O 0.7660(3) -0.0555(3) -0.2083(3) 0.0159(7) Uani 1 1 d . . .
O11 O 0.0013(4) -0.3004(3) 0.7234(3) 0.0243(8) Uani 1 1 d . . .
O12 O 0.9767(3) 0.3313(3) 0.0549(3) 0.0191(8) Uani 1 1 d . . .
O13 O 0.7628(3) 0.6764(3) -0.0976(3) 0.0210(8) Uani 1 1 d . . .
O17 O -0.0410(4) -0.1889(3) 0.1804(3) 0.0244(8) Uani 1 1 d . . .
O18 O 0.2148(3) 0.0465(3) -0.0751(4) 0.0252(9) Uani 1 1 d . . .
O20 O 0.6434(4) 0.6723(4) -0.1914(4) 0.0271(9) Uani 1 1 d . . .
O21 O -0.1443(4) 0.0960(5) 0.3046(4) 0.0387(12) Uani 1 1 d . . .
C2 C -0.0068(4) -0.1440(4) 0.2337(4) 0.0120(9) Uani 1 1 d . . .
C3 C -0.0062(4) -0.2264(4) 0.3518(4) 0.0145(9) Uani 1 1 d . . .
C4 C 0.7108(5) 0.6230(5) -0.1345(5) 0.0185(10) Uani 1 1 d . . .
C7 C 0.2677(4) 0.1264(5) -0.0644(4) 0.0146(10) Uani 1 1 d . . .
C8 C 0.4081(4) 0.1387(4) -0.1067(4) 0.0119(9) Uani 1 1 d . . .
C9 C 0.4671(4) 0.0517(4) -0.1420(4) 0.0134(9) Uani 1 1 d . . .
H9 H 0.4215 -0.0041 -0.1484 0.016 Uiso 1 1 calc R . .
C10 C 0.5917(4) 0.0495(4) -0.1668(4) 0.0128(9) Uani 1 1 d . . .
C11 C 0.6600(4) 0.1331(4) -0.1582(4) 0.0126(9) Uani 1 1 d . . .
H11 H 0.7452 0.1320 -0.1777 0.015 Uiso 1 1 calc R . .
C12 C 0.6039(4) 0.2193(4) -0.1209(4) 0.0111(9) Uani 1 1 d . . .
C13 C 0.4754(4) 0.2212(4) -0.0967(4) 0.0109(9) Uani 1 1 d . . .
H13 H 0.4357 0.2788 -0.0738 0.013 Uiso 1 1 calc R . .
C14 C -0.0234(5) -0.2293(5) 0.6364(4) 0.0170(10) Uani 1 1 d . . .
C15 C 0.9211(4) 0.2686(4) 0.0292(4) 0.0124(9) Uani 1 1 d . . .
C17 C 0.6533(5) -0.0519(4) -0.1913(4) 0.0150(10) Uani 1 1 d . . .
C18 C -0.0098(5) -0.1844(5) 0.4330(4) 0.0153(10) Uani 1 1 d . . .
H18 H -0.0107 -0.1023 0.4150 0.018 Uiso 1 1 calc R . .
O30 O 0.5813(3) -0.1304(3) -0.1911(4) 0.0215(8) Uani 1 1 d . . .
C21 C -0.0039(5) -0.3498(5) 0.3798(4) 0.0176(10) Uani 1 1 d . . .
H21 H -0.0032 -0.3760 0.3245 0.021 Uiso 1 1 calc R . .
C22 C -0.0027(5) -0.4348(5) 0.4865(5) 0.0183(10) Uani 1 1 d . . .
C24 C -0.0083(5) -0.3912(5) 0.5679(5) 0.0212(11) Uani 1 1 d . . .
H24 H -0.0095 -0.4457 0.6414 0.025 Uiso 1 1 calc R . .
C25 C -0.0120(5) -0.2692(5) 0.5424(4) 0.0187(10) Uani 1 1 d . . .
C26 C 0.8162(5) 0.4438(5) -0.0599(5) 0.0163(10) Uani 1 1 d . . .
H26 H 0.8634 0.4924 -0.0472 0.020 Uiso 1 1 calc R . .
C27 C 0.8331(5) 0.3231(5) -0.0302(4) 0.0162(10) Uani 1 1 d . . .
C28 C 0.7635(4) 0.2511(5) -0.0512(4) 0.0152(10) Uani 1 1 d . . .
H28 H 0.7746 0.1700 -0.0315 0.018 Uiso 1 1 calc R . .
C29 C 0.6770(4) 0.2996(4) -0.1016(4) 0.0116(9) Uani 1 1 d . . .
C30 C 0.6590(5) 0.4215(5) -0.1288(5) 0.0175(10) Uani 1 1 d . . .
H30 H 0.6003 0.4541 -0.1602 0.021 Uiso 1 1 calc R . .
C31 C 0.7294(5) 0.4932(4) -0.1084(5) 0.0181(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O18 2.311(4) 2 ?
Eu1 O18 2.311(4) . ?
Eu1 O5 2.363(3) 1_455 ?
Eu1 O5 2.363(3) 2_655 ?
Eu1 O17 2.443(4) 2 ?
Eu1 O17 2.443(4) . ?
Eu1 O3 2.539(3) . ?
Eu1 O3 2.539(3) 2 ?
Eu1 C2 2.871(5) 2 ?
Eu1 C7 3.170(5) 2 ?
Eu1 Eu2 4.0267(9) 2 ?
Eu2 O13 2.335(4) 2_665 ?
Eu2 O9 2.399(3) 2_655 ?
Eu2 O21 2.405(4) . ?
Eu2 O1 2.405(4) . ?
Eu2 O3 2.435(3) . ?
Eu2 O12 2.474(3) 1_455 ?
Eu2 O6 2.476(3) 2_556 ?
Eu2 O11 2.486(3) 2_556 ?
Eu2 O5 2.679(3) 1_455 ?
Eu2 C14 2.837(5) 2_556 ?
Eu2 C15 2.945(5) 1_455 ?
O1 C7 1.257(6) . ?
O3 C2 1.269(6) . ?
O5 C15 1.273(6) . ?
O5 Eu1 2.363(3) 1_655 ?
O5 Eu2 2.679(3) 1_655 ?
O6 C14 1.262(6) . ?
O6 Eu2 2.476(3) 2_556 ?
O9 C17 1.250(6) . ?
O9 Eu2 2.399(3) 2_655 ?
O11 C14 1.264(6) . ?
O11 Eu2 2.486(3) 2_556 ?
O12 C15 1.248(6) . ?
O12 Eu2 2.474(3) 1_655 ?
O13 C4 1.256(6) . ?
O13 Eu2 2.335(4) 2_665 ?
O17 C2 1.244(6) . ?
O18 C7 1.259(6) . ?
O20 C4 1.265(6) . ?
C2 C3 1.491(6) . ?
C3 C21 1.395(7) . ?
C3 C18 1.387(6) . ?
C4 C31 1.502(6) . ?
C7 C8 1.509(6) . ?
C8 C13 1.379(6) . ?
C8 C9 1.407(6) . ?
C9 C10 1.367(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(6) . ?
C10 C17 1.511(6) . ?
C11 C12 1.400(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.412(6) . ?
C12 C29 1.484(6) . ?
C13 H13 0.9300 . ?
C14 C25 1.511(6) . ?
C14 Eu2 2.837(5) 2_556 ?
C15 C27 1.503(6) . ?
C15 Eu2 2.945(5) 1_655 ?
C17 O30 1.295(6) . ?
C18 C25 1.395(7) . ?
C18 H18 0.9300 . ?
C21 C22 1.384(7) . ?
C21 H21 0.9300 . ?
C22 C24 1.398(7) . ?
C22 C22 1.483(10) 2_546 ?
C24 C25 1.387(7) . ?
C24 H24 0.9300 . ?
C26 C27 1.386(7) . ?
C26 C31 1.393(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.397(7) . ?
C28 C29 1.401(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.407(6) . ?
C30 C31 1.393(7) . ?
C30 H30 0.9300 . ?

