# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 723332'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C75 H72 La2 O40, 2(C6 N)'
_chemical_formula_sum            'C87 H72 La2 N2 O40'
_chemical_formula_weight         2063.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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'

_cell_length_a                   20.164(4)
_cell_length_b                   16.345(5)
_cell_length_c                   16.679(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5497(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31231
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.53

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2084
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41258
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9683
_reflns_number_gt                6359
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
dfix 1.5 0.01 c43 c44  c41 c42
dfix 1.5 0.01 n1 c39 n1 c43 c39 c40
isor 0.01 c39 c40 c13 c22 c23 c24 c38 c41 c44 o21 o22 c42 c43
;

_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)+(0.1279P)²+0.5105P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(4)
_refine_ls_number_reflns         9558
_refine_ls_number_parameters     602
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.2095
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2699(5) 0.7758(6) 0.9213(6) 0.060(2) Uani 1 1 d . . .
C2 C 0.2081(6) 0.7919(8) 0.9553(9) 0.089(4) Uani 1 1 d . . .
H2 H 0.2027 0.8325 0.9938 0.107 Uiso 1 1 calc R . .
C3 C 0.1551(7) 0.7450(10) 0.9292(11) 0.107(5) Uani 1 1 d . . .
H3 H 0.1138 0.7539 0.9525 0.128 Uiso 1 1 calc R . .
C4 C 0.1600(7) 0.6869(9) 0.8719(14) 0.120(6) Uani 1 1 d . . .
H4 H 0.1223 0.6610 0.8522 0.144 Uiso 1 1 calc R . .
C5 C 0.2218(9) 0.6669(8) 0.8432(10) 0.107(5) Uani 1 1 d . . .
H5 H 0.2270 0.6226 0.8088 0.128 Uiso 1 1 calc R . .
C6 C 0.2781(6) 0.7146(7) 0.8665(9) 0.086(4) Uani 1 1 d . . .
H6 H 0.3197 0.7040 0.8446 0.103 Uiso 1 1 calc R . .
C7 C 0.3262(5) 0.8289(6) 0.9447(5) 0.054(2) Uani 1 1 d . . .
C8 C 0.4418(4) 0.8568(5) 0.9314(5) 0.050(2) Uani 1 1 d . . .
H8 H 0.4285 0.9138 0.9231 0.060 Uiso 1 1 calc R . .
C9 C 0.4670(5) 0.8473(6) 1.0203(5) 0.055(2) Uani 1 1 d . . .
C10 C 0.5943(7) 0.6541(9) 0.8762(9) 0.096(4) Uani 1 1 d . . .
C11 C 0.5642(8) 0.6099(11) 0.9387(11) 0.128(6) Uani 1 1 d . . .
H11 H 0.5279 0.6326 0.9651 0.153 Uiso 1 1 calc R . .
C12 C 0.5874(9) 0.5323(9) 0.9623(13) 0.132(6) Uani 1 1 d . . .
H12 H 0.5674 0.5041 1.0042 0.159 Uiso 1 1 calc R . .
C13 C 0.6418(9) 0.4983(11) 0.9208(11) 0.126(5) Uani 1 1 d U . .
H13 H 0.6638 0.4528 0.9412 0.151 Uiso 1 1 calc R . .
C14 C 0.6644(10) 0.5377(13) 0.8405(18) 0.191(12) Uani 1 1 d . . .
H14 H 0.6885 0.5087 0.8024 0.229 Uiso 1 1 calc R . .
C15 C 0.6475(7) 0.6141(8) 0.8299(9) 0.095(4) Uani 1 1 d . . .
H15 H 0.6700 0.6446 0.7914 0.114 Uiso 1 1 calc R . .
C16 C 0.5739(5) 0.7311(7) 0.8522(7) 0.070(3) Uani 1 1 d . . .
C17 C 0.4947(6) 0.8364(5) 0.8721(5) 0.0522(19) Uani 1 1 d . . .
H17 H 0.5319 0.8743 0.8799 0.063 Uiso 1 1 calc R . .
C18 C 0.4698(5) 0.8445(5) 0.7843(6) 0.054(2) Uani 1 1 d . . .
C19 C 0.1966(5) 0.8959(6) 0.3898(6) 0.059(2) Uani 1 1 d . . .
C20 C 0.1679(6) 0.8183(7) 0.3878(7) 0.074(3) Uani 1 1 d . . .
H20 H 0.1945 0.7719 0.3895 0.089 Uiso 1 1 calc R . .
C21 C 0.1008(7) 0.8107(8) 0.3834(9) 0.099(5) Uani 1 1 d . . .
H21 H 0.0808 0.7594 0.3829 0.119 Uiso 1 1 calc R . .
C22 C 0.0634(8) 0.8805(11) 0.3797(12) 0.120(5) Uani 1 1 d U . .
H22 H 0.0177 0.8759 0.3733 0.144 Uiso 1 1 calc R . .
C23 C 0.0894(9) 0.9529(12) 0.3848(14) 0.064(5) Uani 0.50 1 d PU . .
H23 H 0.0621 0.9987 0.3852 0.077 Uiso 1 1 calc R . .
C24 C 0.1576(7) 0.9626(8) 0.3896(10) 0.102(4) Uani 1 1 d U . .
H24 H 0.1761 1.0146 0.3926 0.122 Uiso 1 1 calc R . .
C25 C 0.2698(6) 0.9027(7) 0.3935(6) 0.065(3) Uani 1 1 d . . .
C26 C 0.3584(4) 0.9968(6) 0.3836(5) 0.0479(17) Uani 1 1 d . . .
H26 H 0.3862 0.9525 0.4047 0.057 Uiso 1 1 calc R . .
C27 C 0.3668(4) 1.0022(6) 0.2935(5) 0.0498(17) Uani 1 1 d . . .
C28 C 0.3009(5) 1.2774(6) 0.3861(6) 0.064(3) Uani 1 1 d . . .
C29 C 0.2453(6) 1.2566(8) 0.3504(8) 0.080(3) Uani 1 1 d . . .
H29 H 0.2387 1.2019 0.3375 0.096 Uiso 1 1 calc R . .
C30 C 0.1942(8) 1.3142(11) 0.3305(10) 0.107(5) Uani 1 1 d . . .
H30 H 0.1557 1.2987 0.3038 0.128 Uiso 1 1 calc R . .
C31 C 0.2056(9) 1.3912(11) 0.3527(11) 0.118(6) Uani 1 1 d . . .
H31 H 0.1730 1.4303 0.3430 0.142 Uiso 1 1 calc R . .
C32 C 0.2631(9) 1.4151(8) 0.3890(9) 0.101(5) Uani 1 1 d . . .
H32 H 0.2703 1.4702 0.3999 0.121 Uiso 1 1 calc R . .
C33 C 0.3104(8) 1.3586(6) 0.4096(8) 0.097(4) Uani 1 1 d . . .
H33 H 0.3478 1.3739 0.4385 0.116 Uiso 1 1 calc R . .
C34 C 0.3546(6) 1.2170(6) 0.4053(6) 0.060(2) Uani 1 1 d . . .
C35 C 0.3772(4) 1.0781(5) 0.4250(5) 0.0467(19) Uani 1 1 d . . .
H35 H 0.4220 1.0929 0.4076 0.056 Uiso 1 1 calc R . .
C36 C 0.3783(5) 1.0681(5) 0.5172(5) 0.050(2) Uani 1 1 d . . .
C37 C 0.4495(7) 0.8200(6) 0.5276(6) 0.079(3) Uani 1 1 d . . .
H37A H 0.4065 0.7964 0.5364 0.118 Uiso 1 1 calc R . .
H37B H 0.4800 0.7780 0.5116 0.118 Uiso 1 1 calc R . .
H37C H 0.4466 0.8606 0.4862 0.118 Uiso 1 1 calc R . .
C38 C 0.4739(9) 0.8172(10) 0.2770(11) 0.124(6) Uani 1 1 d U . .
H38A H 0.4829 0.8554 0.3193 0.187 Uiso 1 1 calc R . .
H38B H 0.5042 0.7720 0.2806 0.187 Uiso 1 1 calc R . .
H38C H 0.4293 0.7975 0.2818 0.187 Uiso 1 1 calc R . .
C39 C 0.7556(14) 0.9003(19) 0.9138(16) 0.213(12) Uani 1 1 d DU . .
C40 C 0.6891(16) 0.9363(19) 0.898(2) 0.221(12) Uani 1 1 d DU . .
C41 C 0.7744(18) 0.966(2) 0.797(3) 0.275(17) Uani 1 1 d DU . .
C42 C 0.8227(16) 1.0338(19) 0.818(2) 0.214(12) Uani 1 1 d DU . .
C43 C 0.7702(18) 0.8182(13) 0.801(2) 0.285(18) Uani 1 1 d DU . .
C44 C 0.8009(12) 0.7399(16) 0.8260(16) 0.164(8) Uani 1 1 d DU . .
La1 La 0.5000 1.0000 0.65223(3) 0.0456(2) Uani 1 2 d S . .
La2 La 0.5000 1.0000 0.15580(3) 0.0454(2) Uani 1 2 d S . .
N1 N 0.8019(10) 0.8887(11) 0.8437(15) 0.185(9) Uani 1 1 d D . .
O1 O 0.3843(3) 0.8039(4) 0.9152(4) 0.0577(16) Uani 1 1 d . . .
O2 O 0.3215(3) 0.8901(5) 0.9889(5) 0.077(2) Uani 1 1 d . . .
O3 O 0.4463(4) 0.7870(4) 1.0609(4) 0.073(2) Uani 1 1 d . . .
O4 O 0.5062(3) 0.9017(4) 1.0417(3) 0.0572(14) Uani 1 1 d . . .
O5 O 0.6074(4) 0.7784(5) 0.8110(5) 0.079(2) Uani 1 1 d . . .
O6 O 0.5173(3) 0.7550(4) 0.8887(4) 0.0584(16) Uani 1 1 d . . .
O7 O 0.4630(4) 0.7830(4) 0.7438(4) 0.0637(17) Uani 1 1 d . . .
O8 O 0.4568(4) 0.9169(4) 0.7642(4) 0.0629(17) Uani 1 1 d . . .
O9 O 0.2902(3) 0.9815(3) 0.4034(4) 0.0545(15) Uani 1 1 d . . .
O10 O 0.3082(4) 0.8463(4) 0.3845(6) 0.084(2) Uani 1 1 d . . .
O11 O 0.3200(3) 0.9857(5) 0.2476(3) 0.0642(17) Uani 1 1 d . . .
O12 O 0.4248(3) 1.0225(4) 0.2689(3) 0.0613(18) Uani 1 1 d . . .
O13 O 0.3336(3) 1.1393(4) 0.3984(4) 0.0553(15) Uani 1 1 d . . .
O14 O 0.4107(4) 1.2339(4) 0.4248(5) 0.080(2) Uani 1 1 d . . .
O15 O 0.3397(4) 1.1106(4) 0.5589(4) 0.0686(18) Uani 1 1 d . . .
O16 O 0.4207(3) 1.0173(4) 0.5425(3) 0.0577(16) Uani 1 1 d . . .
O17 O 0.3995(3) 1.0851(4) 0.7009(4) 0.0607(16) Uani 1 1 d . . .
H556 H 0.3713 1.0659 0.7338 0.5(3) Uiso 1 1 d R . .
H557 H 0.3785 1.1016 0.6598 0.15(7) Uiso 1 1 d R . .
O18 O 0.4729(4) 0.8580(4) 0.6017(4) 0.0709(19) Uani 1 1 d . . .
H104 H 0.4587 0.8242 0.6365 0.106 Uiso 1 1 d R . .
O19 O 0.3817(3) 0.9820(4) 0.1102(4) 0.0610(16) Uani 1 1 d . . .
H558 H 0.3571 0.9855 0.1514 0.06(3) Uiso 1 1 d R . .
H559 H 0.3634 0.9490 0.0777 0.08(4) Uiso 1 1 d R . .
O20 O 0.4816(4) 0.8553(4) 0.2044(4) 0.084(3) Uani 1 1 d . . .
H108 H 0.4974 0.8331 0.1624 0.125 Uiso 1 1 d 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
C1 C6 1.365(16) . ?
C1 C2 1.395(16) . ?
C1 C7 1.481(13) . ?
C2 C3 1.386(18) . ?
C2 H2 0.9300 . ?
C3 C4 1.35(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.37(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.430(17) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.245(11) . ?
C7 O1 1.335(11) . ?
C8 O1 1.472(10) . ?
C8 C17 1.491(13) . ?
C8 C9 1.575(13) . ?
C8 H8 0.9800 . ?
C9 O4 1.242(11) . ?
C9 O3 1.266(11) . ?
C10 C16 1.384(17) . ?
C10 C11 1.40(2) . ?
C10 C15 1.475(18) . ?
C11 C12 1.41(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.41(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.55(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.31(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.236(13) . ?
C16 O6 1.352(12) . ?
C17 O6 1.434(10) . ?
C17 C18 1.555(13) . ?
C17 H17 0.9800 . ?
C18 O7 1.220(11) . ?
C18 O8 1.256(10) . ?
C19 C24 1.345(17) . ?
C19 C20 1.394(14) . ?
C19 C25 1.481(14) . ?
C20 C21 1.360(18) . ?
C20 H20 0.9300 . ?
C21 C22 1.37(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.30(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.39(2) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O10 1.214(13) . ?
C25 O9 1.363(12) . ?
C26 O9 1.436(10) . ?
C26 C27 1.514(12) . ?
C26 C35 1.544(12) . ?
C26 H26 0.9800 . ?
C27 O11 1.246(10) . ?
C27 O12 1.283(10) . ?
C28 C29 1.315(16) . ?
C28 C33 1.398(15) . ?
C28 C34 1.499(14) . ?
C29 C30 1.434(17) . ?
C29 H29 0.9300 . ?
C30 C31 1.33(2) . ?
C30 H30 0.9300 . ?
C31 C32 1.37(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.371(18) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O14 1.210(12) . ?
C34 O13 1.343(11) . ?
C35 O13 1.404(10) . ?
C35 C36 1.547(12) . ?
C35 H35 0.9800 . ?
C36 O15 1.253(10) . ?
C36 O16 1.262(10) . ?
C37 O18 1.462(12) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.371(19) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.489(10) . ?
C39 N1 1.508(10) . ?
C41 C42 1.522(10) . ?
C41 N1 1.59(4) . ?
C43 C44 1.480(10) . ?
C43 N1 1.494(10) . ?
La1 O16 2.448(6) 2_675 ?
La1 O16 2.448(6) . ?
La1 O8 2.469(6) 2_675 ?
La1 O8 2.469(6) . ?
La1 O18 2.529(7) . ?
La1 O18 2.529(7) 2_675 ?
La1 O17 2.589(7) 2_675 ?
La1 O17 2.589(7) . ?
La2 O12 2.448(6) 2_675 ?
La2 O12 2.448(6) . ?
La2 O4 2.494(6) 1_554 ?
La2 O4 2.494(6) 2_674 ?
La2 O19 2.521(7) 2_675 ?
La2 O19 2.521(7) . ?
La2 O20 2.528(6) 2_675 ?
La2 O20 2.528(6) . ?
O4 La2 2.494(6) 1_556 ?
O17 H556 0.8505 . ?
O17 H557 0.8489 . ?
O18 H104 0.8499 . ?
O19 H558 0.8487 . ?
O19 H559 0.8496 . ?
O20 H108 0.8501 . ?

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
C6 C1 C2 121.2(10) . . ?
C6 C1 C7 120.9(9) . . ?
C2 C1 C7 117.8(10) . . ?
C3 C2 C1 117.2(13) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C4 C3 C2 123.7(14) . . ?
C4 C3 H3 118.2 . . ?
C2 C3 H3 118.2 . . ?
C3 C4 C5 118.7(14) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C4 C5 C6 119.7(14) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 119.0(12) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
O2 C7 O1 122.1(8) . . ?
O2 C7 C1 124.6(9) . . ?
O1 C7 C1 113.3(8) . . ?
O1 C8 C17 108.1(7) . . ?
O1 C8 C9 111.6(7) . . ?
C17 C8 C9 111.8(7) . . ?
O1 C8 H8 108.4 . . ?
C17 C8 H8 108.4 . . ?
C9 C8 H8 108.4 . . ?
O4 C9 O3 127.9(8) . . ?
O4 C9 C8 113.8(8) . . ?
O3 C9 C8 118.3(8) . . ?
C16 C10 C11 123.6(13) . . ?
C16 C10 C15 117.8(12) . . ?
C11 C10 C15 118.5(14) . . ?
C10 C11 C12 121.7(17) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C13 118.5(17) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C12 C13 C14 119.1(16) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 115.9(18) . . ?
C15 C14 H14 122.0 . . ?
C13 C14 H14 122.0 . . ?
C14 C15 C10 122.7(15) . . ?
C14 C15 H15 118.6 . . ?
C10 C15 H15 118.6 . . ?
O5 C16 O6 122.1(10) . . ?
O5 C16 C10 124.6(11) . . ?
O6 C16 C10 112.5(10) . . ?
O6 C17 C8 107.8(7) . . ?
O6 C17 C18 111.3(7) . . ?
C8 C17 C18 112.0(8) . . ?
O6 C17 H17 108.5 . . ?
C8 C17 H17 108.5 . . ?
C18 C17 H17 108.5 . . ?
O7 C18 O8 127.3(9) . . ?
O7 C18 C17 119.2(8) . . ?
O8 C18 C17 113.5(8) . . ?
C24 C19 C20 119.6(11) . . ?
C24 C19 C25 121.5(10) . . ?
C20 C19 C25 119.0(10) . . ?
C21 C20 C19 119.9(12) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 118.3(12) . . ?
C20 C21 H21 120.9 . . ?
C22 C21 H21 120.9 . . ?
C23 C22 C21 122.3(16) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 120.6(18) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C19 C24 C23 119.2(14) . . ?
C19 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
O10 C25 O9 122.7(10) . . ?
O10 C25 C19 125.0(10) . . ?
O9 C25 C19 112.2(9) . . ?
O9 C26 C27 110.2(6) . . ?
O9 C26 C35 106.4(7) . . ?
C27 C26 C35 111.5(7) . . ?
O9 C26 H26 109.6 . . ?
C27 C26 H26 109.6 . . ?
C35 C26 H26 109.6 . . ?
O11 C27 O12 123.4(8) . . ?
O11 C27 C26 120.8(7) . . ?
O12 C27 C26 115.8(7) . . ?
C29 C28 C33 119.3(11) . . ?
C29 C28 C34 122.9(10) . . ?
C33 C28 C34 117.8(11) . . ?
C28 C29 C30 123.3(13) . . ?
C28 C29 H29 118.4 . . ?
C30 C29 H29 118.4 . . ?
C31 C30 C29 115.6(15) . . ?
C31 C30 H30 122.2 . . ?
C29 C30 H30 122.2 . . ?
C30 C31 C32 122.7(14) . . ?
C30 C31 H31 118.7 . . ?
C32 C31 H31 118.7 . . ?
C31 C32 C33 120.6(14) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C28 118.4(14) . . ?
C32 C33 H33 120.8 . . ?
C28 C33 H33 120.8 . . ?
O14 C34 O13 122.2(9) . . ?
O14 C34 C28 125.6(10) . . ?
O13 C34 C28 112.2(9) . . ?
O13 C35 C26 108.6(7) . . ?
O13 C35 C36 113.5(7) . . ?
C26 C35 C36 110.9(7) . . ?
O13 C35 H35 107.9 . . ?
C26 C35 H35 107.9 . . ?
C36 C35 H35 107.9 . . ?
O15 C36 O16 126.8(8) . . ?
O15 C36 C35 118.9(8) . . ?
O16 C36 C35 114.3(7) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N1 118(3) . . ?
C42 C41 N1 104(3) . . ?
C44 C43 N1 111(2) . . ?
O16 La1 O16 83.2(3) 2_675 . ?
O16 La1 O8 113.5(2) 2_675 2_675 ?
O16 La1 O8 137.1(2) . 2_675 ?
O16 La1 O8 137.1(2) 2_675 . ?
O16 La1 O8 113.5(2) . . ?
O8 La1 O8 81.7(3) 2_675 . ?
O16 La1 O18 77.6(2) 2_675 . ?
O16 La1 O18 73.5(2) . . ?
O8 La1 O18 146.5(2) 2_675 . ?
O8 La1 O18 70.8(2) . . ?
O16 La1 O18 73.5(2) 2_675 2_675 ?
O16 La1 O18 77.6(2) . 2_675 ?
O8 La1 O18 70.8(2) 2_675 2_675 ?
O8 La1 O18 146.5(2) . 2_675 ?
O18 La1 O18 141.1(3) . 2_675 ?
O16 La1 O17 70.2(2) 2_675 2_675 ?
O16 La1 O17 143.9(2) . 2_675 ?
O8 La1 O17 77.4(2) 2_675 2_675 ?
O8 La1 O17 75.1(2) . 2_675 ?
O18 La1 O17 77.3(2) . 2_675 ?
O18 La1 O17 115.4(2) 2_675 2_675 ?
O16 La1 O17 143.9(2) 2_675 . ?
O16 La1 O17 70.2(2) . . ?
O8 La1 O17 75.1(2) 2_675 . ?
O8 La1 O17 77.4(2) . . ?
O18 La1 O17 115.4(2) . . ?
O18 La1 O17 77.3(2) 2_675 . ?
O17 La1 O17 143.4(3) 2_675 . ?
O12 La2 O12 79.2(3) 2_675 . ?
O12 La2 O4 117.4(2) 2_675 1_554 ?
O12 La2 O4 135.7(2) . 1_554 ?
O12 La2 O4 135.7(2) 2_675 2_674 ?
O12 La2 O4 117.4(2) . 2_674 ?
O4 La2 O4 80.5(3) 1_554 2_674 ?
O12 La2 O19 70.3(2) 2_675 2_675 ?
O12 La2 O19 143.2(2) . 2_675 ?
O4 La2 O19 78.3(2) 1_554 2_675 ?
O4 La2 O19 75.1(2) 2_674 2_675 ?
O12 La2 O19 143.2(2) 2_675 . ?
O12 La2 O19 70.3(2) . . ?
O4 La2 O19 75.1(2) 1_554 . ?
O4 La2 O19 78.3(2) 2_674 . ?
O19 La2 O19 144.9(3) 2_675 . ?
O12 La2 O20 78.6(3) 2_675 2_675 ?
O12 La2 O20 72.7(2) . 2_675 ?
O4 La2 O20 147.2(2) 1_554 2_675 ?
O4 La2 O20 69.5(2) 2_674 2_675 ?
O19 La2 O20 81.3(2) 2_675 2_675 ?
O19 La2 O20 110.1(3) . 2_675 ?
O12 La2 O20 72.7(2) 2_675 . ?
O12 La2 O20 78.6(3) . . ?
O4 La2 O20 69.5(2) 1_554 . ?
O4 La2 O20 147.2(2) 2_674 . ?
O19 La2 O20 110.1(3) 2_675 . ?
O19 La2 O20 81.3(2) . . ?
O20 La2 O20 142.6(3) 2_675 . ?
C43 N1 C39 101(2) . . ?
C43 N1 C41 103(2) . . ?
C39 N1 C41 94(2) . . ?
C7 O1 C8 116.4(7) . . ?
C9 O4 La2 130.5(6) . 1_556 ?
C16 O6 C17 116.7(8) . . ?
C18 O8 La1 130.2(6) . . ?
C25 O9 C26 115.2(8) . . ?
C27 O12 La2 140.6(5) . . ?
C34 O13 C35 116.7(7) . . ?
C36 O16 La1 140.1(5) . . ?
La1 O17 H556 121.8 . . ?
La1 O17 H557 107.9 . . ?
H556 O17 H557 107.8 . . ?
C37 O18 La1 137.9(6) . . ?
C37 O18 H104 101.1 . . ?
La1 O18 H104 116.2 . . ?
La2 O19 H558 107.4 . . ?
La2 O19 H559 132.6 . . ?
H558 O19 H559 107.9 . . ?
C38 O20 La2 136.5(9) . . ?
C38 O20 H108 125.2 . . ?
La2 O20 H108 94.6 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.111
# 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 0.000 0.195 652.1 36.4
2 1.000 0.500 0.577 652.1 35.6
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 723334'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 Lu O20, C6 N'
_chemical_formula_sum            'C44 H36 Lu N O20'
_chemical_formula_weight         1073.71

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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'

_cell_length_a                   20.052(7)
_cell_length_b                   16.350(4)
_cell_length_c                   16.623(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5450(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    33741
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.75

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2152
_exptl_absorpt_coefficient_mu    1.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38445
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9615
_reflns_number_gt                6950
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
isor 0.01 c5 c22 c23 o21 o22 c39 c41 c42 c c40 c43 c44
dfix 1.50 0.01 c39 c40 c41 c42 n1 c43
dfix 1.50 0.01 n1 c39 c41 n1
DELU     0.010   0.010 C39 C40 C43 C44 N1 C41 C42
SIMU     0.040   0.080   3.800 C39 C40 C43 C44 N1 C41 C42
;

_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)+(0.0893P)²+3.0508P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_number_reflns         9484
_refine_ls_number_parameters     599
_refine_ls_number_restraints     173
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1698
_refine_ls_wR_factor_gt          0.1549
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2730(5) 0.7804(7) 0.9222(6) 0.057(3) Uani 1 1 d . . .
C2 C 0.2102(6) 0.7987(9) 0.9558(10) 0.091(4) Uani 1 1 d . . .
H2 H 0.2048 0.8428 0.9906 0.110 Uiso 1 1 calc R . .
C3 C 0.1555(7) 0.7478(11) 0.9348(12) 0.113(5) Uani 1 1 d . . .
H3 H 0.1144 0.7564 0.9592 0.135 Uiso 1 1 calc R . .
C4 C 0.1620(8) 0.6874(9) 0.8804(11) 0.105(5) Uani 1 1 d . . .
H4 H 0.1245 0.6588 0.8630 0.126 Uiso 1 1 calc R . .
C5 C 0.2268(8) 0.6670(10) 0.8490(10) 0.106(5) Uani 1 1 d U . .
H5 H 0.2335 0.6221 0.8156 0.127 Uiso 1 1 calc R . .
C6 C 0.2799(6) 0.7193(8) 0.8721(9) 0.085(4) Uani 1 1 d . . .
H6 H 0.3220 0.7097 0.8505 0.102 Uiso 1 1 calc R . .
C7 C 0.3288(5) 0.8378(7) 0.9438(6) 0.055(3) Uani 1 1 d . . .
C8 C 0.4440(4) 0.8695(5) 0.9277(5) 0.0377(19) Uani 1 1 d . . .
H8 H 0.4301 0.9266 0.9212 0.045 Uiso 1 1 calc R . .
C9 C 0.4694(5) 0.8565(6) 1.0123(6) 0.048(2) Uani 1 1 d . . .
C10 C 0.6011(7) 0.6668(9) 0.8658(7) 0.078(4) Uani 1 1 d . . .
C11 C 0.5690(7) 0.6185(9) 0.9274(8) 0.092(4) Uani 1 1 d . . .
H11 H 0.5319 0.6391 0.9542 0.110 Uiso 1 1 calc R . .
C12 C 0.5936(8) 0.5398(10) 0.9473(12) 0.119(6) Uani 1 1 d . . .
H12 H 0.5753 0.5086 0.9885 0.142 Uiso 1 1 calc R . .
C13 C 0.6476(10) 0.5121(13) 0.9004(13) 0.154(9) Uani 1 1 d . . .
H13 H 0.6626 0.4590 0.9092 0.184 Uiso 1 1 calc R . .
C14 C 0.6807(11) 0.5586(14) 0.8411(16) 0.155(10) Uani 1 1 d . . .
H14 H 0.7188 0.5399 0.8150 0.186 Uiso 1 1 calc R . .
C15 C 0.6543(6) 0.6288(9) 0.8257(7) 0.084(4) Uani 1 1 d . . .
H15 H 0.6728 0.6577 0.7829 0.100 Uiso 1 1 calc R . .
C16 C 0.5796(5) 0.7445(7) 0.8468(6) 0.057(3) Uani 1 1 d . . .
C17 C 0.4975(5) 0.8498(5) 0.8673(4) 0.0424(18) Uani 1 1 d . . .
H17 H 0.5343 0.8885 0.8741 0.051 Uiso 1 1 calc R . .
C18 C 0.4723(4) 0.8547(6) 0.7798(5) 0.040(2) Uani 1 1 d . . .
C19 C 0.2038(5) 0.8912(7) 0.3913(6) 0.056(2) Uani 1 1 d . . .
C20 C 0.1738(6) 0.8142(8) 0.3869(8) 0.078(4) Uani 1 1 d . . .
H20 H 0.2007 0.7680 0.3831 0.094 Uiso 1 1 calc R . .
C21 C 0.1071(8) 0.8049(9) 0.3881(9) 0.091(4) Uani 1 1 d . . .
H21 H 0.0897 0.7522 0.3867 0.110 Uiso 1 1 calc R . .
C22 C 0.0663(9) 0.8655(12) 0.3911(12) 0.123(5) Uani 1 1 d U . .
H22 H 0.0204 0.8572 0.3891 0.148 Uiso 1 1 calc R . .
C23 C 0.0938(9) 0.9474(11) 0.3977(12) 0.125(6) Uani 1 1 d U . .
H23 H 0.0659 0.9926 0.4029 0.150 Uiso 1 1 calc R . .
C24 C 0.1661(6) 0.9573(8) 0.3961(9) 0.084(4) Uani 1 1 d . . .
H24 H 0.1852 1.0090 0.3984 0.100 Uiso 1 1 calc R . .
C25 C 0.2764(5) 0.8970(7) 0.3874(5) 0.057(3) Uani 1 1 d . . .
C26 C 0.3657(4) 0.9954(7) 0.3780(4) 0.0444(19) Uani 1 1 d . . .
H26 H 0.3943 0.9515 0.3985 0.053 Uiso 1 1 calc R . .
C27 C 0.3736(4) 0.9994(7) 0.2860(4) 0.0407(17) Uani 1 1 d . . .
C28 C 0.3035(5) 1.2716(7) 0.3855(6) 0.056(3) Uani 1 1 d . . .
C29 C 0.2440(7) 1.2458(8) 0.3476(8) 0.082(4) Uani 1 1 d . . .
H29 H 0.2386 1.1920 0.3306 0.098 Uiso 1 1 calc R . .
C30 C 0.1922(7) 1.3048(10) 0.3360(11) 0.101(5) Uani 1 1 d . . .
H30 H 0.1505 1.2892 0.3169 0.121 Uiso 1 1 calc R . .
C31 C 0.2062(10) 1.3874(11) 0.3544(11) 0.112(6) Uani 1 1 d . . .
H31 H 0.1753 1.4280 0.3423 0.135 Uiso 1 1 calc R . .
C32 C 0.2605(8) 1.4055(9) 0.3873(10) 0.094(5) Uani 1 1 d . . .
H32 H 0.2679 1.4605 0.3985 0.113 Uiso 1 1 calc R . .
C33 C 0.3096(6) 1.3518(7) 0.4080(7) 0.073(3) Uani 1 1 d . . .
H33 H 0.3467 1.3693 0.4369 0.088 Uiso 1 1 calc R . .
C34 C 0.3572(5) 1.2122(7) 0.4018(5) 0.053(2) Uani 1 1 d . . .
C35 C 0.3841(4) 1.0725(6) 0.4192(5) 0.041(2) Uani 1 1 d . . .
H35 H 0.4290 1.0881 0.4015 0.049 Uiso 1 1 calc R . .
C36 C 0.3847(5) 1.0656(6) 0.5121(5) 0.044(2) Uani 1 1 d . . .
C37 C 0.4546(7) 0.8298(7) 0.5256(7) 0.074(4) Uani 1 1 d . . .
H37A H 0.4070 0.8310 0.5197 0.111 Uiso 1 1 calc R . .
H37B H 0.4697 0.7740 0.5255 0.111 Uiso 1 1 calc R . .
H37C H 0.4749 0.8587 0.4817 0.111 Uiso 1 1 calc R . .
C38 C 0.4826(8) 0.8254(10) 0.2698(8) 0.099(5) Uani 1 1 d . . .
H38A H 0.4384 0.8309 0.2914 0.149 Uiso 1 1 calc R . .
H38B H 0.5140 0.8503 0.3058 0.149 Uiso 1 1 calc R . .
H38C H 0.4931 0.7684 0.2637 0.149 Uiso 1 1 calc R . .
C39 C 0.759(2) -0.098(2) 0.910(2) 0.272(9) Uani 1 1 d DU . .
C40 C 0.694(2) -0.058(3) 0.890(3) 0.295(12) Uani 1 1 d DU . .
C43 C 0.798(2) -0.195(3) 0.807(3) 0.269(9) Uani 1 1 d DU . .
C44 C 0.805(2) -0.269(3) 0.836(2) 0.241(11) Uani 1 1 d U . .
Lu1 Lu 0.5000 1.0000 0.64519(2) 0.03730(15) Uani 1 2 d S . .
Lu2 Lu 0.5000 1.0000 0.15152(2) 0.03703(15) Uani 1 2 d S . .
N1 N 0.8054(16) -0.110(2) 0.839(2) 0.268(8) Uani 1 1 d DU . .
O1 O 0.3875(3) 0.8151(4) 0.9089(3) 0.0486(15) Uani 1 1 d . . .
O2 O 0.3231(3) 0.8996(5) 0.9854(4) 0.068(2) Uani 1 1 d . . .
O3 O 0.4507(4) 0.7954(4) 1.0541(4) 0.0596(19) Uani 1 1 d . . .
O4 O 0.5073(3) 0.9132(4) 1.0389(3) 0.0511(15) Uani 1 1 d . . .
O5 O 0.6089(4) 0.7907(5) 0.8036(4) 0.073(2) Uani 1 1 d . . .
O6 O 0.5217(3) 0.7678(4) 0.8841(3) 0.0499(16) Uani 1 1 d . . .
O7 O 0.4659(3) 0.7910(4) 0.7405(4) 0.0559(17) Uani 1 1 d . . .
O8 O 0.4613(3) 0.9263(4) 0.7559(4) 0.0513(15) Uani 1 1 d . . .
O9 O 0.2977(3) 0.9759(4) 0.3976(3) 0.0442(14) Uani 1 1 d . . .
O10 O 0.3155(4) 0.8412(5) 0.3760(6) 0.078(2) Uani 1 1 d . . .
O11 O 0.3247(3) 0.9840(5) 0.2422(3) 0.062(2) Uani 1 1 d . . .
O12 O 0.4313(3) 1.0176(4) 0.2625(3) 0.0509(18) Uani 1 1 d . . .
O13 O 0.3384(3) 1.1346(4) 0.3934(4) 0.0469(14) Uani 1 1 d . . .
O14 O 0.4143(4) 1.2321(5) 0.4182(5) 0.072(2) Uani 1 1 d . . .
O15 O 0.3449(3) 1.1051(4) 0.5537(4) 0.0564(17) Uani 1 1 d . . .
O16 O 0.4300(3) 1.0153(4) 0.5372(3) 0.0507(17) Uani 1 1 d . . .
O17 O 0.4040(3) 1.0721(4) 0.6919(3) 0.0521(16) Uani 1 1 d . . .
H445 H 0.3709 1.0643 0.7230 0.063 Uiso 1 1 d R . .
H446 H 0.3907 1.1053 0.6550 0.063 Uiso 1 1 d R . .
O18 O 0.4732(3) 0.8685(4) 0.6010(4) 0.0531(16) Uani 1 1 d . . .
H104 H 0.4590 0.8346 0.6358 0.080 Uiso 1 1 d R . .
O19 O 0.3908(3) 0.9876(4) 0.1087(3) 0.0483(15) Uani 1 1 d . . .
H556 H 0.3648 0.9935 0.1479 0.058 Uiso 1 1 d R . .
H557 H 0.3685 0.9636 0.0709 0.058 Uiso 1 1 d R . .
O20 O 0.4860(3) 0.8651(4) 0.1928(3) 0.0560(19) Uani 1 1 d . . .
H108 H 0.5017 0.8428 0.1507 0.084 Uiso 1 1 d R . .
C41 C 0.800(2) -0.038(2) 0.783(2) 0.274(9) Uani 1 1 d DU . .
C42 C 0.829(2) 0.043(2) 0.811(2) 0.272(11) Uani 1 1 d DU . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.307(15) . ?
C1 C2 1.409(16) . ?
C1 C7 1.505(14) . ?
C2 C3 1.421(18) . ?
C2 H2 0.9300 . ?
C3 C4 1.35(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.44(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.419(18) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.229(11) . ?
C7 O1 1.363(11) . ?
C8 O1 1.475(10) . ?
C8 C17 1.504(12) . ?
C8 C9 1.511(13) . ?
C8 H8 0.9800 . ?
C9 O3 1.272(12) . ?
C9 O4 1.278(11) . ?
C10 C16 1.378(17) . ?
C10 C15 1.404(16) . ?
C10 C11 1.446(17) . ?
C11 C12 1.416(18) . ?
C11 H11 0.9300 . ?
C12 C13 1.41(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.41(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.29(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.196(12) . ?
C16 O6 1.370(12) . ?
C17 O6 1.452(10) . ?
C17 C18 1.542(11) . ?
C17 H17 0.9800 . ?
C18 O7 1.237(11) . ?
C18 O8 1.255(11) . ?
C19 C24 1.321(15) . ?
C19 C20 1.398(15) . ?
C19 C25 1.460(14) . ?
C20 C21 1.346(18) . ?
C20 H20 0.9300 . ?
C21 C22 1.29(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.45(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.46(2) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O10 1.218(13) . ?
C25 O9 1.369(12) . ?
C26 O9 1.436(9) . ?
C26 C35 1.483(13) . ?
C26 C27 1.540(9) . ?
C26 H26 0.9800 . ?
C27 O11 1.248(9) . ?
C27 O12 1.257(9) . ?
C28 C33 1.369(14) . ?
C28 C29 1.414(17) . ?
C28 C34 1.476(14) . ?
C29 C30 1.430(16) . ?
C29 H29 0.9300 . ?
C30 C31 1.41(2) . ?
C30 H30 0.9300 . ?
C31 C32 1.25(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.365(17) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O14 1.221(11) . ?
C34 O13 1.330(11) . ?
C35 O13 1.433(10) . ?
C35 C36 1.548(11) . ?
C35 H35 0.9800 . ?
C36 O15 1.237(11) . ?
C36 O16 1.294(10) . ?
C37 O18 1.453(11) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.436(14) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.491(10) . ?
C39 N1 1.510(10) . ?
C43 C44 1.30(4) . ?
C43 N1 1.501(10) . ?
Lu1 O16 2.293(5) 2_675 ?
Lu1 O16 2.293(5) . ?
Lu1 O8 2.333(6) 2_675 ?
Lu1 O8 2.333(6) . ?
Lu1 O18 2.336(6) . ?
Lu1 O18 2.336(6) 2_675 ?
Lu1 O17 2.387(6) 2_675 ?
Lu1 O17 2.387(6) . ?
Lu2 O19 2.312(5) 2_675 ?
Lu2 O19 2.312(5) . ?
Lu2 O12 2.320(5) 2_675 ?
Lu2 O12 2.320(5) . ?
Lu2 O20 2.328(6) 2_675 ?
Lu2 O20 2.328(6) . ?
Lu2 O4 2.354(5) 1_554 ?
Lu2 O4 2.354(5) 2_674 ?
N1 C41 1.508(10) . ?
O4 Lu2 2.354(5) 1_556 ?
O17 H445 0.8496 . ?
O17 H446 0.8617 . ?
O18 H104 0.8500 . ?
O19 H556 0.8404 . ?
O19 H557 0.8645 . ?
O20 H108 0.8500 . ?
C41 C42 1.506(10) . ?

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
C6 C1 C2 120.7(11) . . ?
C6 C1 C7 123.3(10) . . ?
C2 C1 C7 115.9(10) . . ?
C1 C2 C3 117.8(13) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 121.4(14) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.0(13) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 116.1(14) . . ?
C6 C5 H5 122.0 . . ?
C4 C5 H5 122.0 . . ?
C1 C6 C5 123.6(13) . . ?
C1 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
O2 C7 O1 122.9(9) . . ?
O2 C7 C1 125.3(9) . . ?
O1 C7 C1 111.7(8) . . ?
O1 C8 C17 106.0(7) . . ?
O1 C8 C9 111.8(7) . . ?
C17 C8 C9 110.5(7) . . ?
O1 C8 H8 109.5 . . ?
C17 C8 H8 109.5 . . ?
C9 C8 H8 109.5 . . ?
O3 C9 O4 123.8(9) . . ?
O3 C9 C8 121.3(9) . . ?
O4 C9 C8 114.8(9) . . ?
C16 C10 C15 122.5(11) . . ?
C16 C10 C11 121.9(12) . . ?
C15 C10 C11 115.6(13) . . ?
C12 C11 C10 120.5(14) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 115.5(17) . . ?
C11 C12 H12 122.3 . . ?
C13 C12 H12 122.3 . . ?
C14 C13 C12 125.1(18) . . ?
C14 C13 H13 117.4 . . ?
C12 C13 H13 117.4 . . ?
C15 C14 C13 115.2(18) . . ?
C15 C14 H14 122.4 . . ?
C13 C14 H14 122.4 . . ?
C14 C15 C10 127.7(16) . . ?
C14 C15 H15 116.1 . . ?
C10 C15 H15 116.1 . . ?
O5 C16 C10 124.5(10) . . ?
O5 C16 O6 120.8(10) . . ?
C10 C16 O6 114.7(10) . . ?
O6 C17 C8 108.0(6) . . ?
O6 C17 C18 109.8(7) . . ?
C8 C17 C18 112.7(8) . . ?
O6 C17 H17 108.8 . . ?
C8 C17 H17 108.8 . . ?
C18 C17 H17 108.8 . . ?
O7 C18 O8 126.9(8) . . ?
O7 C18 C17 119.2(9) . . ?
O8 C18 C17 113.9(8) . . ?
C24 C19 C20 119.5(11) . . ?
C24 C19 C25 121.4(11) . . ?
C20 C19 C25 119.1(11) . . ?
C21 C20 C19 121.9(14) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C22 C21 C20 123.1(15) . . ?
C22 C21 H21 118.5 . . ?
C20 C21 H21 118.5 . . ?
C21 C22 C23 118.2(17) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 H22 120.9 . . ?
C22 C23 C24 118.5(16) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C19 C24 C23 118.7(13) . . ?
C19 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
O10 C25 O9 121.7(9) . . ?
O10 C25 C19 126.8(10) . . ?
O9 C25 C19 111.5(10) . . ?
O9 C26 C35 108.7(7) . . ?
O9 C26 C27 109.5(6) . . ?
C35 C26 C27 113.4(8) . . ?
O9 C26 H26 108.4 . . ?
C35 C26 H26 108.4 . . ?
C27 C26 H26 108.4 . . ?
O11 C27 O12 126.3(7) . . ?
O11 C27 C26 119.3(7) . . ?
O12 C27 C26 114.5(6) . . ?
C33 C28 C29 119.0(10) . . ?
C33 C28 C34 121.0(10) . . ?
C29 C28 C34 120.1(10) . . ?
C28 C29 C30 118.1(13) . . ?
C28 C29 H29 121.0 . . ?
C30 C29 H29 121.0 . . ?
C29 C30 C31 118.2(15) . . ?
C29 C30 H30 120.9 . . ?
C31 C30 H30 120.9 . . ?
C32 C31 C30 119.5(15) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 125.8(15) . . ?
C31 C32 H32 117.1 . . ?
C33 C32 H32 117.1 . . ?
C32 C33 C28 118.8(12) . . ?
C32 C33 H33 120.6 . . ?
C28 C33 H33 120.6 . . ?
O14 C34 O13 122.9(10) . . ?
O14 C34 C28 123.3(10) . . ?
O13 C34 C28 113.7(9) . . ?
O13 C35 C26 107.8(7) . . ?
O13 C35 C36 110.8(7) . . ?
C26 C35 C36 113.6(7) . . ?
O13 C35 H35 108.2 . . ?
C26 C35 H35 108.2 . . ?
C36 C35 H35 108.2 . . ?
O15 C36 O16 127.1(8) . . ?
O15 C36 C35 121.0(8) . . ?
O16 C36 C35 112.0(8) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N1 115(3) . . ?
C44 C43 N1 136(4) . . ?
O16 Lu1 O16 77.0(3) 2_675 . ?
O16 Lu1 O8 118.0(2) 2_675 2_675 ?
O16 Lu1 O8 139.9(2) . 2_675 ?
O16 Lu1 O8 139.9(2) 2_675 . ?
O16 Lu1 O8 118.0(2) . . ?
O8 Lu1 O8 75.9(3) 2_675 . ?
O16 Lu1 O18 78.1(2) 2_675 . ?
O16 Lu1 O18 73.3(2) . . ?
O8 Lu1 O18 143.2(2) 2_675 . ?
O8 Lu1 O18 72.3(2) . . ?
O16 Lu1 O18 73.3(2) 2_675 2_675 ?
O16 Lu1 O18 78.1(2) . 2_675 ?
O8 Lu1 O18 72.3(2) 2_675 2_675 ?
O8 Lu1 O18 143.2(2) . 2_675 ?
O18 Lu1 O18 143.3(3) . 2_675 ?
O16 Lu1 O17 72.9(2) 2_675 2_675 ?
O16 Lu1 O17 143.4(2) . 2_675 ?
O8 Lu1 O17 74.3(2) 2_675 2_675 ?
O8 Lu1 O17 75.9(2) . 2_675 ?
O18 Lu1 O17 80.4(2) . 2_675 ?
O18 Lu1 O17 111.8(2) 2_675 2_675 ?
O16 Lu1 O17 143.4(2) 2_675 . ?
O16 Lu1 O17 72.9(2) . . ?
O8 Lu1 O17 75.9(2) 2_675 . ?
O8 Lu1 O17 74.3(2) . . ?
O18 Lu1 O17 111.8(2) . . ?
O18 Lu1 O17 80.4(2) 2_675 . ?
O17 Lu1 O17 142.1(3) 2_675 . ?
O19 Lu2 O19 144.2(3) 2_675 . ?
O19 Lu2 O12 72.14(18) 2_675 2_675 ?
O19 Lu2 O12 142.75(19) . 2_675 ?
O19 Lu2 O12 142.75(19) 2_675 . ?
O19 Lu2 O12 72.14(18) . . ?
O12 Lu2 O12 74.6(3) 2_675 . ?
O19 Lu2 O20 83.9(2) 2_675 2_675 ?
O19 Lu2 O20 106.8(2) . 2_675 ?
O12 Lu2 O20 79.1(2) 2_675 2_675 ?
O12 Lu2 O20 73.7(2) . 2_675 ?
O19 Lu2 O20 106.8(2) 2_675 . ?
O19 Lu2 O20 83.9(2) . . ?
O12 Lu2 O20 73.7(2) 2_675 . ?
O12 Lu2 O20 79.1(2) . . ?
O20 Lu2 O20 145.7(3) 2_675 . ?
O19 Lu2 O4 75.5(2) 2_675 1_554 ?
O19 Lu2 O4 76.2(2) . 1_554 ?
O12 Lu2 O4 121.4(2) 2_675 1_554 ?
O12 Lu2 O4 138.1(2) . 1_554 ?
O20 Lu2 O4 143.0(2) 2_675 1_554 ?
O20 Lu2 O4 70.8(2) . 1_554 ?
O19 Lu2 O4 76.2(2) 2_675 2_674 ?
O19 Lu2 O4 75.5(2) . 2_674 ?
O12 Lu2 O4 138.1(2) 2_675 2_674 ?
O12 Lu2 O4 121.4(2) . 2_674 ?
O20 Lu2 O4 70.8(2) 2_675 2_674 ?
O20 Lu2 O4 143.0(2) . 2_674 ?
O4 Lu2 O4 74.6(3) 1_554 2_674 ?
C43 N1 C41 120(4) . . ?
C43 N1 C39 109(4) . . ?
C41 N1 C39 110(3) . . ?
C7 O1 C8 114.1(7) . . ?
C9 O4 Lu2 132.5(6) . 1_556 ?
C16 O6 C17 116.9(7) . . ?
C18 O8 Lu1 132.2(6) . . ?
C25 O9 C26 118.5(8) . . ?
C27 O12 Lu2 139.8(5) . . ?
C34 O13 C35 117.6(7) . . ?
C36 O16 Lu1 138.8(5) . . ?
Lu1 O17 H445 138.8 . . ?
Lu1 O17 H446 109.2 . . ?
H445 O17 H446 106.7 . . ?
C37 O18 Lu1 137.0(6) . . ?
C37 O18 H104 102.6 . . ?
Lu1 O18 H104 117.5 . . ?
Lu2 O19 H556 109.8 . . ?
Lu2 O19 H557 138.8 . . ?
H556 O19 H557 107.2 . . ?
C38 O20 Lu2 134.1(7) . . ?
C38 O20 H108 124.0 . . ?
Lu2 O20 H108 96.7 . . ?
C42 C41 N1 118(4) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.125
# 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 0.000 0.281 631.1 34.1
2 0.500 0.500 0.426 631.2 35.6
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 723336'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 Gd O20, C6 N'
_chemical_formula_sum            'C44 H36 Gd N O20'
_chemical_formula_weight         1055.99

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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'

_cell_length_a                   20.140(4)
_cell_length_b                   16.625(3)
_cell_length_c                   16.701(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5592.0(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    44304
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2124
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43315
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9846
_reflns_number_gt                8540
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
isor 0.01 C39 C40 C41 C42 C43 C44
dfix 1.5 0.01 n1 c39 c39 c40 c41 c42
DELU     0.010   0.010 C39 C40 C41 C42 C43 C44 N1
SIMU     0.040   0.080   3.800 C39 C40 C41 C42 C43 C44 N1
;

_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)+(0.0428P)²+10.5423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(17)
_refine_ls_number_reflns         9823
_refine_ls_number_parameters     599
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2732(3) 0.7805(4) 0.9208(4) 0.0464(15) Uani 1 1 d . . .
C2 C 0.2117(3) 0.7959(5) 0.9528(5) 0.066(2) Uani 1 1 d . . .
H2 H 0.2062 0.8389 0.9878 0.080 Uiso 1 1 calc R . .
C3 C 0.1579(4) 0.7481(6) 0.9333(7) 0.090(3) Uani 1 1 d . . .
H3 H 0.1168 0.7575 0.9571 0.109 Uiso 1 1 calc R . .
C4 C 0.1651(4) 0.6873(6) 0.8794(7) 0.098(3) Uani 1 1 d . . .
H4 H 0.1281 0.6577 0.8639 0.118 Uiso 1 1 calc R . .
C5 C 0.2263(4) 0.6692(6) 0.8477(6) 0.088(3) Uani 1 1 d . . .
H5 H 0.2314 0.6256 0.8134 0.105 Uiso 1 1 calc R . .
C6 C 0.2811(3) 0.7179(5) 0.8679(5) 0.064(2) Uani 1 1 d . . .
H6 H 0.3226 0.7076 0.8456 0.077 Uiso 1 1 calc R . .
C7 C 0.3283(3) 0.8367(4) 0.9393(4) 0.0438(14) Uani 1 1 d . . .
C8 C 0.4428(2) 0.8674(3) 0.9245(3) 0.0301(11) Uani 1 1 d . . .
H8 H 0.4286 0.9233 0.9174 0.036 Uiso 1 1 calc R . .
C9 C 0.4672(3) 0.8566(4) 1.0116(3) 0.0362(13) Uani 1 1 d . . .
C10 C 0.6022(3) 0.6696(4) 0.8643(4) 0.0459(15) Uani 1 1 d . . .
C11 C 0.5725(4) 0.6229(4) 0.9248(5) 0.0604(19) Uani 1 1 d . . .
H11 H 0.5358 0.6428 0.9522 0.072 Uiso 1 1 calc R . .
C12 C 0.5976(4) 0.5466(4) 0.9440(6) 0.074(2) Uani 1 1 d . . .
H12 H 0.5784 0.5158 0.9843 0.088 Uiso 1 1 calc R . .
C13 C 0.6518(4) 0.5187(5) 0.9014(6) 0.081(3) Uani 1 1 d . . .
H13 H 0.6686 0.4679 0.9129 0.098 Uiso 1 1 calc R . .
C14 C 0.6816(4) 0.5640(5) 0.8426(6) 0.074(2) Uani 1 1 d . . .
H14 H 0.7186 0.5446 0.8153 0.089 Uiso 1 1 calc R . .
C15 C 0.6563(3) 0.6365(5) 0.8253(5) 0.0587(18) Uani 1 1 d . . .
H15 H 0.6762 0.6663 0.7847 0.070 Uiso 1 1 calc R . .
C16 C 0.5795(3) 0.7496(4) 0.8448(4) 0.0417(14) Uani 1 1 d . . .
C17 C 0.4959(3) 0.8493(3) 0.8646(3) 0.0306(10) Uani 1 1 d . . .
H17 H 0.5318 0.8884 0.8716 0.037 Uiso 1 1 calc R . .
C18 C 0.4719(3) 0.8539(3) 0.7787(3) 0.0302(12) Uani 1 1 d . . .
C19 C 0.2062(3) 0.8872(4) 0.3908(4) 0.0511(16) Uani 1 1 d . . .
C20 C 0.1796(4) 0.8098(5) 0.3879(5) 0.068(2) Uani 1 1 d . . .
H20 H 0.2080 0.7660 0.3829 0.082 Uiso 1 1 calc R . .
C21 C 0.1127(5) 0.7966(6) 0.3924(6) 0.086(3) Uani 1 1 d . . .
H21 H 0.0957 0.7447 0.3915 0.103 Uiso 1 1 calc R . .
C22 C 0.0724(5) 0.8599(8) 0.3980(8) 0.114(4) Uani 1 1 d . . .
H22 H 0.0268 0.8511 0.3997 0.136 Uiso 1 1 calc R . .
C23 C 0.0958(4) 0.9390(6) 0.4015(8) 0.112(4) Uani 1 1 d . . .
H23 H 0.0666 0.9822 0.4060 0.134 Uiso 1 1 calc R . .
C24 C 0.1651(4) 0.9513(5) 0.3979(6) 0.075(2) Uani 1 1 d . . .
H24 H 0.1825 1.0031 0.4003 0.090 Uiso 1 1 calc R . .
C25 C 0.2792(3) 0.8981(4) 0.3856(4) 0.0484(16) Uani 1 1 d . . .
C26 C 0.3653(2) 0.9945(4) 0.3746(3) 0.0343(11) Uani 1 1 d . . .
H26 H 0.3947 0.9518 0.3942 0.041 Uiso 1 1 calc R . .
C27 C 0.3721(2) 1.0001(4) 0.2840(3) 0.0335(10) Uani 1 1 d . . .
C28 C 0.3019(3) 1.2683(4) 0.3849(4) 0.0477(15) Uani 1 1 d . . .
C29 C 0.2442(4) 1.2461(5) 0.3477(6) 0.075(2) Uani 1 1 d . . .
H29 H 0.2382 1.1931 0.3313 0.090 Uiso 1 1 calc R . .
C30 C 0.1940(5) 1.3032(7) 0.3345(7) 0.102(4) Uani 1 1 d . . .
H30 H 0.1544 1.2885 0.3098 0.122 Uiso 1 1 calc R . .
C31 C 0.2044(5) 1.3811(7) 0.3585(6) 0.095(3) Uani 1 1 d . . .
H31 H 0.1717 1.4197 0.3501 0.114 Uiso 1 1 calc R . .
C32 C 0.2601(5) 1.4014(5) 0.3932(6) 0.083(3) Uani 1 1 d . . .
H32 H 0.2665 1.4546 0.4085 0.100 Uiso 1 1 calc R . .
C33 C 0.3097(4) 1.3455(4) 0.4079(5) 0.064(2) Uani 1 1 d . . .
H33 H 0.3485 1.3613 0.4337 0.077 Uiso 1 1 calc R . .
C34 C 0.3563(3) 1.2089(4) 0.4011(4) 0.0449(14) Uani 1 1 d . . .
C35 C 0.3824(3) 1.0724(3) 0.4177(3) 0.0312(12) Uani 1 1 d . . .
H35 H 0.4270 1.0888 0.4008 0.037 Uiso 1 1 calc R . .
C36 C 0.3830(3) 1.0630(4) 0.5076(3) 0.0354(12) Uani 1 1 d . . .
C37 C 0.4535(4) 0.8294(5) 0.5243(4) 0.066(2) Uani 1 1 d . . .
H37A H 0.4063 0.8350 0.5183 0.098 Uiso 1 1 calc R . .
H37B H 0.4650 0.7733 0.5239 0.098 Uiso 1 1 calc R . .
H37C H 0.4756 0.8562 0.4809 0.098 Uiso 1 1 calc R . .
C38 C 0.4791(6) 0.8231(6) 0.2664(6) 0.101(4) Uani 1 1 d . . .
H38A H 0.4935 0.8589 0.3080 0.152 Uiso 1 1 calc R . .
H38B H 0.5066 0.7759 0.2662 0.152 Uiso 1 1 calc R . .
H38C H 0.4338 0.8079 0.2758 0.152 Uiso 1 1 calc R . .
C39 C 0.7644(10) 0.9145(14) 0.9180(12) 0.218(6) Uani 1 1 d DU . .
C40 C 0.6921(10) 0.9268(14) 0.9046(15) 0.223(6) Uani 1 1 d DU . .
C41 C 0.7856(12) 0.9715(15) 0.7792(16) 0.244(6) Uani 1 1 d DU . .
C42 C 0.8163(12) 1.0493(15) 0.8109(16) 0.242(7) Uani 1 1 d DU . .
C43 C 0.7876(12) 0.8206(16) 0.7995(14) 0.216(5) Uani 1 1 d U . .
C44 C 0.8105(10) 0.7487(14) 0.8347(13) 0.190(6) Uani 1 1 d U . .
Gd1 Gd 0.5000 1.0000 0.642623(18) 0.02966(10) Uani 1 2 d S . .
Gd2 Gd 0.5000 1.0000 0.148025(17) 0.02912(10) Uani 1 2 d S . .
N1 N 0.8027(8) 0.9001(12) 0.8419(11) 0.201(4) Uani 1 1 d DU . .
O1 O 0.38714(18) 0.8149(2) 0.9054(2) 0.0395(9) Uani 1 1 d . . .
O2 O 0.3231(2) 0.8951(3) 0.9827(3) 0.0581(13) Uani 1 1 d . . .
O3 O 0.4504(2) 0.7968(3) 1.0497(2) 0.0480(11) Uani 1 1 d . . .
O4 O 0.5060(2) 0.9116(2) 1.0349(2) 0.0413(9) Uani 1 1 d . . .
O5 O 0.6076(2) 0.7950(3) 0.8005(3) 0.0572(12) Uani 1 1 d . . .
O6 O 0.52178(17) 0.7701(2) 0.8824(2) 0.0364(9) Uani 1 1 d . . .
O7 O 0.4645(2) 0.7908(3) 0.7390(2) 0.0463(10) Uani 1 1 d . . .
O8 O 0.4607(2) 0.9245(2) 0.7539(2) 0.0403(9) Uani 1 1 d . . .
O9 O 0.29709(18) 0.9743(2) 0.3960(2) 0.0386(9) Uani 1 1 d . . .
O10 O 0.3174(3) 0.8443(3) 0.3712(4) 0.0762(17) Uani 1 1 d . . .
O11 O 0.32371(19) 0.9863(4) 0.2411(2) 0.0575(13) Uani 1 1 d . . .
O12 O 0.42967(17) 1.0193(3) 0.2608(2) 0.0424(11) Uani 1 1 d . . .
O13 O 0.33655(18) 1.1329(2) 0.3919(3) 0.0385(9) Uani 1 1 d . . .
O14 O 0.4119(2) 1.2279(3) 0.4192(3) 0.0614(14) Uani 1 1 d . . .
O15 O 0.3428(2) 1.1018(3) 0.5486(3) 0.0541(12) Uani 1 1 d . . .
O16 O 0.42678(19) 1.0145(3) 0.5345(2) 0.0429(10) Uani 1 1 d . . .
O17 O 0.40154(19) 1.0728(3) 0.6896(2) 0.0448(10) Uani 1 1 d . . .
H455 H 0.3696 1.0616 0.7208 0.054 Uiso 1 1 d R . .
H466 H 0.3854 1.0985 0.6498 0.054 Uiso 1 1 d R . .
O18 O 0.4740(2) 0.8648(3) 0.5992(2) 0.0495(11) Uani 1 1 d . . .
H104 H 0.4600 0.8312 0.6337 0.074 Uiso 1 1 d R . .
O19 O 0.38617(17) 0.9854(3) 0.1045(2) 0.0421(10) Uani 1 1 d . . .
H467 H 0.3595 0.9963 0.1417 0.050 Uiso 1 1 d R . .
H468 H 0.3645 0.9608 0.0678 0.050 Uiso 1 1 d R . .
O20 O 0.4840(2) 0.8619(3) 0.1924(2) 0.0522(13) Uani 1 1 d . . .
H108 H 0.4997 0.8398 0.1505 0.078 Uiso 1 1 d 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
C1 C2 1.373(9) . ?
C1 C6 1.374(9) . ?
C1 C7 1.484(8) . ?
C2 C3 1.382(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.361(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.410(10) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.216(7) . ?
C7 O1 1.362(7) . ?
C8 O1 1.455(6) . ?
C8 C17 1.495(7) . ?
C8 C9 1.546(8) . ?
C8 H8 0.9800 . ?
C9 O3 1.227(7) . ?
C9 O4 1.264(7) . ?
C10 C15 1.384(9) . ?
C10 C11 1.406(9) . ?
C10 C16 1.444(9) . ?
C11 C12 1.402(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.375(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.341(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.199(7) . ?
C16 O6 1.366(7) . ?
C17 O6 1.447(6) . ?
C17 C18 1.516(7) . ?
C17 H17 0.9800 . ?
C18 O7 1.250(7) . ?
C18 O8 1.266(7) . ?
C19 C24 1.354(11) . ?
C19 C20 1.396(10) . ?
C19 C25 1.483(9) . ?
C20 C21 1.367(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.332(14) . ?
C21 H21 0.9300 . ?
C22 C23 1.398(15) . ?
C22 H22 0.9300 . ?
C23 C24 1.413(11) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O10 1.204(8) . ?
C25 O9 1.330(7) . ?
C26 O9 1.459(6) . ?
C26 C35 1.521(8) . ?
C26 C27 1.523(6) . ?
C26 H26 0.9800 . ?
C27 O11 1.231(6) . ?
C27 O12 1.263(6) . ?
C28 C33 1.349(10) . ?
C28 C29 1.368(10) . ?
C28 C34 1.501(9) . ?
C29 C30 1.406(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.372(15) . ?
C30 H30 0.9300 . ?
C31 C32 1.306(13) . ?
C31 H31 0.9300 . ?
C32 C33 1.387(10) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O14 1.202(7) . ?
C34 O13 1.333(7) . ?
C35 O13 1.433(6) . ?
C35 C36 1.510(7) . ?
C35 H35 0.9800 . ?
C36 O15 1.242(7) . ?
C36 O16 1.276(7) . ?
C37 O18 1.443(8) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.397(9) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.488(10) . ?
C39 N1 1.506(10) . ?
C41 C42 1.527(10) . ?
C41 N1 1.62(3) . ?
C43 C44 1.41(3) . ?
C43 N1 1.53(3) . ?
Gd1 O16 2.344(3) . ?
Gd1 O16 2.344(3) 2_675 ?
Gd1 O8 2.378(4) 2_675 ?
Gd1 O8 2.378(4) . ?
Gd1 O18 2.420(4) . ?
Gd1 O18 2.420(4) 2_675 ?
Gd1 O17 2.452(4) . ?
Gd1 O17 2.452(4) 2_675 ?
Gd2 O12 2.378(4) 2_675 ?
Gd2 O12 2.378(4) . ?
Gd2 O4 2.397(3) 1_554 ?
Gd2 O4 2.397(3) 2_674 ?
Gd2 O19 2.418(3) . ?
Gd2 O19 2.418(3) 2_675 ?
Gd2 O20 2.435(4) 2_675 ?
Gd2 O20 2.435(4) . ?
O4 Gd2 2.397(3) 1_556 ?
O17 H455 0.8490 . ?
O17 H466 0.8542 . ?
O18 H104 0.8500 . ?
O19 H467 0.8423 . ?
O19 H468 0.8560 . ?
O20 H108 0.8507 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.8(6) . . ?
C2 C1 C7 118.5(6) . . ?
C6 C1 C7 121.6(6) . . ?
C1 C2 C3 120.6(7) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.9(8) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.8(7) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.0(8) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 119.8(7) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
O2 C7 O1 122.4(5) . . ?
O2 C7 C1 124.2(6) . . ?
O1 C7 C1 113.4(5) . . ?
O1 C8 C17 106.5(4) . . ?
O1 C8 C9 112.5(4) . . ?
C17 C8 C9 112.2(4) . . ?
O1 C8 H8 108.5 . . ?
C17 C8 H8 108.5 . . ?
C9 C8 H8 108.5 . . ?
O3 C9 O4 126.6(5) . . ?
O3 C9 C8 119.6(5) . . ?
O4 C9 C8 113.7(5) . . ?
C15 C10 C11 117.0(6) . . ?
C15 C10 C16 120.5(6) . . ?
C11 C10 C16 122.5(6) . . ?
C12 C11 C10 120.7(7) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 118.0(8) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C14 C13 C12 121.9(7) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C15 C14 C13 118.7(7) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C10 123.7(7) . . ?
C14 C15 H15 118.1 . . ?
C10 C15 H15 118.1 . . ?
O5 C16 O6 121.9(6) . . ?
O5 C16 C10 124.9(6) . . ?
O6 C16 C10 113.2(5) . . ?
O6 C17 C8 107.7(4) . . ?
O6 C17 C18 110.8(4) . . ?
C8 C17 C18 113.3(5) . . ?
O6 C17 H17 108.3 . . ?
C8 C17 H17 108.3 . . ?
C18 C17 H17 108.3 . . ?
O7 C18 O8 125.7(5) . . ?
O7 C18 C17 119.8(5) . . ?
O8 C18 C17 114.5(5) . . ?
C24 C19 C20 119.6(7) . . ?
C24 C19 C25 121.0(6) . . ?
C20 C19 C25 119.4(7) . . ?
C21 C20 C19 121.6(9) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 118.6(9) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C21 C22 C23 122.7(9) . . ?
C21 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C22 C23 C24 117.8(10) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 H23 121.1 . . ?
C19 C24 C23 119.6(8) . . ?
C19 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
O10 C25 O9 124.1(6) . . ?
O10 C25 C19 123.8(6) . . ?
O9 C25 C19 112.1(6) . . ?
O9 C26 C35 107.1(4) . . ?
O9 C26 C27 110.0(4) . . ?
C35 C26 C27 113.4(5) . . ?
O9 C26 H26 108.8 . . ?
C35 C26 H26 108.8 . . ?
C27 C26 H26 108.8 . . ?
O11 C27 O12 126.5(4) . . ?
O11 C27 C26 119.7(4) . . ?
O12 C27 C26 113.8(4) . . ?
C33 C28 C29 119.1(7) . . ?
C33 C28 C34 119.3(6) . . ?
C29 C28 C34 121.6(7) . . ?
C28 C29 C30 120.0(9) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 118.8(9) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C32 C31 C30 120.3(9) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C33 121.6(9) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 H32 119.2 . . ?
C28 C33 C32 120.1(8) . . ?
C28 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
O14 C34 O13 123.8(6) . . ?
O14 C34 C28 123.5(6) . . ?
O13 C34 C28 112.6(5) . . ?
O13 C35 C36 112.1(4) . . ?
O13 C35 C26 108.1(4) . . ?
C36 C35 C26 112.6(5) . . ?
O13 C35 H35 108.0 . . ?
C36 C35 H35 108.0 . . ?
C26 C35 H35 108.0 . . ?
O15 C36 O16 125.8(5) . . ?
O15 C36 C35 119.3(5) . . ?
O16 C36 C35 114.9(5) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N1 113.4(18) . . ?
C42 C41 N1 108(2) . . ?
C44 C43 N1 118(2) . . ?
O16 Gd1 O16 79.22(19) . 2_675 ?
O16 Gd1 O8 139.21(14) . 2_675 ?
O16 Gd1 O8 116.56(15) 2_675 2_675 ?
O16 Gd1 O8 116.56(15) . . ?
O16 Gd1 O8 139.21(14) 2_675 . ?
O8 Gd1 O8 77.2(2) 2_675 . ?
O16 Gd1 O18 74.26(15) . . ?
O16 Gd1 O18 79.03(15) 2_675 . ?
O8 Gd1 O18 142.80(14) 2_675 . ?
O8 Gd1 O18 70.84(14) . . ?
O16 Gd1 O18 79.03(15) . 2_675 ?
O16 Gd1 O18 74.26(15) 2_675 2_675 ?
O8 Gd1 O18 70.84(14) 2_675 2_675 ?
O8 Gd1 O18 142.80(14) . 2_675 ?
O18 Gd1 O18 145.1(2) . 2_675 ?
O16 Gd1 O17 71.75(13) . . ?
O16 Gd1 O17 143.73(13) 2_675 . ?
O8 Gd1 O17 76.04(14) 2_675 . ?
O8 Gd1 O17 75.00(14) . . ?
O18 Gd1 O17 112.29(15) . . ?
O18 Gd1 O17 79.19(15) 2_675 . ?
O16 Gd1 O17 143.73(13) . 2_675 ?
O16 Gd1 O17 71.75(13) 2_675 2_675 ?
O8 Gd1 O17 75.00(14) 2_675 2_675 ?
O8 Gd1 O17 76.04(14) . 2_675 ?
O18 Gd1 O17 79.19(15) . 2_675 ?
O18 Gd1 O17 112.29(15) 2_675 2_675 ?
O17 Gd1 O17 142.68(19) . 2_675 ?
O12 Gd2 O12 75.29(18) 2_675 . ?
O12 Gd2 O4 120.76(15) 2_675 1_554 ?
O12 Gd2 O4 137.46(13) . 1_554 ?
O12 Gd2 O4 137.46(13) 2_675 2_674 ?
O12 Gd2 O4 120.76(15) . 2_674 ?
O4 Gd2 O4 75.96(19) 1_554 2_674 ?
O12 Gd2 O19 142.15(13) 2_675 . ?
O12 Gd2 O19 71.76(12) . . ?
O4 Gd2 O19 75.45(14) 1_554 . ?
O4 Gd2 O19 77.11(14) 2_674 . ?
O12 Gd2 O19 71.76(12) 2_675 2_675 ?
O12 Gd2 O19 142.15(13) . 2_675 ?
O4 Gd2 O19 77.11(14) 1_554 2_675 ?
O4 Gd2 O19 75.45(14) 2_674 2_675 ?
O19 Gd2 O19 144.98(18) . 2_675 ?
O12 Gd2 O20 78.89(15) 2_675 2_675 ?
O12 Gd2 O20 73.18(14) . 2_675 ?
O4 Gd2 O20 144.28(13) 1_554 2_675 ?
O4 Gd2 O20 70.61(13) 2_674 2_675 ?
O19 Gd2 O20 108.18(15) . 2_675 ?
O19 Gd2 O20 82.60(14) 2_675 2_675 ?
O12 Gd2 O20 73.18(14) 2_675 . ?
O12 Gd2 O20 78.89(15) . . ?
O4 Gd2 O20 70.61(13) 1_554 . ?
O4 Gd2 O20 144.28(13) 2_674 . ?
O19 Gd2 O20 82.60(14) . . ?
O19 Gd2 O20 108.18(15) 2_675 . ?
O20 Gd2 O20 144.55(19) 2_675 . ?
C39 N1 C43 115(2) . . ?
C39 N1 C41 108.7(17) . . ?
C43 N1 C41 107.0(17) . . ?
C7 O1 C8 114.8(4) . . ?
C9 O4 Gd2 130.9(3) . 1_556 ?
C16 O6 C17 116.1(4) . . ?
C18 O8 Gd1 133.4(3) . . ?
C25 O9 C26 116.3(5) . . ?
C27 O12 Gd2 139.1(3) . . ?
C34 O13 C35 116.0(4) . . ?
C36 O16 Gd1 140.5(4) . . ?
Gd1 O17 H455 134.6 . . ?
Gd1 O17 H466 107.7 . . ?
H455 O17 H466 107.4 . . ?
C37 O18 Gd1 134.5(4) . . ?
C37 O18 H104 103.0 . . ?
Gd1 O18 H104 118.6 . . ?
Gd2 O19 H467 111.2 . . ?
Gd2 O19 H468 138.3 . . ?
H467 O19 H468 107.9 . . ?
C38 O20 Gd2 135.5(5) . . ?
C38 O20 H108 123.7 . . ?
Gd2 O20 H108 96.2 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.087
# 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 0.000 0.299 609.1 32.4
2 0.500 0.500 0.413 609.1 32.4
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 848922'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 O20 Pr, C6 N'
_chemical_formula_sum            'C44 H36 N O20 Pr'
_chemical_formula_weight         1039.65