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
O18 Eu1 O18 180.00(7) 2 . ?
O18 Eu1 O5 78.28(12) 2 1_455 ?
O18 Eu1 O5 101.72(12) . 1_455 ?
O18 Eu1 O5 101.72(12) 2 2_655 ?
O18 Eu1 O5 78.28(12) . 2_655 ?
O5 Eu1 O5 180.0(3) 1_455 2_655 ?
O18 Eu1 O17 101.85(15) 2 2 ?
O18 Eu1 O17 78.15(15) . 2 ?
O5 Eu1 O17 72.06(12) 1_455 2 ?
O5 Eu1 O17 107.94(12) 2_655 2 ?
O18 Eu1 O17 78.15(15) 2 . ?
O18 Eu1 O17 101.85(15) . . ?
O5 Eu1 O17 107.94(12) 1_455 . ?
O5 Eu1 O17 72.06(12) 2_655 . ?
O17 Eu1 O17 180.00(18) 2 . ?
O18 Eu1 O3 99.85(14) 2 . ?
O18 Eu1 O3 80.15(14) . . ?
O5 Eu1 O3 67.34(11) 1_455 . ?
O5 Eu1 O3 112.66(11) 2_655 . ?
O17 Eu1 O3 128.30(11) 2 . ?
O17 Eu1 O3 51.70(11) . . ?
O18 Eu1 O3 80.15(14) 2 2 ?
O18 Eu1 O3 99.85(14) . 2 ?
O5 Eu1 O3 112.66(11) 1_455 2 ?
O5 Eu1 O3 67.34(11) 2_655 2 ?
O17 Eu1 O3 51.70(11) 2 2 ?
O17 Eu1 O3 128.30(11) . 2 ?
O3 Eu1 O3 180.00(4) . 2 ?
O18 Eu1 C2 90.66(15) 2 2 ?
O18 Eu1 C2 89.34(15) . 2 ?
O5 Eu1 C2 91.77(12) 1_455 2 ?
O5 Eu1 C2 88.23(12) 2_655 2 ?
O17 Eu1 C2 25.49(12) 2 2 ?
O17 Eu1 C2 154.51(12) . 2 ?
O3 Eu1 C2 153.77(12) . 2 ?
O3 Eu1 C2 26.23(12) 2 2 ?
O18 Eu1 C7 19.59(13) 2 2 ?
O18 Eu1 C7 160.41(13) . 2 ?
O5 Eu1 C7 97.60(12) 1_455 2 ?
O5 Eu1 C7 82.40(12) 2_655 2 ?
O17 Eu1 C7 105.08(13) 2 2 ?
O17 Eu1 C7 74.92(13) . 2 ?
O3 Eu1 C7 110.67(12) . 2 ?
O3 Eu1 C7 69.33(12) 2 2 ?
C2 Eu1 C7 86.84(13) 2 2 ?
O18 Eu1 Eu2 73.86(10) 2 2 ?
O18 Eu1 Eu2 106.14(10) . 2 ?
O5 Eu1 Eu2 140.21(8) 1_455 2 ?
O5 Eu1 Eu2 39.79(8) 2_655 2 ?
O17 Eu1 Eu2 86.42(8) 2 2 ?
O17 Eu1 Eu2 93.58(8) . 2 ?
O3 Eu1 Eu2 144.91(8) . 2 ?
O3 Eu1 Eu2 35.09(8) 2 2 ?
C2 Eu1 Eu2 61.15(9) 2 2 ?
C7 Eu1 Eu2 55.50(9) 2 2 ?
O13 Eu2 O9 77.65(12) 2_665 2_655 ?
O13 Eu2 O21 144.17(14) 2_665 . ?
O9 Eu2 O21 121.35(16) 2_655 . ?
O13 Eu2 O1 71.88(14) 2_665 . ?
O9 Eu2 O1 75.76(12) 2_655 . ?
O21 Eu2 O1 138.71(13) . . ?
O13 Eu2 O3 140.95(12) 2_665 . ?
O9 Eu2 O3 71.13(11) 2_655 . ?
O21 Eu2 O3 74.09(15) . . ?
O1 Eu2 O3 78.09(13) . . ?
O13 Eu2 O12 86.20(12) 2_665 1_455 ?
O9 Eu2 O12 156.15(13) 2_655 1_455 ?
O21 Eu2 O12 81.77(16) . 1_455 ?
O1 Eu2 O12 82.64(12) . 1_455 ?
O3 Eu2 O12 114.36(11) . 1_455 ?
O13 Eu2 O6 86.53(13) 2_665 2_556 ?
O9 Eu2 O6 71.27(12) 2_655 2_556 ?
O21 Eu2 O6 73.76(14) . 2_556 ?
O1 Eu2 O6 143.74(13) . 2_556 ?
O3 Eu2 O6 104.49(12) . 2_556 ?
O12 Eu2 O6 125.63(12) 1_455 2_556 ?
O13 Eu2 O11 72.67(13) 2_665 2_556 ?
O9 Eu2 O11 116.82(12) 2_655 2_556 ?
O21 Eu2 O11 71.57(15) . 2_556 ?
O1 Eu2 O11 138.28(13) . 2_556 ?
O3 Eu2 O11 143.05(13) . 2_556 ?
O12 Eu2 O11 73.74(12) 1_455 2_556 ?
O6 Eu2 O11 52.74(12) 2_556 2_556 ?
O13 Eu2 O5 125.36(12) 2_665 1_455 ?
O9 Eu2 O5 128.47(10) 2_655 1_455 ?
O21 Eu2 O5 69.25(12) . 1_455 ?
O1 Eu2 O5 71.36(11) . 1_455 ?
O3 Eu2 O5 64.11(11) . 1_455 ?
O12 Eu2 O5 50.27(10) 1_455 1_455 ?
O6 Eu2 O5 142.98(12) 2_556 1_455 ?
O11 Eu2 O5 114.20(11) 2_556 1_455 ?
O13 Eu2 C14 77.16(14) 2_665 2_556 ?
O9 Eu2 C14 93.47(13) 2_655 2_556 ?
O21 Eu2 C14 71.95(14) . 2_556 ?
O1 Eu2 C14 148.70(14) . 2_556 ?
O3 Eu2 C14 126.70(14) . 2_556 ?
O12 Eu2 C14 99.98(13) 1_455 2_556 ?
O6 Eu2 C14 26.37(13) 2_556 2_556 ?
O11 Eu2 C14 26.43(13) 2_556 2_556 ?
O5 Eu2 C14 133.52(12) 1_455 2_556 ?
O13 Eu2 C15 106.88(13) 2_665 1_455 ?
O9 Eu2 C15 149.34(12) 2_655 1_455 ?
O21 Eu2 C15 72.92(15) . 1_455 ?
O1 Eu2 C15 77.05(13) . 1_455 ?
O3 Eu2 C15 89.65(12) . 1_455 ?
O12 Eu2 C15 24.72(12) 1_455 1_455 ?
O6 Eu2 C15 138.34(12) 2_556 1_455 ?
O11 Eu2 C15 93.00(12) 2_556 1_455 ?
O5 Eu2 C15 25.61(11) 1_455 1_455 ?
C14 Eu2 C15 117.18(13) 2_556 1_455 ?
C7 O1 Eu2 137.2(3) . . ?
C2 O3 Eu2 158.7(3) . . ?
C2 O3 Eu1 91.6(3) . . ?
Eu2 O3 Eu1 108.08(13) . . ?
C15 O5 Eu1 150.8(3) . 1_655 ?
C15 O5 Eu2 89.0(3) . 1_655 ?
Eu1 O5 Eu2 105.84(12) 1_655 1_655 ?
C14 O6 Eu2 93.0(3) . 2_556 ?
C17 O9 Eu2 149.5(3) . 2_655 ?
C14 O11 Eu2 92.5(3) . 2_556 ?
C15 O12 Eu2 99.3(3) . 1_655 ?
C4 O13 Eu2 139.1(4) . 2_665 ?
C2 O17 Eu1 96.9(3) . . ?
C7 O18 Eu1 122.4(3) . . ?
O17 C2 O3 119.7(4) . . ?
O17 C2 C3 118.9(4) . . ?
O3 C2 C3 121.4(4) . . ?
C21 C3 C18 120.3(4) . . ?
C21 C3 C2 117.4(4) . . ?
C18 C3 C2 122.3(4) . . ?
O13 C4 O20 123.5(4) . . ?
O13 C4 C31 117.7(4) . . ?
O20 C4 C31 118.7(4) . . ?
O18 C7 O1 123.5(4) . . ?
O18 C7 C8 116.9(4) . . ?
O1 C7 C8 119.6(4) . . ?
C13 C8 C9 120.3(4) . . ?
C13 C8 C7 121.7(4) . . ?
C9 C8 C7 117.4(4) . . ?
C10 C9 C8 119.7(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 120.2(4) . . ?
C9 C10 C17 120.3(4) . . ?
C11 C10 C17 119.2(4) . . ?
C10 C11 C12 121.6(4) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C13 117.4(4) . . ?
C11 C12 C29 120.2(4) . . ?
C13 C12 C29 122.3(4) . . ?
C8 C13 C12 120.7(4) . . ?
C8 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
O11 C14 O6 121.5(4) . . ?
O11 C14 C25 118.1(4) . . ?
O6 C14 C25 120.3(4) . . ?
O11 C14 Eu2 61.1(2) . 2_556 ?
O6 C14 Eu2 60.6(2) . 2_556 ?
C25 C14 Eu2 173.7(4) . 2_556 ?
O12 C15 O5 121.2(4) . . ?
O12 C15 C27 119.9(4) . . ?
O5 C15 C27 118.9(4) . . ?
O12 C15 Eu2 56.0(2) . 1_655 ?
O5 C15 Eu2 65.4(2) . 1_655 ?
C27 C15 Eu2 171.9(3) . 1_655 ?
O9 C17 O30 125.3(4) . . ?
O9 C17 C10 119.3(4) . . ?
O30 C17 C10 115.4(4) . . ?
C3 C18 C25 118.0(5) . . ?
C3 C18 H18 121.0 . . ?
C25 C18 H18 121.0 . . ?
C22 C21 C3 122.6(4) . . ?
C22 C21 H21 118.7 . . ?
C3 C21 H21 118.7 . . ?
C21 C22 C24 116.3(5) . . ?
C21 C22 C22 121.8(5) . 2_546 ?
C24 C22 C22 121.9(6) . 2_546 ?
C25 C24 C22 122.0(5) . . ?
C25 C24 H24 119.0 . . ?
C22 C24 H24 119.0 . . ?
C24 C25 C18 120.8(4) . . ?
C24 C25 C14 119.2(4) . . ?
C18 C25 C14 120.0(4) . . ?
C27 C26 C31 120.8(4) . . ?
C27 C26 H26 119.6 . . ?
C31 C26 H26 119.6 . . ?
C26 C27 C28 119.3(4) . . ?
C26 C27 C15 120.4(4) . . ?
C28 C27 C15 120.3(4) . . ?
C27 C28 C29 120.7(4) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C28 C29 C30 119.2(4) . . ?
C28 C29 C12 118.9(4) . . ?
C30 C29 C12 121.9(4) . . ?
C31 C30 C29 119.8(4) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C26 C31 C30 120.1(4) . . ?
C26 C31 C4 118.8(4) . . ?
C30 C31 C4 121.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         2.037
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.183
# 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 0.500 0.548 0.500 641.0 16.5
_platon_squeeze_details          
;
;
#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939027'
#######################################################################
#
#                 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          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H18 O26 Tb3 '
_chemical_formula_weight         1487.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.609(2)
_cell_length_b                   12.227(2)
_cell_length_c                   13.554(3)
_cell_angle_alpha                65.00(3)
_cell_angle_beta                 69.14(3)
_cell_angle_gamma                87.75(3)
_cell_volume                     1615.2(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4383
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.48