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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'

_cell_length_a                   20.285(4)
_cell_length_b                   16.776(3)
_cell_length_c                   16.805(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5718.8(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    30632
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      27.57

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2104
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43664
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unitI/netI     0.0836
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10041
_reflns_number_gt                6015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
dfix 1.38 0.01 c30 c31 c28 c33
ISOR 0.001 C39 C40 C41 C42 C43 C44
isor 0.01  o21 c30 c4 c5 c31 o22
dfix 1.50 0.01 n1 c39 c39 c40 c41 c42 c43 c44
DELU     0.010   0.010 N1 C39 C40 C41 C42 C43 C44 
SIMU     0.040   0.080   3.800 N1 C39 C40 C41 C42 C43 C44
;

_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)+(0.0443P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(18)
_refine_ls_number_reflns         10041
_refine_ls_number_parameters     598
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0924
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_restrained_S_all      0.856
_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
N1 N 0.7015(6) 0.9021(8) 0.1567(9) 0.170(4) Uani 1 1 d DU . .
C1 C 0.3972(4) 0.8303(4) -0.1357(3) 0.0462(17) Uani 1 1 d . . .
C2 C 0.4272(4) 0.8770(4) -0.0731(4) 0.063(2) Uani 1 1 d . . .
H2 H 0.4629 0.8574 -0.0445 0.076 Uiso 1 1 calc R . .
C4 C 0.3471(5) 0.9797(4) -0.0956(5) 0.075(2) Uani 1 1 d U . .
H4 H 0.3291 1.0288 -0.0818 0.090 Uiso 1 1 calc R . .
C3 C 0.4011(5) 0.9523(4) -0.0566(5) 0.071(2) Uani 1 1 d . . .
H3 H 0.4212 0.9841 -0.0183 0.086 Uiso 1 1 calc R . .
C5 C 0.3180(5) 0.9344(5) -0.1567(5) 0.072(2) Uani 1 1 d U . .
H5 H 0.2815 0.9539 -0.1840 0.087 Uiso 1 1 calc R . .
C6 C 0.3436(4) 0.8621(4) -0.1756(4) 0.058(2) Uani 1 1 d . . .
H6 H 0.3245 0.8329 -0.2166 0.070 Uiso 1 1 calc R . .
C7 C 0.4203(4) 0.7511(4) -0.1559(3) 0.0436(16) Uani 1 1 d . . .
C8 C 0.5038(5) 0.6525(3) -0.1359(3) 0.0336(12) Uani 1 1 d . . .
H8 H 0.4684 0.6133 -0.1290 0.040 Uiso 1 1 calc R . .
C9 C 0.5290(3) 0.6487(4) -0.2214(3) 0.0375(15) Uani 1 1 d . . .
C10 C 0.7272(4) 0.7214(4) -0.0808(4) 0.0498(18) Uani 1 1 d . . .
C11 C 0.7886(4) 0.7053(5) -0.0488(5) 0.073(2) Uani 1 1 d . . .
H11 H 0.7942 0.6621 -0.0148 0.087 Uiso 1 1 calc R . .
C12 C 0.8414(5) 0.7534(6) -0.0674(6) 0.092(3) Uani 1 1 d . . .
H12 H 0.8820 0.7441 -0.0432 0.111 Uiso 1 1 calc R . .
C13 C 0.8355(5) 0.8138(6) -0.1199(7) 0.101(4) Uani 1 1 d . . .
H13 H 0.8724 0.8433 -0.1343 0.121 Uiso 1 1 calc R . .
C14 C 0.7739(5) 0.8320(5) -0.1527(6) 0.084(3) Uani 1 1 d . . .
H14 H 0.7699 0.8742 -0.1882 0.101 Uiso 1 1 calc R . .
C15 C 0.7169(4) 0.7856(4) -0.1318(4) 0.063(2) Uani 1 1 d . . .
H15 H 0.6752 0.7980 -0.1513 0.075 Uiso 1 1 calc R . .
C16 C 0.6721(4) 0.6652(4) -0.0612(4) 0.0457(17) Uani 1 1 d . . .
C17 C 0.5581(3) 0.6349(3) -0.0778(3) 0.0343(14) Uani 1 1 d . . .
H17 H 0.5723 0.5795 -0.0852 0.041 Uiso 1 1 calc R . .
C18 C 0.5337(3) 0.6455(4) 0.0098(3) 0.0383(16) Uani 1 1 d . . .
C19 C 0.3003(4) 0.7660(4) 0.3870(4) 0.055(2) Uani 1 1 d . . .
C20 C 0.3097(4) 0.8433(4) 0.4106(4) 0.064(2) Uani 1 1 d . . .
H20 H 0.3490 0.8592 0.4343 0.077 Uiso 1 1 calc R . .
C21 C 0.2579(6) 0.8981(5) 0.3978(6) 0.083(3) Uani 1 1 d . . .
H21 H 0.2622 0.9492 0.4186 0.099 Uiso 1 1 calc R . .
C22 C 0.2042(6) 0.8809(6) 0.3582(6) 0.101(4) Uani 1 1 d . . .
H22 H 0.1739 0.9206 0.3459 0.122 Uiso 1 1 calc R . .
C23 C 0.1932(5) 0.8051(7) 0.3357(6) 0.101(4) Uani 1 1 d . . .
H23 H 0.1533 0.7910 0.3124 0.121 Uiso 1 1 calc R . .
C24 C 0.2441(5) 0.7456(5) 0.3480(5) 0.078(3) Uani 1 1 d . . .
H24 H 0.2383 0.6939 0.3294 0.093 Uiso 1 1 calc R . .
C25 C 0.3548(4) 0.7085(4) 0.4019(4) 0.0466(18) Uani 1 1 d . . .
C26 C 0.3811(3) 0.5729(3) 0.4169(3) 0.0359(15) Uani 1 1 d . . .
H26 H 0.4255 0.5892 0.4004 0.043 Uiso 1 1 calc R . .
C27 C 0.3807(4) 0.5623(4) 0.5071(3) 0.0422(16) Uani 1 1 d . . .
C28 C 0.2063(4) 0.3854(4) 0.3900(4) 0.0524(18) Uani 1 1 d D . .
C29 C 0.1648(5) 0.4497(5) 0.3987(6) 0.085(3) Uani 1 1 d . . .
H29 H 0.1810 0.5013 0.4033 0.102 Uiso 1 1 calc R . .
C30 C 0.0961(6) 0.4337(6) 0.4003(6) 0.108(3) Uani 1 1 d DU . .
H30 H 0.0658 0.4752 0.4025 0.129 Uiso 1 1 calc R . .
C31 C 0.0749(5) 0.3542(6) 0.3985(6) 0.096(3) Uani 1 1 d DU . .
H31 H 0.0300 0.3435 0.4019 0.115 Uiso 1 1 calc R . .
C32 C 0.1158(6) 0.2947(5) 0.3921(5) 0.089(3) Uani 1 1 d . . .
H32 H 0.1001 0.2427 0.3906 0.107 Uiso 1 1 calc R . .
C33 C 0.1823(5) 0.3092(4) 0.3877(5) 0.073(3) Uani 1 1 d D . .
H33 H 0.2115 0.2667 0.3831 0.087 Uiso 1 1 calc R . .
C34 C 0.2794(4) 0.3984(4) 0.3850(4) 0.0550(19) Uani 1 1 d . . .
C35 C 0.3633(3) 0.4947(5) 0.3739(3) 0.0388(13) Uani 1 1 d . . .
H35 H 0.3925 0.4523 0.3930 0.047 Uiso 1 1 calc R . .
C36 C 0.3713(3) 0.5023(5) 0.2822(3) 0.0397(13) Uani 1 1 d . . .
C37 C 0.5202(7) 0.6794(6) 0.2653(5) 0.120(5) Uani 1 1 d . . .
H37A H 0.4952 0.6502 0.3040 0.180 Uiso 1 1 calc R . .
H37B H 0.5023 0.7321 0.2598 0.180 Uiso 1 1 calc R . .
H37C H 0.5653 0.6829 0.2822 0.180 Uiso 1 1 calc R . .
C38 C 0.5478(5) 0.6715(5) 0.5202(5) 0.088(3) Uani 1 1 d . . .
H38A H 0.5921 0.6541 0.5099 0.132 Uiso 1 1 calc R . .
H38B H 0.5469 0.7286 0.5233 0.132 Uiso 1 1 calc R . .
H38C H 0.5195 0.6540 0.4779 0.132 Uiso 1 1 calc R . .
C39 C 0.7378(9) 0.9173(10) 0.0811(9) 0.189(5) Uani 1 1 d DU . .
C40 C 0.8096(9) 0.9301(9) 0.0967(11) 0.194(5) Uani 1 1 d DU . .
C41 C 0.7132(10) 0.9713(10) 0.2199(11) 0.206(5) Uani 1 1 d DU . .
C42 C 0.6892(10) 1.0512(10) 0.1884(10) 0.193(6) Uani 1 1 d DU . .
C43 C 0.7131(10) 0.8247(10) 0.2006(10) 0.196(5) Uani 1 1 d DU . .
C44 C 0.6901(9) 0.7500(9) 0.1619(9) 0.174(5) Uani 1 1 d DU . .
Pr1 Pr 0.5000 0.5000 0.14692(2) 0.03119(13) Uani 1 2 d S . .
Pr2 Pr 0.5000 0.5000 0.64184(2) 0.03161(13) Uani 1 2 d S . .
O1 O 0.47824(19) 0.7316(2) -0.1186(2) 0.0357(10) Uani 1 1 d . . .
O2 O 0.3940(3) 0.7062(3) -0.1995(3) 0.0576(14) Uani 1 1 d . . .
O3 O 0.5354(3) 0.7106(2) -0.2620(2) 0.0477(12) Uani 1 1 d . . .
O4 O 0.5406(2) 0.5785(2) -0.2457(2) 0.0423(11) Uani 1 1 d . . .
O5 O 0.6779(3) 0.6077(3) -0.0189(3) 0.0617(14) Uani 1 1 d . . .
O6 O 0.6130(2) 0.6871(2) -0.0954(2) 0.0394(11) Uani 1 1 d . . .
O7 O 0.5510(3) 0.7040(2) 0.0487(2) 0.0496(13) Uani 1 1 d . . .
O8 O 0.4934(3) 0.5905(2) 0.03194(19) 0.0398(10) Uani 1 1 d . . .
O9 O 0.4095(3) 0.7264(3) 0.4197(3) 0.0643(15) Uani 1 1 d . . .
O10 O 0.3348(2) 0.6326(2) 0.3911(3) 0.0416(11) Uani 1 1 d . . .
O11 O 0.3402(3) 0.6005(3) 0.5483(2) 0.0571(14) Uani 1 1 d . . .
O12 O 0.4237(2) 0.5137(3) 0.5327(2) 0.0490(13) Uani 1 1 d . . .
O13 O 0.3170(3) 0.3473(3) 0.3692(4) 0.079(2) Uani 1 1 d . . .
O14 O 0.2957(2) 0.4747(2) 0.3950(2) 0.0430(11) Uani 1 1 d . . .
O15 O 0.3219(2) 0.4875(3) 0.2407(2) 0.0528(13) Uani 1 1 d . . .
O16 O 0.4276(2) 0.5210(2) 0.2599(2) 0.0401(13) Uani 1 1 d . . .
O17 O 0.3831(2) 0.4831(2) 0.1015(2) 0.0427(11) Uani 1 1 d . . .
H103 H 0.3627 0.5052 0.1408 0.064 Uiso 1 1 d R . .
H104 H 0.3551 0.4657 0.0672 0.064 Uiso 1 1 d R . .
O18 O 0.5171(3) 0.6399(2) 0.1916(2) 0.059(2) Uani 1 1 d . . .
H101 H 0.5088 0.6753 0.1555 0.089 Uiso 1 1 d R . .
O19 O 0.3976(2) 0.5751(2) 0.6900(2) 0.0479(12) Uani 1 1 d . . .
H105 H 0.3805 0.5884 0.6451 0.072 Uiso 1 1 d R . .
H106 H 0.4033 0.6179 0.7183 0.072 Uiso 1 1 d R . .
O20 O 0.5251(2) 0.6378(2) 0.5953(2) 0.0542(15) Uani 1 1 d . . .
H102 H 0.5322 0.6676 0.6363 0.081 Uiso 1 1 d 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
N1 C39 1.490(9) . ?
N1 C43 1.512(18) . ?
N1 C41 1.590(18) . ?
C1 C6 1.385(9) . ?
C1 C2 1.445(9) . ?
C1 C7 1.449(8) . ?
C2 C3 1.396(9) . ?
C2 H2 0.9300 . ?
C4 C3 1.358(11) . ?
C4 C5 1.407(11) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C5 C6 1.358(9) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.179(7) . ?
C7 O1 1.372(8) . ?
C8 O1 1.453(6) . ?
C8 C17 1.501(9) . ?
C8 C9 1.527(7) . ?
C8 H8 0.9800 . ?
C9 O3 1.249(7) . ?
C9 O4 1.269(7) . ?
C10 C11 1.384(10) . ?
C10 C15 1.393(8) . ?
C10 C16 1.498(9) . ?
C11 C12 1.378(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.348(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.437(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.204(7) . ?
C16 O6 1.378(8) . ?
C17 O6 1.448(7) . ?
C17 C18 1.563(8) . ?
C17 H17 0.9800 . ?
C18 O7 1.229(7) . ?
C18 O8 1.288(8) . ?
C19 C24 1.360(11) . ?
C19 C20 1.368(9) . ?
C19 C25 1.490(10) . ?
C20 C21 1.413(11) . ?
C20 H20 0.9300 . ?
C21 C22 1.308(13) . ?
C21 H21 0.9300 . ?
C22 C23 1.345(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.451(12) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O9 1.186(9) . ?
C25 O10 1.348(7) . ?
C26 O10 1.440(7) . ?
C26 C27 1.525(7) . ?
C26 C35 1.541(8) . ?
C26 H26 0.9800 . ?
C27 O11 1.251(8) . ?
C27 O12 1.269(8) . ?
C28 C33 1.368(7) . ?
C28 C29 1.376(11) . ?
C28 C34 1.502(10) . ?
C29 C30 1.418(12) . ?
C29 H29 0.9300 . ?
C30 C31 1.403(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.303(12) . ?
C31 H31 0.9300 . ?
C32 C33 1.373(13) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O13 1.178(9) . ?
C34 O14 1.332(7) . ?
C35 O14 1.456(7) . ?
C35 C36 1.554(6) . ?
C35 H35 0.9800 . ?
C36 O16 1.242(7) . ?
C36 O15 1.246(7) . ?
C37 O18 1.405(9) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.459(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.496(9) . ?
C41 C42 1.522(9) . ?
C43 C44 1.487(9) . ?
Pr1 O16 2.426(4) . ?
Pr1 O16 2.426(4) 2_665 ?
Pr1 O8 2.461(3) 2_665 ?
Pr1 O8 2.461(3) . ?
Pr1 O18 2.489(4) 2_665 ?
Pr1 O18 2.489(4) . ?
Pr1 O17 2.508(4) 2_665 ?
Pr1 O17 2.508(4) . ?
Pr2 O12 2.411(4) 2_665 ?
Pr2 O12 2.411(4) . ?
Pr2 O4 2.446(4) 1_556 ?
Pr2 O4 2.446(4) 2_666 ?
Pr2 O20 2.492(4) 2_665 ?
Pr2 O20 2.492(4) . ?
Pr2 O19 2.560(4) . ?
Pr2 O19 2.560(4) 2_665 ?
O4 Pr2 2.446(4) 1_554 ?
O17 H103 0.8616 . ?
O17 H104 0.8607 . ?
O18 H101 0.8655 . ?
O19 H105 0.8599 . ?
O19 H106 0.8686 . ?
O20 H102 0.8638 . ?

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
C39 N1 C43 119.0(15) . . ?
C39 N1 C41 111.7(13) . . ?
C43 N1 C41 106.1(12) . . ?
C6 C1 C2 118.3(6) . . ?
C6 C1 C7 119.5(6) . . ?
C2 C1 C7 122.1(6) . . ?
C3 C2 C1 118.4(7) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C3 C4 C5 120.5(7) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C3 C2 121.1(7) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C6 C5 C4 119.5(8) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 122.1(7) . . ?
C5 C6 H6 119.0 . . ?
C1 C6 H6 119.0 . . ?
O2 C7 O1 121.3(6) . . ?
O2 C7 C1 125.9(7) . . ?
O1 C7 C1 112.9(6) . . ?
O1 C8 C17 108.1(4) . . ?
O1 C8 C9 110.2(4) . . ?
C17 C8 C9 111.0(7) . . ?
O1 C8 H8 109.2 . . ?
C17 C8 H8 109.2 . . ?
C9 C8 H8 109.2 . . ?
O3 C9 O4 125.2(6) . . ?
O3 C9 C8 121.0(5) . . ?
O4 C9 C8 113.8(5) . . ?
C11 C10 C15 121.7(7) . . ?
C11 C10 C16 117.6(6) . . ?
C15 C10 C16 120.6(7) . . ?
C12 C11 C10 119.9(8) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 121.2(9) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.1(9) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 120.3(8) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 116.6(8) . . ?
C10 C15 H15 121.7 . . ?
C14 C15 H15 121.7 . . ?
O5 C16 O6 123.1(6) . . ?
O5 C16 C10 124.0(7) . . ?
O6 C16 C10 112.9(5) . . ?
O6 C17 C8 108.3(5) . . ?
O6 C17 C18 111.5(5) . . ?
C8 C17 C18 110.9(5) . . ?
O6 C17 H17 108.7 . . ?
C8 C17 H17 108.7 . . ?
C18 C17 H17 108.7 . . ?
O7 C18 O8 126.8(5) . . ?
O7 C18 C17 120.1(5) . . ?
O8 C18 C17 113.0(5) . . ?
C24 C19 C20 119.7(8) . . ?
C24 C19 C25 122.7(7) . . ?
C20 C19 C25 117.5(7) . . ?
C19 C20 C21 118.0(8) . . ?
C19 C20 H20 121.0 . . ?
C21 C20 H20 121.0 . . ?
C22 C21 C20 123.6(9) . . ?
C22 C21 H21 118.2 . . ?
C20 C21 H21 118.2 . . ?
C21 C22 C23 119.3(10) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C24 119.5(10) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C19 C24 C23 119.5(9) . . ?
C19 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
O9 C25 O10 123.7(7) . . ?
O9 C25 C19 124.9(7) . . ?
O10 C25 C19 111.5(7) . . ?
O10 C26 C27 112.1(5) . . ?
O10 C26 C35 107.3(5) . . ?
C27 C26 C35 111.4(4) . . ?
O10 C26 H26 108.6 . . ?
C27 C26 H26 108.6 . . ?
C35 C26 H26 108.6 . . ?
O11 C27 O12 126.4(6) . . ?
O11 C27 C26 119.6(6) . . ?
O12 C27 C26 114.1(6) . . ?
C33 C28 C29 121.2(8) . . ?
C33 C28 C34 119.0(8) . . ?
C29 C28 C34 119.8(6) . . ?
C28 C29 C30 117.1(8) . . ?
C28 C29 H29 121.5 . . ?
C30 C29 H29 121.5 . . ?
C31 C30 C29 118.7(10) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C32 C31 C30 122.3(10) . . ?
C32 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
C31 C32 C33 119.7(9) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C28 C33 C32 120.9(9) . . ?
C28 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
O13 C34 O14 124.5(8) . . ?
O13 C34 C28 123.1(7) . . ?
O14 C34 C28 112.2(7) . . ?
O14 C35 C26 107.6(5) . . ?
O14 C35 C36 111.0(4) . . ?
C26 C35 C36 111.7(6) . . ?
O14 C35 H35 108.8 . . ?
C26 C35 H35 108.8 . . ?
C36 C35 H35 108.8 . . ?
O16 C36 O15 128.3(5) . . ?
O16 C36 C35 114.6(5) . . ?
O15 C36 C35 117.1(5) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N1 C39 C40 110.9(14) . . ?
C42 C41 N1 111.3(14) . . ?
C44 C43 N1 117.5(14) . . ?
O16 Pr1 O16 77.0(2) . 2_665 ?
O16 Pr1 O8 137.43(16) . 2_665 ?
O16 Pr1 O8 119.48(15) 2_665 2_665 ?
O16 Pr1 O8 119.48(15) . . ?
O16 Pr1 O8 137.43(16) 2_665 . ?
O8 Pr1 O8 76.53(17) 2_665 . ?
O16 Pr1 O18 79.40(15) . 2_665 ?
O16 Pr1 O18 73.24(14) 2_665 2_665 ?
O8 Pr1 O18 70.28(13) 2_665 2_665 ?
O8 Pr1 O18 144.22(13) . 2_665 ?
O16 Pr1 O18 73.24(14) . . ?
O16 Pr1 O18 79.40(15) 2_665 . ?
O8 Pr1 O18 144.22(13) 2_665 . ?
O8 Pr1 O18 70.28(13) . . ?
O18 Pr1 O18 144.87(18) 2_665 . ?
O16 Pr1 O17 142.61(13) . 2_665 ?
O16 Pr1 O17 71.42(13) 2_665 2_665 ?
O8 Pr1 O17 77.27(16) 2_665 2_665 ?
O8 Pr1 O17 75.10(17) . 2_665 ?
O18 Pr1 O17 109.27(16) 2_665 2_665 ?
O18 Pr1 O17 81.58(15) . 2_665 ?
O16 Pr1 O17 71.42(13) . . ?
O16 Pr1 O17 142.61(13) 2_665 . ?
O8 Pr1 O17 75.10(17) 2_665 . ?
O8 Pr1 O17 77.27(16) . . ?
O18 Pr1 O17 81.58(15) 2_665 . ?
O18 Pr1 O17 109.27(16) . . ?
O17 Pr1 O17 144.59(17) 2_665 . ?
O12 Pr2 O12 80.9(2) 2_665 . ?
O12 Pr2 O4 115.01(16) 2_665 1_556 ?
O12 Pr2 O4 138.81(15) . 1_556 ?
O12 Pr2 O4 138.81(15) 2_665 2_666 ?
O12 Pr2 O4 115.01(16) . 2_666 ?
O4 Pr2 O4 78.9(2) 1_556 2_666 ?
O12 Pr2 O20 78.70(16) 2_665 2_665 ?
O12 Pr2 O20 73.67(15) . 2_665 ?
O4 Pr2 O20 144.13(13) 1_556 2_665 ?
O4 Pr2 O20 70.97(13) 2_666 2_665 ?
O12 Pr2 O20 73.67(15) 2_665 . ?
O12 Pr2 O20 78.70(16) . . ?
O4 Pr2 O20 70.97(13) 1_556 . ?
O4 Pr2 O20 144.13(13) 2_666 . ?
O20 Pr2 O20 143.46(18) 2_665 . ?
O12 Pr2 O19 143.90(14) 2_665 . ?
O12 Pr2 O19 70.90(14) . . ?
O4 Pr2 O19 76.37(15) 1_556 . ?
O4 Pr2 O19 75.38(14) 2_666 . ?
O20 Pr2 O19 112.93(15) 2_665 . ?
O20 Pr2 O19 78.96(14) . . ?
O12 Pr2 O19 70.90(14) 2_665 2_665 ?
O12 Pr2 O19 143.90(14) . 2_665 ?
O4 Pr2 O19 75.38(14) 1_556 2_665 ?
O4 Pr2 O19 76.37(15) 2_666 2_665 ?
O20 Pr2 O19 78.96(14) 2_665 2_665 ?
O20 Pr2 O19 112.93(15) . 2_665 ?
O19 Pr2 O19 143.16(18) . 2_665 ?
C7 O1 C8 115.6(5) . . ?
C9 O4 Pr2 133.3(4) . 1_554 ?
C16 O6 C17 115.0(4) . . ?
C18 O8 Pr1 129.4(4) . . ?
C25 O10 C26 114.8(5) . . ?
C27 O12 Pr2 139.5(4) . . ?
C34 O14 C35 115.1(6) . . ?
C36 O16 Pr1 139.2(4) . . ?
Pr1 O17 H103 99.9 . . ?
Pr1 O17 H104 149.9 . . ?
H103 O17 H104 110.2 . . ?
C37 O18 Pr1 135.8(5) . . ?
C37 O18 H101 107.6 . . ?
Pr1 O18 H101 114.1 . . ?
Pr2 O19 H105 100.3 . . ?
Pr2 O19 H106 118.1 . . ?
H105 O19 H106 108.6 . . ?
C38 O20 Pr2 134.1(4) . . ?
C38 O20 H102 114.3 . . ?
Pr2 O20 H102 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.069
# 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 0.000 0.195 652.1 37.4
2 1.000 0.500 0.577 652.1 37.6
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1A
_database_code_depnum_ccdc_archive 'CCDC 855715'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H47 La2 O31'
_chemical_formula_sum            'C58 H47 La2 O31'
_chemical_formula_weight         1517.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   9.4321(19)
_cell_length_b                   23.555(5)
_cell_length_c                   16.669(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.81(3)
_cell_angle_gamma                90.00
_cell_volume                     3611.2(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25333
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1514
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26944
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12711
_reflns_number_gt                9993
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
ISOR 0.01 C4 C5 C6 C17 C18 C21 C22 C23 C24 C25 C39 C40 C41 C43 C50 C53 C55 C57
ISOR 0.01 O8 O9 O26
isor 0.01 c49 c50 c51 c52 c56 c57 c58
isor 0.01 c21 c22 c23 c24 c33 c38 c39 c40 c41 c42 c43
isor 0.01 c53 c54 c54' o17 o17'
dfix 1.39 0.01 c53 c54 c54 c49
dfix 1.39 0.01 c49 c50 c50 c51 c51 c52 c52 c53
FREE La2  C47
FREE C9   La1
FREE C54' C53
DELU     0.010   0.010 C1 C2 C3 C4 C5 C6 C7
SIMU     0.040   0.080   3.800 C1 C2 C3 C4 C5 C6 C7
DELU     0.010   0.010 C12 C13 C14 C15 C16 C17 C18
SIMU     0.040   0.080   3.800 C12 C13 C14 C15 C16 C17 C18
DELU     0.010   0.010 C19 C20 C21 C22 C23 C24 C25
SIMU     0.040   0.080   3.800 C19 C20 C21 C22 C23 C24 C25
DELU     0.010   0.010 C31 C32 C33 C34 C35 C36
SIMU     0.040   0.080   3.800 C31 C32 C33 C34 C35 C36
DELU     0.010   0.010 C37 C38 C39 C40 C41 C42 C43 Q8
SIMU     0.040   0.080   3.800 C37 C38 C39 C40 C41 C42 C43 Q8
DELU     0.010   0.010 C49 C50 C51 C52 C53 C54 C54'
SIMU     0.040   0.080   3.800 C49 C50 C51 C52 C53 C54 C54'
;

_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)+(0.0958P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(19)
_refine_ls_number_reflns         11801
_refine_ls_number_parameters     829
_refine_ls_number_restraints     1053
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1475
_refine_ls_wR_factor_gt          0.1334
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2880(10) 1.0628(5) 0.0345(7) 0.077(3) Uani 1 1 d U . .
C2 C 0.2526(14) 1.1137(7) -0.0173(9) 0.102(3) Uani 1 1 d U . .
C3 C 0.2138(18) 1.1053(8) -0.1067(10) 0.126(4) Uani 1 1 d U . .
H3 H 0.2050 1.0691 -0.1295 0.151 Uiso 1 1 calc R . .
C4 C 0.191(2) 1.1524(8) -0.1547(12) 0.131(4) Uani 1 1 d U . .
H4 H 0.1701 1.1481 -0.2116 0.157 Uiso 1 1 calc R . .
C5 C 0.199(2) 1.2063(9) -0.1220(13) 0.141(4) Uani 1 1 d U . .
H5 H 0.1706 1.2376 -0.1557 0.169 Uiso 1 1 calc R . .
C6 C 0.2488(19) 1.2128(8) -0.0387(12) 0.129(4) Uani 1 1 d U . .
H6 H 0.2710 1.2491 -0.0177 0.155 Uiso 1 1 calc R . .
C7 C 0.2673(16) 1.1672(6) 0.0155(11) 0.115(4) Uani 1 1 d U . .
H7 H 0.2890 1.1728 0.0721 0.138 Uiso 1 1 calc R . .
C8 C 0.3762(9) 1.0313(4) 0.1717(6) 0.055(2) Uani 1 1 d . . .
H8 H 0.3215 0.9962 0.1555 0.066 Uiso 1 1 calc R . .
C9 C 0.5378(8) 1.0206(4) 0.1747(5) 0.054(2) Uani 1 1 d . . .
C10 C 0.3514(9) 1.0508(3) 0.2540(5) 0.0534(19) Uani 1 1 d . . .
H10 H 0.3915 1.0224 0.2958 0.064 Uiso 1 1 calc R . .
C11 C 0.1906(10) 1.0591(5) 0.2526(7) 0.071(3) Uani 1 1 d . . .
C12 C 0.4511(12) 1.1229(6) 0.3499(8) 0.086(3) Uani 1 1 d U . .
C13 C 0.5044(13) 1.1814(6) 0.3585(9) 0.095(3) Uani 1 1 d U . .
C14 C 0.5330(12) 1.2118(6) 0.2963(9) 0.097(3) Uani 1 1 d U . .
H14 H 0.5190 1.1954 0.2445 0.116 Uiso 1 1 calc R . .
C15 C 0.5845(16) 1.2688(7) 0.3074(11) 0.113(4) Uani 1 1 d U . .
H15 H 0.6078 1.2897 0.2648 0.135 Uiso 1 1 calc R . .
C16 C 0.5971(15) 1.2904(6) 0.3831(11) 0.115(4) Uani 1 1 d U . .
H16 H 0.6236 1.3283 0.3911 0.138 Uiso 1 1 calc R . .
C17 C 0.574(2) 1.2608(8) 0.4487(12) 0.129(4) Uani 1 1 d U . .
H17 H 0.5935 1.2776 0.5005 0.154 Uiso 1 1 calc R . .
C18 C 0.5211(17) 1.2054(7) 0.4388(10) 0.115(3) Uani 1 1 d U . .
H18 H 0.4980 1.1851 0.4820 0.138 Uiso 1 1 calc R . .
C19 C 0.5410(13) 0.8883(7) -0.1141(8) 0.098(3) Uani 1 1 d U . .
C20 C 0.5240(19) 0.9286(8) -0.1804(11) 0.119(4) Uani 1 1 d U . .
C21 C 0.558(2) 0.9117(9) -0.2512(13) 0.140(4) Uani 1 1 d U . .
H21 H 0.5861 0.8746 -0.2587 0.167 Uiso 1 1 calc R . .
C22 C 0.549(2) 0.9525(9) -0.3125(14) 0.150(4) Uani 1 1 d U . .
H22 H 0.5808 0.9420 -0.3595 0.180 Uiso 1 1 calc R . .
C23 C 0.497(2) 1.0083(10) -0.3096(14) 0.154(4) Uani 1 1 d U . .
H23 H 0.4942 1.0338 -0.3526 0.185 Uiso 1 1 calc R . .
C24 C 0.449(2) 1.0238(10) -0.2373(15) 0.160(4) Uani 1 1 d U . .
H24 H 0.4083 1.0590 -0.2317 0.192 Uiso 1 1 calc R . .
C25 C 0.469(2) 0.9803(9) -0.1721(14) 0.147(4) Uani 1 1 d U . .
H25 H 0.4424 0.9891 -0.1231 0.176 Uiso 1 1 calc R . .
C26 C 0.5067(10) 0.8687(4) 0.0192(6) 0.066(2) Uani 1 1 d . . .
H26 H 0.5322 0.8302 0.0051 0.079 Uiso 1 1 calc R . .
C27 C 0.6291(10) 0.8925(6) 0.0892(6) 0.073(3) Uani 1 1 d . . .
C28 C 0.3569(9) 0.8680(4) 0.0398(6) 0.063(2) Uani 1 1 d . . .
H28 H 0.3160 0.9064 0.0346 0.076 Uiso 1 1 calc R . .
C29 C 0.3575(9) 0.8453(4) 0.1232(6) 0.062(2) Uani 1 1 d . . .
C30 C 0.1305(12) 0.8376(4) -0.0387(7) 0.073(3) Uani 1 1 d . . .
C31 C 0.0585(14) 0.8041(5) -0.1128(8) 0.088(3) Uani 1 1 d U . .
C32 C 0.1370(16) 0.7743(6) -0.1629(9) 0.111(4) Uani 1 1 d U . .
H32 H 0.2379 0.7765 -0.1523 0.133 Uiso 1 1 calc R . .
C33 C 0.0622(17) 0.7423(6) -0.2272(9) 0.108(4) Uani 1 1 d U . .
H33 H 0.1118 0.7200 -0.2580 0.129 Uiso 1 1 calc R . .
C34 C -0.0872(17) 0.7435(6) -0.2453(11) 0.119(4) Uani 1 1 d U . .
H34 H -0.1361 0.7241 -0.2919 0.143 Uiso 1 1 calc R . .
C35 C -0.1686(16) 0.7715(7) -0.1990(10) 0.115(4) Uani 1 1 d U . .
H35 H -0.2696 0.7702 -0.2128 0.139 Uiso 1 1 calc R . .
C36 C -0.0941(15) 0.8024(6) -0.1298(10) 0.110(4) Uani 1 1 d U . .
H36 H -0.1452 0.8212 -0.0961 0.132 Uiso 1 1 calc R . .
C37 C 1.1219(17) 0.9550(6) 0.5102(10) 0.106(4) Uani 1 1 d U . .
C38 C 1.0797(11) 0.9482(5) 0.5912(6) 0.106(3) Uani 1 1 d GU . .
C39 C 1.0676(13) 0.8938(4) 0.6214(7) 0.138(4) Uani 1 1 d GU . .
H39 H 1.0862 0.8623 0.5916 0.166 Uiso 1 1 calc R . .
C40 C 1.0277(14) 0.8864(4) 0.6961(8) 0.153(4) Uani 1 1 d GU . .
H40 H 1.0196 0.8501 0.7164 0.183 Uiso 1 1 calc R . .
C41 C 1.0000(14) 0.9335(6) 0.7407(6) 0.144(4) Uani 1 1 d GU . .
H41 H 0.9733 0.9285 0.7907 0.172 Uiso 1 1 calc R . .
C42 C 1.0121(14) 0.9878(5) 0.7105(7) 0.148(4) Uani 1 1 d GU . .
H42 H 0.9936 1.0193 0.7403 0.177 Uiso 1 1 calc R . .
C43 C 1.0520(13) 0.9952(4) 0.6357(7) 0.132(4) Uani 1 1 d GU . .
H43 H 1.0601 1.0315 0.6155 0.159 Uiso 1 1 calc R . .
C44 C 1.1740(8) 0.9174(4) 0.3928(5) 0.0514(18) Uani 1 1 d . . .
H44 H 1.1533 0.9562 0.3723 0.062 Uiso 1 1 calc R . .
C45 C 1.3385(8) 0.9085(3) 0.4099(5) 0.0470(18) Uani 1 1 d . . .
C46 C 1.0948(7) 0.8768(4) 0.3275(5) 0.0500(19) Uani 1 1 d . . .
H46 H 1.1223 0.8858 0.2756 0.060 Uiso 1 1 calc R . .
C47 C 0.9300(7) 0.8817(4) 0.3139(5) 0.0518(19) Uani 1 1 d . . .
C48 C 1.1152(10) 0.7827(5) 0.2883(9) 0.076(3) Uani 1 1 d . . .
C49 C 1.1581(18) 0.7246(7) 0.3142(11) 0.121(4) Uani 1 1 d DU . .
C50 C 1.170(2) 0.6856(7) 0.2536(11) 0.140(4) Uani 1 1 d DU . .
H50 H 1.1501 0.6974 0.1990 0.167 Uiso 1 1 calc R . .
C51 C 1.210(2) 0.6291(7) 0.2718(12) 0.152(5) Uani 1 1 d DU . .
H51 H 1.2277 0.6036 0.2325 0.182 Uiso 1 1 calc R B .
C52 C 1.221(2) 0.6145(9) 0.3526(12) 0.152(5) Uani 1 1 d DU B .
H52 H 1.2485 0.5770 0.3647 0.183 Uiso 1 1 calc R A 1
C53 C 1.200(3) 0.6454(9) 0.4192(13) 0.158(5) Uani 1 1 d DU B 1
H53 H 1.1922 0.6317 0.4705 0.190 Uiso 0.50 1 calc PR B 1
C54 C 1.192(5) 0.7014(12) 0.3925(16) 0.145(6) Uani 0.50 1 d PDU B 1
H54 H 1.2132 0.7281 0.4346 0.174 Uiso 0.50 1 calc PR B 1
C54' C 1.134(4) 0.7117(15) 0.390(2) 0.124(7) Uani 0.50 1 d PU B 2
C55 C 0.576(3) 0.7353(12) 0.3100(16) 0.189(9) Uani 1 1 d U . .
H55A H 0.6575 0.7406 0.3551 0.284 Uiso 1 1 calc R . .
H55B H 0.6047 0.7136 0.2676 0.284 Uiso 1 1 calc R . .
H55C H 0.5003 0.7153 0.3289 0.284 Uiso 1 1 calc R . .
C56 C 0.810(2) 1.1001(8) 0.3313(12) 0.131(6) Uani 1 1 d U . .
H56A H 0.8724 1.1164 0.3790 0.197 Uiso 1 1 calc R . .
H56B H 0.7146 1.0943 0.3419 0.197 Uiso 1 1 calc R . .
H56C H 0.8028 1.1253 0.2853 0.197 Uiso 1 1 calc R . .
C57 C 0.679(3) 0.9953(15) 0.4640(18) 0.223(11) Uani 1 1 d U . .
H57A H 0.7675 1.0056 0.5022 0.335 Uiso 1 1 d R . .
H57B H 0.6282 0.9673 0.4886 0.335 Uiso 1 1 d R . .
H57C H 0.6192 1.0283 0.4502 0.335 Uiso 1 1 d R . .
C58 C 0.8862(19) 0.9972(9) -0.0429(11) 0.130(5) Uani 1 1 d U . .
H58A H 0.9243 0.9596 -0.0302 0.195 Uiso 1 1 calc R . .
H58B H 0.9457 1.0171 -0.0734 0.195 Uiso 1 1 calc R . .
H58C H 0.7886 0.9947 -0.0752 0.195 Uiso 1 1 calc R . .
O1 O 0.3189(6) 1.0755(3) 0.1137(4) 0.0649(16) Uani 1 1 d . . .
O2 O 0.2895(12) 1.0151(4) 0.0119(5) 0.112(3) Uani 1 1 d . . .
O3 O 0.6025(6) 1.0519(3) 0.1323(4) 0.0656(16) Uani 1 1 d . . .
O4 O 0.5990(5) 0.9822(2) 0.2215(4) 0.0515(14) Uani 1 1 d . . .
O5 O 0.1101(6) 1.0171(3) 0.2270(5) 0.075(2) Uani 1 1 d . . .
O6 O 0.1508(10) 1.1057(5) 0.2710(10) 0.158(6) Uani 1 1 d . . .
O7 O 0.4306(7) 1.1026(3) 0.2729(4) 0.0668(16) Uani 1 1 d . . .
O8 O 0.4227(13) 1.0952(5) 0.4052(8) 0.131(4) Uani 1 1 d U . .
O9 O 0.5761(15) 0.8400(6) -0.1203(9) 0.146(4) Uani 1 1 d U . .
O10 O 0.4926(10) 0.9040(3) -0.0506(5) 0.093(2) Uani 1 1 d . . .
O11 O 0.6959(11) 0.9360(4) 0.0756(6) 0.106(3) Uani 1 1 d . . .
O12 O 0.6521(7) 0.8646(3) 0.1552(5) 0.0720(19) Uani 1 1 d . . .
O13 O 0.3731(6) 0.8794(3) 0.1804(4) 0.0648(16) Uani 1 1 d . . .
O14 O 0.3509(9) 0.7916(3) 0.1319(5) 0.086(2) Uani 1 1 d . . .
O15 O 0.0711(9) 0.8654(5) 0.0005(6) 0.122(4) Uani 1 1 d . . .
O16 O 0.2757(8) 0.8324(3) -0.0258(4) 0.0764(19) Uani 1 1 d . . .
O17 O 1.077(2) 1.0068(9) 0.4690(13) 0.113(6) Uani 0.50 1 d PU . .
O17' O 1.2098(17) 0.9944(7) 0.5084(9) 0.081(4) Uani 0.50 1 d PU . .
O18 O 1.1198(6) 0.9114(2) 0.4654(4) 0.0540(13) Uani 1 1 d . . .
O19 O 1.3947(6) 0.9179(3) 0.3494(4) 0.0571(15) Uani 1 1 d . . .
O20 O 1.4046(6) 0.8941(4) 0.4802(4) 0.079(2) Uani 1 1 d . . .
O21 O 0.8568(6) 0.8435(3) 0.3330(5) 0.0649(17) Uani 1 1 d . . .
O22 O 0.8783(5) 0.9284(2) 0.2828(4) 0.0537(13) Uani 1 1 d . . .
O23 O 1.0625(10) 0.7988(4) 0.2188(7) 0.099(3) Uani 1 1 d . . .
O24 O 1.1414(6) 0.8203(3) 0.3504(5) 0.0674(18) Uani 1 1 d . . .
O25 O 0.8862(10) 1.0254(4) 0.0277(6) 0.108(3) Uani 1 1 d . . .
O26 O 1.0146(11) 0.9197(5) 0.1316(7) 0.115(3) Uani 1 1 d U . .
O27 O 0.8646(8) 1.0496(3) 0.3138(6) 0.089(2) Uani 1 1 d . . .
O28 O 0.5249(10) 0.7864(3) 0.2797(6) 0.103(3) Uani 1 1 d . . .
O29 O 0.6406(6) 0.8496(3) 0.4404(4) 0.0724(18) Uani 1 1 d . . .
O30 O 0.7092(9) 0.9673(4) 0.3958(5) 0.086(2) Uani 1 1 d . . .
O31 O 0.8893(9) 1.1061(4) 0.1564(7) 0.109(3) Uani 1 1 d . . .
La1 La 0.85364(4) 0.999319(19) 0.17023(3) 0.05187(14) Uani 1 1 d . . .
La2 La 0.60122(4) 0.888588(16) 0.29298(3) 0.04598(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.185(13) . ?
C1 O1 1.323(13) . ?
C1 C2 1.473(19) . ?
C2 C7 1.37(2) . ?
C2 C3 1.47(2) . ?
C3 C4 1.36(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.39(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O1 1.442(10) . ?
C8 C10 1.512(13) . ?
C8 C9 1.535(11) . ?
C8 H8 0.9800 . ?
C9 O4 1.251(10) . ?
C9 O3 1.267(11) . ?
C10 O7 1.430(10) . ?
C10 C11 1.524(12) . ?
C10 H10 0.9800 . ?
C11 O6 1.220(14) . ?
C11 O5 1.263(12) . ?
C12 O8 1.208(15) . ?
C12 O7 1.341(14) . ?
C12 C13 1.464(18) . ?
C13 C14 1.335(19) . ?
C13 C18 1.43(2) . ?
C14 C15 1.425(19) . ?
C14 H14 0.9300 . ?
C15 C16 1.34(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.35(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.40(2) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O9 1.195(18) . ?
C19 O10 1.297(14) . ?
C19 C20 1.44(2) . ?
C20 C25 1.34(2) . ?
C20 C21 1.35(2) . ?
C21 C22 1.39(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.41(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.42(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.48(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O10 1.411(13) . ?
C26 C28 1.527(13) . ?
C26 C27 1.552(13) . ?
C26 H26 0.9800 . ?
C27 O11 1.249(14) . ?
C27 O12 1.258(14) . ?
C28 O16 1.455(10) . ?
C28 C29 1.487(14) . ?
C28 H28 0.9800 . ?
C29 O13 1.230(11) . ?
C29 O14 1.277(12) . ?
C30 O15 1.155(12) . ?
C30 O16 1.344(13) . ?
C30 C31 1.496(14) . ?
C31 C36 1.404(19) . ?
C31 C32 1.418(19) . ?
C32 C33 1.371(17) . ?
C32 H32 0.9300 . ?
C33 C34 1.37(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.37(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.412(18) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O17' 1.25(2) . ?
C37 O18 1.268(15) . ?
C37 O17 1.42(3) . ?
C37 C38 1.499(17) . ?
C38 C39 1.3900 . ?
C38 C43 1.3900 . ?
C39 C40 1.3900 . ?
C39 H39 0.9300 . ?
C40 C41 1.3900 . ?
C40 H40 0.9300 . ?
C41 C42 1.3900 . ?
C41 H41 0.9300 . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 O18 1.422(10) . ?
C44 C46 1.516(12) . ?
C44 C45 1.529(10) . ?
C44 H44 0.9800 . ?
C45 O20 1.247(10) . ?
C45 O19 1.258(10) . ?
C46 O24 1.426(10) . ?
C46 C47 1.525(9) . ?
C46 H46 0.9800 . ?
C47 O21 1.217(10) . ?
C47 O22 1.267(10) . ?
C48 O23 1.216(14) . ?
C48 O24 1.344(14) . ?
C48 C49 1.46(2) . ?
C49 C54' 1.37(4) . ?
C49 C54 1.385(10) . ?
C49 C50 1.387(9) . ?
C50 C51 1.399(9) . ?
C50 H50 0.9300 . ?
C51 C52 1.371(9) . ?
C51 H51 0.9300 . ?
C52 C53 1.380(10) . ?
C52 H52 0.9300 . ?
C53 C54 1.391(10) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 O28 1.35(3) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 O27 1.354(18) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 O30 1.40(3) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9599 . ?
C58 O25 1.351(19) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
O3 La1 2.623(6) . ?
O4 La2 2.504(5) . ?
O4 La1 2.752(5) . ?
O5 La1 2.430(6) 1_455 ?
O11 La1 2.426(8) . ?
O12 La2 2.513(7) . ?
O13 La2 2.532(6) . ?
O17 O17' 1.31(2) . ?
O19 La2 2.442(6) 1_655 ?
O21 La2 2.583(5) . ?
O22 La1 2.484(6) . ?
O22 La2 2.817(5) . ?
O25 La1 2.538(9) . ?
O26 La1 2.583(10) . ?
O27 La1 2.652(8) . ?
O28 La2 2.508(7) . ?
O29 La2 2.572(7) . ?
O30 La2 2.576(7) . ?
O31 La1 2.554(9) . ?
La1 O5 2.430(6) 1_655 ?
La2 O19 2.442(6) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 121.2(11) . . ?
O2 C1 C2 127.0(12) . . ?
O1 C1 C2 111.8(10) . . ?
C7 C2 C3 120.7(15) . . ?
C7 C2 C1 121.7(13) . . ?
C3 C2 C1 117.4(14) . . ?
C4 C3 C2 117.5(18) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C3 C4 C5 122(2) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C6 C5 C4 119(2) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C7 122.4(19) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C2 C7 C6 117.7(17) . . ?
C2 C7 H7 121.1 . . ?
C6 C7 H7 121.1 . . ?
O1 C8 C10 106.2(7) . . ?
O1 C8 C9 111.2(7) . . ?
C10 C8 C9 111.9(7) . . ?
O1 C8 H8 109.2 . . ?
C10 C8 H8 109.2 . . ?
C9 C8 H8 109.2 . . ?
O4 C9 O3 123.8(7) . . ?
O4 C9 C8 117.2(8) . . ?
O3 C9 C8 119.0(8) . . ?
O7 C10 C8 106.3(7) . . ?
O7 C10 C11 111.3(7) . . ?
C8 C10 C11 112.2(7) . . ?
O7 C10 H10 109.0 . . ?
C8 C10 H10 109.0 . . ?
C11 C10 H10 109.0 . . ?
O6 C11 O5 126.4(9) . . ?
O6 C11 C10 118.2(10) . . ?
O5 C11 C10 115.3(8) . . ?
O8 C12 O7 122.0(12) . . ?
O8 C12 C13 124.3(14) . . ?
O7 C12 C13 113.7(11) . . ?
C14 C13 C18 121.1(14) . . ?
C14 C13 C12 123.6(13) . . ?
C18 C13 C12 115.3(14) . . ?
C13 C14 C15 121.8(14) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C16 C15 C14 115.8(16) . . ?
C16 C15 H15 122.1 . . ?
C14 C15 H15 122.1 . . ?
C15 C16 C17 124.7(16) . . ?
C15 C16 H16 117.7 . . ?
C17 C16 H16 117.7 . . ?
C16 C17 C18 120.1(18) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 116.3(16) . . ?
C17 C18 H18 121.8 . . ?
C13 C18 H18 121.8 . . ?
O9 C19 O10 119.8(16) . . ?
O9 C19 C20 123.2(14) . . ?
O10 C19 C20 116.0(15) . . ?
C25 C20 C21 122(2) . . ?
C25 C20 C19 120.0(17) . . ?
C21 C20 C19 118.0(17) . . ?
C20 C21 C22 117(2) . . ?
C20 C21 H21 121.6 . . ?
C22 C21 H21 121.6 . . ?
C21 C22 C23 126(2) . . ?
C21 C22 H22 117.2 . . ?
C23 C22 H22 117.2 . . ?
C22 C23 C24 117(2) . . ?
C22 C23 H23 121.7 . . ?
C24 C23 H23 121.7 . . ?
C23 C24 C25 116(2) . . ?
C23 C24 H24 122.1 . . ?
C25 C24 H24 122.1 . . ?
C20 C25 C24 123(2) . . ?
C20 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
O10 C26 C28 105.6(9) . . ?
O10 C26 C27 109.0(8) . . ?
C28 C26 C27 113.9(7) . . ?
O10 C26 H26 109.4 . . ?
C28 C26 H26 109.4 . . ?
C27 C26 H26 109.4 . . ?
O11 C27 O12 126.1(10) . . ?
O11 C27 C26 118.7(11) . . ?
O12 C27 C26 115.1(10) . . ?
O16 C28 C29 112.8(8) . . ?
O16 C28 C26 101.3(7) . . ?
C29 C28 C26 113.7(8) . . ?
O16 C28 H28 109.6 . . ?
C29 C28 H28 109.6 . . ?
C26 C28 H28 109.6 . . ?
O13 C29 O14 123.9(10) . . ?
O13 C29 C28 117.7(9) . . ?
O14 C29 C28 118.2(8) . . ?
O15 C30 O16 124.5(9) . . ?
O15 C30 C31 125.3(11) . . ?
O16 C30 C31 110.1(9) . . ?
C36 C31 C32 120.8(11) . . ?
C36 C31 C30 116.0(12) . . ?
C32 C31 C30 123.1(11) . . ?
C33 C32 C31 119.1(14) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C32 C33 C34 119.1(15) . . ?
C32 C33 H33 120.5 . . ?
C34 C33 H33 120.5 . . ?
C35 C34 C33 124.1(14) . . ?
C35 C34 H34 118.0 . . ?
C33 C34 H34 118.0 . . ?
C34 C35 C36 117.9(14) . . ?
C34 C35 H35 121.0 . . ?
C36 C35 H35 121.0 . . ?
C31 C36 C35 118.8(15) . . ?
C31 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
O17' C37 O18 120.9(14) . . ?
O17' C37 O17 58.5(13) . . ?
O18 C37 O17 116.7(15) . . ?
O17' C37 C38 114.3(14) . . ?
O18 C37 C38 118.0(12) . . ?
O17 C37 C38 114.8(14) . . ?
C39 C38 C43 120.0 . . ?
C39 C38 C37 119.1(9) . . ?
C43 C38 C37 120.9(9) . . ?
C40 C39 C38 120.0 . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C41 120.0 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C40 C41 C42 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C38 120.0 . . ?
C42 C43 H43 120.0 . . ?
C38 C43 H43 120.0 . . ?
O18 C44 C46 109.6(6) . . ?
O18 C44 C45 111.7(7) . . ?
C46 C44 C45 111.4(7) . . ?
O18 C44 H44 108.0 . . ?
C46 C44 H44 108.0 . . ?
C45 C44 H44 108.0 . . ?
O20 C45 O19 126.2(7) . . ?
O20 C45 C44 119.1(7) . . ?
O19 C45 C44 114.7(7) . . ?
O24 C46 C44 108.9(7) . . ?
O24 C46 C47 110.7(7) . . ?
C44 C46 C47 112.5(7) . . ?
O24 C46 H46 108.2 . . ?
C44 C46 H46 108.2 . . ?
C47 C46 H46 108.2 . . ?
O21 C47 O22 124.0(6) . . ?
O21 C47 C46 121.6(7) . . ?
O22 C47 C46 114.4(7) . . ?
O23 C48 O24 119.6(11) . . ?
O23 C48 C49 127.0(13) . . ?
O24 C48 C49 113.5(12) . . ?
C54' C49 C54 25(2) . . ?
C54' C49 C50 126(2) . . ?
C54 C49 C50 113(2) . . ?
C54' C49 C48 112.9(19) . . ?
C54 C49 C48 129.5(18) . . ?
C50 C49 C48 117.7(16) . . ?
C49 C50 C51 122.2(18) . . ?
C49 C50 H50 118.9 . . ?
C51 C50 H50 118.9 . . ?
C52 C51 C50 114.2(19) . . ?
C52 C51 H51 122.9 . . ?
C50 C51 H51 122.9 . . ?
C51 C52 C53 132(2) . . ?
C51 C52 H52 114.1 . . ?
C53 C52 H52 114.1 . . ?
C52 C53 C54 104(3) . . ?
C52 C53 H53 127.8 . . ?
C54 C53 H53 127.8 . . ?
C49 C54 C53 131(3) . . ?
C49 C54 H54 114.3 . . ?
C53 C54 H54 114.3 . . ?
O28 C55 H55A 109.5 . . ?
O28 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
O28 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O27 C56 H56A 109.5 . . ?
O27 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O27 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O30 C57 H57A 110.9 . . ?
O30 C57 H57B 103.6 . . ?
H57A C57 H57B 109.5 . . ?
O30 C57 H57C 113.8 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O25 C58 H58A 109.5 . . ?
O25 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O25 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C1 O1 C8 118.2(8) . . ?
C9 O3 La1 96.4(5) . . ?
C9 O4 La2 152.7(5) . . ?
C9 O4 La1 90.8(5) . . ?
La2 O4 La1 111.18(18) . . ?
C11 O5 La1 137.7(6) . 1_455 ?
C12 O7 C10 118.2(8) . . ?
C19 O10 C26 121.2(11) . . ?
C27 O11 La1 130.4(8) . . ?
C27 O12 La2 130.7(7) . . ?
C29 O13 La2 124.5(6) . . ?
C30 O16 C28 114.5(7) . . ?
O17' O17 C37 54.4(13) . . ?
C37 O17' O17 67.2(14) . . ?
C37 O18 C44 117.2(9) . . ?
C45 O19 La2 140.6(5) . 1_655 ?
C47 O21 La2 100.4(5) . . ?
C47 O22 La1 148.9(5) . . ?
C47 O22 La2 88.0(4) . . ?
La1 O22 La2 109.68(19) . . ?
C48 O24 C46 114.6(8) . . ?
C58 O25 La1 136.0(11) . . ?
C56 O27 La1 130.2(10) . . ?
C55 O28 La2 138.7(13) . . ?
C57 O30 La2 139.5(14) . . ?
O11 La1 O5 140.6(3) . 1_655 ?
O11 La1 O22 91.0(3) . . ?
O5 La1 O22 84.5(2) 1_655 . ?
O11 La1 O25 74.0(3) . . ?
O5 La1 O25 90.4(3) 1_655 . ?
O22 La1 O25 149.2(3) . . ?
O11 La1 O31 128.4(4) . . ?
O5 La1 O31 74.1(2) 1_655 . ?
O22 La1 O31 137.6(3) . . ?
O25 La1 O31 68.4(4) . . ?
O11 La1 O26 72.6(3) . . ?
O5 La1 O26 68.5(3) 1_655 . ?
O22 La1 O26 74.8(3) . . ?
O25 La1 O26 75.1(4) . . ?
O31 La1 O26 126.6(3) . . ?
O11 La1 O3 75.1(3) . . ?
O5 La1 O3 141.3(2) 1_655 . ?
O22 La1 O3 115.34(18) . . ?
O25 La1 O3 87.1(3) . . ?
O31 La1 O3 69.1(2) . . ?
O26 La1 O3 146.3(3) . . ?
O11 La1 O27 139.2(3) . . ?
O5 La1 O27 74.6(3) 1_655 . ?
O22 La1 O27 68.9(2) . . ?
O25 La1 O27 138.5(3) . . ?
O31 La1 O27 70.3(3) . . ?
O26 La1 O27 129.9(3) . . ?
O3 La1 O27 81.9(2) . . ?
O11 La1 O4 70.1(2) . . ?
O5 La1 O4 140.0(2) 1_655 . ?
O22 La1 O4 66.96(16) . . ?
O25 La1 O4 128.4(3) . . ?
O31 La1 O4 108.3(3) . . ?
O26 La1 O4 124.9(3) . . ?
O3 La1 O4 48.74(17) . . ?
O27 La1 O4 69.3(2) . . ?
O19 La2 O4 90.64(19) 1_455 . ?
O19 La2 O28 93.9(3) 1_455 . ?
O4 La2 O28 146.2(2) . . ?
O19 La2 O12 138.2(2) 1_455 . ?
O4 La2 O12 75.3(2) . . ?
O28 La2 O12 79.2(3) . . ?
O19 La2 O13 71.97(19) 1_455 . ?
O4 La2 O13 78.9(2) . . ?
O28 La2 O13 70.9(3) . . ?
O12 La2 O13 66.80(19) . . ?
O19 La2 O29 72.0(2) 1_455 . ?
O4 La2 O29 138.9(2) . . ?
O28 La2 O29 73.7(3) . . ?
O12 La2 O29 141.0(2) . . ?
O13 La2 O29 126.6(2) . . ?
O19 La2 O30 76.8(2) 1_455 . ?
O4 La2 O30 69.1(2) . . ?
O28 La2 O30 144.4(3) . . ?
O12 La2 O30 130.0(2) . . ?
O13 La2 O30 134.5(3) . . ?
O29 La2 O30 70.7(3) . . ?
O19 La2 O21 142.6(2) 1_455 . ?
O4 La2 O21 113.18(18) . . ?
O28 La2 O21 82.0(3) . . ?
O12 La2 O21 77.7(2) . . ?
O13 La2 O21 138.4(2) . . ?
O29 La2 O21 71.2(2) . . ?
O30 La2 O21 85.1(3) . . ?
O19 La2 O22 139.4(2) 1_455 . ?
O4 La2 O22 65.68(16) . . ?
O28 La2 O22 124.5(3) . . ?
O12 La2 O22 69.6(2) . . ?
O13 La2 O22 129.14(19) . . ?
O29 La2 O22 103.73(19) . . ?
O30 La2 O22 64.3(2) . . ?
O21 La2 O22 47.70(18) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.097
# 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 0.156 0.206 0.493 144.9 5.9
2 -0.156 0.706 0.507 144.9 5.6
3 0.301 0.663 0.030 131.6 7.1
4 0.698 0.163 0.970 131.7 6.9
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2A
_database_code_depnum_ccdc_archive 'CCDC 855716'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H48 Ce2 O31'
_chemical_formula_sum            'C58 H48 Ce2 O31'
_chemical_formula_weight         1521.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   9.4048(19)
_cell_length_b                   23.598(5)
_cell_length_c                   16.683(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.47(3)
_cell_angle_gamma                90.00
_cell_volume                     3615.2(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25739
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.49

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27803
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12722
_reflns_number_gt                9544
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
dfix 1.39 0.01 c49 c50 c50 c51 c51 c52 c52 c53
dfix 1.39 0.01 c53 c54 c54 c49 c23 c24 c16 c17
isor 0.01 C3 C4 C5 C6 C18 C21 C22 C23 C24 C25 C39 C40 C41 C42 C43 C50 C52
ISOR 0.01 C53 C54 C55 C56 C57 O8 O9 O26
isor 0.01 o17 o17' c33 c38 c49 c51 c58 c16 c17
FREE Ce2  C47
FREE C9   Ce1
DELU     0.010   0.010 C1 C2 C3 C4 C5 C6 C7
SIMU     0.040   0.080   1.700 C1 C2 C3 C4 C5 C6 C7
DELU     0.010   0.010 C19 C20 C21 C22 C23 C24 C25
SIMU     0.040   0.080   1.700 C19 C20 C21 C22 C23 C24 C25
DELU     0.010   0.010 C37 C38 C39 C40 C41 C42 C43 Q20
SIMU     0.040   0.080   1.700 C37 C38 C39 C40 C41 C42 C43 Q20
DELU     0.010   0.010 C49 C50 C51 C52 C53 C54
SIMU     0.040   0.080   1.700 C49 C50 C51 C52 C53 C54
DELU     0.010   0.010 C56 O27
SIMU     0.040   0.080   1.700 C56 O27
DELU     0.010   0.010 C57 O30
SIMU     0.040   0.080   1.700 C57 O30
;