_exptl_crystal_description       sheet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             709
_exptl_absorpt_coefficient_mu    3.319
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6053
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16046
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7327
_reflns_number_gt                6053
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0649P)²+3.6852P] 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         7327
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_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
O13 O 0.6410(5) 0.9024(6) 0.2005(5) 0.0452(14) Uani 1 1 d . . .
O11 O 0.5619(5) 1.1299(4) -0.1306(4) 0.0282(11) Uani 1 1 d . . .
O12 O 0.4986(5) 1.3006(4) -0.2244(4) 0.0322(12) Uani 1 1 d . . .
C21 C 0.5238(6) 1.2287(5) -0.1363(5) 0.0224(13) Uani 1 1 d . . .
O5 O 1.2908(4) 0.8067(4) 0.5155(4) 0.0247(9) Uani 1 1 d . . .
O6 O 1.2891(4) 0.9537(4) 0.5705(4) 0.0287(10) Uani 1 1 d . . .
C12 C 1.2362(5) 0.8728(5) 0.5605(5) 0.0172(11) Uani 1 1 d . . .
C10 C 1.0264(5) 0.7785(5) 0.5953(5) 0.0154(11) Uani 1 1 d . . .
H8 H 1.0657 0.7211 0.5717 0.018 Uiso 1 1 calc R . .
C11 C 1.0958(5) 0.8626(5) 0.6043(5) 0.0159(11) Uani 1 1 d . . .
C13 C 1.0375(5) 0.9487(5) 0.6400(5) 0.0165(11) Uani 1 1 d . . .
H25 H 1.0836 1.0045 0.6460 0.020 Uiso 1 1 calc R . .
O8 O 0.7388(4) 1.0552(4) 0.7088(4) 0.0242(9) Uani 1 1 d . . .
O7 O 0.9202(4) 1.1299(4) 0.6919(5) 0.0292(11) Uani 1 1 d . . .
C15 C 0.8496(6) 1.0521(5) 0.6926(5) 0.0191(12) Uani 1 1 d . . .
C14 C 0.9113(5) 0.9511(5) 0.6665(5) 0.0150(11) Uani 1 1 d . . .
C16 C 0.8427(5) 0.8671(5) 0.6576(5) 0.0167(11) Uani 1 1 d . . .
H13 H 0.7576 0.8688 0.6763 0.020 Uiso 1 1 calc R . .
C9 C 0.8990(5) 0.7800(5) 0.6211(5) 0.0162(11) Uani 1 1 d . . .
O3 O 0.7331(4) 0.3220(4) 0.6035(4) 0.0269(10) Uani 1 1 d . . .
C5 C 0.7892(6) 0.3777(6) 0.6344(6) 0.0249(14) Uani 1 1 d . . .
C4 C 0.7714(6) 0.5072(5) 0.6086(6) 0.0206(12) Uani 1 1 d . . .
C3 C 0.6826(6) 0.5559(6) 0.5606(6) 0.0230(13) Uani 1 1 d . . .
H18 H 0.6341 0.5074 0.5488 0.028 Uiso 1 1 calc R . .
C2 C 0.6668(6) 0.6786(5) 0.5304(6) 0.0194(12) Uani 1 1 d . . .
Tb1 Tb 0.5000 1.0000 0.5000 0.01138(10) Uani 1 2 d S . .
Tb2 Tb 0.42632(2) 0.83031(2) 0.32690(2) 0.01373(9) Uani 1 1 d . . .
O2 O 0.5637(4) 0.8453(4) 0.4441(4) 0.0179(8) Uani 1 1 d . . .
O10 O 0.4681(5) 1.0297(4) 0.3129(4) 0.0244(10) Uani 1 1 d . . .
O1 O 0.5213(4) 0.6715(4) 0.4452(4) 0.0232(9) Uani 1 1 d . . .
O9 O 0.5339(6) 1.1856(4) 0.3233(4) 0.0365(13) Uani 1 1 d . . .
O4 O 0.8595(5) 0.3283(4) 0.6910(5) 0.0424(15) Uani 1 1 d . . .
C17 C 0.5023(5) 1.1412(5) 0.2667(5) 0.0160(11) Uani 1 1 d . . .
C1 C 0.5774(5) 0.7330(5) 0.4714(5) 0.0160(11) Uani 1 1 d . . .
C7 C 0.8254(5) 0.7006(5) 0.6021(5) 0.0173(11) Uani 1 1 d . . .
C18 C 0.5039(6) 1.2257(5) 0.1487(5) 0.0195(12) Uani 1 1 d . . .
C6 C 0.8418(6) 0.5791(5) 0.6290(6) 0.0206(12) Uani 1 1 d . . .
H11 H 0.9008 0.5456 0.6610 0.025 Uiso 1 1 calc R . .
C19 C 0.5078(6) 1.1854(5) 0.0663(5) 0.0214(12) Uani 1 1 d . . .
H15 H 0.5078 1.1031 0.0844 0.026 Uiso 1 1 calc R . .
C8 C 0.7380(5) 0.7491(5) 0.5514(6) 0.0197(12) Uani 1 1 d . . .
H20 H 0.7272 0.8305 0.5311 0.024 Uiso 1 1 calc R . .
C24 C 0.5013(7) 1.3476(6) 0.1220(5) 0.0258(14) Uani 1 1 d . . .
H21 H 0.4995 1.3733 0.1780 0.031 Uiso 1 1 calc R . .
C23 C 0.5011(7) 1.4337(5) 0.0143(5) 0.0239(14) Uani 1 1 d . . .
C20 C 0.5118(7) 1.2686(6) -0.0432(5) 0.0244(13) Uani 1 1 d . . .
C22 C 0.5087(7) 1.3905(6) -0.0681(6) 0.0302(15) Uani 1 1 d . . .
H24 H 0.5117 1.4455 -0.1420 0.036 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

O13 Tb2 2.404(5) . ?
O11 C21 1.250(7) . ?
O11 Tb2 2.447(4) 2_675 ?
O12 C21 1.276(7) . ?
O12 Tb2 2.482(4) 2_675 ?
C21 C20 1.495(8) . ?
O5 C12 1.236(7) . ?
O5 Tb2 2.375(4) 1_655 ?
O6 C12 1.263(7) . ?
O6 Tb1 2.284(4) 1_655 ?
C12 C11 1.512(8) . ?
C10 C9 1.395(8) . ?
C10 C11 1.401(7) . ?
C11 C13 1.393(7) . ?
C13 C14 1.382(8) . ?
O8 C15 1.228(7) . ?
O8 Tb2 2.396(4) 2_676 ?
O7 C15 1.275(7) . ?
C15 C14 1.511(7) . ?
C14 C16 1.393(8) . ?
C16 C9 1.402(7) . ?
C9 C7 1.473(7) . ?
O3 C5 1.238(7) . ?
O3 Tb2 2.308(5) 2_666 ?
C5 O4 1.278(7) . ?
C5 C4 1.493(8) . ?
C4 C6 1.393(8) . ?
C4 C3 1.394(8) . ?
C3 C2 1.401(8) . ?
C2 C8 1.392(8) . ?
C2 C1 1.500(7) . ?
Tb1 O6 2.284(4) 1_455 ?
Tb1 O6 2.284(4) 2_776 ?
Tb1 O2 2.324(4) . ?
Tb1 O2 2.324(4) 2_676 ?
Tb1 O9 2.418(4) . ?
Tb1 O9 2.418(4) 2_676 ?
Tb1 O10 2.565(4) . ?
Tb1 O10 2.565(4) 2_676 ?
Tb1 C17 2.883(5) 2_676 ?
Tb2 O3 2.308(5) 2_666 ?
Tb2 O5 2.375(4) 1_455 ?
Tb2 O8 2.396(4) 2_676 ?
Tb2 O10 2.419(4) . ?
Tb2 O11 2.447(4) 2_675 ?
Tb2 O1 2.453(4) . ?
Tb2 O12 2.482(4) 2_675 ?
Tb2 O2 2.679(4) . ?
Tb2 C21 2.830(6) 2_675 ?
O2 C1 1.281(6) . ?
O10 C17 1.246(7) . ?
O1 C1 1.243(7) . ?
O9 C17 1.260(7) . ?
C17 C18 1.485(8) . ?
C7 C6 1.395(7) . ?
C7 C8 1.400(8) . ?
C18 C24 1.379(8) . ?
C18 C19 1.385(8) . ?
C19 C20 1.385(8) . ?
C24 C23 1.394(8) . ?
C23 C22 1.401(8) . ?
C23 C23 1.500(11) 2_685 ?
C20 C22 1.385(8) . ?