_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)+(0.0865P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_number_reflns         12626
_refine_ls_number_parameters     819
_refine_ls_number_restraints     446
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1472
_refine_ls_wR_factor_gt          0.1364
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2865(13) 1.0644(6) 0.0359(10) 0.086(3) Uani 1 1 d U . .
C2 C 0.2536(18) 1.1136(8) -0.0160(10) 0.112(4) Uani 1 1 d U . .
C3 C 0.217(2) 1.1038(9) -0.1052(12) 0.134(4) Uani 1 1 d U . .
H3 H 0.2120 1.0674 -0.1269 0.161 Uiso 1 1 calc R . .
C4 C 0.189(2) 1.1514(10) -0.1559(14) 0.141(4) Uani 1 1 d U . .
H4 H 0.1651 1.1469 -0.2126 0.170 Uiso 1 1 calc R . .
C5 C 0.197(2) 1.2017(10) -0.1246(14) 0.145(5) Uani 1 1 d U . .
H5 H 0.1734 1.2328 -0.1590 0.174 Uiso 1 1 calc R . .
C6 C 0.240(2) 1.2099(10) -0.0419(13) 0.147(5) Uani 1 1 d U . .
H6 H 0.2577 1.2466 -0.0219 0.176 Uiso 1 1 calc R . .
C7 C 0.258(2) 1.1647(8) 0.0139(13) 0.128(5) Uani 1 1 d U . .
H7 H 0.2725 1.1709 0.0701 0.153 Uiso 1 1 calc R . .
C8 C 0.3736(10) 1.0311(5) 0.1724(6) 0.059(2) Uani 1 1 d . . .
H8 H 0.3177 0.9964 0.1558 0.071 Uiso 1 1 calc R . .
C9 C 0.5347(10) 1.0198(5) 0.1751(6) 0.058(3) Uani 1 1 d . . .
C10 C 0.3497(10) 1.0499(4) 0.2541(6) 0.056(2) Uani 1 1 d . . .
H10 H 0.3893 1.0214 0.2957 0.068 Uiso 1 1 calc R . .
C11 C 0.1889(12) 1.0588(5) 0.2523(8) 0.072(3) Uani 1 1 d . . .
C12 C 0.4472(13) 1.1220(6) 0.3498(8) 0.079(3) Uani 1 1 d . . .
C13 C 0.5037(13) 1.1808(6) 0.3593(9) 0.085(4) Uani 1 1 d . . .
C14 C 0.5314(14) 1.2099(6) 0.2961(10) 0.093(4) Uani 1 1 d . . .
H14 H 0.5204 1.1927 0.2449 0.112 Uiso 1 1 calc R . .
C15 C 0.5788(16) 1.2686(7) 0.3068(12) 0.114(5) Uani 1 1 d . . .
H15 H 0.5964 1.2902 0.2633 0.136 Uiso 1 1 calc R . .
C16 C 0.5956(19) 1.2898(7) 0.3815(11) 0.118(5) Uani 1 1 d DU . .
H16 H 0.6279 1.3270 0.3900 0.141 Uiso 1 1 calc R . .
C17 C 0.568(2) 1.2600(8) 0.4481(12) 0.142(7) Uani 1 1 d DU . .
H17 H 0.5836 1.2770 0.4996 0.171 Uiso 1 1 calc R . .
C18 C 0.516(2) 1.2032(8) 0.4375(11) 0.124(5) Uani 1 1 d U . .
H18 H 0.4922 1.1826 0.4801 0.148 Uiso 1 1 calc R . .
C19 C 0.5428(15) 0.8867(7) -0.1131(8) 0.094(3) Uani 1 1 d U . .
C20 C 0.5215(17) 0.9279(7) -0.1804(10) 0.107(4) Uani 1 1 d U . .
C21 C 0.562(2) 0.9110(8) -0.2500(11) 0.130(4) Uani 1 1 d U . .
H21 H 0.5987 0.8750 -0.2545 0.156 Uiso 1 1 calc R . .
C22 C 0.545(2) 0.9494(9) -0.3138(14) 0.147(4) Uani 1 1 d U . .
H22 H 0.5680 0.9381 -0.3629 0.177 Uiso 1 1 calc R . .
C23 C 0.496(2) 1.0039(11) -0.3070(12) 0.152(4) Uani 1 1 d DU . .
H23 H 0.4962 1.0296 -0.3492 0.183 Uiso 1 1 calc R . .
C24 C 0.446(3) 1.0210(10) -0.2381(13) 0.163(5) Uani 1 1 d DU . .
H24 H 0.4064 1.0566 -0.2336 0.196 Uiso 1 1 calc R . .
C25 C 0.463(2) 0.9775(9) -0.1724(13) 0.144(4) Uani 1 1 d U . .
H25 H 0.4307 0.9856 -0.1247 0.172 Uiso 1 1 calc R . .
C26 C 0.5093(12) 0.8683(5) 0.0216(6) 0.068(3) Uani 1 1 d . . .
H26 H 0.5345 0.8297 0.0076 0.081 Uiso 1 1 calc R . .
C27 C 0.6310(11) 0.8911(6) 0.0933(6) 0.069(3) Uani 1 1 d . . .
C28 C 0.3579(12) 0.8678(5) 0.0403(6) 0.068(3) Uani 1 1 d . . .
H28 H 0.3180 0.9064 0.0356 0.082 Uiso 1 1 calc R . .
C29 C 0.3577(10) 0.8447(5) 0.1240(6) 0.058(2) Uani 1 1 d . . .
C30 C 0.1334(14) 0.8375(5) -0.0391(7) 0.077(3) Uani 1 1 d . . .
C31 C 0.0589(14) 0.8030(5) -0.1113(7) 0.081(3) Uani 1 1 d . . .
C32 C 0.136(2) 0.7724(7) -0.1584(9) 0.119(6) Uani 1 1 d . . .
H32 H 0.2376 0.7730 -0.1447 0.143 Uiso 1 1 calc R . .
C33 C 0.067(2) 0.7415(7) -0.2247(10) 0.118(5) Uani 1 1 d U . .
H33 H 0.1199 0.7210 -0.2559 0.142 Uiso 1 1 calc R . .
C34 C -0.088(2) 0.7413(7) -0.2448(12) 0.130(6) Uani 1 1 d . . .
H34 H -0.1371 0.7217 -0.2909 0.156 Uiso 1 1 calc R . .
C35 C -0.1657(16) 0.7698(8) -0.1972(11) 0.118(5) Uani 1 1 d . . .
H35 H -0.2669 0.7684 -0.2100 0.141 Uiso 1 1 calc R . .
C36 C -0.0931(17) 0.8011(6) -0.1291(10) 0.106(4) Uani 1 1 d . . .
H36 H -0.1455 0.8204 -0.0963 0.128 Uiso 1 1 calc R . .
C37 C 1.1125(16) 0.9544(7) 0.5086(9) 0.096(4) Uani 1 1 d U . .
C38 C 1.0745(11) 0.9479(5) 0.5914(5) 0.093(3) Uani 1 1 d GU . .
C39 C 1.0683(12) 0.8937(4) 0.6230(7) 0.126(4) Uani 1 1 d GU . .
H39 H 1.0895 0.8624 0.5937 0.151 Uiso 1 1 calc R . .
C40 C 1.0303(14) 0.8862(4) 0.6984(7) 0.141(4) Uani 1 1 d GU . .
H40 H 1.0262 0.8499 0.7195 0.169 Uiso 1 1 calc R . .
C41 C 0.9986(14) 0.9329(6) 0.7421(5) 0.137(4) Uani 1 1 d GU . .
H41 H 0.9732 0.9279 0.7925 0.164 Uiso 1 1 calc R . .
C42 C 1.0048(13) 0.9871(5) 0.7105(6) 0.131(4) Uani 1 1 d GU . .
H42 H 0.9835 1.0184 0.7397 0.157 Uiso 1 1 calc R . .
C43 C 1.0427(12) 0.9946(4) 0.6351(7) 0.130(4) Uani 1 1 d GU . .
H43 H 1.0469 1.0309 0.6140 0.156 Uiso 1 1 calc R . .
C44 C 1.1708(9) 0.9181(4) 0.3936(6) 0.050(2) Uani 1 1 d . . .
H44 H 1.1492 0.9568 0.3732 0.060 Uiso 1 1 calc R . .
C45 C 1.3358(9) 0.9089(4) 0.4092(5) 0.049(2) Uani 1 1 d . . .
C46 C 1.0948(9) 0.8771(4) 0.3288(6) 0.056(2) Uani 1 1 d . . .
H46 H 1.1235 0.8862 0.2772 0.067 Uiso 1 1 calc R . .
C47 C 0.9268(10) 0.8819(5) 0.3142(6) 0.056(2) Uani 1 1 d . . .
C48 C 1.1133(12) 0.7843(6) 0.2875(10) 0.080(3) Uani 1 1 d . . .
C49 C 1.1581(18) 0.7258(7) 0.3127(10) 0.117(4) Uani 1 1 d DU . .
C50 C 1.172(2) 0.6873(7) 0.2521(12) 0.148(5) Uani 1 1 d DU . .
H50 H 1.1550 0.6986 0.1974 0.177 Uiso 1 1 calc R . .
C51 C 1.213(2) 0.6314(8) 0.2738(13) 0.153(5) Uani 1 1 d DU . .
H51 H 1.2334 0.6066 0.2343 0.183 Uiso 1 1 calc R . .
C52 C 1.224(2) 0.6129(10) 0.3526(12) 0.158(5) Uani 1 1 d DU . .
H52 H 1.2435 0.5748 0.3649 0.190 Uiso 1 1 calc R . .
C53 C 1.206(3) 0.6492(8) 0.4141(14) 0.167(5) Uani 1 1 d DU . .
H53 H 1.2179 0.6372 0.4682 0.201 Uiso 1 1 calc R . .
C54 C 1.168(2) 0.7052(9) 0.3912(11) 0.153(5) Uani 1 1 d DU . .
H54 H 1.1487 0.7298 0.4310 0.184 Uiso 1 1 calc R . .
C55 C 0.580(3) 0.7360(14) 0.3135(17) 0.208(11) Uani 1 1 d U . .
H55A H 0.6548 0.7257 0.2849 0.311 Uiso 1 1 calc R . .
H55B H 0.5071 0.7070 0.3060 0.311 Uiso 1 1 calc R . .
H55C H 0.6225 0.7402 0.3710 0.311 Uiso 1 1 calc R . .
C56 C 0.809(2) 1.0974(9) 0.3330(13) 0.144(6) Uani 1 1 d U . .
H56A H 0.8834 1.1216 0.3636 0.216 Uiso 1 1 d R . .
H56B H 0.7348 1.0915 0.3636 0.216 Uiso 1 1 d R . .
H56C H 0.7670 1.1149 0.2814 0.216 Uiso 1 1 d R . .
C57 C 0.684(2) 0.9896(10) 0.4687(12) 0.152(6) Uani 1 1 d U . .
H57A H 0.5815 0.9953 0.4631 0.227 Uiso 1 1 d R . .
H57B H 0.7340 1.0252 0.4804 0.227 Uiso 1 1 d R . .
H57C H 0.7190 0.9636 0.5127 0.227 Uiso 1 1 d R . .
C58 C 0.880(2) 0.9958(9) -0.0418(10) 0.127(5) Uani 1 1 d U . .
H58A H 0.9226 0.9590 -0.0291 0.191 Uiso 1 1 calc R . .
H58B H 0.9363 1.0165 -0.0739 0.191 Uiso 1 1 calc R . .
H58C H 0.7821 0.9918 -0.0725 0.191 Uiso 1 1 calc R . .
O1 O 0.3194(7) 1.0757(3) 0.1149(5) 0.0644(18) Uani 1 1 d . . .
O2 O 0.2870(12) 1.0151(4) 0.0115(5) 0.107(3) Uani 1 1 d . . .
O3 O 0.6020(8) 1.0504(3) 0.1330(5) 0.072(2) Uani 1 1 d . . .
O4 O 0.5979(7) 0.9814(3) 0.2225(4) 0.0543(16) Uani 1 1 d . . .
O5 O 0.1087(7) 1.0172(3) 0.2283(6) 0.076(2) Uani 1 1 d . . .
O6 O 0.1465(9) 1.1057(5) 0.2692(10) 0.141(5) Uani 1 1 d . . .
O7 O 0.4288(8) 1.1021(3) 0.2731(4) 0.0687(19) Uani 1 1 d . . .
O8 O 0.4196(13) 1.0953(5) 0.4056(7) 0.124(3) Uani 1 1 d U . .
O9 O 0.5717(14) 0.8374(6) -0.1196(8) 0.135(4) Uani 1 1 d U . .
O10 O 0.4957(11) 0.9034(4) -0.0490(5) 0.094(3) Uani 1 1 d . . .
O11 O 0.6965(11) 0.9347(4) 0.0785(6) 0.103(3) Uani 1 1 d . . .
O12 O 0.6542(8) 0.8634(4) 0.1585(5) 0.072(2) Uani 1 1 d . . .
O13 O 0.3752(8) 0.8799(3) 0.1814(4) 0.0699(19) Uani 1 1 d . . .
O14 O 0.3485(9) 0.7921(4) 0.1341(5) 0.082(2) Uani 1 1 d . . .
O15 O 0.0725(10) 0.8641(5) 0.0029(6) 0.123(4) Uani 1 1 d . . .
O16 O 0.2761(9) 0.8331(3) -0.0238(5) 0.076(2) Uani 1 1 d . . .
O17 O 1.076(3) 1.0064(10) 0.4698(12) 0.112(6) Uani 0.50 1 d PU . .
O17' O 1.1947(19) 0.9968(9) 0.5063(11) 0.089(4) Uani 0.50 1 d PU . .
O18 O 1.1173(6) 0.9111(3) 0.4655(4) 0.0558(15) Uani 1 1 d . . .
O19 O 1.3920(6) 0.9176(3) 0.3485(4) 0.0576(17) Uani 1 1 d . . .
O20 O 1.4004(7) 0.8939(4) 0.4798(4) 0.078(2) Uani 1 1 d . . .
O21 O 0.8541(7) 0.8440(3) 0.3328(5) 0.0632(19) Uani 1 1 d . . .
O22 O 0.8758(6) 0.9282(3) 0.2824(4) 0.0540(15) Uani 1 1 d . . .
O23 O 1.0599(12) 0.7986(5) 0.2170(7) 0.104(3) Uani 1 1 d . . .
O24 O 1.1370(7) 0.8209(3) 0.3500(5) 0.0662(18) Uani 1 1 d . . .
O25 O 0.8808(11) 1.0245(4) 0.0293(5) 0.096(3) Uani 1 1 d . . .
O26 O 1.0105(11) 0.9209(4) 0.1327(6) 0.102(3) Uani 1 1 d U . .
O27 O 0.8618(10) 1.0490(4) 0.3131(6) 0.096(3) Uani 1 1 d U . .
O28 O 0.5169(12) 0.7876(4) 0.2822(6) 0.103(3) Uani 1 1 d . . .
O29 O 0.6387(8) 0.8506(4) 0.4402(5) 0.077(2) Uani 1 1 d . . .
O30 O 0.7070(9) 0.9677(4) 0.3941(5) 0.085(2) Uani 1 1 d U . .
O31 O 0.8850(9) 1.1050(4) 0.1581(7) 0.104(3) Uani 1 1 d . . .
Ce1 Ce 0.85215(5) 0.99897(2) 0.17124(3) 0.05263(15) Uani 1 1 d . . .
Ce2 Ce 0.59873(5) 0.888757(19) 0.29326(3) 0.04690(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.231(15) . ?
C1 O1 1.315(16) . ?
C1 C2 1.44(2) . ?
C2 C7 1.30(2) . ?
C2 C3 1.47(2) . ?
C3 C4 1.40(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.29(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.36(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.40(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O1 1.440(12) . ?
C8 C10 1.496(13) . ?
C8 C9 1.529(13) . ?
C8 H8 0.9800 . ?
C9 O4 1.263(12) . ?
C9 O3 1.269(11) . ?
C10 O7 1.437(12) . ?
C10 C11 1.521(13) . ?
C10 H10 0.9800 . ?
C11 O6 1.230(14) . ?
C11 O5 1.250(13) . ?
C12 O8 1.198(15) . ?
C12 O7 1.340(14) . ?
C12 C13 1.481(18) . ?
C13 C14 1.331(19) . ?
C13 C18 1.39(2) . ?
C14 C15 1.45(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.32(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.42(2) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O9 1.205(19) . ?
C19 O10 1.305(13) . ?
C19 C20 1.47(2) . ?
C20 C25 1.31(2) . ?
C20 C21 1.35(2) . ?
C21 C22 1.38(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.38(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.390(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.48(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O10 1.424(13) . ?
C26 C28 1.523(15) . ?
C26 C27 1.562(15) . ?
C26 H26 0.9800 . ?
C27 O12 1.246(14) . ?
C27 O11 1.251(14) . ?
C28 O16 1.433(12) . ?
C28 C29 1.499(15) . ?
C28 H28 0.9800 . ?
C29 O13 1.253(11) . ?
C29 O14 1.258(13) . ?
C30 O15 1.177(13) . ?
C30 O16 1.316(14) . ?
C30 C31 1.498(16) . ?
C31 C32 1.38(2) . ?
C31 C36 1.396(19) . ?
C32 C33 1.37(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.43(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.36(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.40(2) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O18 1.256(15) . ?
C37 O17' 1.27(2) . ?
C37 O17 1.40(3) . ?
C37 C38 1.507(15) . ?
C38 C39 1.3900 . ?
C38 C43 1.3900 . ?
C39 C40 1.3900 . ?
C39 H39 0.9300 . ?
C40 C41 1.3900 . ?
C40 H40 0.9300 . ?
C41 C42 1.3900 . ?
C41 H41 0.9300 . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 O18 1.407(10) . ?
C44 C46 1.509(14) . ?
C44 C45 1.532(11) . ?
C44 H44 0.9800 . ?
C45 O20 1.254(10) . ?
C45 O19 1.257(10) . ?
C46 O24 1.407(12) . ?
C46 C47 1.550(11) . ?
C46 H46 0.9800 . ?
C47 O21 1.207(12) . ?
C47 O22 1.264(12) . ?
C48 O23 1.222(16) . ?
C48 O24 1.336(15) . ?
C48 C49 1.48(2) . ?
C49 C54 1.381(10) . ?
C49 C50 1.388(10) . ?
C50 C51 1.401(10) . ?
C50 H50 0.9300 . ?
C51 C52 1.369(10) . ?
C51 H51 0.9300 . ?
C52 C53 1.375(10) . ?
C52 H52 0.9300 . ?
C53 C54 1.399(10) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 O28 1.41(3) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 O27 1.32(2) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 O30 1.406(19) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 O25 1.366(19) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
O3 Ce1 2.601(7) . ?
O4 Ce2 2.484(6) . ?
O4 Ce1 2.739(6) . ?
O5 Ce1 2.433(7) 1_455 ?
O11 Ce1 2.421(9) . ?
O12 Ce2 2.488(7) . ?
O13 Ce2 2.500(7) . ?
O17 O17' 1.17(2) . ?
O19 Ce2 2.422(5) 1_655 ?
O21 Ce2 2.576(6) . ?
O22 Ce1 2.469(6) . ?
O22 Ce2 2.809(6) . ?
O25 Ce1 2.514(8) . ?
O26 Ce1 2.538(10) . ?
O27 Ce1 2.628(9) . ?
O28 Ce2 2.502(8) . ?
O29 Ce2 2.561(7) . ?
O30 Ce2 2.569(8) . ?
O31 Ce1 2.537(9) . ?
Ce1 O5 2.433(7) 1_655 ?
Ce2 O19 2.422(5) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 120.4(14) . . ?
O2 C1 C2 125.3(15) . . ?
O1 C1 C2 114.3(13) . . ?
C7 C2 C1 122.1(16) . . ?
C7 C2 C3 121.0(19) . . ?
C1 C2 C3 116.9(16) . . ?
C4 C3 C2 117(2) . . ?
C4 C3 H3 121.4 . . ?
C2 C3 H3 121.4 . . ?
C5 C4 C3 120(2) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 121(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C7 122(2) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C2 C7 C6 117(2) . . ?
C2 C7 H7 121.3 . . ?
C6 C7 H7 121.3 . . ?
O1 C8 C10 106.8(8) . . ?
O1 C8 C9 110.7(8) . . ?
C10 C8 C9 111.6(9) . . ?
O1 C8 H8 109.2 . . ?
C10 C8 H8 109.2 . . ?
C9 C8 H8 109.2 . . ?
O4 C9 O3 122.1(9) . . ?
O4 C9 C8 118.3(8) . . ?
O3 C9 C8 119.6(10) . . ?
O7 C10 C8 106.4(7) . . ?
O7 C10 C11 110.6(8) . . ?
C8 C10 C11 111.5(9) . . ?
O7 C10 H10 109.4 . . ?
C8 C10 H10 109.4 . . ?
C11 C10 H10 109.4 . . ?
O6 C11 O5 125.3(10) . . ?
O6 C11 C10 119.3(11) . . ?
O5 C11 C10 115.3(9) . . ?
O8 C12 O7 123.6(12) . . ?
O8 C12 C13 122.9(13) . . ?
O7 C12 C13 113.5(11) . . ?
C14 C13 C18 123.7(14) . . ?
C14 C13 C12 121.8(12) . . ?
C18 C13 C12 114.4(14) . . ?
C13 C14 C15 120.1(15) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 116.5(17) . . ?
C16 C15 H15 121.7 . . ?
C14 C15 H15 121.7 . . ?
C15 C16 C17 124.1(17) . . ?
C15 C16 H16 117.9 . . ?
C17 C16 H16 117.9 . . ?
C16 C17 C18 119.7(17) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C13 C18 C17 115.7(17) . . ?
C13 C18 H18 122.2 . . ?
C17 C18 H18 122.2 . . ?
O9 C19 O10 119.3(15) . . ?
O9 C19 C20 124.7(13) . . ?
O10 C19 C20 114.3(15) . . ?
C25 C20 C21 123.4(19) . . ?
C25 C20 C19 120.3(15) . . ?
C21 C20 C19 116.3(16) . . ?
C20 C21 C22 117.6(19) . . ?
C20 C21 H21 121.2 . . ?
C22 C21 H21 121.2 . . ?
C23 C22 C21 122(2) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C22 C23 C24 121(2) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 114(2) . . ?
C23 C24 H24 122.9 . . ?
C25 C24 H24 122.9 . . ?
C20 C25 C24 121.3(19) . . ?
C20 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
O10 C26 C28 104.6(10) . . ?
O10 C26 C27 110.7(9) . . ?
C28 C26 C27 114.1(8) . . ?
O10 C26 H26 109.1 . . ?
C28 C26 H26 109.1 . . ?
C27 C26 H26 109.1 . . ?
O12 C27 O11 127.1(11) . . ?
O12 C27 C26 116.7(10) . . ?
O11 C27 C26 116.2(11) . . ?
O16 C28 C29 112.2(9) . . ?
O16 C28 C26 103.0(8) . . ?
C29 C28 C26 112.5(9) . . ?
O16 C28 H28 109.7 . . ?
C29 C28 H28 109.7 . . ?
C26 C28 H28 109.7 . . ?
O13 C29 O14 123.6(10) . . ?
O13 C29 C28 116.3(10) . . ?
O14 C29 C28 119.9(9) . . ?
O15 C30 O16 122.3(12) . . ?
O15 C30 C31 124.5(12) . . ?
O16 C30 C31 113.2(10) . . ?
C32 C31 C36 120.3(13) . . ?
C32 C31 C30 121.9(12) . . ?
C36 C31 C30 117.8(12) . . ?
C33 C32 C31 121.3(17) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C34 118.5(17) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C35 C34 C33 120.7(16) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 120.2(15) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C31 C36 C35 119.0(15) . . ?
C31 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
O18 C37 O17' 121.7(13) . . ?
O18 C37 O17 119.0(15) . . ?
O17' C37 O17 52.0(13) . . ?
O18 C37 C38 119.1(12) . . ?
O17' C37 C38 112.0(14) . . ?
O17 C37 C38 115.6(14) . . ?
C39 C38 C43 120.0 . . ?
C39 C38 C37 118.6(9) . . ?
C43 C38 C37 121.3(9) . . ?
C38 C39 C40 120.0 . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C38 120.0 . . ?
C42 C43 H43 120.0 . . ?
C38 C43 H43 120.0 . . ?
O18 C44 C46 109.5(7) . . ?
O18 C44 C45 111.9(7) . . ?
C46 C44 C45 109.7(7) . . ?
O18 C44 H44 108.5 . . ?
C46 C44 H44 108.5 . . ?
C45 C44 H44 108.5 . . ?
O20 C45 O19 126.9(8) . . ?
O20 C45 C44 117.9(7) . . ?
O19 C45 C44 115.2(7) . . ?
O24 C46 C44 111.1(8) . . ?
O24 C46 C47 109.3(8) . . ?
C44 C46 C47 112.0(7) . . ?
O24 C46 H46 108.1 . . ?
C44 C46 H46 108.1 . . ?
C47 C46 H46 108.1 . . ?
O21 C47 O22 124.3(8) . . ?
O21 C47 C46 121.4(9) . . ?
O22 C47 C46 114.3(8) . . ?
O23 C48 O24 122.6(13) . . ?
O23 C48 C49 124.3(14) . . ?
O24 C48 C49 113.1(13) . . ?
C54 C49 C50 117.6(19) . . ?
C54 C49 C48 123.8(16) . . ?
C50 C49 C48 118.1(16) . . ?
C49 C50 C51 120(2) . . ?
C49 C50 H50 120.2 . . ?
C51 C50 H50 120.2 . . ?
C52 C51 C50 121(2) . . ?
C52 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
C51 C52 C53 122(2) . . ?
C51 C52 H52 119.2 . . ?
C53 C52 H52 119.2 . . ?
C52 C53 C54 117(2) . . ?
C52 C53 H53 121.6 . . ?
C54 C53 H53 121.6 . . ?
C49 C54 C53 124(2) . . ?
C49 C54 H54 118.2 . . ?
C53 C54 H54 118.2 . . ?
O28 C55 H55A 109.5 . . ?
O28 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
O28 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O27 C56 H56A 112.3 . . ?
O27 C56 H56B 111.4 . . ?
H56A C56 H56B 109.5 . . ?
O27 C56 H56C 104.6 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O30 C57 H57A 108.0 . . ?
O30 C57 H57B 109.9 . . ?
H57A C57 H57B 109.5 . . ?
O30 C57 H57C 110.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O25 C58 H58A 109.5 . . ?
O25 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O25 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C1 O1 C8 119.5(9) . . ?
C9 O3 Ce1 97.5(6) . . ?
C9 O4 Ce2 151.8(6) . . ?
C9 O4 Ce1 91.2(5) . . ?
Ce2 O4 Ce1 111.6(2) . . ?
C11 O5 Ce1 137.9(6) . 1_455 ?
C12 O7 C10 117.7(8) . . ?
C19 O10 C26 121.1(12) . . ?
C27 O11 Ce1 130.1(8) . . ?
C27 O12 Ce2 129.1(7) . . ?
C29 O13 Ce2 125.3(7) . . ?
C30 O16 C28 117.4(9) . . ?
O17' O17 C37 58.5(15) . . ?
O17 O17' C37 69.5(16) . . ?
C37 O18 C44 117.2(9) . . ?
C45 O19 Ce2 140.5(6) . 1_655 ?
C47 O21 Ce2 100.3(6) . . ?
C47 O22 Ce1 149.8(6) . . ?
C47 O22 Ce2 87.7(5) . . ?
Ce1 O22 Ce2 109.8(2) . . ?
C48 O24 C46 115.0(10) . . ?
C58 O25 Ce1 136.0(10) . . ?
C56 O27 Ce1 132.5(12) . . ?
C55 O28 Ce2 134.4(15) . . ?
C57 O30 Ce2 137.0(10) . . ?
O11 Ce1 O5 140.6(3) . 1_655 ?
O11 Ce1 O22 90.0(3) . . ?
O5 Ce1 O22 84.5(2) 1_655 . ?
O11 Ce1 O25 73.8(3) . . ?
O5 Ce1 O25 91.5(3) 1_655 . ?
O22 Ce1 O25 149.2(3) . . ?
O11 Ce1 O31 129.1(4) . . ?
O5 Ce1 O31 74.4(3) 1_655 . ?
O22 Ce1 O31 137.6(3) . . ?
O25 Ce1 O31 69.0(4) . . ?
O11 Ce1 O26 71.9(3) . . ?
O5 Ce1 O26 68.9(3) 1_655 . ?
O22 Ce1 O26 74.7(3) . . ?
O25 Ce1 O26 75.4(3) . . ?
O31 Ce1 O26 127.3(3) . . ?
O11 Ce1 O3 75.3(3) . . ?
O5 Ce1 O3 141.4(2) 1_655 . ?
O22 Ce1 O3 115.5(2) . . ?
O25 Ce1 O3 86.1(3) . . ?
O31 Ce1 O3 68.8(3) . . ?
O26 Ce1 O3 145.7(3) . . ?
O11 Ce1 O27 139.1(3) . . ?
O5 Ce1 O27 74.4(3) 1_655 . ?
O22 Ce1 O27 69.4(3) . . ?
O25 Ce1 O27 138.6(3) . . ?
O31 Ce1 O27 69.7(3) . . ?
O26 Ce1 O27 130.2(3) . . ?
O3 Ce1 O27 82.2(3) . . ?
O11 Ce1 O4 69.9(2) . . ?
O5 Ce1 O4 139.8(2) 1_655 . ?
O22 Ce1 O4 66.82(19) . . ?
O25 Ce1 O4 127.5(3) . . ?
O31 Ce1 O4 107.9(3) . . ?
O26 Ce1 O4 124.7(3) . . ?
O3 Ce1 O4 48.9(2) . . ?
O27 Ce1 O4 69.5(2) . . ?
O19 Ce2 O4 90.7(2) 1_455 . ?
O19 Ce2 O12 138.9(2) 1_455 . ?
O4 Ce2 O12 76.2(2) . . ?
O19 Ce2 O13 72.1(2) 1_455 . ?
O4 Ce2 O13 78.6(2) . . ?
O12 Ce2 O13 67.2(2) . . ?
O19 Ce2 O28 92.1(3) 1_455 . ?
O4 Ce2 O28 146.6(3) . . ?
O12 Ce2 O28 80.0(3) . . ?
O13 Ce2 O28 70.7(3) . . ?
O19 Ce2 O29 72.5(2) 1_455 . ?
O4 Ce2 O29 138.5(3) . . ?
O12 Ce2 O29 139.8(3) . . ?
O13 Ce2 O29 127.6(2) . . ?
O28 Ce2 O29 73.4(3) . . ?
O19 Ce2 O30 77.5(3) 1_455 . ?
O4 Ce2 O30 68.5(3) . . ?
O12 Ce2 O30 129.4(3) . . ?
O13 Ce2 O30 134.4(3) . . ?
O28 Ce2 O30 144.3(3) . . ?
O29 Ce2 O30 70.9(3) . . ?
O19 Ce2 O21 143.0(2) 1_455 . ?
O4 Ce2 O21 112.94(19) . . ?
O12 Ce2 O21 76.5(2) . . ?
O13 Ce2 O21 138.1(2) . . ?
O28 Ce2 O21 83.3(3) . . ?
O29 Ce2 O21 71.0(2) . . ?
O30 Ce2 O21 85.0(3) . . ?
O19 Ce2 O22 139.7(2) 1_455 . ?
O4 Ce2 O22 65.50(19) . . ?
O12 Ce2 O22 69.1(2) . . ?
O13 Ce2 O22 128.4(2) . . ?
O28 Ce2 O22 125.9(3) . . ?
O29 Ce2 O22 103.4(2) . . ?
O30 Ce2 O22 63.9(2) . . ?
O21 Ce2 O22 47.63(19) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.103
# 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 0.164 0.205 0.499 148.8 6.9
2 -0.165 0.705 0.501 148.8 6.8
3 0.310 0.661 1.029 132.4 7.9
4 0.689 0.161 0.971 132.5 7.5
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3A
_database_code_depnum_ccdc_archive 'CCDC 855717'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H48 O31 Pr2'
_chemical_formula_sum            'C58 H48 O31 Pr2'
_chemical_formula_weight         1522.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   9.3330(9)
_cell_length_b                   23.444(2)
_cell_length_c                   16.4638(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.6280(10)
_cell_angle_gamma                90.00
_cell_volume                     3500.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8555
_cell_measurement_theta_min      2.464
_cell_measurement_theta_max      27.311

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_absorpt_coefficient_mu    1.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15820
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12306
_reflns_number_gt                8920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
isor 0.01 C5 C39 C40 C42 C43 C51 C52 O9 C49 C50 C53 C54
isor 0.01  c56 c57 c58
isor 0.01 c21 c22 c23 c24 c33 c38 c39 c41
isor 0.01  o17 o17'
FREE Pr2  C47
FREE C9   Pr1
FLAT     0.100 C48 C49 C50 C51 C52 C53 C54 O23 O24
DELU     0.010   0.010 C48 C49 C50 C51 C52 C53 C54
SIMU     0.040   0.080   1.700 C48 C49 C50 C51 C52 C53 C54
;