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
C21 O11 Tb2 94.3(4) . 2_675 ?
C21 O12 Tb2 92.0(3) . 2_675 ?
O11 C21 O12 120.6(5) . . ?
O11 C21 C20 121.3(5) . . ?
O12 C21 C20 118.0(5) . . ?
O11 C21 Tb2 59.6(3) . 2_675 ?
O12 C21 Tb2 61.2(3) . 2_675 ?
C20 C21 Tb2 173.4(5) . 2_675 ?
C12 O5 Tb2 137.4(4) . 1_655 ?
C12 O6 Tb1 123.3(4) . 1_655 ?
O5 C12 O6 124.8(6) . . ?
O5 C12 C11 119.8(5) . . ?
O6 C12 C11 115.3(5) . . ?
C9 C10 C11 120.8(5) . . ?
C13 C11 C10 120.0(5) . . ?
C13 C11 C12 118.6(5) . . ?
C10 C11 C12 120.9(5) . . ?
C14 C13 C11 120.0(5) . . ?
C15 O8 Tb2 149.4(4) . 2_676 ?
O8 C15 O7 125.6(5) . . ?
O8 C15 C14 118.5(5) . . ?
O7 C15 C14 115.9(5) . . ?
C13 C14 C16 119.8(5) . . ?
C13 C14 C15 120.4(5) . . ?
C16 C14 C15 119.5(5) . . ?
C14 C16 C9 121.5(5) . . ?
C10 C9 C16 117.9(5) . . ?
C10 C9 C7 122.2(5) . . ?
C16 C9 C7 119.7(5) . . ?
C5 O3 Tb2 143.3(5) . 2_666 ?
O3 C5 O4 122.9(5) . . ?
O3 C5 C4 119.1(5) . . ?
O4 C5 C4 117.9(5) . . ?
C6 C4 C3 120.2(5) . . ?
C6 C4 C5 122.1(5) . . ?
C3 C4 C5 117.7(5) . . ?
C4 C3 C2 119.5(5) . . ?
C8 C2 C3 119.5(5) . . ?
C8 C2 C1 121.0(5) . . ?
C3 C2 C1 119.4(5) . . ?
O6 Tb1 O6 180.000(1) 1_455 2_776 ?
O6 Tb1 O2 100.52(15) 1_455 . ?
O6 Tb1 O2 79.48(15) 2_776 . ?
O6 Tb1 O2 79.48(15) 1_455 2_676 ?
O6 Tb1 O2 100.52(15) 2_776 2_676 ?
O2 Tb1 O2 180.000(1) . 2_676 ?
O6 Tb1 O9 100.98(19) 1_455 . ?
O6 Tb1 O9 79.02(19) 2_776 . ?
O2 Tb1 O9 107.62(15) . . ?
O2 Tb1 O9 72.38(15) 2_676 . ?
O6 Tb1 O9 79.02(19) 1_455 2_676 ?
O6 Tb1 O9 100.98(19) 2_776 2_676 ?
O2 Tb1 O9 72.38(15) . 2_676 ?
O2 Tb1 O9 107.62(15) 2_676 2_676 ?
O9 Tb1 O9 180.000(1) . 2_676 ?
O6 Tb1 O10 79.28(17) 1_455 . ?
O6 Tb1 O10 100.72(17) 2_776 . ?
O2 Tb1 O10 66.87(14) . . ?
O2 Tb1 O10 113.13(14) 2_676 . ?
O9 Tb1 O10 51.23(14) . . ?
O9 Tb1 O10 128.77(14) 2_676 . ?
O6 Tb1 O10 100.72(17) 1_455 2_676 ?
O6 Tb1 O10 79.28(17) 2_776 2_676 ?
O2 Tb1 O10 113.13(14) . 2_676 ?
O2 Tb1 O10 66.87(14) 2_676 2_676 ?
O9 Tb1 O10 128.77(14) . 2_676 ?
O9 Tb1 O10 51.23(14) 2_676 2_676 ?
O10 Tb1 O10 180.000(1) . 2_676 ?
O6 Tb1 C17 89.91(18) 1_455 2_676 ?
O6 Tb1 C17 90.09(18) 2_776 2_676 ?
O2 Tb1 C17 92.84(14) . 2_676 ?
O2 Tb1 C17 87.16(14) 2_676 2_676 ?
O9 Tb1 C17 154.38(15) . 2_676 ?
O9 Tb1 C17 25.62(15) 2_676 2_676 ?
O10 Tb1 C17 154.40(14) . 2_676 ?
O10 Tb1 C17 25.60(14) 2_676 2_676 ?
O3 Tb2 O5 72.41(17) 2_666 1_455 ?
O3 Tb2 O8 78.13(15) 2_666 2_676 ?
O5 Tb2 O8 75.67(16) 1_455 2_676 ?
O3 Tb2 O13 143.37(18) 2_666 . ?
O5 Tb2 O13 138.08(17) 1_455 . ?
O8 Tb2 O13 122.51(19) 2_676 . ?
O3 Tb2 O10 142.35(16) 2_666 . ?
O5 Tb2 O10 78.98(16) 1_455 . ?
O8 Tb2 O10 71.37(15) 2_676 . ?
O13 Tb2 O10 73.62(18) . . ?
O3 Tb2 O11 86.20(17) 2_666 2_675 ?
O5 Tb2 O11 144.37(16) 1_455 2_675 ?
O8 Tb2 O11 72.18(15) 2_676 2_675 ?
O13 Tb2 O11 74.29(18) . 2_675 ?
O10 Tb2 O11 104.40(15) . 2_675 ?
O3 Tb2 O1 85.71(15) 2_666 . ?
O5 Tb2 O1 81.67(15) 1_455 . ?
O8 Tb2 O1 155.24(16) 2_676 . ?
O13 Tb2 O1 81.32(19) . . ?
O10 Tb2 O1 114.09(14) . . ?
O11 Tb2 O1 125.72(14) 2_675 . ?
O3 Tb2 O12 71.96(17) 2_666 2_675 ?
O5 Tb2 O12 137.70(16) 1_455 2_675 ?
O8 Tb2 O12 117.72(15) 2_676 2_675 ?
O13 Tb2 O12 71.54(19) . 2_675 ?
O10 Tb2 O12 142.55(17) . 2_675 ?
O11 Tb2 O12 52.86(14) 2_675 2_675 ?
O1 Tb2 O12 73.67(14) . 2_675 ?
O3 Tb2 O2 125.78(15) 2_666 . ?
O5 Tb2 O2 71.35(14) 1_455 . ?
O8 Tb2 O2 128.00(13) 2_676 . ?
O13 Tb2 O2 68.27(16) . . ?
O10 Tb2 O2 63.76(13) . . ?
O11 Tb2 O2 142.53(16) 2_675 . ?
O1 Tb2 O2 50.34(12) . . ?
O12 Tb2 O2 113.80(15) 2_675 . ?
O3 Tb2 C21 76.83(18) 2_666 2_675 ?
O5 Tb2 C21 148.96(18) 1_455 2_675 ?
O8 Tb2 C21 94.24(17) 2_676 2_675 ?
O13 Tb2 C21 72.06(19) . 2_675 ?
O10 Tb2 C21 126.14(17) . 2_675 ?
O11 Tb2 C21 26.14(15) 2_675 2_675 ?
O1 Tb2 C21 100.24(16) . 2_675 ?
O12 Tb2 C21 26.77(15) 2_675 2_675 ?
O2 Tb2 C21 133.09(16) . 2_675 ?
C1 O2 Tb1 150.1(4) . . ?
C1 O2 Tb2 88.5(3) . . ?
Tb1 O2 Tb2 107.02(14) . . ?
C17 O10 Tb2 158.7(4) . . ?
C17 O10 Tb1 91.6(3) . . ?
Tb2 O10 Tb1 107.82(15) . . ?
C1 O1 Tb2 100.2(3) . . ?
C17 O9 Tb1 98.3(4) . . ?
O10 C17 O9 118.8(5) . . ?
O10 C17 C18 123.1(5) . . ?
O9 C17 C18 118.1(5) . . ?
O1 C1 O2 120.6(5) . . ?
O1 C1 C2 120.4(5) . . ?
O2 C1 C2 118.9(5) . . ?
C6 C7 C8 118.0(5) . . ?
C6 C7 C9 122.7(5) . . ?
C8 C7 C9 119.3(5) . . ?
C24 C18 C19 119.8(5) . . ?
C24 C18 C17 118.2(5) . . ?
C19 C18 C17 122.0(5) . . ?
C4 C6 C7 121.2(5) . . ?
C18 C19 C20 119.6(5) . . ?
C2 C8 C7 121.6(5) . . ?
C18 C24 C23 122.5(5) . . ?
C24 C23 C22 116.2(5) . . ?
C24 C23 C23 122.2(6) . 2_685 ?
C22 C23 C23 121.5(7) . 2_685 ?
C22 C20 C19 119.6(5) . . ?
C22 C20 C21 119.6(5) . . ?
C19 C20 C21 120.7(5) . . ?
C20 C22 C23 122.2(6) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.548
_refine_diff_density_min         -2.416
_refine_diff_density_rms         0.196

# 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 0.000 -0.007 0.000 655.6 17.3
_platon_squeeze_details          
;
;
#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939028'
#######################################################################
#
#                 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          'not measured '
_chemical_formula_moiety         'C48 H18 N0 O26 Sm3'
_chemical_formula_sum            'C48 H18 N0 O26 Sm3'
_chemical_formula_weight         1461.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.647(2)
_cell_length_b                   12.247(2)
_cell_length_c                   13.604(3)
_cell_angle_alpha                65.01(3)
_cell_angle_beta                 67.88(3)
_cell_angle_gamma                88.32(3)
_cell_volume                     1609.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4383
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.00

_exptl_crystal_description       sheet
_exptl_crystal_colour            coloress
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12714
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5624
_reflns_number_gt                5041
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0534P)²+0.7521P] 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         5624
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_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
O2 O 0.4751(3) 1.0307(3) 0.3117(3) 0.0195(7) Uani 1 1 d . . .
O3 O 0.5403(3) 1.1900(3) 0.3197(3) 0.0252(8) Uani 1 1 d . . .
Sm1 Sm 0.5000 1.0000 0.5000 0.00931(9) Uani 1 2 d S . .
Sm2 Sm 0.429475(19) 0.828826(17) 0.328142(17) 0.01020(9) Uani 1 1 d . . .
O5 O 0.2907(3) 0.8080(3) 0.5221(3) 0.0192(7) Uani 1 1 d . . .
O8 O -0.4327(3) 0.8423(2) 0.4421(2) 0.0125(6) Uani 1 1 d . . .
O12 O 0.5600(3) 1.1292(3) -0.1287(3) 0.0212(7) Uani 1 1 d . . .
O10 O -0.2603(3) 0.3255(2) 0.5936(3) 0.0202(7) Uani 1 1 d . . .
O13 O 0.5004(3) 1.3023(3) -0.2240(3) 0.0250(8) Uani 1 1 d . . .
O7 O -0.2648(3) 1.0566(2) 0.7051(3) 0.0169(6) Uani 1 1 d . . .
O9 O -0.4748(3) 0.6681(3) 0.4444(3) 0.0192(7) Uani 1 1 d . . .
C23 C 0.5248(4) 1.2295(4) -0.1364(4) 0.0175(9) Uani 1 1 d . . .
C17 C 0.5090(4) 1.1443(3) 0.2650(4) 0.0130(8) Uani 1 1 d . . .
O4 O 0.2824(3) 0.9522(3) 0.5804(3) 0.0291(8) Uani 1 1 d . . .
O11 O -0.1420(3) 0.3298(3) 0.6868(3) 0.0300(8) Uani 1 1 d . . .
O1 O 0.6476(3) 0.9031(4) 0.1930(3) 0.0378(9) Uani 1 1 d . . .
C14 C -0.2083(4) 0.3784(4) 0.6300(4) 0.0195(10) Uani 1 1 d . . .
C13 C -0.2274(4) 0.5101(4) 0.6031(4) 0.0155(9) Uani 1 1 d . . .
C18 C 0.5077(4) 1.2273(4) 0.1476(3) 0.0137(9) Uani 1 1 d . . .
C19 C 0.5038(4) 1.3500(4) 0.1205(4) 0.0195(10) Uani 1 1 d . . .
H19 H 0.5021 1.3760 0.1761 0.023 Uiso 1 1 calc R . .
C24 C 0.5109(4) 1.1852(4) 0.0662(4) 0.0157(9) Uani 1 1 d . . .
H24 H 0.5109 1.1030 0.0843 0.019 Uiso 1 1 calc R . .
C1 C 0.2309(4) 0.8725(4) 0.5678(4) 0.0154(9) Uani 1 1 d . . .
C16 C -0.4198(4) 0.7320(4) 0.4701(4) 0.0137(9) Uani 1 1 d . . .
C11 C -0.3300(4) 0.6777(4) 0.5275(4) 0.0139(9) Uani 1 1 d . . .
O6 O -0.0826(3) 1.1311(3) 0.6897(3) 0.0217(7) Uani 1 1 d . . .
C2 C 0.0918(4) 0.8627(3) 0.6072(3) 0.0125(8) Uani 1 1 d . . .
C3 C 0.0317(4) 0.9486(4) 0.6425(4) 0.0157(9) Uani 1 1 d . . .
H3 H 0.0765 1.0038 0.6504 0.019 Uiso 1 1 calc R . .
C8 C 0.0240(4) 0.7790(3) 0.5967(3) 0.0126(8) Uani 1 1 d . . .
H8 H 0.0640 0.7217 0.5736 0.015 Uiso 1 1 calc R . .
C5 C -0.1555(4) 1.0518(3) 0.6912(4) 0.0156(9) Uani 1 1 d . . .
C21 C 0.5091(5) 1.3910(4) -0.0685(4) 0.0206(10) Uani 1 1 d . . .
H21 H 0.5102 1.4447 -0.1418 0.025 Uiso 1 1 calc R . .
C4 C -0.0928(4) 0.9514(4) 0.6655(3) 0.0146(9) Uani 1 1 d . . .
C22 C 0.5141(4) 1.2689(4) -0.0422(4) 0.0194(10) Uani 1 1 d . . .
C7 C -0.1028(4) 0.7808(3) 0.6204(3) 0.0128(8) Uani 1 1 d . . .
C6 C -0.1608(4) 0.8681(4) 0.6562(4) 0.0145(9) Uani 1 1 d . . .
H6 H -0.2459 0.8697 0.6738 0.017 Uiso 1 1 calc R . .
C10 C -0.2605(4) 0.7488(4) 0.5492(3) 0.0131(8) Uani 1 1 d . . .
H10 H -0.2715 0.8298 0.5295 0.016 Uiso 1 1 calc R . .
C12 C -0.3134(4) 0.5567(4) 0.5561(4) 0.0174(9) Uani 1 1 d . . .
H12 H -0.3603 0.5077 0.5434 0.021 Uiso 1 1 calc R . .
C15 C -0.1585(4) 0.5803(4) 0.6255(4) 0.0154(9) Uani 1 1 d . . .
H15 H -0.1009 0.5467 0.6579 0.018 Uiso 1 1 calc R . .
C9 C -0.1752(4) 0.7019(3) 0.5995(4) 0.0135(9) Uani 1 1 d . . .
C20 C 0.5023(4) 1.4355(4) 0.0136(4) 0.0185(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