_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)+(0.0790P)²+6.9056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(19)
_refine_ls_number_reflns         9605
_refine_ls_number_parameters     809
_refine_ls_number_restraints     232
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1321
_refine_ls_wR_factor_gt          0.1284
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2911(13) 1.0664(5) 0.0310(7) 0.054(3) Uani 1 1 d . . .
C2 C 0.2644(18) 1.1206(7) -0.0195(9) 0.079(4) Uani 1 1 d . . .
C3 C 0.2252(19) 1.1165(9) -0.1095(8) 0.094(5) Uani 1 1 d . . .
H3 H 0.2144 1.0811 -0.1356 0.113 Uiso 1 1 calc R . .
C4 C 0.205(2) 1.1633(10) -0.1536(10) 0.109(7) Uani 1 1 d . . .
H4 H 0.1765 1.1589 -0.2113 0.131 Uiso 1 1 calc R . .
C5 C 0.221(2) 1.2159(11) -0.1256(14) 0.115(6) Uani 1 1 d U . .
H5 H 0.2050 1.2474 -0.1611 0.137 Uiso 1 1 calc R . .
C6 C 0.263(2) 1.2215(9) -0.0392(13) 0.113(6) Uani 1 1 d . . .
H6 H 0.2819 1.2577 -0.0161 0.136 Uiso 1 1 calc R . .
C7 C 0.2785(16) 1.1733(5) 0.0151(9) 0.070(4) Uani 1 1 d . . .
H7 H 0.2976 1.1779 0.0728 0.084 Uiso 1 1 calc R . .
C8 C 0.3787(11) 1.0318(4) 0.1686(6) 0.039(2) Uani 1 1 d . . .
H8 H 0.3220 0.9969 0.1514 0.046 Uiso 1 1 calc R . .
C9 C 0.5420(10) 1.0212(4) 0.1705(6) 0.034(2) Uani 1 1 d . . .
C10 C 0.3629(11) 1.0501(4) 0.2565(6) 0.041(2) Uani 1 1 d . . .
H10 H 0.4012 1.0205 0.2980 0.049 Uiso 1 1 calc R . .
C11 C 0.1961(13) 1.0615(5) 0.2511(7) 0.055(3) Uani 1 1 d . . .
C12 C 0.4567(13) 1.1197(6) 0.3551(8) 0.061(3) Uani 1 1 d . . .
C13 C 0.5174(14) 1.1766(6) 0.3664(8) 0.064(3) Uani 1 1 d . . .
C14 C 0.5462(14) 1.2093(6) 0.3009(8) 0.065(3) Uani 1 1 d . . .
H14 H 0.5305 1.1930 0.2480 0.078 Uiso 1 1 calc R . .
C15 C 0.598(2) 1.2661(8) 0.3119(14) 0.109(7) Uani 1 1 d . . .
H15 H 0.6198 1.2877 0.2689 0.131 Uiso 1 1 calc R . .
C16 C 0.6138(19) 1.2872(7) 0.3942(14) 0.103(6) Uani 1 1 d . . .
H16 H 0.6460 1.3247 0.4040 0.123 Uiso 1 1 calc R . .
C17 C 0.585(2) 1.2565(8) 0.4631(14) 0.117(7) Uani 1 1 d . . .
H17 H 0.6046 1.2718 0.5167 0.140 Uiso 1 1 calc R . .
C18 C 0.5259(19) 1.2025(8) 0.4458(11) 0.096(5) Uani 1 1 d . . .
H18 H 0.4913 1.1828 0.4864 0.115 Uiso 1 1 calc R . .
C19 C 0.5289(14) 0.8912(7) -0.1250(8) 0.068(3) Uani 1 1 d . . .
C20 C 0.5123(16) 0.9337(8) -0.1912(8) 0.074(4) Uani 1 1 d . . .
C21 C 0.539(2) 0.9207(10) -0.2665(11) 0.116(6) Uani 1 1 d U . .
H21 H 0.5652 0.8837 -0.2769 0.139 Uiso 1 1 calc R . .
C22 C 0.528(3) 0.9594(11) -0.3245(15) 0.128(7) Uani 1 1 d U . .
H22 H 0.5392 0.9472 -0.3764 0.154 Uiso 1 1 calc R . .
C23 C 0.502(3) 1.0151(11) -0.3165(14) 0.134(8) Uani 1 1 d U . .
H23 H 0.5041 1.0414 -0.3585 0.161 Uiso 1 1 calc R . .
C24 C 0.469(3) 1.0317(10) -0.2368(13) 0.123(7) Uani 1 1 d U . .
H24 H 0.4425 1.0688 -0.2271 0.147 Uiso 1 1 calc R . .
C25 C 0.4798(18) 0.9892(10) -0.1760(9) 0.101(6) Uani 1 1 d . . .
H25 H 0.4645 0.9988 -0.1239 0.122 Uiso 1 1 calc R . .
C26 C 0.5051(13) 0.8729(4) 0.0128(6) 0.052(3) Uani 1 1 d . . .
H26 H 0.5287 0.8346 -0.0040 0.062 Uiso 1 1 calc R . .
C27 C 0.6280(11) 0.8923(5) 0.0856(6) 0.044(2) Uani 1 1 d . . .
C28 C 0.3476(12) 0.8716(5) 0.0309(6) 0.047(3) Uani 1 1 d . . .
H28 H 0.3064 0.9102 0.0262 0.057 Uiso 1 1 calc R . .
C29 C 0.3493(11) 0.8476(5) 0.1168(6) 0.042(2) Uani 1 1 d . . .
C30 C 0.1241(16) 0.8389(5) -0.0483(6) 0.056(3) Uani 1 1 d . . .
C31 C 0.0467(15) 0.8055(5) -0.1209(7) 0.055(3) Uani 1 1 d . . .
C32 C 0.1173(16) 0.7732(6) -0.1683(7) 0.066(3) Uani 1 1 d . . .
H32 H 0.2198 0.7725 -0.1536 0.079 Uiso 1 1 calc R . .
C33 C 0.0469(19) 0.7419(6) -0.2363(8) 0.077(4) Uani 1 1 d U . .
H33 H 0.0988 0.7204 -0.2673 0.092 Uiso 1 1 calc R . .
C34 C -0.1080(18) 0.7439(6) -0.2565(9) 0.085(5) Uani 1 1 d . . .
H34 H -0.1602 0.7246 -0.3035 0.102 Uiso 1 1 calc R . .
C35 C -0.184(2) 0.7740(7) -0.2083(9) 0.093(5) Uani 1 1 d . . .
H35 H -0.2868 0.7734 -0.2210 0.111 Uiso 1 1 calc R . .
C36 C -0.1069(18) 0.8047(6) -0.1413(8) 0.079(4) Uani 1 1 d . . .
H36 H -0.1578 0.8253 -0.1088 0.095 Uiso 1 1 calc R . .
C37 C 1.1330(15) 0.9532(6) 0.5117(9) 0.066(4) Uani 1 1 d . . .
C38 C 1.0862(12) 0.9466(5) 0.5896(6) 0.064(3) Uani 1 1 d GU . .
C39 C 1.0585(17) 0.8930(5) 0.6187(8) 0.147(8) Uani 1 1 d GU . .
H39 H 1.0663 0.8607 0.5873 0.177 Uiso 1 1 calc R . .
C40 C 1.0193(19) 0.8878(5) 0.6947(9) 0.216(13) Uani 1 1 d GU . .
H40 H 1.0007 0.8519 0.7142 0.259 Uiso 1 1 calc R . .
C41 C 1.0077(17) 0.9361(7) 0.7417(6) 0.105(5) Uani 1 1 d GU . .
H41 H 0.9814 0.9326 0.7925 0.126 Uiso 1 1 calc R . .
C42 C 1.0353(19) 0.9897(6) 0.7126(8) 0.182(11) Uani 1 1 d GU . .
H42 H 1.0276 1.0220 0.7440 0.218 Uiso 1 1 calc R . .
C43 C 1.0746(17) 0.9949(4) 0.6366(8) 0.149(8) Uani 1 1 d GU . .
H43 H 1.0931 1.0308 0.6171 0.178 Uiso 1 1 calc R . .
C44 C 1.1761(9) 0.9148(4) 0.3899(5) 0.0332(19) Uani 1 1 d . . .
H44 H 1.1527 0.9532 0.3672 0.040 Uiso 1 1 calc R . .
C45 C 1.3450(9) 0.9065(4) 0.4089(5) 0.0307(19) Uani 1 1 d . . .
C46 C 1.0992(10) 0.8725(4) 0.3266(6) 0.037(2) Uani 1 1 d . . .
H46 H 1.1299 0.8799 0.2747 0.045 Uiso 1 1 calc R . .
C47 C 0.9288(9) 0.8795(4) 0.3074(5) 0.0310(19) Uani 1 1 d . . .
C48 C 1.1197(17) 0.7759(12) 0.2945(15) 0.117(5) Uani 1 1 d DU . .
C49 C 1.1430(15) 0.7193(8) 0.3096(16) 0.185(6) Uani 1 1 d GDU . .
C50 C 1.169(2) 0.6770(12) 0.2555(11) 0.182(6) Uani 1 1 d GDU . .
H50 H 1.1754 0.6865 0.2017 0.219 Uiso 1 1 calc R . .
C51 C 1.184(2) 0.6205(10) 0.2819(15) 0.199(7) Uani 1 1 d GDU . .
H51 H 1.2012 0.5922 0.2457 0.238 Uiso 1 1 calc R . .
C52 C 1.174(2) 0.6063(9) 0.3623(17) 0.205(7) Uani 1 1 d GDU . .
H52 H 1.1842 0.5686 0.3800 0.246 Uiso 1 1 calc R . .
C53 C 1.148(2) 0.6486(12) 0.4164(11) 0.212(7) Uani 1 1 d GDU . .
H53 H 1.1414 0.6391 0.4702 0.254 Uiso 1 1 calc R . .
C54 C 1.133(2) 0.7051(11) 0.3900(14) 0.197(7) Uani 1 1 d GDU . .
H54 H 1.1157 0.7334 0.4262 0.236 Uiso 1 1 calc R . .
C55 C 0.568(2) 0.7330(7) 0.3101(11) 0.097(6) Uani 1 1 d . . .
H55A H 0.6634 0.7373 0.3470 0.146 Uiso 1 1 calc R . .
H55B H 0.5740 0.7074 0.2656 0.146 Uiso 1 1 calc R . .
H55C H 0.5003 0.7180 0.3405 0.146 Uiso 1 1 calc R . .
C56 C 0.819(3) 1.0980(11) 0.3364(16) 0.143(8) Uani 1 1 d U . .
H56A H 0.9012 1.1189 0.3692 0.215 Uiso 1 1 calc R . .
H56B H 0.7438 1.0946 0.3669 0.215 Uiso 1 1 calc R . .
H56C H 0.7807 1.1178 0.2848 0.215 Uiso 1 1 calc R . .
C57 C 0.691(2) 0.9829(8) 0.4701(10) 0.103(5) Uani 1 1 d U . .
H57A H 0.5947 0.9999 0.4624 0.154 Uiso 1 1 calc R . .
H57B H 0.7645 1.0104 0.4944 0.154 Uiso 1 1 calc R . .
H57C H 0.6975 0.9505 0.5065 0.154 Uiso 1 1 calc R . .
C58 C 0.8875(16) 1.0000(8) -0.0438(7) 0.071(3) Uani 1 1 d U . .
H58A H 0.9877 0.9969 -0.0487 0.106 Uiso 1 1 calc R . .
H58B H 0.8308 1.0205 -0.0910 0.106 Uiso 1 1 calc R . .
H58C H 0.8467 0.9625 -0.0423 0.106 Uiso 1 1 calc R . .
O1 O 0.3199(7) 1.0773(3) 0.1120(4) 0.0427(16) Uani 1 1 d . . .
O2 O 0.2882(11) 1.0178(4) 0.0040(5) 0.070(2) Uani 1 1 d . . .
O3 O 0.6055(8) 1.0503(3) 0.1277(4) 0.0435(16) Uani 1 1 d . . .
O4 O 0.6016(8) 0.9809(3) 0.2166(4) 0.0372(15) Uani 1 1 d . . .
O5 O 0.1152(8) 1.0184(3) 0.2319(5) 0.0477(18) Uani 1 1 d . . .
O6 O 0.1588(8) 1.1099(4) 0.2671(7) 0.083(3) Uani 1 1 d . . .
O7 O 0.4432(8) 1.0996(3) 0.2743(4) 0.0493(18) Uani 1 1 d . . .
O8 O 0.4235(13) 1.0922(5) 0.4100(6) 0.091(3) Uani 1 1 d . . .
O9 O 0.5592(15) 0.8424(6) -0.1328(8) 0.109(4) Uani 1 1 d U . .
O10 O 0.4946(11) 0.9104(4) -0.0565(5) 0.071(2) Uani 1 1 d . . .
O11 O 0.7019(10) 0.9348(3) 0.0744(5) 0.061(2) Uani 1 1 d . . .
O12 O 0.6481(7) 0.8633(3) 0.1511(4) 0.0412(16) Uani 1 1 d . . .
O13 O 0.3718(7) 0.8835(4) 0.1763(4) 0.0511(19) Uani 1 1 d . . .
O14 O 0.3425(9) 0.7943(4) 0.1248(5) 0.058(2) Uani 1 1 d . . .
O15 O 0.0596(10) 0.8671(4) -0.0045(5) 0.077(3) Uani 1 1 d . . .
O16 O 0.2684(10) 0.8377(4) -0.0355(5) 0.061(2) Uani 1 1 d . . .
O17 O 1.099(3) 1.0054(10) 0.4687(13) 0.086(5) Uani 0.50 1 d PU . .
O17' O 1.2217(18) 0.9895(7) 0.5119(10) 0.058(4) Uani 0.50 1 d PU . .
O18 O 1.1213(6) 0.9091(3) 0.4642(4) 0.0385(15) Uani 1 1 d . . .
O19 O 1.3997(6) 0.9165(3) 0.3460(4) 0.0336(14) Uani 1 1 d . . .
O20 O 1.4117(7) 0.8904(4) 0.4793(4) 0.0523(17) Uani 1 1 d . . .
O21 O 0.8556(8) 0.8406(3) 0.3259(5) 0.0423(16) Uani 1 1 d . . .
O22 O 0.8802(7) 0.9268(3) 0.2796(4) 0.0331(14) Uani 1 1 d . . .
O23 O 1.0731(13) 0.7891(5) 0.2206(9) 0.098(4) Uani 1 1 d D . .
O24 O 1.1391(8) 0.8163(3) 0.3505(5) 0.0532(19) Uani 1 1 d D . .
O25 O 0.8837(9) 1.0293(3) 0.0302(5) 0.056(2) Uani 1 1 d . . .
O26 O 1.0245(12) 0.9248(4) 0.1311(6) 0.080(3) Uani 1 1 d . . .
O27 O 0.8637(11) 1.0465(3) 0.3202(6) 0.068(3) Uani 1 1 d . . .
O28 O 0.5155(10) 0.7883(3) 0.2753(6) 0.065(2) Uani 1 1 d . . .
O29 O 0.6450(8) 0.8471(3) 0.4353(4) 0.0467(17) Uani 1 1 d . . .
O30 O 0.7122(9) 0.9654(3) 0.3931(4) 0.0521(19) Uani 1 1 d . . .
O31 O 0.8908(9) 1.1062(3) 0.1684(6) 0.060(2) Uani 1 1 d . . .
Pr1 Pr 0.85643(5) 1.000011(19) 0.17103(3) 0.03341(14) Uani 1 1 d . . .
Pr2 Pr 0.60241(5) 0.888148(17) 0.28919(3) 0.03047(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.221(13) . ?
C1 O1 1.322(13) . ?
C1 C2 1.506(17) . ?
C2 C7 1.35(2) . ?
C2 C3 1.442(19) . ?
C3 C4 1.31(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.31(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.39(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.43(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O1 1.437(12) . ?
C8 C9 1.537(13) . ?
C8 C10 1.550(13) . ?
C8 H8 0.9800 . ?
C9 O3 1.229(11) . ?
C9 O4 1.257(11) . ?
C10 O7 1.376(12) . ?
C10 C11 1.561(14) . ?
C10 H10 0.9800 . ?
C11 O6 1.233(13) . ?
C11 O5 1.256(13) . ?
C12 O8 1.209(16) . ?
C12 O7 1.388(14) . ?
C12 C13 1.444(19) . ?
C13 C14 1.40(2) . ?
C13 C18 1.43(2) . ?
C14 C15 1.41(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.42(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.42(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.38(2) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O9 1.191(19) . ?
C19 O10 1.323(14) . ?
C19 C20 1.46(2) . ?
C20 C21 1.36(2) . ?
C20 C25 1.37(3) . ?
C21 C22 1.30(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.34(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.47(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.40(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O10 1.424(13) . ?
C26 C27 1.519(15) . ?
C26 C28 1.568(15) . ?
C26 H26 0.9800 . ?
C27 O11 1.251(13) . ?
C27 O12 1.251(12) . ?
C28 O16 1.412(12) . ?
C28 C29 1.519(14) . ?
C28 H28 0.9800 . ?
C29 O14 1.261(13) . ?
C29 O13 1.271(12) . ?
C30 O15 1.234(14) . ?
C30 O16 1.314(16) . ?
C30 C31 1.468(16) . ?
C31 C32 1.363(18) . ?
C31 C36 1.39(2) . ?
C32 C33 1.371(17) . ?
C32 H32 0.9300 . ?
C33 C34 1.41(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.38(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.372(18) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O17' 1.188(19) . ?
C37 O18 1.286(14) . ?
C37 O17 1.41(3) . ?
C37 C38 1.457(15) . ?
C38 C39 1.3900 . ?
C38 C43 1.3900 . ?
C39 C40 1.3900 . ?
C39 H39 0.9300 . ?
C40 C41 1.3900 . ?
C40 H40 0.9300 . ?
C41 C42 1.3900 . ?
C41 H41 0.9300 . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 O18 1.439(10) . ?
C44 C46 1.494(13) . ?
C44 C45 1.545(12) . ?
C44 H44 0.9800 . ?
C45 O20 1.239(11) . ?
C45 O19 1.279(10) . ?
C46 O24 1.400(12) . ?
C46 C47 1.555(12) . ?
C46 H46 0.9800 . ?
C47 O21 1.222(11) . ?
C47 O22 1.244(11) . ?
C48 O23 1.23(2) . ?
C48 O24 1.30(2) . ?
C48 C49 1.36(3) . ?
C49 C50 1.3900 . ?
C49 C54 1.3900 . ?
C50 C51 1.3900 . ?
C50 H50 0.9300 . ?
C51 C52 1.3900 . ?
C51 H51 0.9300 . ?
C52 C53 1.3900 . ?
C52 H52 0.9300 . ?
C53 C54 1.3900 . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 O28 1.453(17) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 O27 1.32(3) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 O30 1.392(17) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 O25 1.407(15) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
O3 Pr1 2.569(7) . ?
O4 Pr2 2.480(6) . ?
O4 Pr1 2.695(6) . ?
O5 Pr1 2.426(7) 1_455 ?
O11 Pr1 2.422(8) . ?
O12 Pr2 2.480(6) . ?
O13 Pr2 2.493(6) . ?
O17 O17' 1.25(3) . ?
O19 Pr2 2.394(6) 1_655 ?
O21 Pr2 2.553(7) . ?
O22 Pr1 2.450(6) . ?
O22 Pr2 2.786(6) . ?
O25 Pr1 2.488(7) . ?
O26 Pr1 2.547(7) . ?
O27 Pr1 2.674(8) . ?
O28 Pr2 2.471(8) . ?
O29 Pr2 2.533(6) . ?
O30 Pr2 2.535(7) . ?
O31 Pr1 2.511(8) . ?
Pr1 O5 2.426(8) 1_655 ?
Pr2 O19 2.394(6) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 121.9(10) . . ?
O2 C1 C2 126.9(12) . . ?
O1 C1 C2 111.2(10) . . ?
C7 C2 C3 117.9(14) . . ?
C7 C2 C1 123.3(13) . . ?
C3 C2 C1 118.7(14) . . ?
C4 C3 C2 119.0(18) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 127.2(19) . . ?
C3 C4 H4 116.4 . . ?
C5 C4 H4 116.4 . . ?
C4 C5 C6 115(2) . . ?
C4 C5 H5 122.3 . . ?
C6 C5 H5 122.3 . . ?
C5 C6 C7 122(2) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C2 C7 C6 118.2(15) . . ?
C2 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
O1 C8 C9 111.1(8) . . ?
O1 C8 C10 107.2(7) . . ?
C9 C8 C10 109.8(8) . . ?
O1 C8 H8 109.6 . . ?
C9 C8 H8 109.6 . . ?
C10 C8 H8 109.6 . . ?
O3 C9 O4 124.0(8) . . ?
O3 C9 C8 120.5(8) . . ?
O4 C9 C8 115.5(8) . . ?
O7 C10 C8 105.4(7) . . ?
O7 C10 C11 110.6(8) . . ?
C8 C10 C11 107.9(8) . . ?
O7 C10 H10 110.9 . . ?
C8 C10 H10 110.9 . . ?
C11 C10 H10 110.9 . . ?
O6 C11 O5 127.7(10) . . ?
O6 C11 C10 118.3(10) . . ?
O5 C11 C10 114.0(9) . . ?
O8 C12 O7 123.6(12) . . ?
O8 C12 C13 124.0(12) . . ?
O7 C12 C13 112.4(11) . . ?
C14 C13 C18 119.6(14) . . ?
C14 C13 C12 123.2(11) . . ?
C18 C13 C12 116.5(14) . . ?
C13 C14 C15 122.6(14) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C16 114(2) . . ?
C14 C15 H15 123.0 . . ?
C16 C15 H15 123.0 . . ?
C15 C16 C17 126.1(16) . . ?
C15 C16 H16 117.0 . . ?
C17 C16 H16 117.0 . . ?
C18 C17 C16 116.2(18) . . ?
C18 C17 H17 121.9 . . ?
C16 C17 H17 121.9 . . ?
C17 C18 C13 120.8(18) . . ?
C17 C18 H18 119.6 . . ?
C13 C18 H18 119.6 . . ?
O9 C19 O10 121.9(14) . . ?
O9 C19 C20 124.2(13) . . ?
O10 C19 C20 113.6(13) . . ?
C21 C20 C25 118.4(17) . . ?
C21 C20 C19 121.3(17) . . ?
C25 C20 C19 120.1(12) . . ?
C22 C21 C20 121(2) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 126(2) . . ?
C21 C22 H22 116.9 . . ?
C23 C22 H22 116.9 . . ?
C22 C23 C24 115(2) . . ?
C22 C23 H23 122.4 . . ?
C24 C23 H23 122.4 . . ?
C25 C24 C23 117(2) . . ?
C25 C24 H24 121.4 . . ?
C23 C24 H24 121.4 . . ?
C20 C25 C24 121.8(18) . . ?
C20 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
O10 C26 C27 110.1(9) . . ?
O10 C26 C28 105.9(9) . . ?
C27 C26 C28 115.0(7) . . ?
O10 C26 H26 108.5 . . ?
C27 C26 H26 108.5 . . ?
C28 C26 H26 108.5 . . ?
O11 C27 O12 125.8(10) . . ?
O11 C27 C26 117.5(9) . . ?
O12 C27 C26 116.7(9) . . ?
O16 C28 C29 113.6(9) . . ?
O16 C28 C26 102.0(7) . . ?
C29 C28 C26 112.4(9) . . ?
O16 C28 H28 109.6 . . ?
C29 C28 H28 109.6 . . ?
C26 C28 H28 109.6 . . ?
O14 C29 O13 125.5(10) . . ?
O14 C29 C28 118.3(9) . . ?
O13 C29 C28 115.8(9) . . ?
O15 C30 O16 122.7(11) . . ?
O15 C30 C31 123.2(13) . . ?
O16 C30 C31 114.1(10) . . ?
C32 C31 C36 117.6(12) . . ?
C32 C31 C30 123.4(13) . . ?
C36 C31 C30 118.9(12) . . ?
C31 C32 C33 124.2(14) . . ?
C31 C32 H32 117.9 . . ?
C33 C32 H32 117.9 . . ?
C32 C33 C34 116.3(14) . . ?
C32 C33 H33 121.9 . . ?
C34 C33 H33 121.9 . . ?
C35 C34 C33 121.6(13) . . ?
C35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C36 C35 C34 119.1(17) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C31 121.2(16) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?
O17' C37 O18 122.4(12) . . ?
O17' C37 O17 56.8(13) . . ?
O18 C37 O17 114.4(14) . . ?
O17' C37 C38 115.4(13) . . ?
O18 C37 C38 116.8(11) . . ?
O17 C37 C38 117.2(13) . . ?
C39 C38 C43 120.0 . . ?
C39 C38 C37 121.2(10) . . ?
C43 C38 C37 118.8(10) . . ?
C40 C39 C38 120.0 . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C38 120.0 . . ?
C42 C43 H43 120.0 . . ?
C38 C43 H43 120.0 . . ?
O18 C44 C46 108.8(7) . . ?
O18 C44 C45 111.5(7) . . ?
C46 C44 C45 111.0(7) . . ?
O18 C44 H44 108.5 . . ?
C46 C44 H44 108.5 . . ?
C45 C44 H44 108.5 . . ?
O20 C45 O19 127.2(8) . . ?
O20 C45 C44 119.5(7) . . ?
O19 C45 C44 113.4(7) . . ?
O24 C46 C44 112.1(8) . . ?
O24 C46 C47 110.4(8) . . ?
C44 C46 C47 111.8(7) . . ?
O24 C46 H46 107.4 . . ?
C44 C46 H46 107.4 . . ?
C47 C46 H46 107.4 . . ?
O21 C47 O22 125.6(8) . . ?
O21 C47 C46 118.3(8) . . ?
O22 C47 C46 115.9(8) . . ?
O23 C48 O24 118(2) . . ?
O23 C48 C49 116(2) . . ?
O24 C48 C49 126(2) . . ?
C48 C49 C50 129(2) . . ?
C48 C49 C54 111(2) . . ?
C50 C49 C54 120.0 . . ?
C51 C50 C49 120.0 . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C50 C51 C52 120.0 . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C53 C52 C51 120.0 . . ?
C53 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
C52 C53 C54 120.0 . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C53 C54 C49 120.0 . . ?
C53 C54 H54 120.0 . . ?
C49 C54 H54 120.0 . . ?
O28 C55 H55A 109.5 . . ?
O28 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
O28 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O27 C56 H56A 109.5 . . ?
O27 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O27 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O30 C57 H57A 109.5 . . ?
O30 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O30 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O25 C58 H58A 109.5 . . ?
O25 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O25 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C1 O1 C8 117.8(8) . . ?
C9 O3 Pr1 96.7(6) . . ?
C9 O4 Pr2 154.2(6) . . ?
C9 O4 Pr1 90.0(5) . . ?
Pr2 O4 Pr1 112.2(2) . . ?
C11 O5 Pr1 136.7(7) . 1_455 ?
C10 O7 C12 114.4(9) . . ?
C19 O10 C26 119.2(10) . . ?
C27 O11 Pr1 132.1(7) . . ?
C27 O12 Pr2 129.7(6) . . ?
C29 O13 Pr2 124.1(6) . . ?
C30 O16 C28 116.3(8) . . ?
O17' O17 C37 52.5(13) . . ?
C37 O17' O17 70.7(15) . . ?
C37 O18 C44 116.5(8) . . ?
C45 O19 Pr2 140.2(6) . 1_655 ?
C47 O21 Pr2 98.9(6) . . ?
C47 O22 Pr1 148.8(5) . . ?
C47 O22 Pr2 87.3(5) . . ?
Pr1 O22 Pr2 110.1(2) . . ?
C48 O24 C46 120.1(14) . . ?
C58 O25 Pr1 134.5(8) . . ?
C56 O27 Pr1 128.0(13) . . ?
C55 O28 Pr2 137.4(10) . . ?
C57 O30 Pr2 134.7(9) . . ?
O11 Pr1 O5 139.9(3) . 1_655 ?
O11 Pr1 O22 88.6(2) . . ?
O5 Pr1 O22 85.0(2) 1_655 . ?
O11 Pr1 O25 74.8(3) . . ?
O5 Pr1 O25 91.4(3) 1_655 . ?
O22 Pr1 O25 149.5(2) . . ?
O11 Pr1 O31 132.3(3) . . ?
O5 Pr1 O31 73.2(2) 1_655 . ?
O22 Pr1 O31 135.8(3) . . ?
O25 Pr1 O31 70.7(3) . . ?
O11 Pr1 O26 72.6(3) . . ?
O5 Pr1 O26 67.4(3) 1_655 . ?
O22 Pr1 O26 75.4(2) . . ?
O25 Pr1 O26 75.3(3) . . ?
O31 Pr1 O26 126.4(3) . . ?
O11 Pr1 O3 75.2(3) . . ?
O5 Pr1 O3 141.9(2) 1_655 . ?
O22 Pr1 O3 116.4(2) . . ?
O25 Pr1 O3 84.3(2) . . ?
O31 Pr1 O3 69.6(2) . . ?
O26 Pr1 O3 145.4(3) . . ?
O11 Pr1 O27 138.0(2) . . ?
O5 Pr1 O27 75.0(3) 1_655 . ?
O22 Pr1 O27 68.7(2) . . ?
O25 Pr1 O27 139.2(3) . . ?
O31 Pr1 O27 68.6(3) . . ?
O26 Pr1 O27 129.5(3) . . ?
O3 Pr1 O27 83.8(3) . . ?
O11 Pr1 O4 69.5(2) . . ?
O5 Pr1 O4 140.6(2) 1_655 . ?
O22 Pr1 O4 67.32(19) . . ?
O25 Pr1 O4 126.6(2) . . ?
O31 Pr1 O4 107.1(2) . . ?
O26 Pr1 O4 126.4(3) . . ?
O3 Pr1 O4 49.23(19) . . ?
O27 Pr1 O4 69.2(2) . . ?
O19 Pr2 O28 91.5(3) 1_455 . ?
O19 Pr2 O12 138.3(2) 1_455 . ?
O28 Pr2 O12 79.4(3) . . ?
O19 Pr2 O4 91.8(2) 1_455 . ?
O28 Pr2 O4 145.3(3) . . ?
O12 Pr2 O4 75.3(2) . . ?
O19 Pr2 O13 71.36(19) 1_455 . ?
O28 Pr2 O13 71.5(3) . . ?
O12 Pr2 O13 67.1(2) . . ?
O4 Pr2 O13 77.0(3) . . ?
O19 Pr2 O29 72.3(2) 1_455 . ?
O28 Pr2 O29 72.7(3) . . ?
O12 Pr2 O29 139.3(2) . . ?
O4 Pr2 O29 140.6(2) . . ?
O13 Pr2 O29 127.3(2) . . ?
O19 Pr2 O30 76.6(2) 1_455 . ?
O28 Pr2 O30 144.2(3) . . ?
O12 Pr2 O30 131.1(2) . . ?
O4 Pr2 O30 69.8(2) . . ?
O13 Pr2 O30 132.4(3) . . ?
O29 Pr2 O30 71.5(2) . . ?
O19 Pr2 O21 143.2(2) 1_455 . ?
O28 Pr2 O21 82.7(3) . . ?
O12 Pr2 O21 76.4(2) . . ?
O4 Pr2 O21 113.2(2) . . ?
O13 Pr2 O21 138.2(2) . . ?
O29 Pr2 O21 71.3(2) . . ?
O30 Pr2 O21 87.0(3) . . ?
O19 Pr2 O22 139.8(2) 1_455 . ?
O28 Pr2 O22 126.4(3) . . ?
O12 Pr2 O22 70.2(2) . . ?
O4 Pr2 O22 65.5(2) . . ?
O13 Pr2 O22 128.6(2) . . ?
O29 Pr2 O22 103.7(2) . . ?
O30 Pr2 O22 64.7(2) . . ?
O21 Pr2 O22 48.25(19) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.121
# 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 -0.274 0.166 -0.024 117.0 21.5
2 0.194 0.209 0.483 100.6 21.0
3 -0.194 0.709 0.517 100.6 20.8
4 0.273 0.666 1.024 117.0 21.9
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4A
_database_code_depnum_ccdc_archive 'CCDC 855718'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H45 Nd2 O31'
_chemical_formula_sum            'C57 H45 Nd2 O31'
_chemical_formula_weight         1514.41

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'
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   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   9.3238(19)
_cell_length_b                   23.424(5)
_cell_length_c                   16.730(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.70(3)
_cell_angle_gamma                90.00
_cell_volume                     3564.5(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12370
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1510
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27892
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12538
_reflns_number_gt                9510
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
ISOR 0.01  C3 C4 C5 C6 C18 C21 C22 C23 C24 C32 C39 C40 C41 C42 C43
ISOR 0.01 C50 C51 C52 C53 C54 C55 C57 O8 O9 o17' O17
isor 0.01 c49  c58 c17 c25 c33 c38
dfix 1.39 0.01 c53 c54 c54 c49 c24 c25
dfix 1.39 0.01 c49 c50 c50 c51 c51 c52 c52 c53
dfix 1.50 0.01 c57 o30
FREE Nd2  C47
FREE C9   Nd1
DELU     0.010   0.010 C1 C2 C3 C4 C5 C6 C7
SIMU     0.040   0.080   1.700 C1 C2 C3 C4 C5 C6 C7
DELU     0.010   0.010 C19 C20 C21 C22 C23 C24 C25
SIMU     0.040   0.080   1.700 C19 C20 C21 C22 C23 C24 C25
DELU     0.010   0.010 C37 C38 C39 C40 C41 C42 C43
SIMU     0.040   0.080   1.700 C37 C38 C39 C40 C41 C42 C43
DELU     0.010   0.010 C49 C50 C51 C52 C53 C54
SIMU     0.040   0.080   1.700 C49 C50 C51 C52 C53 C54
DELU     0.010   0.010 C55 O28
SIMU     0.040   0.080   1.700 C55 O28
DELU     0.010   0.010 C57 O30
SIMU     0.040   0.080   1.700 C57 O30
DELU     0.010   0.010 C13 C14 C15 C16 C17 C18
SIMU     0.040   0.080   1.700 C13 C14 C15 C16 C17 C18
;

_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)+(0.1044P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_number_reflns         12370
_refine_ls_number_parameters     808
_refine_ls_number_restraints     482
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1784
_refine_ls_wR_factor_gt          0.1435
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2891(14) 1.0637(6) 0.0374(10) 0.089(3) Uani 1 1 d U . .
C2 C 0.2510(18) 1.1133(8) -0.0136(11) 0.112(4) Uani 1 1 d U . .
C3 C 0.217(2) 1.1058(10) -0.1031(14) 0.135(4) Uani 1 1 d U . .
H3 H 0.2111 1.0695 -0.1262 0.162 Uiso 1 1 calc R . .
C4 C 0.194(3) 1.1537(11) -0.1517(16) 0.147(5) Uani 1 1 d U . .
H4 H 0.1681 1.1495 -0.2083 0.176 Uiso 1 1 calc R . .
C5 C 0.209(3) 1.2063(11) -0.1192(16) 0.147(5) Uani 1 1 d U . .
H5 H 0.1920 1.2383 -0.1529 0.176 Uiso 1 1 calc R . .
C6 C 0.250(3) 1.2126(10) -0.0368(15) 0.143(5) Uani 1 1 d U . .
H6 H 0.2716 1.2490 -0.0153 0.172 Uiso 1 1 calc R . .
C7 C 0.261(2) 1.1666(7) 0.0170(14) 0.123(5) Uani 1 1 d U . .
H7 H 0.2746 1.1727 0.0731 0.147 Uiso 1 1 calc R . .
C8 C 0.3712(10) 1.0314(5) 0.1735(7) 0.057(2) Uani 1 1 d . . .
H8 H 0.3137 0.9966 0.1570 0.068 Uiso 1 1 calc R . .
C9 C 0.5373(10) 1.0182(5) 0.1769(7) 0.058(3) Uani 1 1 d . . .
C10 C 0.3488(11) 1.0500(4) 0.2551(7) 0.058(2) Uani 1 1 d . . .
H10 H 0.3857 1.0206 0.2961 0.070 Uiso 1 1 calc R . .
C11 C 0.1909(11) 1.0628(5) 0.2546(8) 0.068(3) Uani 1 1 d . . .
C12 C 0.4491(14) 1.1238(6) 0.3519(8) 0.077(3) Uani 1 1 d . . .
C13 C 0.5097(15) 1.1825(7) 0.3609(10) 0.092(3) Uani 1 1 d U . .
C14 C 0.5416(16) 1.2103(6) 0.2955(11) 0.097(4) Uani 1 1 d U . .
H14 H 0.5346 1.1918 0.2456 0.117 Uiso 1 1 calc R . .
C15 C 0.587(2) 1.2698(8) 0.3060(14) 0.124(5) Uani 1 1 d U . .
H15 H 0.5989 1.2925 0.2623 0.149 Uiso 1 1 calc R . .
C16 C 0.611(2) 1.2904(8) 0.3861(14) 0.120(5) Uani 1 1 d U . .
H16 H 0.6519 1.3267 0.3964 0.144 Uiso 1 1 calc R . .
C17 C 0.580(2) 1.2607(9) 0.4507(15) 0.135(5) Uani 1 1 d U . .
H17 H 0.6013 1.2764 0.5030 0.162 Uiso 1 1 calc R . .
C18 C 0.516(2) 1.2080(8) 0.4382(13) 0.120(4) Uani 1 1 d U . .
H18 H 0.4796 1.1896 0.4787 0.144 Uiso 1 1 calc R . .
C19 C 0.5400(16) 0.8849(8) -0.1098(9) 0.093(3) Uani 1 1 d U . .
C20 C 0.5201(17) 0.9291(8) -0.1748(12) 0.105(4) Uani 1 1 d U . .
C21 C 0.548(2) 0.9130(10) -0.2471(14) 0.133(4) Uani 1 1 d U . .
H21 H 0.5792 0.8759 -0.2533 0.160 Uiso 1 1 calc R . .
C22 C 0.532(3) 0.9489(10) -0.3100(16) 0.149(5) Uani 1 1 d U . .
H22 H 0.5413 0.9357 -0.3611 0.179 Uiso 1 1 calc R . .
C23 C 0.500(3) 1.0115(11) -0.2985(16) 0.150(5) Uani 1 1 d U . .
H23 H 0.5116 1.0397 -0.3355 0.181 Uiso 1 1 calc R . .
C24 C 0.452(3) 1.0225(10) -0.2300(15) 0.148(5) Uani 1 1 d DU . .
H24 H 0.4048 1.0569 -0.2250 0.178 Uiso 1 1 calc R . .
C25 C 0.472(3) 0.9827(9) -0.1661(14) 0.143(5) Uani 1 1 d DU . .
H25 H 0.4508 0.9934 -0.1163 0.171 Uiso 1 1 calc R . .
C26 C 0.5114(14) 0.8696(5) 0.0247(8) 0.071(3) Uani 1 1 d . . .
H26 H 0.5354 0.8308 0.0101 0.085 Uiso 1 1 calc R . .
C27 C 0.6312(11) 0.8912(6) 0.0952(6) 0.066(3) Uani 1 1 d . . .
C28 C 0.3551(13) 0.8703(5) 0.0412(7) 0.066(3) Uani 1 1 d . . .
H28 H 0.3149 0.9091 0.0360 0.080 Uiso 1 1 calc R . .
C29 C 0.3521(11) 0.8452(5) 0.1263(7) 0.060(3) Uani 1 1 d . . .
C30 C 0.1241(16) 0.8380(5) -0.0386(9) 0.081(4) Uani 1 1 d . . .
C31 C 0.0496(16) 0.8050(6) -0.1080(8) 0.081(3) Uani 1 1 d . . .
C32 C 0.130(2) 0.7754(8) -0.1582(11) 0.111(5) Uani 1 1 d U . .
H32 H 0.2325 0.7775 -0.1465 0.133 Uiso 1 1 calc R . .
C33 C 0.056(2) 0.7433(7) -0.2249(11) 0.110(5) Uani 1 1 d U . .
H33 H 0.1068 0.7233 -0.2582 0.132 Uiso 1 1 calc R . .
C34 C -0.103(3) 0.7424(7) -0.2398(14) 0.130(7) Uani 1 1 d . . .
H34 H -0.1554 0.7202 -0.2823 0.156 Uiso 1 1 calc R . .
C35 C -0.1756(18) 0.7733(9) -0.1932(14) 0.123(7) Uani 1 1 d . . .
H35 H -0.2777 0.7744 -0.2067 0.148 Uiso 1 1 calc R . .
C36 C -0.1006(15) 0.8032(7) -0.1257(10) 0.095(4) Uani 1 1 d . . .
H36 H -0.1525 0.8221 -0.0921 0.114 Uiso 1 1 calc R . .
C37 C 1.125(2) 0.9549(7) 0.5146(13) 0.111(5) Uani 1 1 d U . .
C38 C 1.0743(15) 0.9465(7) 0.5909(8) 0.122(4) Uani 1 1 d GU . .
C39 C 1.0392(17) 0.8924(6) 0.6149(9) 0.155(5) Uani 1 1 d GU . .
H39 H 1.0458 0.8610 0.5819 0.187 Uiso 1 1 calc R . .
C40 C 0.9942(19) 0.8853(6) 0.6881(10) 0.173(5) Uani 1 1 d GU . .
H40 H 0.9707 0.8491 0.7042 0.208 Uiso 1 1 calc R . .
C41 C 0.9843(18) 0.9322(8) 0.7374(8) 0.162(5) Uani 1 1 d GU . .
H41 H 0.9541 0.9275 0.7864 0.195 Uiso 1 1 calc R . .
C42 C 1.0194(18) 0.9863(7) 0.7134(9) 0.165(5) Uani 1 1 d GU . .
H42 H 1.0128 1.0178 0.7464 0.197 Uiso 1 1 calc R . .
C43 C 1.0644(17) 0.9935(5) 0.6402(10) 0.157(5) Uani 1 1 d GU . .
H43 H 1.0879 1.0297 0.6241 0.188 Uiso 1 1 calc R . .
C44 C 1.1687(10) 0.9180(5) 0.3909(7) 0.060(3) Uani 1 1 d . . .
H44 H 1.1454 0.9566 0.3692 0.072 Uiso 1 1 calc R . .
C45 C 1.3362(10) 0.9082(4) 0.4088(6) 0.052(2) Uani 1 1 d . . .
C46 C 1.0947(9) 0.8748(5) 0.3304(7) 0.056(2) Uani 1 1 d . . .
H46 H 1.1238 0.8827 0.2787 0.067 Uiso 1 1 calc R . .
C47 C 0.9262(10) 0.8814(5) 0.3143(7) 0.060(2) Uani 1 1 d . . .
C48 C 1.1122(13) 0.7794(7) 0.2925(15) 0.103(6) Uani 1 1 d . . .
C49 C 1.150(3) 0.7231(11) 0.3085(15) 0.155(6) Uani 1 1 d DU . .
C50 C 1.166(3) 0.6820(11) 0.2509(18) 0.179(6) Uani 1 1 d DU . .
H50 H 1.1532 0.6922 0.1960 0.215 Uiso 1 1 calc R . .
C51 C 1.199(3) 0.6256(11) 0.2749(17) 0.180(6) Uani 1 1 d DU . .
H51 H 1.2159 0.5989 0.2367 0.216 Uiso 1 1 calc R . .
C52 C 1.208(3) 0.6094(13) 0.3556(16) 0.181(6) Uani 1 1 d DU . .
H52 H 1.2291 0.5714 0.3695 0.217 Uiso 1 1 calc R . .
C53 C 1.188(3) 0.6464(11) 0.4165(18) 0.184(6) Uani 1 1 d DU . .
H53 H 1.1916 0.6355 0.4703 0.220 Uiso 1 1 calc R . .
C54 C 1.163(3) 0.7022(11) 0.3871(16) 0.169(6) Uani 1 1 d DU . .
H54 H 1.1525 0.7293 0.4262 0.203 Uiso 1 1 calc R . .
C55 C 0.586(3) 0.7350(13) 0.3220(18) 0.177(8) Uani 1 1 d U . .
H55A H 0.6707 0.7223 0.3030 0.265 Uiso 1 1 d R . .
H55B H 0.5098 0.7068 0.3088 0.265 Uiso 1 1 d R . .
H55C H 0.6122 0.7403 0.3803 0.265 Uiso 1 1 d R . .
C57 C 0.675(3) 0.9969(13) 0.4689(14) 0.196(8) Uani 1 1 d DU . .
H57A H 0.5701 0.9931 0.4592 0.293 Uiso 1 1 d R . .
H57B H 0.7010 1.0366 0.4734 0.293 Uiso 1 1 d R . .
H57C H 0.7195 0.9777 0.5189 0.293 Uiso 1 1 d R . .
C58 C 0.884(2) 1.0017(11) -0.0332(13) 0.139(6) Uani 1 1 d U . .
H58A H 0.8960 0.9615 -0.0225 0.208 Uiso 1 1 d R . .
H58B H 0.9641 1.0155 -0.0551 0.208 Uiso 1 1 d R . .
H58C H 0.7930 1.0081 -0.0722 0.208 Uiso 1 1 d R . .
O1 O 0.3171(8) 1.0754(3) 0.1166(5) 0.0681(19) Uani 1 1 d . . .
O2 O 0.2854(14) 1.0149(5) 0.0138(6) 0.116(4) Uani 1 1 d . . .
O3 O 0.6020(8) 1.0489(4) 0.1353(5) 0.073(2) Uani 1 1 d . . .
O4 O 0.5966(7) 0.9808(3) 0.2238(5) 0.0564(17) Uani 1 1 d . . .
O5 O 0.1051(7) 1.0194(3) 0.2341(6) 0.073(2) Uani 1 1 d . . .
O6 O 0.1462(11) 1.1104(4) 0.2657(9) 0.111(4) Uani 1 1 d . . .
O7 O 0.4351(8) 1.1021(4) 0.2750(5) 0.073(2) Uani 1 1 d . . .
O8 O 0.4164(14) 1.0966(5) 0.4070(8) 0.117(4) Uani 1 1 d U . .
O9 O 0.5576(16) 0.8371(6) -0.1193(9) 0.130(4) Uani 1 1 d U . .
O10 O 0.5010(12) 0.9056(4) -0.0434(5) 0.089(3) Uani 1 1 d . . .
O11 O 0.7025(11) 0.9342(4) 0.0841(6) 0.096(3) Uani 1 1 d . . .
O12 O 0.6481(8) 0.8621(4) 0.1613(5) 0.077(3) Uani 1 1 d . . .
O13 O 0.3705(7) 0.8811(4) 0.1832(5) 0.070(2) Uani 1 1 d . . .
O14 O 0.3397(11) 0.7930(4) 0.1333(6) 0.086(2) Uani 1 1 d . . .
O15 O 0.0670(11) 0.8658(6) 0.0072(8) 0.129(5) Uani 1 1 d . . .
O16 O 0.2732(9) 0.8337(3) -0.0233(5) 0.072(2) Uani 1 1 d . . .
O17 O 1.101(4) 1.0077(16) 0.478(2) 0.158(10) Uani 0.50 1 d PU . .
O17' O 1.199(2) 0.9939(9) 0.5050(12) 0.087(5) Uani 0.50 1 d PU . .
O18 O 1.1152(7) 0.9102(3) 0.4648(5) 0.0634(19) Uani 1 1 d . . .
O19 O 1.3907(8) 0.9172(3) 0.3483(5) 0.0646(19) Uani 1 1 d . . .
O20 O 1.4032(8) 0.8936(5) 0.4803(4) 0.080(2) Uani 1 1 d . . .
O21 O 0.8518(7) 0.8424(4) 0.3334(5) 0.068(2) Uani 1 1 d . . .
O22 O 0.8729(7) 0.9281(3) 0.2832(5) 0.0585(17) Uani 1 1 d . . .
O23 O 1.0582(13) 0.7959(6) 0.2198(10) 0.118(4) Uani 1 1 d . . .
O24 O 1.1355(9) 0.8190(4) 0.3521(6) 0.080(2) Uani 1 1 d . . .
O25 O 0.8779(11) 1.0273(4) 0.0380(6) 0.090(3) Uani 1 1 d . . .
O26 O 1.0163(12) 0.9251(4) 0.1389(6) 0.095(3) Uani 1 1 d . . .
O27 O 0.8455(13) 1.0468(4) 0.3151(8) 0.109(4) Uani 1 1 d . . .
O28 O 0.5139(13) 0.7890(4) 0.2843(7) 0.107(3) Uani 1 1 d U . .
O29 O 0.6400(8) 0.8492(4) 0.4361(5) 0.075(2) Uani 1 1 d . . .
O30 O 0.7035(11) 0.9656(5) 0.3954(6) 0.097(3) Uani 1 1 d DU . .
O31 O 0.8842(10) 1.1049(4) 0.1671(9) 0.115(4) Uani 1 1 d . . .
Nd1 Nd 0.85135(5) 0.99974(2) 0.17633(4) 0.05737(17) Uani 1 1 d . . .
Nd2 Nd 0.59602(5) 0.88816(2) 0.29316(3) 0.05242(15) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.208(16) . ?
C1 O1 1.320(17) . ?
C1 C2 1.44(2) . ?
C2 C7 1.35(2) . ?
C2 C3 1.47(3) . ?
C3 C4 1.38(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.34(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.35(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.39(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O1 1.419(13) . ?
C8 C10 1.491(15) . ?
C8 C9 1.568(13) . ?
C8 H8 0.9800 . ?
C9 O4 1.223(12) . ?
C9 O3 1.245(13) . ?
C10 O7 1.459(13) . ?
C10 C11 1.501(14) . ?
C10 H10 0.9800 . ?
C11 O6 1.219(15) . ?
C11 O5 1.292(14) . ?
C12 O8 1.212(16) . ?
C12 O7 1.364(15) . ?
C12 C13 1.48(2) . ?
C13 C14 1.36(2) . ?
C13 C18 1.41(2) . ?
C14 C15 1.46(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.40(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.37(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.36(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O9 1.15(2) . ?
C19 O10 1.334(16) . ?
C19 C20 1.48(2) . ?
C20 C21 1.35(3) . ?
C20 C25 1.35(3) . ?
C21 C22 1.33(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.52(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.34(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.401(10) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 O10 1.403(14) . ?
C26 C27 1.521(16) . ?
C26 C28 1.542(17) . ?
C26 H26 0.9800 . ?
C27 O11 1.244(15) . ?
C27 O12 1.280(15) . ?
C28 O16 1.455(13) . ?
C28 C29 1.545(16) . ?
C28 H28 0.9800 . ?
C29 O14 1.237(14) . ?
C29 O13 1.255(13) . ?
C30 O15 1.214(15) . ?
C30 O16 1.361(16) . ?
C30 C31 1.440(18) . ?
C31 C36 1.367(19) . ?
C31 C32 1.43(2) . ?
C32 C33 1.40(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.45(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.35(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.38(2) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 O17' 1.17(2) . ?
C37 O18 1.329(18) . ?
C37 O17 1.38(4) . ?
C37 C38 1.47(2) . ?
C38 C39 1.3900 . ?
C38 C43 1.3900 . ?
C39 C40 1.3900 . ?
C39 H39 0.9300 . ?
C40 C41 1.3900 . ?
C40 H40 0.9300 . ?
C41 C42 1.3900 . ?
C41 H41 0.9300 . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 O18 1.444(13) . ?
C44 C46 1.488(15) . ?
C44 C45 1.542(13) . ?
C44 H44 0.9800 . ?
C45 O19 1.247(12) . ?
C45 O20 1.269(12) . ?
C46 O24 1.388(13) . ?
C46 C47 1.542(12) . ?
C46 H46 0.9800 . ?
C47 O21 1.231(13) . ?
C47 O22 1.263(13) . ?
C48 O23 1.27(2) . ?
C48 O24 1.34(2) . ?
C48 C49 1.38(3) . ?
C49 C54 1.383(10) . ?
C49 C50 1.392(10) . ?
C50 C51 1.396(10) . ?
C50 H50 0.9300 . ?
C51 C52 1.387(10) . ?
C51 H51 0.9300 . ?
C52 C53 1.380(10) . ?
C52 H52 0.9300 . ?
C53 C54 1.399(10) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 O28 1.51(3) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C57 O30 1.506(10) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9599 . ?
C57 H57C 0.9600 . ?
C58 O25 1.35(2) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
O3 Nd1 2.550(7) . ?
O4 Nd2 2.462(6) . ?
O4 Nd1 2.702(6) . ?
O5 Nd1 2.396(7) 1_455 ?
O11 Nd1 2.392(9) . ?
O12 Nd2 2.439(7) . ?
O13 Nd2 2.476(7) . ?
O17 O17' 0.98(3) . ?
O19 Nd2 2.399(7) 1_655 ?
O21 Nd2 2.566(7) . ?
O22 Nd1 2.429(7) . ?
O22 Nd2 2.785(6) . ?
O25 Nd1 2.467(9) . ?
O26 Nd1 2.498(9) . ?
O27 Nd1 2.582(11) . ?
O28 Nd2 2.439(9) . ?
O29 Nd2 2.508(8) . ?
O30 Nd2 2.542(10) . ?
O31 Nd1 2.492(9) . ?
Nd1 O5 2.396(7) 1_655 ?
Nd2 O19 2.399(7) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 120.6(15) . . ?
O2 C1 C2 125.7(15) . . ?
O1 C1 C2 113.4(12) . . ?
C7 C2 C1 122.4(17) . . ?
C7 C2 C3 118.7(19) . . ?
C1 C2 C3 118.5(16) . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C5 C4 C3 121(3) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 120(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 123(2) . . ?
C5 C6 H6 118.7 . . ?
C7 C6 H6 118.7 . . ?
C2 C7 C6 119(2) . . ?
C2 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
O1 C8 C10 107.5(8) . . ?
O1 C8 C9 111.7(8) . . ?
C10 C8 C9 111.1(9) . . ?
O1 C8 H8 108.8 . . ?
C10 C8 H8 108.8 . . ?
C9 C8 H8 108.8 . . ?
O4 C9 O3 124.5(9) . . ?
O4 C9 C8 117.9(9) . . ?
O3 C9 C8 117.5(10) . . ?
O7 C10 C8 105.8(8) . . ?
O7 C10 C11 109.0(9) . . ?
C8 C10 C11 112.8(9) . . ?
O7 C10 H10 109.7 . . ?
C8 C10 H10 109.7 . . ?
C11 C10 H10 109.7 . . ?
O6 C11 O5 123.2(10) . . ?
O6 C11 C10 123.3(11) . . ?
O5 C11 C10 113.2(10) . . ?
O8 C12 O7 122.3(13) . . ?
O8 C12 C13 124.3(14) . . ?
O7 C12 C13 113.4(12) . . ?
C14 C13 C18 124.1(16) . . ?
C14 C13 C12 120.5(14) . . ?
C18 C13 C12 115.1(15) . . ?
C13 C14 C15 118.0(16) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
C16 C15 C14 115.4(19) . . ?
C16 C15 H15 122.3 . . ?
C14 C15 H15 122.3 . . ?
C17 C16 C15 124.2(18) . . ?
C17 C16 H16 117.9 . . ?
C15 C16 H16 117.9 . . ?
C18 C17 C16 120(2) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C13 117(2) . . ?
C17 C18 H18 121.5 . . ?
C13 C18 H18 121.5 . . ?
O9 C19 O10 122.9(16) . . ?
O9 C19 C20 125.3(16) . . ?
O10 C19 C20 110.2(15) . . ?
C21 C20 C25 119(2) . . ?
C21 C20 C19 116.5(17) . . ?
C25 C20 C19 124.0(18) . . ?
C22 C21 C20 122(2) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C22 C23 120(2) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 114(2) . . ?
C24 C23 H23 122.9 . . ?
C22 C23 H23 122.9 . . ?
C23 C24 C25 121(2) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C20 C25 C24 122(2) . . ?
C20 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
O10 C26 C27 109.7(10) . . ?
O10 C26 C28 103.9(10) . . ?
C27 C26 C28 114.9(9) . . ?
O10 C26 H26 109.4 . . ?
C27 C26 H26 109.4 . . ?
C28 C26 H26 109.4 . . ?
O11 C27 O12 126.4(11) . . ?
O11 C27 C26 118.6(11) . . ?
O12 C27 C26 115.0(11) . . ?
O16 C28 C26 102.9(8) . . ?
O16 C28 C29 110.2(9) . . ?
C26 C28 C29 111.7(9) . . ?
O16 C28 H28 110.6 . . ?
C26 C28 H28 110.6 . . ?
C29 C28 H28 110.6 . . ?
O14 C29 O13 126.3(11) . . ?
O14 C29 C28 119.0(10) . . ?
O13 C29 C28 114.6(10) . . ?
O15 C30 O16 119.5(12) . . ?
O15 C30 C31 126.6(13) . . ?
O16 C30 C31 113.8(11) . . ?
C36 C31 C32 120.4(14) . . ?
C36 C31 C30 118.8(13) . . ?
C32 C31 C30 120.8(14) . . ?
C33 C32 C31 120.0(17) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 116.9(18) . . ?
C32 C33 H33 121.6 . . ?
C34 C33 H33 121.6 . . ?
C35 C34 C33 121.3(16) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C34 C35 C36 120.9(16) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C31 C36 C35 120.2(16) . . ?
C31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
O17' C37 O18 119.4(19) . . ?
O17' C37 O17 44.1(16) . . ?
O18 C37 O17 116(2) . . ?
O17' C37 C38 122.2(18) . . ?
O18 C37 C38 116.5(13) . . ?
O17 C37 C38 117(2) . . ?
C39 C38 C43 120.0 . . ?
C39 C38 C37 121.0(12) . . ?
C43 C38 C37 119.0(12) . . ?
C40 C39 C38 120.0 . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C38 120.0 . . ?
C42 C43 H43 120.0 . . ?
C38 C43 H43 120.0 . . ?
O18 C44 C46 107.5(8) . . ?
O18 C44 C45 109.9(8) . . ?
C46 C44 C45 109.2(8) . . ?
O18 C44 H44 110.1 . . ?
C46 C44 H44 110.1 . . ?
C45 C44 H44 110.1 . . ?
O19 C45 O20 127.4(9) . . ?
O19 C45 C44 113.1(9) . . ?
O20 C45 C44 119.4(8) . . ?
O24 C46 C44 113.8(9) . . ?
O24 C46 C47 110.5(8) . . ?
C44 C46 C47 110.7(8) . . ?
O24 C46 H46 107.2 . . ?
C44 C46 H46 107.2 . . ?
C47 C46 H46 107.2 . . ?
O21 C47 O22 123.7(9) . . ?
O21 C47 C46 119.4(9) . . ?
O22 C47 C46 116.9(9) . . ?
O23 C48 O24 117.8(14) . . ?
O23 C48 C49 121(2) . . ?
O24 C48 C49 122(2) . . ?
C48 C49 C54 119(2) . . ?
C48 C49 C50 126(2) . . ?
C54 C49 C50 115(3) . . ?
C49 C50 C51 120(3) . . ?
C49 C50 H50 119.8 . . ?
C51 C50 H50 119.8 . . ?
C52 C51 C50 120(3) . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C53 C52 C51 124(3) . . ?
C53 C52 H52 118.1 . . ?
C51 C52 H52 118.1 . . ?
C52 C53 C54 112(3) . . ?
C52 C53 H53 124.2 . . ?
C54 C53 H53 124.2 . . ?
C49 C54 C53 129(3) . . ?
C49 C54 H54 115.3 . . ?
C53 C54 H54 115.3 . . ?
O28 C55 H55A 116.4 . . ?
O28 C55 H55B 103.9 . . ?
H55A C55 H55B 109.5 . . ?
O28 C55 H55C 107.9 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O30 C57 H57A 99.9 . . ?
O30 C57 H57B 116.7 . . ?
H57A C57 H57B 109.5 . . ?
O30 C57 H57C 111.3 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O25 C58 H58A 107.3 . . ?
O25 C58 H58B 111.9 . . ?
H58A C58 H58B 109.5 . . ?
O25 C58 H58C 109.2 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C1 O1 C8 119.0(10) . . ?
C9 O3 Nd1 96.5(6) . . ?
C9 O4 Nd2 152.3(6) . . ?
C9 O4 Nd1 89.8(6) . . ?
Nd2 O4 Nd1 112.1(2) . . ?
C11 O5 Nd1 139.2(6) . 1_455 ?
C12 O7 C10 117.4(9) . . ?
C19 O10 C26 118.4(12) . . ?
C27 O11 Nd1 132.6(8) . . ?
C27 O12 Nd2 129.6(7) . . ?
C29 O13 Nd2 124.1(7) . . ?
C30 O16 C28 116.3(9) . . ?
O17' O17 C37 57(2) . . ?
O17 O17' C37 79(3) . . ?
C37 O18 C44 116.5(10) . . ?
C45 O19 Nd2 140.0(6) . 1_655 ?
C47 O21 Nd2 99.6(6) . . ?
C47 O22 Nd1 149.5(7) . . ?
C47 O22 Nd2 88.4(5) . . ?
Nd1 O22 Nd2 110.4(3) . . ?
C48 O24 C46 117.8(12) . . ?
C58 O25 Nd1 138.2(12) . . ?
C55 O28 Nd2 132.0(14) . . ?
C57 O30 Nd2 141.5(13) . . ?
O11 Nd1 O5 139.9(3) . 1_655 ?
O11 Nd1 O22 88.5(3) . . ?
O5 Nd1 O22 85.5(3) 1_655 . ?
O11 Nd1 O25 74.1(3) . . ?
O5 Nd1 O25 92.0(3) 1_655 . ?
O22 Nd1 O25 149.6(3) . . ?
O11 Nd1 O31 131.0(4) . . ?
O5 Nd1 O31 73.2(3) 1_655 . ?
O22 Nd1 O31 137.5(4) . . ?
O25 Nd1 O31 69.1(4) . . ?
O11 Nd1 O26 72.0(4) . . ?
O5 Nd1 O26 68.1(3) 1_655 . ?
O22 Nd1 O26 75.2(3) . . ?
O25 Nd1 O26 75.7(3) . . ?
O31 Nd1 O26 125.9(4) . . ?
O11 Nd1 O3 75.6(3) . . ?
O5 Nd1 O3 141.5(3) 1_655 . ?
O22 Nd1 O3 115.7(3) . . ?
O25 Nd1 O3 84.4(3) . . ?
O31 Nd1 O3 69.8(3) . . ?
O26 Nd1 O3 145.5(3) . . ?
O11 Nd1 O27 136.9(3) . . ?
O5 Nd1 O27 76.7(3) 1_655 . ?
O22 Nd1 O27 69.4(3) . . ?
O25 Nd1 O27 139.3(4) . . ?
O31 Nd1 O27 70.2(4) . . ?
O26 Nd1 O27 131.3(4) . . ?
O3 Nd1 O27 81.4(4) . . ?
O11 Nd1 O4 70.2(3) . . ?
O5 Nd1 O4 140.1(3) 1_655 . ?
O22 Nd1 O4 66.8(2) . . ?
O25 Nd1 O4 126.5(3) . . ?
O31 Nd1 O4 108.0(3) . . ?
O26 Nd1 O4 126.1(3) . . ?
O3 Nd1 O4 49.0(2) . . ?
O27 Nd1 O4 67.1(3) . . ?
O19 Nd2 O12 138.9(3) 1_455 . ?
O19 Nd2 O28 91.6(4) 1_455 . ?
O12 Nd2 O28 80.1(4) . . ?
O19 Nd2 O4 90.9(2) 1_455 . ?
O12 Nd2 O4 76.9(3) . . ?
O28 Nd2 O4 147.5(3) . . ?
O19 Nd2 O13 71.7(2) 1_455 . ?
O12 Nd2 O13 67.5(2) . . ?
O28 Nd2 O13 71.8(3) . . ?
O4 Nd2 O13 78.4(3) . . ?
O19 Nd2 O29 73.3(3) 1_455 . ?
O12 Nd2 O29 138.5(3) . . ?
O28 Nd2 O29 72.3(3) . . ?
O4 Nd2 O29 138.9(3) . . ?
O13 Nd2 O29 128.2(3) . . ?
O19 Nd2 O30 76.6(3) 1_455 . ?
O12 Nd2 O30 131.3(3) . . ?
O28 Nd2 O30 142.4(3) . . ?
O4 Nd2 O30 69.3(3) . . ?
O13 Nd2 O30 133.8(3) . . ?
O29 Nd2 O30 70.1(3) . . ?
O19 Nd2 O21 142.4(3) 1_455 . ?
O12 Nd2 O21 77.0(3) . . ?
O28 Nd2 O21 83.1(3) . . ?
O4 Nd2 O21 113.2(2) . . ?
O13 Nd2 O21 139.1(3) . . ?
O29 Nd2 O21 69.5(3) . . ?
O30 Nd2 O21 85.1(3) . . ?
O19 Nd2 O22 139.1(3) 1_455 . ?
O12 Nd2 O22 70.0(3) . . ?
O28 Nd2 O22 126.8(3) . . ?
O4 Nd2 O22 65.0(2) . . ?
O13 Nd2 O22 128.7(2) . . ?
O29 Nd2 O22 102.7(2) . . ?
O30 Nd2 O22 64.4(3) . . ?
O21 Nd2 O22 48.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.122
# 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 0.144 0.196 0.490 157.4 7.6
2 -0.144 0.696 0.510 157.3 7.5
3 0.311 0.664 1.033 128.5 7.5
4 0.689 0.164 0.967 128.5 7.4
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 859164'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 Ce O20, C6 N'
_chemical_formula_sum            'C44 H36 Ce N O20'
_chemical_formula_weight         1038.86

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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'

_cell_length_a                   20.195(4)
_cell_length_b                   16.765(3)
_cell_length_c                   16.778(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5680.5(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    45810
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44683
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10017
_reflns_number_gt                9286
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
dfix 0.85 0.01 h108 o20
dfix 1.5 0.01 n1 c39 c39 c40 c41 c42
isor 0.01 c41 c42
FREE Ce1  H102
;

_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)+(0.0592P)²+2.2866P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(15)
_refine_ls_number_reflns         9994
_refine_ls_number_parameters     597
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.27338(18) 0.7777(2) 0.9194(2) 0.0520(9) Uani 1 1 d . . .
C2 C 0.2110(2) 0.7940(3) 0.9516(3) 0.0687(12) Uani 1 1 d . . .
H2 H 0.2054 0.8371 0.9859 0.082 Uiso 1 1 calc R . .
C3 C 0.1576(2) 0.7459(3) 0.9325(4) 0.0938(18) Uani 1 1 d . . .
H3 H 0.1161 0.7558 0.9545 0.113 Uiso 1 1 calc R . .
C4 C 0.1669(3) 0.6829(4) 0.8801(5) 0.101(2) Uani 1 1 d . . .
H4 H 0.1310 0.6510 0.8662 0.121 Uiso 1 1 calc R . .
C5 C 0.2271(3) 0.6673(3) 0.8490(4) 0.0883(17) Uani 1 1 d . . .
H5 H 0.2325 0.6242 0.8147 0.106 Uiso 1 1 calc R . .
C6 C 0.2809(2) 0.7149(3) 0.8678(3) 0.0685(12) Uani 1 1 d . . .
H6 H 0.3221 0.7044 0.8455 0.082 Uiso 1 1 calc R . .
C7 C 0.32787(17) 0.8327(2) 0.9395(2) 0.0466(8) Uani 1 1 d . . .
C8 C 0.44131(16) 0.86376(19) 0.92430(19) 0.0380(7) Uani 1 1 d . . .
H8 H 0.4271 0.9192 0.9172 0.046 Uiso 1 1 calc R . .
C9 C 0.46638(17) 0.8533(2) 1.0101(2) 0.0387(7) Uani 1 1 d . . .
C10 C 0.60131(19) 0.6678(2) 0.8662(2) 0.0477(8) Uani 1 1 d . . .
C11 C 0.5725(2) 0.6223(2) 0.9271(3) 0.0608(10) Uani 1 1 d . . .
H11 H 0.5365 0.6420 0.9556 0.073 Uiso 1 1 calc R . .
C12 C 0.5982(3) 0.5479(3) 0.9442(3) 0.0749(13) Uani 1 1 d . . .
H12 H 0.5789 0.5171 0.9841 0.090 Uiso 1 1 calc R . .
C13 C 0.6506(2) 0.5194(3) 0.9041(3) 0.0746(13) Uani 1 1 d . . .
H13 H 0.6670 0.4691 0.9165 0.090 Uiso 1 1 calc R . .
C14 C 0.6807(2) 0.5639(3) 0.8446(3) 0.0724(13) Uani 1 1 d . . .
H14 H 0.7174 0.5441 0.8175 0.087 Uiso 1 1 calc R . .
C15 C 0.6556(2) 0.6366(3) 0.8267(3) 0.0621(10) Uani 1 1 d . . .
H15 H 0.6754 0.6665 0.7866 0.075 Uiso 1 1 calc R . .
C16 C 0.57786(18) 0.7476(2) 0.8456(2) 0.0444(8) Uani 1 1 d . . .
C17 C 0.49526(18) 0.84568(19) 0.86437(17) 0.0372(7) Uani 1 1 d . . .
H17 H 0.5309 0.8847 0.8714 0.045 Uiso 1 1 calc R . .
C18 C 0.47069(17) 0.8508(2) 0.7784(2) 0.0367(7) Uani 1 1 d . . .
C19 C 0.2052(2) 0.8880(3) 0.3899(2) 0.0603(10) Uani 1 1 d . . .
C20 C 0.1797(3) 0.8108(3) 0.3877(3) 0.0771(14) Uani 1 1 d . . .
H20 H 0.2086 0.7680 0.3826 0.093 Uiso 1 1 calc R . .
C21 C 0.1134(3) 0.7964(4) 0.3929(4) 0.0953(18) Uani 1 1 d . . .
H21 H 0.0972 0.7445 0.3925 0.114 Uiso 1 1 calc R . .
C22 C 0.0731(3) 0.8566(5) 0.3984(4) 0.115(3) Uani 1 1 d . . .
H22 H 0.0278 0.8467 0.4000 0.138 Uiso 1 1 calc R . .
C23 C 0.0951(3) 0.9362(4) 0.4022(5) 0.117(3) Uani 1 1 d . . .
H23 H 0.0653 0.9781 0.4078 0.140 Uiso 1 1 calc R . .
C24 C 0.1635(2) 0.9503(3) 0.3972(4) 0.0833(15) Uani 1 1 d . . .
H24 H 0.1799 1.0021 0.3989 0.100 Uiso 1 1 calc R . .
C25 C 0.2775(2) 0.9000(3) 0.3837(2) 0.0549(10) Uani 1 1 d . . .
C26 C 0.36215(15) 0.9957(2) 0.37471(17) 0.0395(7) Uani 1 1 d . . .
H26 H 0.3918 0.9535 0.3937 0.047 Uiso 1 1 calc R . .
C27 C 0.36925(14) 1.0026(2) 0.28372(17) 0.0399(6) Uani 1 1 d . . .
C28 C 0.3005(2) 1.2672(2) 0.3846(2) 0.0511(9) Uani 1 1 d . . .
C29 C 0.2424(3) 1.2469(3) 0.3466(4) 0.0789(15) Uani 1 1 d . . .
H29 H 0.2356 1.1947 0.3297 0.095 Uiso 1 1 calc R . .
C30 C 0.1945(3) 1.3036(4) 0.3336(5) 0.104(2) Uani 1 1 d . . .
H30 H 0.1556 1.2894 0.3077 0.125 Uiso 1 1 calc R . .
C31 C 0.2030(3) 1.3790(4) 0.3576(4) 0.106(2) Uani 1 1 d . . .
H31 H 0.1706 1.4168 0.3469 0.127 Uiso 1 1 calc R . .
C32 C 0.2593(3) 1.4009(3) 0.3980(4) 0.0917(17) Uani 1 1 d . . .
H32 H 0.2640 1.4525 0.4175 0.110 Uiso 1 1 calc R . .
C33 C 0.3092(3) 1.3450(2) 0.4092(3) 0.0674(12) Uani 1 1 d . . .
H33 H 0.3487 1.3602 0.4334 0.081 Uiso 1 1 calc R . .
C34 C 0.35424(19) 1.2085(2) 0.4008(2) 0.0501(9) Uani 1 1 d . . .
C35 C 0.37957(16) 1.0728(2) 0.41717(18) 0.0382(7) Uani 1 1 d . . .
H35 H 0.4242 1.0888 0.4006 0.046 Uiso 1 1 calc R . .
C36 C 0.37946(17) 1.0629(2) 0.50766(19) 0.0407(7) Uani 1 1 d . . .
C37 C 0.4527(3) 0.8268(3) 0.5220(3) 0.0696(13) Uani 1 1 d . . .
H37A H 0.4076 0.8426 0.5123 0.104 Uiso 1 1 d R . .
H37B H 0.4554 0.7695 0.5236 0.104 Uiso 1 1 d R . .
H37C H 0.4805 0.8467 0.4801 0.104 Uiso 1 1 d R . .
C38 C 0.4757(4) 0.8208(4) 0.2656(4) 0.112(3) Uani 1 1 d . . .
H38A H 0.4451 0.8497 0.2987 0.168 Uiso 1 1 d R . .
H38B H 0.5187 0.8207 0.2900 0.168 Uiso 1 1 d R . .
H38C H 0.4606 0.7667 0.2594 0.168 Uiso 1 1 d R . .
C39 C 0.7585(6) 0.9140(6) 0.9178(6) 0.180(5) Uani 1 1 d D . .
C40 C 0.6856(6) 0.9256(8) 0.9060(10) 0.222(7) Uani 1 1 d D . .
C41 C 0.7854(8) 0.9719(9) 0.7772(9) 0.217(5) Uani 1 1 d DU . .
C42 C 0.8150(8) 1.0484(8) 0.8112(9) 0.213(5) Uani 1 1 d DU . .
C43 C 0.7801(6) 0.8214(8) 0.7983(8) 0.191(5) Uani 1 1 d . . .
C44 C 0.8097(5) 0.7527(8) 0.8322(8) 0.187(5) Uani 1 1 d . . .
Ce1 Ce 0.5000 1.0000 0.642540(12) 0.03362(8) Uani 1 2 d S . .
Ce2 Ce 0.5000 1.0000 0.147428(12) 0.03345(8) Uani 1 2 d S . .
N1 N 0.7963(4) 0.9006(5) 0.8397(6) 0.163(3) Uani 1 1 d D . .
O1 O 0.38628(11) 0.81201(13) 0.90576(14) 0.0430(5) Uani 1 1 d . . .
O2 O 0.32198(13) 0.89105(17) 0.98136(18) 0.0625(7) Uani 1 1 d . . .
O3 O 0.44853(15) 0.79503(15) 1.04926(15) 0.0549(7) Uani 1 1 d . . .
O4 O 0.50499(12) 0.90811(14) 1.03289(12) 0.0451(5) Uani 1 1 d . . .
O5 O 0.60592(13) 0.79239(17) 0.80043(16) 0.0582(7) Uani 1 1 d . . .
O6 O 0.52098(10) 0.76777(13) 0.88241(13) 0.0404(5) Uani 1 1 d . . .
O7 O 0.46417(14) 0.78903(15) 0.73915(15) 0.0517(6) Uani 1 1 d . . .
O8 O 0.45944(13) 0.92029(14) 0.75494(14) 0.0471(6) Uani 1 1 d . . .
O9 O 0.29504(12) 0.97523(14) 0.39603(14) 0.0453(5) Uani 1 1 d . . .
O10 O 0.31638(18) 0.8472(2) 0.3710(3) 0.0843(11) Uani 1 1 d . . .
O11 O 0.32117(12) 0.9888(2) 0.24122(14) 0.0610(7) Uani 1 1 d . . .
O12 O 0.42632(11) 1.02130(16) 0.26086(13) 0.0496(6) Uani 1 1 d . . .
O13 O 0.33368(12) 1.13318(14) 0.39159(15) 0.0443(5) Uani 1 1 d . . .
O14 O 0.40898(14) 1.22649(17) 0.4208(2) 0.0689(8) Uani 1 1 d . . .
O15 O 0.33995(13) 1.10116(18) 0.54881(15) 0.0599(7) Uani 1 1 d . . .
O16 O 0.42285(12) 1.01464(15) 0.53341(13) 0.0503(6) Uani 1 1 d . . .
O17 O 0.39776(12) 1.07650(16) 0.69088(14) 0.0511(6) Uani 1 1 d . . .
H101 H 0.3730 1.0975 0.7263 0.077 Uiso 1 1 d R . .
H102 H 0.4207 1.1139 0.6700 0.077 Uiso 1 1 d R . .
O18 O 0.47435(15) 0.86040(15) 0.59573(15) 0.0569(7) Uani 1 1 d . . .
H104 H 0.4603 0.8269 0.6302 0.085 Uiso 1 1 d R . .
O19 O 0.38154(12) 0.98260(15) 0.10296(14) 0.0490(6) Uani 1 1 d . . .
H105 H 0.3600 1.0255 0.0934 0.074 Uiso 1 1 d R . .
H106 H 0.3951 0.9641 0.0584 0.074 Uiso 1 1 d R . .
O20 O 0.48198(16) 0.85839(16) 0.19270(14) 0.0657(9) Uani 1 1 d D . .
H108 H 0.4976 0.8363 0.1508 0.099 Uiso 1 1 d RD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.370(6) . ?
C1 C2 1.397(6) . ?
C1 C7 1.475(5) . ?
C2 C3 1.384(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.349(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.210(4) . ?
C7 O1 1.353(4) . ?
C8 O1 1.444(4) . ?
C8 C17 1.513(5) . ?
C8 C9 1.536(5) . ?
C8 H8 0.9800 . ?
C9 O3 1.231(4) . ?
C9 O4 1.264(4) . ?
C10 C15 1.383(5) . ?
C10 C11 1.401(5) . ?
C10 C16 1.461(5) . ?
C11 C12 1.382(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.342(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.354(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.208(4) . ?
C16 O6 1.347(4) . ?
C17 O6 1.438(4) . ?
C17 C18 1.528(4) . ?
C17 H17 0.9800 . ?
C18 O7 1.235(4) . ?
C18 O8 1.250(4) . ?
C19 C24 1.347(7) . ?
C19 C20 1.392(6) . ?
C19 C25 1.480(6) . ?
C20 C21 1.364(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.300(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.408(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O10 1.202(5) . ?
C25 O9 1.325(5) . ?
C26 O9 1.443(4) . ?
C26 C35 1.516(5) . ?
C26 C27 1.538(4) . ?
C26 H26 0.9800 . ?
C27 O11 1.227(4) . ?
C27 O12 1.254(4) . ?
C28 C29 1.379(6) . ?
C28 C33 1.380(6) . ?
C28 C34 1.490(5) . ?
C29 C30 1.374(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.336(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.374(9) . ?
C31 H31 0.9300 . ?
C32 C33 1.388(7) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O14 1.194(5) . ?
C34 O13 1.338(4) . ?
C35 O13 1.439(4) . ?
C35 C36 1.527(5) . ?
C35 H35 0.9800 . ?
C36 O15 1.235(4) . ?
C36 O16 1.269(4) . ?
C37 O18 1.428(5) . ?
C37 H37A 0.9613 . ?
C37 H37B 0.9625 . ?
C37 H37C 0.9613 . ?
C38 O20 1.382(6) . ?
C38 H38A 0.9615 . ?
C38 H38B 0.9612 . ?
C38 H38C 0.9623 . ?
C39 C40 1.498(9) . ?
C39 N1 1.533(8) . ?
C41 C42 1.526(9) . ?
C41 N1 1.605(16) . ?
C43 C44 1.417(15) . ?
C43 N1 1.535(13) . ?
Ce1 O16 2.417(2) . ?
Ce1 O16 2.417(2) 2_675 ?
Ce1 O8 2.452(2) 2_675 ?
Ce1 O8 2.452(2) . ?
Ce1 O18 2.522(2) . ?
Ce1 O18 2.522(2) 2_675 ?
Ce1 O17 2.562(2) 2_675 ?
Ce1 O17 2.562(2) . ?
Ce1 H102 2.5351 . ?
Ce2 O12 2.442(2) 2_675 ?
Ce2 O12 2.442(2) . ?
Ce2 O4 2.465(2) 1_554 ?
Ce2 O4 2.465(2) 2_674 ?
Ce2 O20 2.519(3) 2_675 ?
Ce2 O20 2.519(3) . ?
Ce2 O19 2.523(2) . ?
Ce2 O19 2.523(2) 2_675 ?
O4 Ce2 2.465(2) 1_556 ?
O17 H101 0.8538 . ?
O17 H102 0.8552 . ?
O18 H104 0.8551 . ?
O19 H105 0.8558 . ?
O19 H106 0.8540 . ?
O20 H108 0.8550 . ?