O2 C17 1.262(5) . ?
O2 Sm2 2.442(3) . ?
O2 Sm1 2.555(3) . ?
O3 C17 1.253(5) . ?
O3 Sm1 2.455(3) . ?
Sm1 O4 2.328(3) 2_676 ?
Sm1 O4 2.328(3) . ?
Sm1 O8 2.387(3) 1_655 ?
Sm1 O8 2.387(3) 2_576 ?
Sm1 O3 2.455(3) 2_676 ?
Sm1 O2 2.555(3) 2_676 ?
Sm1 C17 2.887(4) 2_676 ?
Sm2 O10 2.351(3) 2_566 ?
Sm2 O7 2.411(3) 2_576 ?
Sm2 O1 2.422(4) . ?
Sm2 O5 2.426(3) . ?
Sm2 O9 2.488(3) 1_655 ?
Sm2 O12 2.493(3) 2_675 ?
Sm2 O13 2.496(3) 2_675 ?
Sm2 O8 2.667(3) 1_655 ?
Sm2 C23 2.847(4) 2_675 ?
Sm2 C16 2.952(4) 1_655 ?
O5 C1 1.246(5) . ?
O8 C16 1.261(5) . ?
O8 Sm1 2.387(3) 1_455 ?
O8 Sm2 2.667(3) 1_455 ?
O12 C23 1.258(5) . ?
O12 Sm2 2.493(3) 2_675 ?
O10 C14 1.245(5) . ?
O10 Sm2 2.351(3) 2_566 ?
O13 C23 1.280(5) . ?
O13 Sm2 2.496(3) 2_675 ?
O7 C5 1.219(5) . ?
O7 Sm2 2.411(3) 2_576 ?
O9 C16 1.255(5) . ?
O9 Sm2 2.488(3) 1_455 ?
C23 C22 1.514(6) . ?
C23 Sm2 2.847(4) 2_675 ?
C17 C18 1.494(6) . ?
O4 C1 1.263(5) . ?
O11 C14 1.259(5) . ?
C14 C13 1.525(6) . ?
C13 C12 1.370(6) . ?
C13 C15 1.387(5) . ?
C18 C19 1.391(6) . ?
C18 C24 1.394(6) . ?
C19 C20 1.395(6) . ?
C19 H19 0.9300 . ?
C24 C22 1.382(6) . ?
C24 H24 0.9300 . ?
C1 C2 1.493(6) . ?
C16 C11 1.510(6) . ?
C16 Sm2 2.952(4) 1_455 ?
C11 C12 1.392(6) . ?
C11 C10 1.393(5) . ?
O6 C5 1.297(5) . ?
C2 C8 1.397(5) . ?
C2 C3 1.399(6) . ?
C3 C4 1.366(6) . ?
C3 H3 0.9300 . ?
C8 C7 1.390(6) . ?
C8 H8 0.9300 . ?
C5 C4 1.512(6) . ?
C21 C22 1.387(6) . ?
C21 C20 1.412(6) . ?
C21 H21 0.9300 . ?
C4 C6 1.384(5) . ?
C7 C6 1.409(6) . ?
C7 C9 1.477(5) . ?
C6 H6 0.9300 . ?
C10 C9 1.391(6) . ?
C10 H10 0.9300 . ?
C12 H12 0.9300 . ?
C15 C9 1.404(6) . ?
C15 H15 0.9300 . ?
C20 C20 1.467(8) 2_685 ?

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
C17 O2 Sm2 159.5(3) . . ?
C17 O2 Sm1 91.9(2) . . ?
Sm2 O2 Sm1 107.41(11) . . ?
C17 O3 Sm1 96.9(2) . . ?
O4 Sm1 O4 180.000(1) 2_676 . ?
O4 Sm1 O8 77.41(11) 2_676 1_655 ?
O4 Sm1 O8 102.59(11) . 1_655 ?
O4 Sm1 O8 102.59(11) 2_676 2_576 ?
O4 Sm1 O8 77.41(11) . 2_576 ?
O8 Sm1 O8 180.000(1) 1_655 2_576 ?
O4 Sm1 O3 102.11(13) 2_676 2_676 ?
O4 Sm1 O3 77.89(13) . 2_676 ?
O8 Sm1 O3 72.07(10) 1_655 2_676 ?
O8 Sm1 O3 107.93(10) 2_576 2_676 ?
O4 Sm1 O3 77.89(13) 2_676 . ?
O4 Sm1 O3 102.11(13) . . ?
O8 Sm1 O3 107.93(10) 1_655 . ?
O8 Sm1 O3 72.07(10) 2_576 . ?
O3 Sm1 O3 180.000(1) 2_676 . ?
O4 Sm1 O2 97.96(12) 2_676 . ?
O4 Sm1 O2 82.04(12) . . ?
O8 Sm1 O2 66.97(10) 1_655 . ?
O8 Sm1 O2 113.03(10) 2_576 . ?
O3 Sm1 O2 128.60(9) 2_676 . ?
O3 Sm1 O2 51.40(9) . . ?
O4 Sm1 O2 82.04(12) 2_676 2_676 ?
O4 Sm1 O2 97.96(12) . 2_676 ?
O8 Sm1 O2 113.03(10) 1_655 2_676 ?
O8 Sm1 O2 66.97(10) 2_576 2_676 ?
O3 Sm1 O2 51.40(9) 2_676 2_676 ?
O3 Sm1 O2 128.60(9) . 2_676 ?
O2 Sm1 O2 180.000(1) . 2_676 ?
O4 Sm1 C17 91.95(13) 2_676 2_676 ?
O4 Sm1 C17 88.05(13) . 2_676 ?
O8 Sm1 C17 92.24(10) 1_655 2_676 ?
O8 Sm1 C17 87.76(10) 2_576 2_676 ?
O3 Sm1 C17 25.51(10) 2_676 2_676 ?
O3 Sm1 C17 154.49(10) . 2_676 ?
O2 Sm1 C17 154.11(10) . 2_676 ?
O2 Sm1 C17 25.89(10) 2_676 2_676 ?
O4 Sm1 Sm2 75.02(9) 2_676 2_676 ?
O4 Sm1 Sm2 104.98(9) . 2_676 ?
O8 Sm1 Sm2 140.37(6) 1_655 2_676 ?
O8 Sm1 Sm2 39.63(6) 2_576 2_676 ?
O3 Sm1 Sm2 86.51(7) 2_676 2_676 ?
O3 Sm1 Sm2 93.49(7) . 2_676 ?
O2 Sm1 Sm2 144.65(7) . 2_676 ?
O2 Sm1 Sm2 35.35(6) 2_676 2_676 ?
C17 Sm1 Sm2 61.12(8) 2_676 2_676 ?
O10 Sm2 O7 77.47(10) 2_566 2_576 ?
O10 Sm2 O1 144.17(12) 2_566 . ?
O7 Sm2 O1 121.83(12) 2_576 . ?
O10 Sm2 O5 72.10(11) 2_566 . ?
O7 Sm2 O5 75.35(10) 2_576 . ?
O1 Sm2 O5 138.43(11) . . ?
O10 Sm2 O2 140.97(11) 2_566 . ?
O7 Sm2 O2 71.17(10) 2_576 . ?
O1 Sm2 O2 74.10(13) . . ?
O5 Sm2 O2 77.87(11) . . ?
O10 Sm2 O9 86.22(10) 2_566 1_655 ?
O7 Sm2 O9 155.99(10) 2_576 1_655 ?
O1 Sm2 O9 81.46(13) . 1_655 ?
O5 Sm2 O9 82.97(11) . 1_655 ?
O2 Sm2 O9 114.49(9) . 1_655 ?
O10 Sm2 O12 86.85(11) 2_566 2_675 ?
O7 Sm2 O12 71.34(11) 2_576 2_675 ?
O1 Sm2 O12 73.80(12) . 2_675 ?
O5 Sm2 O12 143.72(11) . 2_675 ?
O2 Sm2 O12 104.04(10) . 2_675 ?
O9 Sm2 O12 125.74(10) 1_655 2_675 ?
O10 Sm2 O13 72.62(11) 2_566 2_675 ?
O7 Sm2 O13 116.71(10) 2_576 2_675 ?
O1 Sm2 O13 71.65(12) . 2_675 ?
O5 Sm2 O13 138.65(11) . 2_675 ?
O2 Sm2 O13 142.97(11) . 2_675 ?
O9 Sm2 O13 73.83(10) 1_655 2_675 ?
O12 Sm2 O13 52.83(10) 2_675 2_675 ?
O10 Sm2 O8 124.97(9) 2_566 1_655 ?
O7 Sm2 O8 128.45(9) 2_576 1_655 ?
O1 Sm2 O8 69.40(10) . 1_655 ?
O5 Sm2 O8 71.04(10) . 1_655 ?
O2 Sm2 O8 64.42(9) . 1_655 ?
O9 Sm2 O8 50.09(9) 1_655 1_655 ?
O12 Sm2 O8 143.16(10) 2_675 1_655 ?
O13 Sm2 O8 114.42(10) 2_675 1_655 ?
O10 Sm2 C23 77.53(12) 2_566 2_675 ?
O7 Sm2 C23 93.33(12) 2_576 2_675 ?
O1 Sm2 C23 71.84(12) . 2_675 ?
O5 Sm2 C23 149.20(12) . 2_675 ?
O2 Sm2 C23 126.10(11) . 2_675 ?
O9 Sm2 C23 100.28(11) 1_655 2_675 ?
O12 Sm2 C23 26.19(11) 2_675 2_675 ?
O13 Sm2 C23 26.69(11) 2_675 2_675 ?
O8 Sm2 C23 133.77(12) 1_655 2_675 ?
O10 Sm2 C16 106.70(11) 2_566 1_655 ?
O7 Sm2 C16 148.82(10) 2_576 1_655 ?
O1 Sm2 C16 73.05(13) . 1_655 ?
O5 Sm2 C16 76.73(11) . 1_655 ?
O2 Sm2 C16 89.64(10) . 1_655 ?
O9 Sm2 C16 24.85(10) 1_655 1_655 ?
O12 Sm2 C16 138.81(11) 2_675 1_655 ?
O13 Sm2 C16 93.52(11) 2_675 1_655 ?
O8 Sm2 C16 25.28(9) 1_655 1_655 ?
C23 Sm2 C16 117.83(12) 2_675 1_655 ?
C1 O5 Sm2 138.9(3) . . ?
C16 O8 Sm1 149.5(3) . 1_455 ?
C16 O8 Sm2 90.1(2) . 1_455 ?
Sm1 O8 Sm2 105.56(10) 1_455 1_455 ?
C23 O12 Sm2 92.8(2) . 2_675 ?
C14 O10 Sm2 138.4(3) . 2_566 ?
C23 O13 Sm2 92.1(2) . 2_675 ?
C5 O7 Sm2 150.8(3) . 2_576 ?
C16 O9 Sm2 98.8(2) . 1_455 ?
O12 C23 O13 122.0(4) . . ?
O12 C23 C22 119.9(4) . . ?
O13 C23 C22 118.1(4) . . ?
O12 C23 Sm2 61.0(2) . 2_675 ?
O13 C23 Sm2 61.2(2) . 2_675 ?
C22 C23 Sm2 173.9(3) . 2_675 ?
O3 C17 O2 119.7(4) . . ?
O3 C17 C18 118.6(3) . . ?
O2 C17 C18 121.7(3) . . ?
C1 O4 Sm1 120.6(3) . . ?
O10 C14 O11 124.0(4) . . ?
O10 C14 C13 117.2(4) . . ?
O11 C14 C13 118.9(4) . . ?
C12 C13 C15 121.3(4) . . ?
C12 C13 C14 118.3(4) . . ?
C15 C13 C14 120.3(4) . . ?
C19 C18 C24 120.2(4) . . ?
C19 C18 C17 117.9(3) . . ?
C24 C18 C17 121.9(4) . . ?
C18 C19 C20 122.7(4) . . ?
C18 C19 H19 118.6 . . ?
C20 C19 H19 118.6 . . ?
C22 C24 C18 118.2(4) . . ?
C22 C24 H24 120.9 . . ?
C18 C24 H24 120.9 . . ?
O5 C1 O4 123.3(4) . . ?
O5 C1 C2 121.0(4) . . ?
O4 C1 C2 115.7(4) . . ?
O9 C16 O8 120.8(4) . . ?
O9 C16 C11 119.0(3) . . ?
O8 C16 C11 120.0(3) . . ?
O9 C16 Sm2 56.4(2) . 1_455 ?
O8 C16 Sm2 64.6(2) . 1_455 ?
C11 C16 Sm2 171.1(3) . 1_455 ?
C12 C11 C10 119.4(4) . . ?
C12 C11 C16 120.2(3) . . ?
C10 C11 C16 120.5(4) . . ?
C8 C2 C3 119.9(4) . . ?
C8 C2 C1 121.2(4) . . ?
C3 C2 C1 118.5(3) . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C7 C8 C2 120.5(4) . . ?
C7 C8 H8 119.8 . . ?
C2 C8 H8 119.8 . . ?
O7 C5 O6 125.4(4) . . ?
O7 C5 C4 119.5(4) . . ?
O6 C5 C4 114.9(4) . . ?
C22 C21 C20 121.5(4) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C3 C4 C6 120.3(4) . . ?
C3 C4 C5 120.5(4) . . ?
C6 C4 C5 119.0(4) . . ?
C24 C22 C21 121.4(4) . . ?
C24 C22 C23 120.5(4) . . ?
C21 C22 C23 118.1(4) . . ?
C8 C7 C6 118.3(4) . . ?
C8 C7 C9 122.2(4) . . ?
C6 C7 C9 119.3(4) . . ?
C4 C6 C7 120.9(4) . . ?
C4 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C9 C10 C11 121.7(4) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C13 C15 C9 120.2(4) . . ?
C13 C15 H15 119.9 . . ?
C9 C15 H15 119.9 . . ?
C10 C9 C15 117.8(4) . . ?
C10 C9 C7 119.9(4) . . ?
C15 C9 C7 122.3(4) . . ?
C19 C20 C21 115.9(4) . . ?
C19 C20 C20 122.1(5) . 2_685 ?
C21 C20 C20 122.0(5) . 2_685 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.150