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
C6 C1 C2 119.6(4) . . ?
C6 C1 C7 122.8(4) . . ?
C2 C1 C7 117.5(4) . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.0(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 121.0(4) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 120.4(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 120.0(4) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
O2 C7 O1 122.4(3) . . ?
O2 C7 C1 124.4(3) . . ?
O1 C7 C1 113.2(3) . . ?
O1 C8 C17 106.9(2) . . ?
O1 C8 C9 112.8(3) . . ?
C17 C8 C9 111.3(3) . . ?
O1 C8 H8 108.6 . . ?
C17 C8 H8 108.6 . . ?
C9 C8 H8 108.6 . . ?
O3 C9 O4 126.6(3) . . ?
O3 C9 C8 119.6(3) . . ?
O4 C9 C8 113.8(3) . . ?
C15 C10 C11 118.2(4) . . ?
C15 C10 C16 119.3(4) . . ?
C11 C10 C16 122.4(3) . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C13 C12 C11 120.8(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 121.1(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 118.6(4) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C10 122.1(4) . . ?
C14 C15 H15 119.0 . . ?
C10 C15 H15 119.0 . . ?
O5 C16 O6 122.1(3) . . ?
O5 C16 C10 124.4(3) . . ?
O6 C16 C10 113.5(3) . . ?
O6 C17 C8 107.6(2) . . ?
O6 C17 C18 111.6(3) . . ?
C8 C17 C18 112.5(3) . . ?
O6 C17 H17 108.4 . . ?
C8 C17 H17 108.4 . . ?
C18 C17 H17 108.4 . . ?
O7 C18 O8 126.5(3) . . ?
O7 C18 C17 119.4(3) . . ?
O8 C18 C17 114.1(3) . . ?
C24 C19 C20 119.5(4) . . ?
C24 C19 C25 121.1(4) . . ?
C20 C19 C25 119.4(5) . . ?
C21 C20 C19 121.7(6) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C22 C21 C20 118.8(6) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C21 C22 C23 122.8(6) . . ?
C21 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C24 C23 C22 117.9(6) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
C19 C24 C23 119.3(5) . . ?
C19 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
O10 C25 O9 123.7(4) . . ?
O10 C25 C19 123.8(4) . . ?
O9 C25 C19 112.5(4) . . ?
O9 C26 C35 107.7(3) . . ?
O9 C26 C27 110.6(2) . . ?
C35 C26 C27 112.4(3) . . ?
O9 C26 H26 108.7 . . ?
C35 C26 H26 108.7 . . ?
C27 C26 H26 108.7 . . ?
O11 C27 O12 126.6(3) . . ?
O11 C27 C26 119.3(3) . . ?
O12 C27 C26 114.1(3) . . ?
C29 C28 C33 118.7(4) . . ?
C29 C28 C34 122.8(4) . . ?
C33 C28 C34 118.6(4) . . ?
C30 C29 C28 120.1(5) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 121.1(6) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C32 120.5(5) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C33 119.1(5) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C28 C33 C32 120.4(5) . . ?
C28 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
O14 C34 O13 124.0(4) . . ?
O14 C34 C28 123.9(4) . . ?
O13 C34 C28 112.1(3) . . ?
O13 C35 C26 108.1(3) . . ?
O13 C35 C36 111.8(3) . . ?
C26 C35 C36 112.0(3) . . ?
O13 C35 H35 108.3 . . ?
C26 C35 H35 108.3 . . ?
C36 C35 H35 108.3 . . ?
O15 C36 O16 126.0(3) . . ?
O15 C36 C35 120.0(3) . . ?
O16 C36 C35 114.0(3) . . ?
O18 C37 H37A 109.2 . . ?
O18 C37 H37B 110.6 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 108.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.9 . . ?
O20 C38 H38B 107.1 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 111.3 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.4 . . ?
C40 C39 N1 113.4(9) . . ?
C42 C41 N1 109.1(11) . . ?
C44 C43 N1 115.6(9) . . ?
O16 Ce1 O16 81.49(11) . 2_675 ?
O16 Ce1 O8 137.96(8) . 2_675 ?
O16 Ce1 O8 115.00(9) 2_675 2_675 ?
O16 Ce1 O8 115.00(9) . . ?
O16 Ce1 O8 137.96(8) 2_675 . ?
O8 Ce1 O8 79.46(12) 2_675 . ?
O16 Ce1 O18 74.09(9) . . ?
O16 Ce1 O18 78.60(9) 2_675 . ?
O8 Ce1 O18 144.46(8) 2_675 . ?
O8 Ce1 O18 70.44(8) . . ?
O16 Ce1 O18 78.60(9) . 2_675 ?
O16 Ce1 O18 74.09(9) 2_675 2_675 ?
O8 Ce1 O18 70.44(8) 2_675 2_675 ?
O8 Ce1 O18 144.46(8) . 2_675 ?
O18 Ce1 O18 143.72(11) . 2_675 ?
O16 Ce1 O17 144.11(8) . 2_675 ?
O16 Ce1 O17 70.70(8) 2_675 2_675 ?
O8 Ce1 O17 76.13(8) 2_675 2_675 ?
O8 Ce1 O17 75.70(8) . 2_675 ?
O18 Ce1 O17 78.44(9) . 2_675 ?
O18 Ce1 O17 113.42(9) 2_675 2_675 ?
O16 Ce1 O17 70.70(8) . . ?
O16 Ce1 O17 144.11(8) 2_675 . ?
O8 Ce1 O17 75.70(8) 2_675 . ?
O8 Ce1 O17 76.13(8) . . ?
O18 Ce1 O17 113.42(9) . . ?
O18 Ce1 O17 78.44(9) 2_675 . ?
O17 Ce1 O17 143.10(11) 2_675 . ?
O16 Ce1 H102 69.7 . . ?
O16 Ce1 H102 128.4 2_675 . ?
O8 Ce1 H102 70.2 2_675 . ?
O8 Ce1 H102 93.4 . . ?
O18 Ce1 H102 128.8 . . ?
O18 Ce1 H102 59.1 2_675 . ?
O17 Ce1 H102 146.0 2_675 . ?
O17 Ce1 H102 19.3 . . ?
O12 Ce2 O12 77.60(11) 2_675 . ?
O12 Ce2 O4 119.42(9) 2_675 1_554 ?
O12 Ce2 O4 136.37(8) . 1_554 ?
O12 Ce2 O4 136.37(8) 2_675 2_674 ?
O12 Ce2 O4 119.42(9) . 2_674 ?
O4 Ce2 O4 77.55(11) 1_554 2_674 ?
O12 Ce2 O20 79.33(9) 2_675 2_675 ?
O12 Ce2 O20 73.45(8) . 2_675 ?
O4 Ce2 O20 144.90(8) 1_554 2_675 ?
O4 Ce2 O20 69.63(8) 2_674 2_675 ?
O12 Ce2 O20 73.45(8) 2_675 . ?
O12 Ce2 O20 79.33(9) . . ?
O4 Ce2 O20 69.63(8) 1_554 . ?
O4 Ce2 O20 144.90(8) 2_674 . ?
O20 Ce2 O20 144.90(11) 2_675 . ?
O12 Ce2 O19 142.31(8) 2_675 . ?
O12 Ce2 O19 70.71(8) . . ?
O4 Ce2 O19 74.69(8) 1_554 . ?
O4 Ce2 O19 78.63(8) 2_674 . ?
O20 Ce2 O19 109.58(10) 2_675 . ?
O20 Ce2 O19 80.98(9) . . ?
O12 Ce2 O19 70.71(8) 2_675 2_675 ?
O12 Ce2 O19 142.31(8) . 2_675 ?
O4 Ce2 O19 78.63(8) 1_554 2_675 ?
O4 Ce2 O19 74.69(8) 2_674 2_675 ?
O20 Ce2 O19 80.98(9) 2_675 2_675 ?
O20 Ce2 O19 109.58(10) . 2_675 ?
O19 Ce2 O19 145.60(11) . 2_675 ?
C39 N1 C43 114.0(10) . . ?
C39 N1 C41 112.4(8) . . ?
C43 N1 C41 108.6(9) . . ?
C7 O1 C8 115.3(2) . . ?
C9 O4 Ce2 131.7(2) . 1_556 ?
C16 O6 C17 116.1(3) . . ?
C18 O8 Ce1 133.6(2) . . ?
C25 O9 C26 116.0(3) . . ?
C27 O12 Ce2 139.6(2) . . ?
C34 O13 C35 115.5(3) . . ?
C36 O16 Ce1 140.2(2) . . ?
Ce1 O17 H101 154.2 . . ?
Ce1 O17 H102 78.5 . . ?
H101 O17 H102 107.5 . . ?
C37 O18 Ce1 134.4(3) . . ?
C37 O18 H104 103.0 . . ?
Ce1 O18 H104 117.9 . . ?
Ce2 O19 H105 116.1 . . ?
Ce2 O19 H106 89.8 . . ?
H105 O19 H106 107.8 . . ?
C38 O20 Ce2 135.3(3) . . ?
C38 O20 H108 124.3 . . ?
Ce2 O20 H108 96.2 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.076
# 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 0.000 0.281 631.1 35.1
2 0.500 0.500 0.426 631.2 34.6
_platon_squeeze_details          
; ?
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 859165'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 Nd O20, C6 N'
_chemical_formula_sum            'C44 H36 N Nd O20'
_chemical_formula_weight         1042.98

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           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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'

_cell_length_a                   20.169(4)
_cell_length_b                   16.722(3)
_cell_length_c                   16.759(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5652.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    43250
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2108
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55249
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         27.47
_reflns_number_total             12928
_reflns_number_gt                11030
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_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.
dfix 1.5 0.01 n1 c39 c39 c40 c41 c42
isor 0.01 c41 c42
;

_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)+(0.0777P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(14)
_refine_ls_number_reflns         12928
_refine_ls_number_parameters     597
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1181
_refine_ls_wR_factor_gt          0.1152
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.27324(17) 0.7788(2) 0.9193(2) 0.0520(9) Uani 1 1 d . . .
C2 C 0.2115(2) 0.7947(3) 0.9521(3) 0.0678(11) Uani 1 1 d . . .
H2 H 0.2060 0.8372 0.9873 0.081 Uiso 1 1 calc R . .
C3 C 0.1574(2) 0.7461(4) 0.9318(4) 0.0967(19) Uani 1 1 d . . .
H3 H 0.1157 0.7563 0.9532 0.116 Uiso 1 1 calc R . .
C4 C 0.1666(3) 0.6830(4) 0.8798(4) 0.0986(19) Uani 1 1 d . . .
H4 H 0.1308 0.6509 0.8656 0.118 Uiso 1 1 calc R . .
C5 C 0.2272(3) 0.6677(3) 0.8496(4) 0.0877(17) Uani 1 1 d . . .
H5 H 0.2330 0.6240 0.8160 0.105 Uiso 1 1 calc R . .
C6 C 0.2808(2) 0.7156(3) 0.8675(3) 0.0669(12) Uani 1 1 d . . .
H6 H 0.3219 0.7053 0.8446 0.080 Uiso 1 1 calc R . .
C7 C 0.32822(16) 0.8334(2) 0.9395(2) 0.0472(8) Uani 1 1 d . . .
C8 C 0.44177(14) 0.86509(19) 0.92429(19) 0.0377(6) Uani 1 1 d . . .
H8 H 0.4275 0.9206 0.9171 0.045 Uiso 1 1 calc R . .
C9 C 0.46712(17) 0.8544(2) 1.0101(2) 0.0389(7) Uani 1 1 d . . .
C10 C 0.60166(17) 0.6681(2) 0.8664(2) 0.0468(8) Uani 1 1 d . . .
C11 C 0.5721(2) 0.6231(2) 0.9262(3) 0.0616(10) Uani 1 1 d . . .
H11 H 0.5358 0.6428 0.9543 0.074 Uiso 1 1 calc R . .
C12 C 0.5985(3) 0.5460(3) 0.9436(3) 0.0778(13) Uani 1 1 d . . .
H12 H 0.5793 0.5150 0.9834 0.093 Uiso 1 1 calc R . .
C13 C 0.6503(2) 0.5179(3) 0.9035(3) 0.0752(13) Uani 1 1 d . . .
H13 H 0.6666 0.4673 0.9155 0.090 Uiso 1 1 calc R . .
C14 C 0.6809(2) 0.5633(3) 0.8436(3) 0.0754(13) Uani 1 1 d . . .
H14 H 0.7177 0.5436 0.8165 0.090 Uiso 1 1 calc R . .
C15 C 0.6559(2) 0.6361(3) 0.8258(3) 0.0627(10) Uani 1 1 d . . .
H15 H 0.6755 0.6658 0.7852 0.075 Uiso 1 1 calc R . .
C16 C 0.57857(17) 0.7478(2) 0.8451(2) 0.0432(7) Uani 1 1 d . . .
C17 C 0.49630(17) 0.84667(18) 0.86412(16) 0.0363(6) Uani 1 1 d . . .
H17 H 0.5321 0.8857 0.8708 0.044 Uiso 1 1 calc R . .
C18 C 0.47050(16) 0.8517(2) 0.7780(2) 0.0373(7) Uani 1 1 d . . .
C19 C 0.2060(2) 0.8882(3) 0.3897(2) 0.0594(10) Uani 1 1 d . . .
C20 C 0.1788(3) 0.8100(3) 0.3876(3) 0.0753(13) Uani 1 1 d . . .
H20 H 0.2075 0.7668 0.3820 0.090 Uiso 1 1 calc R . .
C21 C 0.1130(3) 0.7954(4) 0.3935(4) 0.0921(17) Uani 1 1 d . . .
H21 H 0.0965 0.7435 0.3934 0.111 Uiso 1 1 calc R . .
C22 C 0.0731(3) 0.8579(5) 0.3994(4) 0.119(3) Uani 1 1 d . . .
H22 H 0.0276 0.8488 0.4017 0.142 Uiso 1 1 calc R . .
C23 C 0.0958(3) 0.9369(4) 0.4024(5) 0.110(2) Uani 1 1 d . . .
H23 H 0.0662 0.9792 0.4082 0.132 Uiso 1 1 calc R . .
C24 C 0.1644(2) 0.9506(3) 0.3966(4) 0.0818(15) Uani 1 1 d . . .
H24 H 0.1808 1.0026 0.3976 0.098 Uiso 1 1 calc R . .
C25 C 0.2782(2) 0.8991(2) 0.3842(2) 0.0547(9) Uani 1 1 d . . .
C26 C 0.36346(15) 0.9950(2) 0.37477(17) 0.0400(6) Uani 1 1 d . . .
H26 H 0.3930 0.9526 0.3938 0.048 Uiso 1 1 calc R . .
C27 C 0.37009(14) 1.0015(2) 0.28331(16) 0.0398(6) Uani 1 1 d . . .
C28 C 0.30123(18) 1.2673(2) 0.3841(2) 0.0511(8) Uani 1 1 d . . .
C29 C 0.2435(3) 1.2468(3) 0.3474(4) 0.0823(16) Uani 1 1 d . . .
H29 H 0.2372 1.1943 0.3308 0.099 Uiso 1 1 calc R . .
C30 C 0.1937(3) 1.3028(4) 0.3344(5) 0.108(2) Uani 1 1 d . . .
H30 H 0.1544 1.2879 0.3095 0.129 Uiso 1 1 calc R . .
C31 C 0.2034(3) 1.3810(5) 0.3590(4) 0.112(2) Uani 1 1 d . . .
H31 H 0.1713 1.4194 0.3484 0.134 Uiso 1 1 calc R . .
C32 C 0.2596(3) 1.4020(3) 0.3984(4) 0.0918(16) Uani 1 1 d . . .
H32 H 0.2645 1.4536 0.4182 0.110 Uiso 1 1 calc R . .
C33 C 0.3099(2) 1.3461(2) 0.4089(3) 0.0678(11) Uani 1 1 d . . .
H33 H 0.3495 1.3614 0.4327 0.081 Uiso 1 1 calc R . .
C34 C 0.35494(19) 1.2096(2) 0.4006(2) 0.0499(8) Uani 1 1 d . . .
C35 C 0.38095(16) 1.07248(19) 0.41741(18) 0.0398(7) Uani 1 1 d . . .
H35 H 0.4256 1.0887 0.4008 0.048 Uiso 1 1 calc R . .
C36 C 0.38060(16) 1.06309(19) 0.50727(18) 0.0393(7) Uani 1 1 d . . .
C37 C 0.4530(3) 0.8272(3) 0.5226(3) 0.0689(12) Uani 1 1 d . . .
H37A H 0.4080 0.8430 0.5129 0.103 Uiso 1 1 d R . .
H37B H 0.4557 0.7699 0.5242 0.103 Uiso 1 1 d R . .
H37C H 0.4809 0.8471 0.4807 0.103 Uiso 1 1 d R . .
C38 C 0.4784(4) 0.8218(4) 0.2647(4) 0.115(3) Uani 1 1 d . . .
H38A H 0.4478 0.8507 0.2978 0.172 Uiso 1 1 d R . .
H38B H 0.5214 0.8218 0.2892 0.172 Uiso 1 1 d R . .
H38C H 0.4633 0.7677 0.2585 0.172 Uiso 1 1 d R . .
C39 C 0.7565(7) 0.9147(6) 0.9184(6) 0.210(7) Uani 1 1 d D . .
C40 C 0.6852(6) 0.9309(11) 0.8995(11) 0.269(10) Uani 1 1 d D . .
C41 C 0.7885(9) 0.9732(10) 0.7762(11) 0.268(7) Uani 1 1 d DU . .
C42 C 0.8208(7) 1.0489(8) 0.8096(9) 0.199(5) Uani 1 1 d DU . .
C43 C 0.7789(7) 0.8177(9) 0.8036(9) 0.221(7) Uani 1 1 d . . .
C44 C 0.8110(6) 0.7501(10) 0.8314(10) 0.228(7) Uani 1 1 d . . .
Nd1 Nd 0.5000 1.0000 0.642503(11) 0.03303(7) Uani 1 2 d S . .
Nd2 Nd 0.5000 1.0000 0.147502(11) 0.03255(7) Uani 1 2 d S . .
N1 N 0.7949(4) 0.8975(6) 0.8413(6) 0.170(4) Uani 1 1 d D . .
O1 O 0.38671(11) 0.81261(13) 0.90587(14) 0.0422(5) Uani 1 1 d . . .
O2 O 0.32249(12) 0.89219(17) 0.98167(18) 0.0627(7) Uani 1 1 d . . .
O3 O 0.44926(14) 0.79588(15) 1.04936(15) 0.0542(6) Uani 1 1 d . . .
O4 O 0.50544(12) 0.90910(14) 1.03353(12) 0.0458(5) Uani 1 1 d . . .
O5 O 0.60620(13) 0.79314(16) 0.79995(16) 0.0583(7) Uani 1 1 d . . .
O6 O 0.52140(10) 0.76848(13) 0.88241(13) 0.0402(5) Uani 1 1 d . . .
O7 O 0.46418(13) 0.78976(14) 0.73935(15) 0.0501(6) Uani 1 1 d . . .
O8 O 0.45978(12) 0.92163(14) 0.75440(14) 0.0455(5) Uani 1 1 d . . .
O9 O 0.29590(11) 0.97468(13) 0.39620(13) 0.0433(5) Uani 1 1 d . . .
O10 O 0.31720(18) 0.84602(19) 0.3725(3) 0.0842(11) Uani 1 1 d . . .
O11 O 0.32227(11) 0.98710(19) 0.24107(14) 0.0597(7) Uani 1 1 d . . .
O12 O 0.42782(11) 1.01999(15) 0.26045(13) 0.0496(6) Uani 1 1 d . . .
O13 O 0.33477(11) 1.13296(14) 0.39162(15) 0.0443(5) Uani 1 1 d . . .
O14 O 0.41040(13) 1.22734(16) 0.4196(2) 0.0671(8) Uani 1 1 d . . .
O15 O 0.34083(12) 1.10130(17) 0.54889(15) 0.0586(7) Uani 1 1 d . . .
O16 O 0.42446(11) 1.01508(14) 0.53342(13) 0.0491(6) Uani 1 1 d . . .
O17 O 0.39975(12) 1.07587(15) 0.69005(14) 0.0505(6) Uani 1 1 d . . .
H107 H 0.3695 1.0606 0.7218 0.061 Uiso 1 1 d R . .
H331 H 0.3809 1.0964 0.6494 0.061 Uiso 1 1 d R . .
O18 O 0.47453(14) 0.86191(14) 0.59651(14) 0.0548(6) Uani 1 1 d . . .
H104 H 0.4605 0.8284 0.6310 0.082 Uiso 1 1 d R . .
O19 O 0.38327(11) 0.98387(14) 0.10283(13) 0.0472(5) Uani 1 1 d . . .
H201 H 0.3562 0.9956 0.1395 0.057 Uiso 1 1 d R . .
H202 H 0.3642 0.9510 0.0714 0.057 Uiso 1 1 d R . .
O20 O 0.48267(15) 0.85971(15) 0.19196(14) 0.0621(8) Uani 1 1 d D . .
H108 H 0.4983 0.8376 0.1501 0.093 Uiso 1 1 d RD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.376(5) . ?
C1 C2 1.387(5) . ?
C1 C7 1.476(5) . ?
C2 C3 1.402(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.348(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.216(4) . ?
C7 O1 1.353(4) . ?
C8 O1 1.449(4) . ?
C8 C17 1.523(4) . ?
C8 C9 1.537(5) . ?
C8 H8 0.9800 . ?
C9 O3 1.233(4) . ?
C9 O4 1.260(4) . ?
C10 C11 1.388(5) . ?
C10 C15 1.396(5) . ?
C10 C16 1.456(5) . ?
C11 C12 1.426(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.327(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.402(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.350(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.207(4) . ?
C16 O6 1.357(4) . ?
C17 O6 1.435(4) . ?
C17 C18 1.537(4) . ?
C17 H17 0.9800 . ?
C18 O7 1.227(4) . ?
C18 O8 1.254(4) . ?
C19 C24 1.344(7) . ?
C19 C20 1.419(6) . ?
C19 C25 1.471(6) . ?
C20 C21 1.353(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.324(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.399(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.406(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O10 1.201(5) . ?
C25 O9 1.329(4) . ?
C26 O9 1.450(4) . ?
C26 C35 1.521(5) . ?
C26 C27 1.542(4) . ?
C26 H26 0.9800 . ?
C27 O11 1.220(4) . ?
C27 O12 1.264(4) . ?
C28 C29 1.361(6) . ?
C28 C33 1.393(6) . ?
C28 C34 1.477(5) . ?
C29 C30 1.390(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.385(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.359(9) . ?
C31 H31 0.9300 . ?
C32 C33 1.390(7) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O14 1.200(4) . ?
C34 O13 1.353(4) . ?
C35 O13 1.441(4) . ?
C35 C36 1.514(4) . ?
C35 H35 0.9800 . ?
C36 O15 1.240(4) . ?
C36 O16 1.272(4) . ?
C37 O18 1.434(5) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.377(7) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.499(9) . ?
C39 N1 1.533(9) . ?
C41 C42 1.528(9) . ?
C41 N1 1.676(19) . ?
C43 C44 1.385(18) . ?
C43 N1 1.512(14) . ?
Nd1 O16 2.393(2) 2_675 ?
Nd1 O16 2.393(2) . ?
Nd1 O8 2.427(2) 2_675 ?
Nd1 O8 2.427(2) . ?
Nd1 O18 2.488(2) . ?
Nd1 O18 2.488(2) 2_675 ?
Nd1 O17 2.516(2) 2_675 ?
Nd1 O17 2.516(2) . ?
Nd2 O12 2.411(2) 2_675 ?
Nd2 O12 2.411(2) . ?
Nd2 O4 2.444(2) 1_554 ?
Nd2 O4 2.444(2) 2_674 ?
Nd2 O19 2.485(2) . ?
Nd2 O19 2.485(2) 2_675 ?
Nd2 O20 2.486(2) 2_675 ?
Nd2 O20 2.486(2) . ?
O4 Nd2 2.444(2) 1_556 ?
O17 H107 0.8494 . ?
O17 H331 0.8525 . ?
O18 H104 0.8536 . ?
O19 H201 0.8452 . ?
O19 H202 0.8530 . ?
O20 H108 0.8538 . ?

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
C6 C1 C2 119.8(4) . . ?
C6 C1 C7 122.5(3) . . ?
C2 C1 C7 117.7(3) . . ?
C1 C2 C3 119.4(4) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.3(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 119.8(4) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
O2 C7 O1 122.2(3) . . ?
O2 C7 C1 124.2(3) . . ?
O1 C7 C1 113.6(3) . . ?
O1 C8 C17 106.8(2) . . ?
O1 C8 C9 112.6(3) . . ?
C17 C8 C9 110.8(2) . . ?
O1 C8 H8 108.8 . . ?
C17 C8 H8 108.8 . . ?
C9 C8 H8 108.8 . . ?
O3 C9 O4 126.1(3) . . ?
O3 C9 C8 119.6(3) . . ?
O4 C9 C8 114.3(3) . . ?
C11 C10 C15 118.7(3) . . ?
C11 C10 C16 122.4(3) . . ?
C15 C10 C16 118.8(3) . . ?
C10 C11 C12 118.5(4) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
C13 C12 C11 120.8(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 121.2(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 118.8(4) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C10 122.1(4) . . ?
C14 C15 H15 119.0 . . ?
C10 C15 H15 119.0 . . ?
O5 C16 O6 121.4(3) . . ?
O5 C16 C10 125.5(3) . . ?
O6 C16 C10 113.1(3) . . ?
O6 C17 C8 107.3(2) . . ?
O6 C17 C18 111.7(2) . . ?
C8 C17 C18 111.5(3) . . ?
O6 C17 H17 108.8 . . ?
C8 C17 H17 108.8 . . ?
C18 C17 H17 108.8 . . ?
O7 C18 O8 127.1(3) . . ?
O7 C18 C17 119.0(3) . . ?
O8 C18 C17 113.9(3) . . ?
C24 C19 C20 118.5(4) . . ?
C24 C19 C25 121.9(4) . . ?
C20 C19 C25 119.6(4) . . ?
C21 C20 C19 122.9(6) . . ?
C21 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
C22 C21 C20 117.4(5) . . ?
C22 C21 H21 121.3 . . ?
C20 C21 H21 121.3 . . ?
C21 C22 C23 123.3(5) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C22 C23 C24 118.3(6) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 H23 120.8 . . ?
C19 C24 C23 119.6(5) . . ?
C19 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
O10 C25 O9 123.5(4) . . ?
O10 C25 C19 124.6(4) . . ?
O9 C25 C19 111.9(4) . . ?
O9 C26 C35 107.6(3) . . ?
O9 C26 C27 110.1(2) . . ?
C35 C26 C27 112.8(3) . . ?
O9 C26 H26 108.8 . . ?
C35 C26 H26 108.8 . . ?
C27 C26 H26 108.8 . . ?
O11 C27 O12 126.9(3) . . ?
O11 C27 C26 119.6(3) . . ?
O12 C27 C26 113.5(2) . . ?
C29 C28 C33 118.7(4) . . ?
C29 C28 C34 123.2(4) . . ?
C33 C28 C34 118.1(3) . . ?
C28 C29 C30 121.3(5) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C31 C30 C29 119.1(5) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C32 C31 C30 120.5(5) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C33 119.7(5) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C28 120.5(4) . . ?
C32 C33 H33 119.8 . . ?
C28 C33 H33 119.8 . . ?
O14 C34 O13 123.0(3) . . ?
O14 C34 C28 124.9(4) . . ?
O13 C34 C28 112.2(3) . . ?
O13 C35 C36 111.6(3) . . ?
O13 C35 C26 107.9(2) . . ?
C36 C35 C26 112.2(3) . . ?
O13 C35 H35 108.4 . . ?
C36 C35 H35 108.4 . . ?
C26 C35 H35 108.4 . . ?
O15 C36 O16 125.5(3) . . ?
O15 C36 C35 120.6(3) . . ?
O16 C36 C35 113.9(3) . . ?
O18 C37 H37A 108.8 . . ?
O18 C37 H37B 111.2 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 108.4 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 108.7 . . ?
O20 C38 H38B 108.7 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 111.0 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N1 109.9(9) . . ?
C42 C41 N1 110.7(13) . . ?
C44 C43 N1 118.7(11) . . ?
O16 Nd1 O16 80.38(11) 2_675 . ?
O16 Nd1 O8 115.74(8) 2_675 2_675 ?
O16 Nd1 O8 138.25(8) . 2_675 ?
O16 Nd1 O8 138.25(8) 2_675 . ?
O16 Nd1 O8 115.74(8) . . ?
O8 Nd1 O8 78.83(12) 2_675 . ?
O16 Nd1 O18 78.29(9) 2_675 . ?
O16 Nd1 O18 74.31(8) . . ?
O8 Nd1 O18 144.04(8) 2_675 . ?
O8 Nd1 O18 70.69(8) . . ?
O16 Nd1 O18 74.31(8) 2_675 2_675 ?
O16 Nd1 O18 78.29(9) . 2_675 ?
O8 Nd1 O18 70.69(8) 2_675 2_675 ?
O8 Nd1 O18 144.04(8) . 2_675 ?
O18 Nd1 O18 143.90(11) . 2_675 ?
O16 Nd1 O17 71.17(8) 2_675 2_675 ?
O16 Nd1 O17 143.76(8) . 2_675 ?
O8 Nd1 O17 76.06(8) 2_675 2_675 ?
O8 Nd1 O17 75.62(8) . 2_675 ?
O18 Nd1 O17 78.24(9) . 2_675 ?
O18 Nd1 O17 113.58(9) 2_675 2_675 ?
O16 Nd1 O17 143.76(8) 2_675 . ?
O16 Nd1 O17 71.17(8) . . ?
O8 Nd1 O17 75.62(8) 2_675 . ?
O8 Nd1 O17 76.06(8) . . ?
O18 Nd1 O17 113.58(9) . . ?
O18 Nd1 O17 78.24(9) 2_675 . ?
O17 Nd1 O17 143.07(11) 2_675 . ?
O12 Nd2 O12 76.55(11) 2_675 . ?
O12 Nd2 O4 120.02(9) 2_675 1_554 ?
O12 Nd2 O4 136.64(8) . 1_554 ?
O12 Nd2 O4 136.64(8) 2_675 2_674 ?
O12 Nd2 O4 120.02(8) . 2_674 ?
O4 Nd2 O4 77.17(11) 1_554 2_674 ?
O12 Nd2 O19 142.50(7) 2_675 . ?
O12 Nd2 O19 71.31(7) . . ?
O4 Nd2 O19 74.90(8) 1_554 . ?
O4 Nd2 O19 77.85(8) 2_674 . ?
O12 Nd2 O19 71.31(7) 2_675 2_675 ?
O12 Nd2 O19 142.50(7) . 2_675 ?
O4 Nd2 O19 77.85(8) 1_554 2_675 ?
O4 Nd2 O19 74.90(8) 2_674 2_675 ?
O19 Nd2 O19 144.94(10) . 2_675 ?
O12 Nd2 O20 79.09(9) 2_675 2_675 ?
O12 Nd2 O20 73.67(8) . 2_675 ?
O4 Nd2 O20 144.58(8) 1_554 2_675 ?
O4 Nd2 O20 69.74(8) 2_674 2_675 ?
O19 Nd2 O20 109.02(9) . 2_675 ?
O19 Nd2 O20 81.64(9) 2_675 2_675 ?
O12 Nd2 O20 73.67(8) 2_675 . ?
O12 Nd2 O20 79.09(9) . . ?
O4 Nd2 O20 69.74(8) 1_554 . ?
O4 Nd2 O20 144.58(8) 2_674 . ?
O19 Nd2 O20 81.64(9) . . ?
O19 Nd2 O20 109.02(9) 2_675 . ?
O20 Nd2 O20 145.12(11) 2_675 . ?
C43 N1 C39 114.2(10) . . ?
C43 N1 C41 112.2(10) . . ?
C39 N1 C41 111.6(9) . . ?
C7 O1 C8 115.1(2) . . ?
C9 O4 Nd2 131.9(2) . 1_556 ?
C16 O6 C17 115.7(2) . . ?
C18 O8 Nd1 133.6(2) . . ?
C25 O9 C26 116.0(3) . . ?
C27 O12 Nd2 139.5(2) . . ?
C34 O13 C35 115.9(3) . . ?
C36 O16 Nd1 140.5(2) . . ?
Nd1 O17 H107 128.6 . . ?
Nd1 O17 H331 108.0 . . ?
H107 O17 H331 107.5 . . ?
C37 O18 Nd1 134.8(3) . . ?
C37 O18 H104 102.6 . . ?
Nd1 O18 H104 117.9 . . ?
Nd2 O19 H201 111.6 . . ?
Nd2 O19 H202 133.1 . . ?
H201 O19 H202 107.9 . . ?
C38 O20 Nd2 135.1(3) . . ?
C38 O20 H108 123.5 . . ?
Nd2 O20 H108 96.3 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.093
# 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 0.000 0.280 622.6 30.8
2 0.500 0.500 0.424 622.6 30.6
_platon_squeeze_details          
; ?
;