# 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 0.000 -0.005 0.000 643.9 14.7
_platon_squeeze_details          
;
;
#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939029'
#######################################################################
#
#                 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         'not measured'
_chemical_formula_sum            'C48 H18 Dy3 N0 O26'
_chemical_formula_weight         1498.12

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5976(11)
_cell_length_b                   12.2130(11)
_cell_length_c                   13.5187(12)
_cell_angle_alpha                65.039(6)
_cell_angle_beta                 68.351(6)
_cell_angle_gamma                87.858(6)
_cell_volume                     1597.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4383
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      24.98

_exptl_crystal_description       sheet
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    3.544
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6053
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9009
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         24.98
_reflns_number_total             5572
_reflns_number_gt                4344
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0409P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5572
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0830
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_restrained_S_all      0.927
_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
O11 O 0.9950(5) 0.7999(4) -0.2244(4) 0.0349(12) Uani 1 1 d . . .
O12 O 1.0580(5) 0.6296(3) -0.1308(4) 0.0313(11) Uani 1 1 d . . .
C21 C 1.0209(6) 0.7294(5) -0.1379(5) 0.0247(14) Uani 1 1 d . . .
Dy1 Dy 0.92876(3) 0.33001(2) 0.32744(2) 0.01703(9) Uani 1 1 d . . .
Dy2 Dy 1.0000 0.5000 0.5000 0.01374(10) Uani 1 2 d S . .
O1 O 0.7918(4) 0.3057(4) 0.5170(4) 0.0271(10) Uani 1 1 d . . .
O10 O 0.9715(4) 0.5286(3) 0.3120(4) 0.0273(10) Uani 1 1 d . . .
O5 O 0.0647(4) 0.3448(3) 0.4443(4) 0.0221(9) Uani 1 1 d . . .
O4 O 0.2362(4) 0.5572(3) 0.7062(4) 0.0276(10) Uani 1 1 d . . .
O2 O 0.7895(4) 0.4534(4) 0.5720(4) 0.0344(11) Uani 1 1 d . . .
O6 O 0.0211(4) 0.1722(3) 0.4452(4) 0.0273(10) Uani 1 1 d . . .
O9 O 1.0393(5) 0.6847(4) 0.3217(4) 0.0392(13) Uani 1 1 d . . .
O13 O 1.1452(5) 0.4039(5) 0.1975(4) 0.0499(14) Uani 1 1 d . . .
O3 O 0.4164(4) 0.6288(4) 0.6952(4) 0.0325(11) Uani 1 1 d . . .
O7 O 0.3584(5) -0.1716(4) 0.6885(5) 0.0432(14) Uani 1 1 d . . .
O8 O 0.2338(4) -0.1775(3) 0.6010(4) 0.0323(11) Uani 1 1 d . . .
C1 C 0.7347(6) 0.3722(5) 0.5622(5) 0.0210(13) Uani 1 1 d . . .
C2 C 0.5940(5) 0.3617(5) 0.6061(5) 0.0179(12) Uani 1 1 d . . .
C3 C 0.5345(6) 0.4467(5) 0.6427(5) 0.0207(13) Uani 1 1 d . . .
H3 H 0.5801 0.5017 0.6501 0.025 Uiso 1 1 calc R . .
C17 C 1.0063(6) 0.6409(5) 0.2665(5) 0.0192(12) Uani 1 1 d . . .
C18 C 1.0053(6) 0.7252(5) 0.1478(5) 0.0224(13) Uani 1 1 d . . .
C19 C 1.0073(6) 0.6834(5) 0.0662(5) 0.0222(13) Uani 1 1 d . . .
H19 H 1.0058 0.6007 0.0850 0.027 Uiso 1 1 calc R . .
C5 C 0.3457(6) 0.5506(5) 0.6931(5) 0.0207(13) Uani 1 1 d . . .
C12 C 0.0773(5) 0.2330(5) 0.4717(5) 0.0188(12) Uani 1 1 d . . .
C11 C 0.1662(6) 0.1778(5) 0.5303(5) 0.0212(13) Uani 1 1 d . . .
C10 C 0.2374(5) 0.2483(5) 0.5512(5) 0.0213(13) Uani 1 1 d . . .
H10 H 0.2272 0.3298 0.5307 0.026 Uiso 1 1 calc R . .
C9 C 0.3246(6) 0.1994(5) 0.6026(5) 0.0204(13) Uani 1 1 d . . .
C7 C 0.3987(6) 0.2805(4) 0.6217(5) 0.0188(13) Uani 1 1 d . . .
C6 C 0.3410(6) 0.3657(5) 0.6585(5) 0.0210(13) Uani 1 1 d . . .
H6 H 0.2554 0.3668 0.6773 0.025 Uiso 1 1 calc R . .
C4 C 0.4096(6) 0.4502(5) 0.6678(5) 0.0201(13) Uani 1 1 d . . .
C8 C 0.5253(5) 0.2773(5) 0.5970(5) 0.0182(12) Uani 1 1 d . . .
H8 H 0.5647 0.2190 0.5743 0.022 Uiso 1 1 calc R . .
C24 C 1.0026(6) 0.8497(5) 0.1206(5) 0.0287(15) Uani 1 1 d . . .
H24 H 1.0014 0.8760 0.1763 0.034 Uiso 1 1 calc R . .
C22 C 1.0058(6) 0.8919(5) -0.0684(5) 0.0279(15) Uani 1 1 d . . .
H22 H 1.0047 0.9465 -0.1411 0.033 Uiso 1 1 calc R . .
C20 C 1.0116(7) 0.7674(5) -0.0437(5) 0.0283(15) Uani 1 1 d . . .
C23 C 1.0017(7) 0.9343(5) 0.0130(5) 0.0288(15) Uani 1 1 d . . .
C16 C 0.3403(6) 0.0785(5) 0.6293(5) 0.0256(14) Uani 1 1 d . . .
H16 H 0.3981 0.0446 0.6624 0.031 Uiso 1 1 calc R . .
C13 C 0.1827(6) 0.0567(5) 0.5596(5) 0.0230(13) Uani 1 1 d . . .
H13 H 0.1346 0.0081 0.5474 0.028 Uiso 1 1 calc R . .
C14 C 0.2712(6) 0.0072(5) 0.6075(6) 0.0243(14) Uani 1 1 d . . .
C15 C 0.2884(6) -0.1223(5) 0.6346(6) 0.0250(14) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag


O11 C21 1.260(7) . ?
O11 Dy1 2.468(4) 2_765 ?
O12 C21 1.253(7) . ?
O12 Dy1 2.435(4) 2_765 ?
C21 C20 1.498(8) . ?
C21 Dy1 2.804(6) 2_765 ?
Dy1 O8 2.314(4) 2_656 ?
Dy1 O1 2.360(4) . ?
Dy1 O4 2.383(4) 2_666 ?
Dy1 O10 2.400(3) . ?
Dy1 O13 2.404(5) . ?
Dy1 O6 2.431(4) 1_655 ?
Dy1 O12 2.435(4) 2_765 ?
Dy1 O11 2.468(4) 2_765 ?
Dy1 O5 2.667(4) 1_655 ?
Dy2 O2 2.261(4) 2_766 ?
Dy2 O2 2.261(4) . ?
Dy2 O5 2.325(4) 2_666 ?
Dy2 O5 2.325(4) 1_655 ?
Dy2 O9 2.404(4) 2_766 ?
Dy2 O9 2.404(4) . ?
Dy2 O10 2.561(4) 2_766 ?
Dy2 O10 2.561(4) . ?
O1 C1 1.245(7) . ?
O10 C17 1.253(6) . ?
O5 C12 1.273(6) . ?
O5 Dy2 2.325(4) 1_455 ?
O5 Dy1 2.667(4) 1_455 ?
O4 C5 1.220(7) . ?
O4 Dy1 2.383(4) 2_666 ?
O2 C1 1.275(6) . ?
O6 C12 1.241(6) . ?
O6 Dy1 2.431(4) 1_455 ?
O9 C17 1.246(6) . ?
O3 C5 1.298(6) . ?
O7 C15 1.259(7) . ?
O8 C15 1.250(6) . ?
O8 Dy1 2.314(4) 2_656 ?
C1 C2 1.506(8) . ?
C2 C3 1.388(8) . ?
C2 C8 1.398(7) . ?
C3 C4 1.363(8) . ?
C3 H3 0.9300 . ?
C17 C18 1.501(7) . ?
C18 C19 1.390(7) . ?
C18 C24 1.408(8) . ?
C19 C20 1.388(8) . ?
C19 H19 0.9300 . ?
C5 C4 1.506(8) . ?
C12 C11 1.498(7) . ?
C12 Dy1 2.924(5) 1_455 ?
C11 C13 1.387(7) . ?
C11 C10 1.391(7) . ?
C10 C9 1.409(8) . ?
C10 H10 0.9300 . ?
C9 C16 1.387(7) . ?
C9 C7 1.493(7) . ?
C7 C8 1.383(8) . ?
C7 C6 1.384(8) . ?
C6 C4 1.400(7) . ?
C6 H6 0.9300 . ?
C8 H8 0.9300 . ?
C24 C23 1.387(8) . ?
C24 H24 0.9300 . ?
C22 C23 1.387(8) . ?
C22 C20 1.417(7) . ?
C22 H22 0.9300 . ?
C23 C23 1.494(11) 2_775 ?
C16 C14 1.389(7) . ?
C16 H16 0.9300 . ?
C13 C14 1.397(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.490(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 O11 Dy1 91.7(3) . 2_765 ?
C21 O12 Dy1 93.4(3) . 2_765 ?
O12 C21 O11 121.5(5) . . ?
O12 C21 C20 119.2(5) . . ?
O11 C21 C20 119.3(5) . . ?
O12 C21 Dy1 60.1(3) . 2_765 ?
O11 C21 Dy1 61.6(3) . 2_765 ?
C20 C21 Dy1 172.6(5) . 2_765 ?
O8 Dy1 O1 72.16(15) 2_656 . ?
O8 Dy1 O4 77.51(14) 2_656 2_666 ?
O1 Dy1 O4 75.51(14) . 2_666 ?
O8 Dy1 O10 142.09(16) 2_656 . ?
O1 Dy1 O10 79.32(14) . . ?
O4 Dy1 O10 71.47(13) 2_666 . ?
O8 Dy1 O13 143.75(16) 2_656 . ?
O1 Dy1 O13 138.33(14) . . ?
O4 Dy1 O13 122.42(17) 2_666 . ?
O10 Dy1 O13 73.35(16) . . ?
O8 Dy1 O6 85.83(14) 2_656 1_655 ?
O1 Dy1 O6 81.48(15) . 1_655 ?
O4 Dy1 O6 154.80(15) 2_666 1_655 ?
O10 Dy1 O6 114.40(12) . 1_655 ?
O13 Dy1 O6 81.91(17) . 1_655 ?
O8 Dy1 O12 86.26(15) 2_656 2_765 ?
O1 Dy1 O12 144.28(15) . 2_765 ?
O4 Dy1 O12 72.16(15) 2_666 2_765 ?
O10 Dy1 O12 103.96(13) . 2_765 ?
O13 Dy1 O12 74.02(16) . 2_765 ?
O6 Dy1 O12 125.94(14) 1_655 2_765 ?
O8 Dy1 O11 72.46(16) 2_656 2_765 ?
O1 Dy1 O11 137.71(14) . 2_765 ?
O4 Dy1 O11 117.91(13) 2_666 2_765 ?
O10 Dy1 O11 142.17(16) . 2_765 ?
O13 Dy1 O11 71.36(16) . 2_765 ?
O6 Dy1 O11 73.57(13) 1_655 2_765 ?
O12 Dy1 O11 53.12(13) 2_765 2_765 ?
O8 Dy1 O5 125.76(13) 2_656 1_655 ?
O1 Dy1 O5 71.22(13) . 1_655 ?
O4 Dy1 O5 128.02(12) 2_666 1_655 ?
O10 Dy1 O5 64.04(12) . 1_655 ?
O13 Dy1 O5 68.73(14) . 1_655 ?
O6 Dy1 O5 50.37(11) 1_655 1_655 ?
O12 Dy1 O5 142.71(15) 2_765 1_655 ?
O11 Dy1 O5 113.64(13) 2_765 1_655 ?
O8 Dy1 C21 76.74(16) 2_656 2_765 ?
O1 Dy1 C21 148.67(16) . 2_765 ?
O4 Dy1 C21 94.35(16) 2_666 2_765 ?
O10 Dy1 C21 126.11(15) . 2_765 ?
O13 Dy1 C21 72.10(17) . 2_765 ?
O6 Dy1 C21 100.13(15) 1_655 2_765 ?
O12 Dy1 C21 26.50(15) 2_765 2_765 ?
O11 Dy1 C21 26.70(15) 2_765 2_765 ?
O5 Dy1 C21 133.25(16) 1_655 2_765 ?
O8 Dy1 C12 106.74(14) 2_656 1_655 ?
O1 Dy1 C12 76.36(15) . 1_655 ?
O4 Dy1 C12 148.55(15) 2_666 1_655 ?
O10 Dy1 C12 89.76(13) . 1_655 ?
O13 Dy1 C12 72.73(17) . 1_655 ?
O6 Dy1 C12 24.65(13) 1_655 1_655 ?
O12 Dy1 C12 138.37(16) 2_765 1_655 ?
O11 Dy1 C12 92.50(14) 2_765 1_655 ?
O5 Dy1 C12 25.79(12) 1_655 1_655 ?
C21 Dy1 C12 117.05(17) 2_765 1_655 ?
O2 Dy2 O2 180.00(9) 2_766 . ?
O2 Dy2 O5 100.73(14) 2_766 2_666 ?
O2 Dy2 O5 79.27(14) . 2_666 ?
O2 Dy2 O5 79.27(14) 2_766 1_655 ?
O2 Dy2 O5 100.73(14) . 1_655 ?
O5 Dy2 O5 180.000(1) 2_666 1_655 ?
O2 Dy2 O9 101.89(17) 2_766 2_766 ?
O2 Dy2 O9 78.11(17) . 2_766 ?
O5 Dy2 O9 107.39(14) 2_666 2_766 ?
O5 Dy2 O9 72.61(14) 1_655 2_766 ?
O2 Dy2 O9 78.11(17) 2_766 . ?
O2 Dy2 O9 101.89(17) . . ?
O5 Dy2 O9 72.61(14) 2_666 . ?
O5 Dy2 O9 107.39(14) 1_655 . ?
O9 Dy2 O9 180.000(1) 2_766 . ?
O2 Dy2 O10 79.71(16) 2_766 2_766 ?
O2 Dy2 O10 100.29(16) . 2_766 ?
O5 Dy2 O10 66.78(13) 2_666 2_766 ?
O5 Dy2 O10 113.22(13) 1_655 2_766 ?
O9 Dy2 O10 51.50(12) 2_766 2_766 ?
O9 Dy2 O10 128.50(12) . 2_766 ?
O2 Dy2 O10 100.29(16) 2_766 . ?
O2 Dy2 O10 79.71(16) . . ?
O5 Dy2 O10 113.22(13) 2_666 . ?
O5 Dy2 O10 66.78(13) 1_655 . ?
O9 Dy2 O10 128.50(12) 2_766 . ?
O9 Dy2 O10 51.50(12) . . ?
O10 Dy2 O10 180.000(1) 2_766 . ?
O2 Dy2 C17 90.49(17) 2_766 2_766 ?
O2 Dy2 C17 89.51(17) . 2_766 ?
O5 Dy2 C17 87.45(14) 2_666 2_766 ?
O5 Dy2 C17 92.55(14) 1_655 2_766 ?
O9 Dy2 C17 25.54(13) 2_766 2_766 ?
O9 Dy2 C17 154.46(13) . 2_766 ?
O10 Dy2 C17 25.97(13) 2_766 2_766 ?
O10 Dy2 C17 154.03(13) . 2_766 ?
C1 O1 Dy1 137.1(4) . . ?
C17 O10 Dy1 160.0(4) . . ?
C17 O10 Dy2 90.5(3) . . ?
Dy1 O10 Dy2 107.81(13) . . ?
C12 O5 Dy2 150.2(4) . 1_455 ?
C12 O5 Dy1 88.5(3) . 1_455 ?
Dy2 O5 Dy1 106.65(14) 1_455 1_455 ?
C5 O4 Dy1 151.9(4) . 2_666 ?
C1 O2 Dy2 123.9(4) . . ?
C12 O6 Dy1 100.5(3) . 1_455 ?
C17 O9 Dy2 98.2(3) . . ?
C15 O8 Dy1 141.7(4) . 2_656 ?
O1 C1 O2 123.3(6) . . ?
O1 C1 C2 120.5(5) . . ?
O2 C1 C2 116.3(5) . . ?
C3 C2 C8 120.0(5) . . ?
C3 C2 C1 118.9(5) . . ?
C8 C2 C1 120.7(5) . . ?
C4 C3 C2 120.6(5) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
O9 C17 O10 119.8(5) . . ?
O9 C17 C18 119.0(5) . . ?
O10 C17 C18 121.2(5) . . ?
C19 C18 C24 120.3(5) . . ?
C19 C18 C17 121.9(5) . . ?
C24 C18 C17 117.7(5) . . ?
C20 C19 C18 118.7(5) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
O4 C5 O3 124.2(5) . . ?
O4 C5 C4 120.6(5) . . ?
O3 C5 C4 115.2(5) . . ?
O6 C12 O5 120.3(5) . . ?
O6 C12 C11 120.4(5) . . ?
O5 C12 C11 119.2(4) . . ?
O6 C12 Dy1 54.8(3) . 1_455 ?
O5 C12 Dy1 65.7(3) . 1_455 ?
C11 C12 Dy1 170.8(4) . 1_455 ?
C13 C11 C10 119.0(5) . . ?
C13 C11 C12 120.2(5) . . ?
C10 C11 C12 120.7(5) . . ?
C11 C10 C9 121.8(5) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C16 C9 C10 117.9(5) . . ?
C16 C9 C7 123.1(5) . . ?
C10 C9 C7 118.9(5) . . ?
C8 C7 C6 119.3(5) . . ?
C8 C7 C9 121.5(5) . . ?
C6 C7 C9 119.1(5) . . ?
C7 C6 C4 120.9(5) . . ?
C7 C6 H6 119.6 . . ?
C4 C6 H6 119.6 . . ?
C3 C4 C6 119.4(5) . . ?
C3 C4 C5 121.8(5) . . ?
C6 C4 C5 118.5(5) . . ?
C7 C8 C2 119.9(5) . . ?
C7 C8 H8 120.1 . . ?
C2 C8 H8 120.1 . . ?
C23 C24 C18 121.8(5) . . ?
C23 C24 H24 119.1 . . ?
C18 C24 H24 119.1 . . ?
C23 C22 C20 121.6(5) . . ?
C23 C22 H22 119.2 . . ?
C20 C22 H22 119.2 . . ?
C19 C20 C22 120.1(5) . . ?
C19 C20 C21 121.4(5) . . ?
C22 C20 C21 118.5(5) . . ?
C24 C23 C22 117.4(5) . . ?
C24 C23 C23 120.5(6) . 2_775 ?
C22 C23 C23 122.1(7) . 2_775 ?
C9 C16 C14 121.1(5) . . ?
C9 C16 H16 119.4 . . ?
C14 C16 H16 119.4 . . ?
C11 C13 C14 120.3(5) . . ?
C11 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C16 C14 C13 120.0(5) . . ?
C16 C14 C15 121.6(5) . . ?
C13 C14 C15 118.4(5) . . ?
O8 C15 O7 122.4(5) . . ?
O8 C15 C14 118.5(5) . . ?
O7 C15 C14 119.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.805
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.147

# SQUEEZE RESULTS 
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 0.500 1.047 0.000 638.3 137.5
_platon_squeeze_details          
;
;
#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939030'
#######################################################################
#
#                 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            'C19 H6 Er2 O16 '
_chemical_formula_weight         824.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.318(4)
_cell_length_b                   14.082(3)
_cell_length_c                   8.8793(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.31(3)
_cell_angle_gamma                90.00
_cell_volume                     2376.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4383
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.45

_exptl_crystal_description       sheet
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    7.093
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_T_max  0.242
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2713
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.45
_reflns_number_total             2713
_reflns_number_gt                2562
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

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

_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)+(0.0178P)²+7.1298P] 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         2713
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0193
_refine_ls_wR_factor_ref         0.0476
_refine_ls_wR_factor_gt          0.0471
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.004
_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
O2 O 0.19967(11) 0.30406(14) 0.1467(2) 0.0159(4) Uani 1 1 d . . .
O1 O 0.09074(11) 0.25276(15) 0.0893(3) 0.0201(5) Uani 1 1 d . . .
C1 C 0.13606(16) 0.31634(19) 0.0833(3) 0.0127(5) Uani 1 1 d . . .
C9 C 0.5000 0.6330(3) 0.2500 0.0232(10) Uani 1 2 d S . .
O8 O 0.30365(15) 0.62736(16) 0.4930(3) 0.0263(6) Uani 1 1 d . . .
Er1 Er 0.328467(6) 0.651634(7) 0.241836(13) 0.00868(5) Uani 1 1 d . . .
O4 O 0.21438(12) 0.66769(15) 0.1335(3) 0.0192(5) Uani 1 1 d . . .
O3 O 0.35120(12) 0.76107(13) 0.0656(2) 0.0170(4) Uani 1 1 d . . .
O6 O 0.31189(14) 0.48837(14) 0.2787(3) 0.0214(5) Uani 1 1 d . . .
C6 C 0.12755(15) 0.57595(18) -0.0266(3) 0.0116(5) Uani 1 1 d . . .
O7 O 0.44270(11) 0.59175(16) 0.2513(3) 0.0249(5) Uani 1 1 d . . .
C8 C 0.16701(15) 0.66745(18) 0.0168(3) 0.0107(5) Uani 1 1 d . . .
O5 O 0.32601(15) 0.56182(14) 0.0171(3) 0.0257(5) Uani 1 1 d . . .
C10 C 0.30864(17) 0.4261(2) 0.3778(3) 0.0181(6) Uani 1 1 d . . .
C7 C 0.15136(15) 0.49123(19) 0.0460(3) 0.0129(5) Uani 1 1 d . . .
H7 H 0.1915 0.4903 0.1215 0.016 Uiso 1 1 calc R . .
C5 C 0.06882(15) 0.57657(18) -0.1428(3) 0.0120(5) Uani 1 1 d . . .
H5 H 0.0543 0.6334 -0.1918 0.014 Uiso 1 1 calc R . .
C2 C 0.11385(15) 0.40789(19) 0.0032(3) 0.0134(5) Uani 1 1 d . . .
C4 C 0.03120(15) 0.49317(19) -0.1875(3) 0.0119(5) Uani 1 1 d . . .
C3 C 0.05401(16) 0.41034(19) -0.1092(3) 0.0143(6) Uani 1 1 d . . .
H3 H 0.0283 0.3548 -0.1329 0.017 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C1 1.268(4) . ?
O2 Er1 2.465(2) 4_545 ?
O1 C1 1.260(3) . ?
O1 Er1 2.423(2) 4_545 ?
C1 C2 1.498(4) . ?
C1 Er1 2.807(3) 4_545 ?
C9 O7 1.252(3) 2_655 ?
C9 O7 1.252(3) . ?
O8 Er1 2.388(2) . ?
Er1 O4 2.253(2) . ?
Er1 O3 2.294(2) . ?
Er1 O7 2.350(2) . ?
Er1 O6 2.352(2) . ?
Er1 O5 2.356(2) . ?
Er1 O1 2.423(2) 4 ?
Er1 O2 2.465(2) 4 ?
Er1 C1 2.807(3) 4 ?
O4 C8 1.253(4) . ?
O3 C8 1.257(3) 7_565 ?
O6 C10 1.252(4) . ?
C6 C5 1.390(4) . ?
C6 C7 1.394(4) . ?
C6 C8 1.512(4) . ?
C8 O3 1.257(3) 7_565 ?
O5 C10 1.234(4) 6_565 ?
C10 O5 1.234(4) 6_566 ?
C7 C2 1.396(4) . ?
C5 C4 1.401(4) . ?
C2 C3 1.386(4) . ?
C4 C3 1.389(4) . ?
C4 C4 1.485(6) 2_554 ?

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
C1 O2 Er1 91.78(16) . 4_545 ?
C1 O1 Er1 93.92(17) . 4_545 ?
O1 C1 O2 120.6(2) . . ?
O1 C1 C2 119.3(3) . . ?
O2 C1 C2 120.0(2) . . ?
O1 C1 Er1 59.47(15) . 4_545 ?
O2 C1 Er1 61.37(14) . 4_545 ?
C2 C1 Er1 174.2(2) . 4_545 ?
O7 C9 O7 124.8(4) 2_655 . ?
O4 Er1 O3 86.19(8) . . ?
O4 Er1 O7 153.14(8) . . ?
O3 Er1 O7 88.41(8) . . ?
O4 Er1 O6 90.59(8) . . ?
O3 Er1 O6 143.03(8) . . ?
O7 Er1 O6 78.15(8) . . ?
O4 Er1 O5 79.77(9) . . ?
O3 Er1 O5 76.12(7) . . ?
O7 Er1 O5 73.39(9) . . ?
O6 Er1 O5 67.08(7) . . ?
O4 Er1 O8 93.92(10) . . ?
O3 Er1 O8 145.92(7) . . ?
O7 Er1 O8 105.03(9) . . ?
O6 Er1 O8 71.03(8) . . ?
O5 Er1 O8 137.49(8) . . ?
O4 Er1 O1 132.66(7) . 4 ?
O3 Er1 O1 81.17(8) . 4 ?
O7 Er1 O1 72.06(8) . 4 ?
O6 Er1 O1 125.23(8) . 4 ?
O5 Er1 O1 138.80(8) . 4 ?
O8 Er1 O1 73.82(9) . 4 ?
O4 Er1 O2 79.33(7) . 4 ?
O3 Er1 O2 76.82(7) . 4 ?
O7 Er1 O2 124.84(7) . 4 ?
O6 Er1 O2 138.59(7) . 4 ?
O5 Er1 O2 146.65(8) . 4 ?
O8 Er1 O2 69.76(7) . 4 ?
O1 Er1 O2 53.40(7) 4 4 ?
O4 Er1 C1 106.05(8) . 4 ?
O3 Er1 C1 76.39(8) . 4 ?
O7 Er1 C1 98.16(8) . 4 ?
O6 Er1 C1 139.16(8) . 4 ?
O5 Er1 C1 151.41(8) . 4 ?
O8 Er1 C1 70.84(8) . 4 ?
O1 Er1 C1 26.61(8) 4 4 ?
O2 Er1 C1 26.85(8) 4 4 ?
C8 O4 Er1 150.0(2) . . ?
C8 O3 Er1 150.1(2) 7_565 . ?
C10 O6 Er1 143.9(2) . . ?
C5 C6 C7 120.4(2) . . ?
C5 C6 C8 119.4(2) . . ?
C7 C6 C8 120.1(3) . . ?
C9 O7 Er1 131.3(2) . . ?
O4 C8 O3 124.5(3) . 7_565 ?
O4 C8 C6 118.3(2) . . ?
O3 C8 C6 117.3(3) 7_565 . ?
C10 O5 Er1 137.3(2) 6_565 . ?
O5 C10 O6 124.7(3) 6_566 . ?
C6 C7 C2 118.8(3) . . ?
C6 C5 C4 121.2(2) . . ?
C3 C2 C7 120.0(2) . . ?
C3 C2 C1 119.6(2) . . ?
C7 C2 C1 120.2(3) . . ?
C3 C4 C5 117.4(3) . . ?
C3 C4 C4 121.10(17) . 2_554 ?
C5 C4 C4 121.49(17) . 2_554 ?
C2 C3 C4 122.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.161

#End of Crystallographic Information File
_database_code_depnum_ccdc_archive 'CCDC 939031'
